EP4588369A1

EP4588369A1 - Botanical material treatment

Info

Publication number: EP4588369A1
Application number: EP24152224.2A
Authority: EP
Inventors: Batir ABDURAHMANOV
Original assignee: Nicoventures Trading Ltd
Current assignee: Nicoventures Trading Ltd
Priority date: 2024-01-16
Filing date: 2024-01-16
Publication date: 2025-07-23
Also published as: WO2025153627A1

Abstract

The invention provides a process for producing expanded botanical material for use in a non-combustible aerosol delivery system or an aerosol-free delivery system. The process comprises dry ice expansion of a treated botanical material. The treated botanical material has previously been formed by a treatment process comprising heating a botanical material which is enclosed within a moisture-retaining material. Also provided is expanded botanical material obtainable by the process and a non-combustible aerosol delivery system comprising the expanded botanical material, or an aerosol-generating material or consumable therefor. Also provided is an aerosol-free delivery system comprising the expanded botanical material.

Description

Field

The present invention relates to a process and in particular a process for the production of dry ice expanded botanical material, such as dry ice expanded tobacco (DIET).

Background

After harvesting, tobacco material can be cured to prepare the leaf for consumption. The tobacco material may be further treated, for example by aging or fermentation, to enhance the organoleptic properties of the tobacco. However, these processes can be lengthy and the quality of the resulting tobacco material can be variable. Treatments to enhance or add flavours and aromas to the tobacco material at a later stage of tobacco processing often involve the addition of one or more additive(s) to the tobacco and can require additional processing steps and equipment, which can be costly and time-consuming.

Summary

According to a first aspect of the invention, a process is provided for producing expanded botanical material, the process comprising:
dry ice expansion of a treated botanical material, wherein the treated botanical material has previously been formed by a treatment process comprising:
heating a botanical material which is enclosed within a moisture-retaining material.
The expanded botanical material may optionally be suitable for use in a non-combustible aerosol delivery system or an aerosol-free delivery system. Thus, according to a second aspect of the invention, a process is provided for producing expanded botanical material for use in (or for) a non-combustible aerosol delivery system or an aerosol-free delivery system, the process comprising:
dry ice expansion of a treated botanical material, wherein the treated botanical material has previously been formed by a treatment process comprising:
heating a botanical material which is enclosed within a moisture-retaining material.
Features of aspects and embodiments described herein are applicable to both the first and second aspects of the invention.
In all of the aspects and embodiments described herein, the botanical material that is treated in the treatment process may be tobacco. Thus, the processes of the first and second aspects may comprise dry ice expansion of tobacco material which has previously been treated by the treatment process.
The processes of the first and second aspects may comprise treating the botanical material according to the treatment process to provide the treated botanical material, and dry ice expansion of the treated botanical material (to provide the dry ice expanded botanical material). That is, the processes may comprise carrying out the treatment process to provide the treated botanical material.
In the treatment process, the step of heating the botanical material may comprise exposing the botanical material to an ambient processing temperature of at least about 45°C, wherein the botanical material has a packing density on a dry matter weight base of at least 200 kg/m³ at the start of the treatment process and has a moisture content of between about 10% and 23% before and during the treatment process. The treatment process may produce a botanical material with desirable organoleptic properties.
A third aspect provides expanded botanical material which is obtainable by (or obtained by) the process of the first or second aspects.
A fourth aspect provides an aerosol-generating material for use in a non-combustible aerosol provision system, the aerosol-generating material comprising the expanded botanical material of the third aspect.
A fifth aspect provides a consumable for use in a non-combustible aerosol provision system, the consumable comprising the expanded botanical material of the third aspect, or the aerosol-generating material of the fourth aspect.
A further aspect provides a non-combustible aerosol provision system comprising the expanded botanical material of the third aspect, the aerosol-generating material of the fourth aspect, or the consumable of the fifth aspect.
The processes described herein may also further comprise incorporating the dry ice expanded botanical material into a non-combustible aerosol provision system, or an aerosol-generating material or consumable therefor.
The processes described herein may further comprise incorporating the dry ice expanded botanical material into a blend. The blend may be suitable for use in a non-combustible aerosol provision system, or an aerosol-generating material or consumable therefor. Suitable amounts of the dry ice expanded botanical material in the blend are set out below.
A further aspect provides the use of the dry ice expanded botanical material of the third aspect for the manufacture of an aerosol-generating material for use in a non-combustible aerosol provision system, or a consumable for use in a non-combustible aerosol provision system, or for the manufacture of an aerosol-free delivery system.
A further aspect provides an aerosol-free delivery system comprising the expanded botanical material of the third aspect. The processes described herein may also further comprise incorporating the dry ice expanded botanical material into an aerosol-free delivery system.
The dry ice expanded botanical material may be used to make an extract, such as a tobacco extract when the botanical material is tobacco. A further aspect provides an extract manufactured from the dry ice expanded botanical material of the third aspect. The processes described herein may comprise one of more further steps of producing an extract from the dry ice expanded botanical material.

Brief Description of the Figures

For the purposes of illustration only, embodiments of the invention are described below with reference to the accompanying drawings, in which:

Figure 1 is a process flow diagram for the manufacture of dry ice expanded tobacco;
Figure 2 shows a cross section through a tobacco leaf before (top) and after (bottom) dry ice expansion. The scale bar (centre, bottom) of each image corresponds to a distance of 100 microns.

Detailed Description

The present invention relates to a process for the production of dry ice expanded botanical material. The process comprises dry ice expansion of a treated botanical material which has previously been formed by a treatment process. As used herein, the term "treated botanical material" refers to botanical material, such as tobacco, that has undergone the treatment process described herein. The term "untreated botanical material" refers to botanical material that has not undergone the treatment process.
Expanded botanical material is botanical material that has been subjected to an expansion process. Expansion involves increasing the volume of the cell structure of the tobacco material which may result in an increase in the area and spacing between any fibres present in the botanical material, such as tobacco material. After being subjected to the expansion process, the botanical material has a higher fill value, but lower density, than the botanical material prior to the expansion process. Expanded botanical material may be blended with other types of botanical material, for example to provide consumables for non-combustible aerosol provision systems, or aerosol-free delivery systems, having a lower overall weight than convention consumables or aerosol-free delivery systems. Reducing the overall weight can provide numerous advantages, such as reduced transportation costs. Furthermore, reducing the weight may also have a positive impact on the environment because less energy may be required for transportation. In addition, consumers may prefer to carry and use a lighter-weight consumable or delivery system. Types of expanded tobacco include dry ice expanded tobacco and expanded stem. Expanded stem is formed by steam expansion of stem tobacco.
It has been established that treatment processes as described herein can favourably change the organoleptic properties of dry ice expanded botanical materials. On the other hand, it has been found that these desirable changes in organoleptic properties are not observed when the same treatment is performed on other types of expanded botanical material. In particular, no significant change in taste profile between treated and untreated expanded stem (i.e. steam expanded stem tobacco before and after a treatment process as described herein) was determined by expert smokers. In contrast, a change in taste profile was found between treated and untreated dry ice expanded tobacco (i.e. dry ice expanded tobacco before and after carrying out a treatment process as described herein). That is, it has been surprisingly found that the treatment process described herein is particularly suitable for improving the organoleptic properties of dry ice expanded botanical materials, whereas it is not suitable for improving the organoleptic properties of steam expanded stem.
Furthermore, by carrying out the dry ice expansion on botanical material which has already been treated according to the treatment process described herein, the processes described herein provide a number of additional advantages.
Firstly, the inventors have found that conducting the treatment process on dry ice expanded botanical material (i.e. using dry ice expanded botanical material as the starting material for the treatment process) may lead to the formation of hard clumps (which may also be referred to as blocks or pads) of dry ice expanded botanical material. Such clumps may need to be removed before the dry ice expanded botanical material can be used in products such as non-combustible aerosol provision systems, or aerosol-generating materials or consumables therefor, and aerosol-free delivery systems. Without wishing to be bound by theory, the inventor believes that the clumps form due the compressible, or fluffy, nature of the dry ice expanded botanical material. During the treatment process in which the temperature of the dry ice expanded botanical is increased, the dry ice expanded botanical material at the top of the moisture retaining material may compress the dry ice expanded botanical material beneath it, leading to the formation of compacted layers, or clumps, in the lower portion of the body, or batch, of dry ice expanded botanical material being treated. Advantageously, the formation of these clumps can be avoided by carrying out the dry ice expansion after the treatment process described herein.
On the other hand, dry ice expansion can compromise the organoleptic properties of untreated botanical materials, such as untreated tobacco materials. Conventional dry ice expanded botanical materials, such as dry ice expanded tobacco, can exhibit poor irritation and dryness taste characteristics. Surprisingly, the organoleptic properties and taste profile of the dry expanded botanical material, such as dry ice expanded tobacco, provided by the processes described herein are still favourable even after the dry ice expansion. Without wishing to be bound by theory, the inventors believe that the chemical transformations which occur during the treatment process described herein are surprisingly sufficient to impart favourable organoleptic properties to the treated botanical material even after the treated botanical material has been subjected to the steps of the dry ice expansion. For example, dry ice expanded botanical material (e.g. tobacco) obtainable by (or obtained by) the processes described herein may exhibit favourable sensorial properties, such as low dryness and favourable mouth-coating.
As used herein the term "botanical material" includes any material derived from plants and having a cell structure including, but not limited to, extracts, leaves, bark, fibres, stems, roots, seeds, flowers, fruits, pollen, husk, shells or the like. The material may be in the form of solid, crushed particles, shreds, strips, sheets, or the like. Example botanicals are tobacco, eucalyptus, star anise, hemp, cocoa, cannabis, fennel, lemongrass, peppermint, spearmint, rooibos, chamomile, flax, ginger, ginkgo biloba, hazel, hibiscus, laurel, licorice (liquorice), matcha, mate, orange skin, papaya, rose, sage, tea such as green tea or black tea, thyme, clove, cinnamon, coffee, aniseed (anise), basil, bay leaves, cardamom, coriander, cumin, nutmeg, oregano, paprika, rosemary, saffron, lavender, lemon peel, mint, juniper, elderflower, vanilla, wintergreen, beefsteak plant, curcuma, turmeric, sandalwood, cilantro, bergamot, orange blossom, myrtle, cassis, valerian, pimento, mace, damien, marjoram, olive, lemon balm, lemon basil, chive, carvi, verbena, tarragon, geranium, mulberry, ginseng, theanine, theacrine, maca, ashwagandha, damiana, guarana, chlorophyll, baobab or any combination thereof. The mint may be chosen from the following mint varieties: Mentha Arventis, Mentha c.v.,Mentha niliaca, Mentha piperita, Mentha piperita citrata c.v.,Mentha piperita c.v, Mentha spicata crispa, Mentha cardifolia, Memtha longifolia, Mentha suaveolens variegata, Mentha pulegium, Mentha spicata c.v. and Mentha suaveolens In particular embodiments, the botanical material is tobacco.
Tobacco undergoes a number of steps prior to consumption by the consumer. On the field the following steps are usually carried out by the farmer: seeding; transplanting; growing; harvesting; and curing.
Tobacco is generally cured after harvesting to reduce the moisture content of the tobacco, usually from around 80% to around 20% or lower. Tobacco can be cured in a number of different ways, including air-, fire-, flue- and sun-curing. During the curing period, the tobacco undergoes certain chemical changes and turns from a green colour to yellow, orange or brown. The temperature, relative humidity and packing density are carefully controlled to try to prevent houseburn and rot, which are common problems encountered during curing.
At a Green Leaf Threshing (GLT) plant the tobacco is sold by the farmer and then usually undergoes the following steps: re-grading; green-leaf blending; conditioning; stem removal by de-stemming or threshing (or not in the case of whole leaf); drying; and packing.
Usually after curing, the stem may be removed from the lamina. This may be done by threshing, in which the midribs and partially the lamina ribs are separated from the lamina by machine threshing. An alternative way to remove the stem from lamina is manually, with the so-called 'hand stripping' process. Alternatively, tobacco may be 'butted', which means that the thick part of the stem is cut, while the rest of the tobacco leaf remains integral.
In addition to curing, the tobacco may be further processed to enhance its taste and aroma. Aging and fermentation are known techniques for enhancing the taste and aroma of tobacco. These processes can be applied to tobacco materials such as threshed lamina, hand-stripped lamina, butted lamina and/or whole leaf tobacco.
Aging usually takes place after the tobacco has been cured, threshed (or butted or hand-stripped) and packed. Tobaccos that undergo aging include Oriental, flue-cured and air-cured tobaccos. During aging the tobacco might be stored generally at temperatures of around 20°C to around 40°C and relative humidities present at the respective country of origin/aging or under controlled warehouse conditions for around 1 to 3 years.
It is important that the moisture content of the tobacco is kept at a relatively low level during aging, for example up to around 10-13%, as mould will form in tobacco with higher moisture content.
Fermentation is a process that is applied to particular tobaccos, including dark air-cured tobacco, cured Oriental tobacco and cigar tobacco, to give the tobacco a more uniform colour and to change the aroma and taste. Fermentation is generally not applied to flue-cured and light air-cured tobacco. Fermentation is also generally not applied to dry ice expanded tobacco (DIET).
The fermentation parameters, such as the moisture content of the tobacco and the ambient conditions, vary depending on the type of tobacco that is undergoing fermentation. Generally, the fermentation moisture is either similar to the moisture content of the tobacco when it has been received from the farmer (around 16-20%), or the tobacco is conditioned to a slightly higher moisture content. Care has to be taken to avoid the production of different rots, which occur when the tobacco is fermented at a moisture content that is too high. The duration of the fermentation period can vary, ranging from several weeks to several years.
Generally, fermentation involves the treatment of tobacco in large volumes and is applied to whole leaf, with subsequent removal of the stem after process. The tobacco can be arranged into large piles, which is then turned at intervals to move the tobacco at the periphery into the centre of the pile. Alternatively, the tobacco is placed into chambers with a volume of several square meters. Treatment of such large volumes of tobacco can be cumbersome and/or time-consuming.
The density of the tobacco during fermentation is generally around 150 to 200 kg/m³ (on a dry matter weight base). For comparison, the density of cut rag tobacco may be as low as 70 kg/m³ and is more likely to be from about 80 to 90 kg/m³.
Significantly, fermentation relies on the activity of microorganisms to effect changes in the tobacco material and the fermentation conditions, including temperature and moisture content of the tobacco, are selected to enhance the microbiological activity during fermentation. For example, during fermentation treatment temperatures must typically be controlled within the range of 38-40 °C. In most, if not all, cases the fermentation of tobacco relies upon microorganisms already present in the tobacco material. However, suitable microorganisms could potentially be added to the tobacco material at the start of the fermentation process.
After the above treatments, generally the tobacco is transported to other locations to be further processed, for example before it is incorporated into a tobacco-containing product.
Botanical materials, such as tobacco, may additionally or alternatively be treated with additives to improve or enhance the flavour and aroma of the botanical material. However, this requires additional processing steps and apparatus, making the botanical material preparation process more lengthy and often more costly. In addition, it can be desirable to have a botanical material that has a taste and aroma that is enjoyed by consumers but has not had any additives applied to it to achieve this. This would be the case for consumers who would like a natural botanical product that also has a pleasant flavour and/or taste, for example.

Treatment process

In some embodiments, the treatment process as described herein produces a botanical material, such as tobacco material, with desirable organoleptic properties within a period of time that may be shorter than the more traditional techniques such as fermentation and aging and without the addition of flavour or aromatising additives. In some embodiments, the treatment process involves no fermentation or essentially no fermentation. This may be demonstrated by the presence of little or no microbial content of the botanical material, such as tobacco material, at the end of the process. Thus, in one embodiment the microbial content of the treated botanical material provided by the treatment process is lower than the microbial content of the botanical material at the start of the treatment process.
In some embodiments, the treatment process as described herein produces a botanical material, such as tobacco, with an enhanced flavour profile or enhanced organoleptic properties (compared to the flavour profile of botanical material which has not been treated or which has been treated using only conventional curing processes). This means that there is a reduction in off-notes or irritants, whilst retaining the taste characteristics of the botanical as would be seen following conventional curing. As used herein, the terms "enhance" or "enhancement" are used in the context of the flavour or organoleptic properties to mean that there is an improvement or refinement in the taste or in the quality of the taste, as identified by expert smokers. This may, but does not necessarily, include a strengthening of the taste.
In some embodiments, the treatment process as described herein produces a botanical material, such as tobacco material, wherein at least one undesirable taste or flavour characteristic has been reduced.
In some embodiments, the treatment process may be used to enhance the organoleptic properties of a botanical starting material, such as a tobacco starting material, which has poor organoleptic (e.g. taste) properties. It has been found that at least one effect that the processing has on the botanical material, such as tobacco material, is the removal or reduction of organoleptic factors that have a negative impact on the overall organoleptic properties of the botanical material. In some embodiments, the process may also result in the increase of positive organoleptic properties.
In some embodiments, the treatment process may be adjusted to produce a treated material with particular selected organoleptic characteristics. This may, for example, involve the adjustment of one or more of the parameters of the process.
In some embodiments, the treatment process as described herein transforms the flavour profile of the botanical material, such as tobacco (compared to the flavour profile of botanical material, such as tobacco, which has not been treated or which has been treated using only conventional curing processes). This means that there is a significant change in the organoleptic properties of the botanical material following the processing, so that the taste characteristics of the botanical material are changed compared to those of the same botanical material following conventional curing. As used herein, the terms "transform" or "transformation" are used in the context of the flavour or organoleptic properties to mean that there is change from one overall taste or sensory character to another, as identified by expert smokers. This may include an improvement and/or refinement in the taste or in the quality of the taste.
In some embodiments, including those where the organoleptic properties of the botanical starting material, such as tobacco, are transformed, the processing has the effect of not only reducing or removing organoleptic factors that have a negative effect, but also introducing or increasing organoleptic factors that have a positive effect. For example, in some embodiments, the process described herein leads to an increase in the products of the Maillard Reaction, many of which are known to contribute to desirable organoleptic properties.
Reference made herein to the organoleptic properties of the botanical material may be reference to the organoleptic properties of the botanical material itself, for example when used orally by a consumer. Additionally or alternatively, the reference is to the organoleptic properties of vapour produced by heating the botanical material. In some embodiments, the treated botanical material affords a product including said botanical material with desirable organoleptic properties when said product is used or consumed.
As used herein, the term 'tobacco material' includes any part and any related byproduct, such as for example the leaves or stems, of any member of the genus Nicotiana. The tobacco material for use in the treatment process in the present invention is preferably from the species Nicotiana tabacum.
Any type, style and/or variety of tobacco may be treated. Examples of tobacco which may be used include but are not limited to Virginia, Burley, Oriental, Comum, Amarelinho and Maryland tobaccos, and blends of any of these types. The skilled person will be aware that the treatment of different types, styles and/or varieties will result in tobacco with different organoleptic properties.
In particular embodiments, the tobacco material to be treated in the treatment process comprises lamina tobacco, such as a lamina tobacco comprising lamina Virginia tobacco.
In particular embodiments the tobacco material to be treated in the treatment process comprises at least 50 wt% (i.e. from 50 to 100 wt) such as at least 60 wt%, at least 70 wt%, at least 80 wt%, or at least 90 wt%, of Virginia tobacco. In some embodiments the tobacco material to be treated in the treatment process is Virginia tobacco. In these embodiments, the Virginia tobacco may be lamina tobacco.
The botanical material, such as tobacco material, may be pre-treated according to known practices before being used in the treatment process described herein.
For example, tobacco material to be treated in the treatment process may comprise and/or consist of post-curing tobacco. As used herein, the term 'post-curing tobacco' refers to tobacco that has been cured but has not undergone any further treatment process to alter the taste and/or aroma of the tobacco material. The post-curing tobacco may have been blended with other styles, varieties and/or types. Post-curing tobacco does not comprise or consist of cut rag tobacco.
Alternatively or in addition, tobacco material to be treated in the treatment process may comprise and/or consist of tobacco that has been processed to a stage that takes place at a Green Leaf Threshing (GLT) plant. This may comprise tobacco that has been re-graded, green-leaf blended, conditioned, de-stemmed or threshed (or not in the case of whole leaf), dried and/or packed.
In some embodiments, the tobacco material to be treated in the treatment process comprises lamina tobacco material. The tobacco may comprise between about 70% and 100% lamina material.
The tobacco material to be treated in the treatment process may comprise up to 50%, up to 60%, up to 70%, up to 80%, up to 90%, or up to 100% lamina tobacco material. In some embodiments, the tobacco material to be treated in the treatment process comprises up to 100% lamina tobacco material. In other words, the tobacco material to be treated in the treatment process may comprise substantially entirely or entirely lamina tobacco material.
Alternatively or in addition, the tobacco material to be treated in the treatment process may comprise at least 50%, at least 60%, at least 70%, at least 80%, at least 90%, or at least 95% lamina tobacco material.
When the tobacco material to be treated in the treatment process comprises lamina tobacco material, the lamina may be in whole leaf form. In some embodiments, the tobacco material comprises cured whole leaf tobacco. In some embodiments, the tobacco material substantially comprises cured whole leaf tobacco. In some embodiments, the tobacco material consists essentially of cured whole leaf tobacco. In some embodiments, the tobacco material does not comprise cut rag tobacco.
In some embodiments, the tobacco material to be treated in the treatment process comprises stem tobacco material. The tobacco may comprise between about 90% and 100% stem material.
The tobacco material to be treated in the treatment process may comprise up to 50%, up to 60%, up to 70%, up to 80%, up to 90%, or up to 100% stem tobacco material. In some embodiments, the tobacco material comprises up to 100% stem tobacco material. In other words, the tobacco material to be treated in the treatment process may comprise substantially entirely or entirely stem tobacco material.
Alternatively or in addition, the tobacco material to be treated in the treatment process may comprise at least 50%, at least 60%, at least 70%, at least 80%, at least 90%, or at least 95% stem tobacco material.
As set out in the Summary, the treatment process comprises heating a botanical material which is enclosed within (or secured within) a moisture-retaining material. The treatment process may comprise enclosing (or securing) the botanical material within the moisture-retaining material.
The moisture content of the botanical material before and during the treatment process may be between about 10% and about 23%. As used herein, the term 'moisture content' refers to the percentage of oven volatiles present in the botanical material.
In some embodiments, the moisture content of the botanical material before and during the treatment process is between about 10% and 15.5%, optionally between about 11% and 15% or between about 12% and 14%. The moisture content of the botanical material may be about 10%, about 11%, about 12%, about 13%, about 14%, about 15%, about 16%, about 17%, about 18%, about 19%, about 20%, about 21%, about 22% or about 23%.
The botanical material is enclosed within (or secured within) a moisture-retaining material, to limit moisture losses and to retain a desired level of moisture during the treatment process.
The botanical may be completely sealed within the moisture-retaining material. Alternatively, the botanical material may not be completely sealed within the moisture-retaining material. In some embodiments, a moisture-retaining material is wrapped around, or has been wrapped around, the botanical material. In some embodiments, the botanical material is placed within, or has been placed in, a moisture-retaining container.
The moisture-retaining material may be any material that is sufficiently impermeable to moisture to retain the desired amount of moisture during the treatment process. The amount of moisture that is retained in the botanical material may be at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, at least 91%, at least 92%, at least 93%, at least 94%, at least 95%, at least 96%, at least 97%, at least 98%, at least 99%, at least 99.5% or 100% of the moisture which was present in the botanical material prior to treatment. In some embodiments, between 99% and 100% of the moisture content of the botanical material is retained during the process.
It is desirable for the moisture-retaining material to be resistant to degradation during the treatment process. For example, it is desirable for the moisture-retaining material to withstand the temperatures of the treatment process, without breaking down to become moisture-permeable or to release compounds that may be taken up by the botanical material. The temperature reached by the material during the process may therefore be taken into consideration when selecting the moisture-retaining material.
The moisture-retaining material may comprise a flexible material. This flexible material may be wrapped around the botanical material and/or formed into a pouch into which the botanical is placed. In some embodiments, the moisture-retaining material comprises plastic material. In some embodiments, the moisture-retaining material comprises flexible polymeric material, optionally a polymeric or plastic film. In some embodiments, the moisture-retaining material comprises polyethylene. In some embodiments, the moisture-retaining material comprises polyesters, nylon and/or polypropylene. In some embodiments, the moisture-retaining material is Polyliner^®. Polyliner^® is available through a number of suppliers, including Plastrela Flexible Packaging, located in Brazil.
Alternatively or in addition, the moisture-retaining material may comprise a rigid material, such as metal for example, which is formed into a vessel or container. In these embodiments, a separate storage container as discussed below may not be required.
In embodiments where the botanical material reaches a temperature of about 100°C or above, the moisture-retaining material may be pressure-resistant.
In some embodiments, the treatment process may comprise allowing the botanical material to rest when enclosed within the moisture-retaining material for a rest period, before it is heated, e.g. before the botanical material is exposed to the ambient processing temperatures described herein. The rest period may be at least 15 days, such as at least 30 days. For example, the rest period may be from 15-75 days such as 20-60 days or 30-45 days.
At the start of the treatment process, the botanical material may have a packing density of at least 200 kg/m³ (on a dry matter weight base). Additionally or alternatively, at the start of the process, the botanical material may have a packing density up to about 500 kg/m³ (on a dry matter weight base). The botanical material may have a packing density of between about 200 kg/m³ and 330 kg/m³, optionally between about 220 kg/m³ and 330 kg/m³. In some embodiments, the botanical material has a packing density of between about 260 kg/m³ and 300 kg/m³, a packing density of about 200 to about 400 kg/m³, or a packing density of about 250 to about 300 kg/m³.
The packing density of the botanical material may be at least 210 kg/m³, at least 220 kg/m³, at least 230 kg/m³, at least 240 kg/m³, at least 250 kg/m³, at least 260 kg/m³, at least 270 kg/m³, at least 280 kg/m³, at least 290 kg/m³, at least 300 kg/m³, at least 310 kg/m³, at least 320 kg/m³ or at least 330 kg/m³.
Alternatively or in addition, the packing density of the botanical material may be up to 220 kg/m³, up to 230 kg/m³, up to 240 kg/m³, up to 250 kg/m³, up to 260 kg/m³, up to 270 kg/m³, up to 280 kg/m³, up to 290 kg/m³, up to 300 kg/m³, up to 310 kg/m³, up to 320 kg/m³ or up to 330 kg/m³.
The packing density of the botanical material during and/or following treatment may be similar or substantially similar to the packing density of the botanical material at the start of the process. In some cases, the volume occupied by the botanical material decreases during the treatment and so the packing density of the botanical material is increased during and/or following the treatment. In some cases, the botanical material may lose some mass due to the chemical reactions taking place during the treatment process such that the packing density of the botanical material is increased during and/or following the treatment. For example, a 200 kg batch of tobacco material may lose approximately 2 kg of mass during the treatment process.
The botanical material may be placed in a storage container after it has been enclosed or secured within a moisture-retaining material. Alternatively, the botanical material may be placed in a storage container and then enclosed or secured within a moisture-retaining material, such as by wrapping a moisture-retaining material around the storage container. Placing the enclosed or secured botanical material in a container enables the botanical material to be handled easily.
Packing density herein is calculated by dividing the weight of the botanical material by the volume occupied by the botanical material. The packing densities herein are to be calculated based on a dry matter weight base, excluding any water/moisture in the botanical material.
When the volume of the storage container, the volume enclosed by the moisture-retaining material and the volume occupied by the botanical material are substantially the same or exactly the same (for example when the storage container is filled substantially completely or completely with botanical material and tightly enclosed, wrapped or secured within in moisture-retaining material), the packing density may be calculated by dividing the weight of botanical material on a dry matter weight base placed in the storage container by the volume of the storage container.
The volume of the storage container and/or the volume enclosed by the moisture-retaining material (which may be substantially the same) may be selected to achieve the desired packing density for the desired amount of botanical material to be treated, and at the same time allows the treatment of the botanical material to take place at a suitable rate. Alternatively or in addition, the container may be oriented on its side. This arrangement may be particularly beneficial when the botanical material comprises tobacco lamina that is in a horizontal position when placed in the storage container, as placing the storage container on its side achieves a more even packing density.
If the botanical material does not occupy the entire volume of the moisture-retaining material, the volume occupied by the botanical material may be calculated by subtracting the volume of any empty space (e.g. any void space above the botanical material after it has been placed within the moisture-retaining material and optionally the storage container) from the total volume enclosed by the moisture-retaining material.
In some embodiments, the container has a volume of between about 0.2 m³ and about 1.0 m³, optionally between about 0.4 m³ and about 0.8 m³. In some embodiments, the container has a volume of about 0.6 m³.
In some embodiments, the volume occupied by the botanical material at the start of the process is between about 0.2 m³ and about 1.0 m³, optionally between about 0.4 m³ and about 0.8 m³. In some embodiments, the volume occupied by the botanical material at the start of the process is about 0.6 m³.
In some embodiments, the storage container is a case for botanical material, such as tobacco, known as a C-48 box. The C-48 box is generally made of cardboard and has dimensions of about 115 x 70 x 75 cm. For example, a desirable packing density is achieved when 180-200 kg of tobacco with a moisture content of between about 12 and 15% is held within a C-48 box.
The botanical material may be heated within the moisture-retaining material to give rise to an increase in the temperature of the botanical material to a temperature equal to or above a threshold temperature. In some embodiments, the threshold temperature is 55°C, 60°C or 65°C.
The temperature to which the botanical material is raised during the treatment process may be up to about 80°C, up to about 85°C, up to about 90°C, up to about 95°C, or up to about 100°C. For example, the temperature to which the botanical material is raised may be from about 55°C to about 100°C, such as about 55 °C to about 90 °C or about 60 °C to about 85 °C.
In particular embodiments, the step of heating the botanical material comprises exposing the botanical material to an ambient processing temperature of at least about 45°C.
The botanical material may be placed in a processing area. As used herein, the term 'processing area' is the area, which can be a room or chamber, in which the treatment process is carried out. The ambient process conditions, i.e. the conditions of the processing area, may be controlled during the process. This may be achieved by placing the botanical material enclosed or secured within the moisture-retaining material into a controlled environment, such as a chamber. The botanical material may be placed on one or more rack(s) within a chamber, to allow optimal ventilation to maintain constant ambient process conditions around the botanical material. The rack(s) may have one or more shelve(s) comprising bars with gaps between the bars and/or other apertures, to assist in the maintenance of constant ambient process conditions around the botanical material.
The ambient processing humidity may be maintained at a level to avoid significant moisture loss from the botanical material. As used herein, the term 'ambient processing humidity' refers to the humidity of the processing area. As used herein, the term 'ambient relative processing humidity' refers to the relative humidity of the processing area.
In some embodiments, the ambient relative processing humidity is about 65%. The ambient relative processing humidity may be at least 40%, at least 45%, at least 50%, at least 55%, at least 60%, at least 65% or at least 70%.
The ambient processing temperature may be at least about 45°C. In some embodiments, the ambient processing temperature is at least about 50°C. In some embodiments, the ambient processing temperature may be maintained at above 55°C, optionally at about 60°C. As used herein, the term 'ambient processing temperature' refers to the temperature of the processing area.
In some embodiments, the ambient processing temperature is at least 46°C, at least 47°C, at least 48°C, at least 49°C, at least 50°C, at least 51°C, at least 52°C, at least 53°C, at least 54°C, at least 55°C, at least 56°C, at least 57°C, at least 58°C, at least 59°C, at least 60°C, at least 61°C, at least 62°C, at least 63°C, at least 64°C, at least 65°C, at least 66°C, at least 67°C, at least 68°C, at least 69°C or at least 70°C. In some embodiments, the ambient processing temperature is up to 60°C, up to 70°C, up to 75°C, up to 80°C, up to 85°C, up to 90°C, up to 95°C, up to 100°C, up to 105°C, up to 110°C, up to 115°C or up to 120°C.
In embodiments in which the ambient processing temperature is about 45°C, the ambient processing humidity may be about 30-70 g water/m³. In embodiments in which the ambient processing temperature is about 55°C, the ambient processing humidity may be about 40-80 g water/m³. In embodiments in which the ambient processing temperature is about 60°C, the ambient processing humidity may be about 50-110 g water/m³. In embodiments in which the ambient processing temperature is about 70°C, the ambient processing humidity may be about 50-160 g water/m³. In embodiments in which the ambient processing temperature is about 80°C, the ambient processing humidity may be about 50-230 g water/m³. In embodiments in which the ambient processing temperature is about 90°C, the ambient processing humidity may be about 50-340 g water/m³. In embodiments in which the ambient processing temperature is about 100°C or higher, the ambient processing humidity may be about 50-500 g water/m³.
In some embodiments, the ambient processing temperature is 60°C and the ambient relative processing humidity is 60%.
When the botanical material is heated by exposing the material to an ambient processing temperature as described herein, during the treatment process the temperature of the botanical material reaches the ambient processing temperature. The botanical material may reach the ambient processing temperature within a short period of time. For example, the botanical material may reach the ambient processing temperature within 4 to 10 days, optionally within 5 to 9 days, within 7 to 9 days and/or within 4 to 7 days.
To achieve this, the amount of botanical material treated may be optimised for the heat to be transferred to the centre of the botanical material sufficiently rapidly. The rate at which the temperature of the botanical material rises and reaches the ambient processing temperature will be dependent upon a number of factors, including the ambient processing temperature, the density of the botanical material and the overall amount of botanical material being treated.
In some embodiments, the botanical material reaches a temperature of above 55°C and/or at least 60°C within about 9 days. In some embodiments, the botanical material reaches a temperature of above 55°C and/or at least 60°C within about 7 days. In some embodiments, the botanical material reaches a temperature of above 55°C and/or at least 60°C within about 5 days. In such embodiments, the ambient processing temperature may be 60°C. In such embodiments, the botanical material may be treated in 200 kg batches.
In some embodiments, the temperature to which the botanical material should be raised is at least about 55°C or at least about 60°C. Additionally or alternatively, the temperature to which the botanical material should be raised may be up to about 80°C, up to about 85°C, up to about 90°C, up to about 95°C, or up to about 100°C. For example, the temperature to which the botanical material is raised may be from about 55°C to about 100°C, such as about 55 °C to about 90 °C or about 60 °C to about 85 °C.
In some embodiments, the beneficial effects of the processing according to the invention may be achieved within shorter processing periods by employing a higher ambient processing temperature.
In embodiments in which the heating is affected by exposing the botanical material to an ambient processing temperature as described herein, the temperature of the botanical material may rise during the treatment process to reach a second temperature that is higher than ambient processing temperature. This may be achieved with the assistance of exothermic reactions taking place during the treatment process.
In some embodiments, the botanical material reaches a second temperature which is above the ambient processing temperature. In some embodiments, the second temperature is at least 1°C above the ambient processing temperature. at least 2°C, at least 3°C, at least 4°C, at least 5°C, at least 7°C, at least 10°C, at least 12°C, at least 15°C, at least 17°C or at least 20°C above the ambient processing temperature. In some embodiments, the botanical material reaches a second temperature which is above the ambient processing temperature within about 7 to 13 days, and/or the second is reached within about 13 days or within about 11 days. In some embodiments, the botanical material reaches a second temperature of at least 5°C above the ambient processing temperature within about 11 to 13 days.
The temperature of the botanical material may reach up to 60°C, up to 65°C, up to 70°C, up to 75°C, up to 80°C, up to 85°C, up to 90°C, up to 95°C, up to 100°C, up to 105°C, up to 110°C, up to 115°C, up to 120°C, up to 125°C, up to 130°C, up to 135°C, up to 140°C, up to 145°C or up to 150°C during the treatment process.
Alternatively or in addition, the temperature of the botanical material may reach at least 60°C, at least 65°C, at least 70°C, at least 75°C, at least 80°C, at least 85°C, at least 90°C, at least 95°C, at least 100°C, at least 105°C, at least 110°C, at least 115°C, at least 120°C, at least 125°C, at least 130°C, at least 135°C, at least 140°C, at least 145°C or at least 150°C during the treatment process. In practice, the upper temperature may be limited by the thermal tolerance of the moisture-retaining material.
In some embodiments, the temperature of the botanical material may reach between about 55°C and about 90°C, between about 55°C and about 80°C, or between 60°C and about 70°C.
The botanical material may be enclosed (or secured) within the moisture-retaining material for a sufficiently long period of time for the botanical to develop the desirable organoleptic properties, and for a sufficiently short period of time to not cause unwanted delay in the supply chain of the botanical material.
The botanical material may be heated within the moisture-retaining material for a period of time and at an ambient processing temperature and ambient processing humidity suitable to give rise to an increase in the temperature of the botanical material to or above a threshold temperature, wherein the moisture content of the botanical material is between about 10% and 23%. In some embodiments, the threshold temperature is 55°C, 60°C or 65°C.
In some embodiments, the botanical material is heated during the treatment process for between about 5 and 65 days, for between about 8 and 40 days, for between about 10 and 40 days, between about 15 and 40 days, between about 20 and 40 days, between about 25 and 35 days and/or between about 28 and 32 days. For example, where the botanical material is heated by exposing the botanical material to the ambient processing temperature of at least about 45°C (or any of the ambient processing temperatures disclosed herein), the botanical material may be exposed to the ambient processing temperature for between about 5 and 65 days, for between about 8 and 40 days, for between about 10 and 40 days, between about 15 and 40 days, between about 20 and 40 days, between about 25 and 35 days and/or between about 28 and 32 days.
In other words, the duration of the treatment (excluding any period where the botanical material is enclosed or secured within the moisture-retaining material before being heated, such as by being exposed to the ambient processing temperature) may be between about 5 and 65 days, for between about 8 and 40 days, for between about 10 and 40 days, between about 15 and 40 days, between about 20 and 40 days, between about 25 and 35 days and/or between about 28 and 32 days.
In other embodiments, the botanical material is heated for (or exposed to the ambient processing temperature for) for about 30 to 65 days, such as about 40 to 50 days, or about 43 to 48 days. In other words, the duration of the treatment (excluding any period where the botanical material is enclosed or secured within the moisture-retaining material before being heated, such as by being exposed to the ambient processing temperature) may be about 30 to 65 days, such as about 40 to 50 days, or about 43 to 48 days. Increasing the duration of the treatment may increase the quantity of products of the Maillard reaction and may thereby provide a more intense flavour profile of the treated botanical material.
In order to achieve enhancement of the organoleptic properties of the botanical material whilst retaining its original overall taste characteristics, the botanical may be heated under suitable conditions (for example by exposure to a suitable ambient processing temperature and ambient processing humidity) to give rise to an increase in the temperature of the botanical material to at least 55°C with the moisture content of the botanical material being between about 10% and 23% for between about 5 and 16 days. In other embodiments, the organoleptic properties of the botanical material are enhanced by heating the botanical material whilst enclosed within the moisture-retaining material under those conditions for up to 18 days. The treatment period may be between about 6 and 12 days, between about 10 to 12 days, between about 8 to 16 days or between about 8 and 10 days.
In order to achieve transformation of the organoleptic properties of the botanical material to alter the original overall taste characteristics and to produce new taste characteristics, the botanical material may be heated under suitable conditions (for example by exposure to a suitable ambient processing temperature and ambient processing humidity) to give rise to an increase in the temperature of the botanical material to at least 55°C with the moisture content of the botanical material being between about 10% and 23% for between about 20 and 65 days. In other embodiments, the organoleptic properties of the botanical material are transformed by treating the botanical material whilst enclosed within the moisture-retaining material under those conditions for at least 20 days. The treatment period may be between about 25 and 65 days, between about 20 to 40 days, between about 25 to 35 days or between about 30 and 35 days.
In some embodiments, the duration of the treatment is at least 4 days, at least 5 days, at least 6 days, at least 7 days, at least 8 days, at least 9 days, at least 10 days, at least 11 days, at least 12 days, at least 13 days, at least 14 days, at least 15 days, at least 16 days, at least 17 days, at least 18 days, at least 19 days, at least 20 days, at least 21 days, at least 22 days, at least 23 days, at least 24 days, at least 25 days, at least 26 days, at least 27 days, at least 28 days, at least 29 days, at least 30 days, at least 31 days, at least 32 days, at least 33 days, at least 34 days, at least 35 days, at least 36 days, at least 37 days, at least 38 days, at least 39 days, at least 40 days, at least 41 days, at least 42 days, at least 43 days, at least 44 days or at least 45 days.
In some embodiments, the duration of the treatment is up to 5 days, up to 6 days, up to 7 days, up to 8 days, up to 9 days, up to 10 days, up to 11 days, up to 12 days, up to 13 days, up to 14 days, up to 15 days, up to 16 days, up to 17 days, up to 18 days, up to 19 days, up to 20 days, up to 21 days, up to 22 days, up to 23 days, up to 24 days, up to 25 days, up to 26 days, up to 27 days, up to 28 days, up to 29 days, up to 30 days, up to 31 days, up to 32 days, up to 33 days, up to 34 days, up to 35 days, up to 36 days, up to 37 days, up to 38 days, up to 39 days, up to 40 days, up to 41 days, up to 42 days, up to 43 days, up to 44 days, up to 45 days, up to 46 days, up to 47 days, up to 48 days, up to 49 days, up to 50 days, up to 51 days, up to 52 days, up to 53 days, up to 54 days, up to 55 days, up to 56 days, up to 57 days, up to 58 days, up to 59 days, up to 60 days, up to 61 days, up to 62 days, up to 63 days, up to 64 days or up to 65 days.
Embodiments in which the botanical material reaches a higher temperature may require a shorter process period than embodiments in which the botanical material reaches a lower temperature. In some embodiments, the temperature reached by the botanical material during the process is about 5°C above the ambient processing temperature, or between about 2 and 5°C above the ambient processing temperature and the process takes place over a total of 25 to 35 days or a total of 20 to 30 days. This may lead to transformation of the organoleptic properties of the botanical material. In other embodiments, the temperature reached by the botanical material during the process is between about 2 and 5°C above the ambient processing temperature and the process takes place over a total of 5 to 16 days, a total of 6 to 15 days or a total of 8 to 12 days. This may lead to enhancement of the organoleptic properties of the botanical material.
In some embodiments, the botanical material is treated so that it is held at the threshold temperature for a relatively short period of time and the organoleptic properties are enhanced. In some embodiments, the process is halted about 6 hours, 12 hours, 18 hours, 24 hours, or 2, 3, 4, 5, 6, 7 or 8 days after the temperature of the botanical material reaches a threshold temperature. In some embodiments, the threshold temperature is 55°C, 60°C, or 65°C. The period of time for which the botanical material is maintained at or above the threshold temperature may influence the manner and extent to which the organoleptic properties of the botanical material are enhanced by the process. The threshold temperature may differ for different types of botanical material. The period for which the botanical material is maintained at or above the threshold temperature may differ for different types of botanical material.
In other embodiments, the botanical material is treated so that it is held at the threshold temperature for a longer period of time and the organoleptic properties are transformed. In some embodiments, the process is halted no less than 12 days after the temperature of the botanical material reaches a threshold temperature. In some embodiments, the botanical material is 55°C, 60°C, or 65°C. The period of time for which the botanical material is maintained at or above the threshold temperature may influence the manner and extent to which the organoleptic properties of the botanical material are transformed by the process. The threshold temperature may differ for different types of botanical material. The period for which the botanical material is maintained at or above the threshold temperature may differ for different types of botanical material.
In other embodiments, the process involves treating the botanical material until the temperature of the botanical material reaches a target temperature, and then allowing the botanical material to cool. This cooling may be affected by removing the botanical material from the processing area which is being held at an elevated temperature. In some embodiments, the target temperature is 60°C, 61°C, 62°C, 63°C, 64°C, 65°C, 66°C, 67°C, 68°C, 69°C or 70°C. In some embodiments, the target temperature is within the range of 62 to 67°C. The target temperature may differ for different types of botanical material.
After the treatment process described herein, for example after heating the botanical material (such as by exposing the botanical material to the ambient processing temperature) for any of the treatment durations described above, the botanical material may be allowed to rest for a stabilisation period. The botanical material may remain enclosed within, or secured within, the moisture-retaining material during this stabilisation period. The stabilisation period (if used) will occur before the dry ice expansion of the treated botanical material.
The stabilisation period may be initiated by removing the botanical material from the processing area which is being held at an elevated temperature. For example, the botanical material may be transported to a different processing area at a lower temperature, which may be about 30 °C or below (such as from about 18 °C to about 30 °C, or from about 20 °C to about 25 °C, e.g. around 22 °C).
During the stabilisation period the temperature of the treated botanical material gradually reduces, typically to a temperature of about 30 °C or below (such as from about 18 °C to about 30 °C, or from about 20 °C to about 25 °C, e.g. around 22 °C). Moisture may also gradually evaporate from the treated botanical material during the stabilisation period. The moisture content of the botanical material after the stabilisation period may be between about 10% and about 18%, optionally between about 10% and about 15.5%, optionally between about 10.5% and about 15%, such as between about 11% and about 14%.
The duration of the stabilisation period may be at least 15 days, such as at least 30 days. For example, the stabilisation period may be from 15-75 days, such as 20-60 days or 30-45 days. Typically, the stabilisation period is around 40 days.
It has been found that at least one change to the organoleptic properties of the botanical material is a result of a reduction in the negative properties, for example as a result of a reduction in botanical material components that have an unpleasant taste or have an irritant effect. Proline is an example of a component that is associated with such negative properties. In some embodiments, the organoleptic properties are changed by an increase in the positive properties, for example as a result of the increase in or introduction of components that make a positive contribution to the organoleptic properties, such as components having pleasant flavours.
In some embodiments the botanical material is treated so that it has desirable organoleptic properties that are produced in a reliable way and at relatively high volumes. In some embodiments, the treatment process is a batch process.
In an embodiment of the treatment process, 180-200 kg of botanical material, such as tobacco material, with a moisture content of 12 to 14% is wrapped in Polyliner^® material and placed in a C-48 carton. The C-48 carton is placed within a chamber that maintains the relative processing humidity at 60% and the processing temperature at 60°C. After a period of 5 to 9 days the temperature of the botanical material, such as the tobacco material, reaches a temperature of about 60°C and then continues to rise, to reach up a temperature of at least 5°C above the ambient processing temperature after 7 to 13 days. The botanical material, such as the tobacco material, is incubated for a total of 25 to 35 days.
After the botanical material has been incubated for the desired length of time, the treated botanical material may be cooled down while remaining in the moisture-retaining material.
The process parameters are sufficiently gentle for the treated botanical material to maintain some or all of its physical properties. For example, the botanical material remains sufficiently intact following treatment to allow handling and/or processing to ready the botanical material for the dry ice expansion.
The treated botanical material may have a different colour from untreated botanical material. In some embodiments, the botanical material, such as tobacco material, is darker than untreated botanical material.
Importantly, in some embodiments the treated botanical material has organoleptic properties that are acceptable and/or desirable for the consumer. Thus, botanical material with desirable organoleptic properties can be produced by the treatment of botanical material under a specific set of conditions, and without requiring the addition of one or more further chemical(s), which may be hazardous and/or expensive.
The organoleptic properties of the treated botanical material may be developed when the botanical material is secured within the moisture-retaining material, during which period the components in the botanical material undergo chemical changes and modifications, to give desirable organoleptic characteristics to the final product. The treated botanical material may, in some embodiments, have a sweet spicy and/or dark note. The treated botanical material may not, in some embodiments, have a dry and/or bitter note.
In some embodiments the chemical composition of the treated botanical material differs significantly from untreated botanical material. As illustrated in the Examples, in some embodiments the majority of the sugars in the treated botanical material are converted. In some embodiments the treated botanical material contains increased levels of 2,5 deoxyfructosazine and 2,6 deoxyfructosazine, compared with untreated botanical material. The altered levels of these compounds contribute to the desirable taste and aroma of the treated botanical material.
Without being bound by theory, it is thought that the change in the levels of at least some of these compounds is due at least in part to the Maillard reaction taking place during the process. A caramelisation reaction may also be taking place during the process, which may lead to reduced levels of reducing and non-reducing sugars.
In addition, in some embodiments a significant decrease in the content of various amino acids may be seen.
The process may therefore lead to an increase in at least one of the products of the Maillard reaction in the treated botanical material. Products of the Maillard reaction include: 2,6-deoxyfructosazine; 2,5-deoxyfructosazine; 5-acetyl-2,3-dihydro-1H-pyrrolizine; 2,3-dihydro-5-methyl-1H-pyrrolizine-7-carboxaldehyde; 1,2,3,4,5,6-hexahydro-5-(1-hydroxyethylidene)-7H-cyclopenta[b]pyridin-7-one; 1-(1-pyrrolidinyl)-2-butanone; 1-(2,3-dihydro-1H-pyrrolizin-5-yl)-1,4-pentanedione; 2,3,4,5,6,7-hexahydro-cyclopent[b]azepin-8(1H)-one; 5-(2-furanyl)-1,2,3,4,5,6-hexahydro-7H-cyclopenta[b]pyridin-7-one; 4-(2-furanylmethylene)-3,4-dihydro-2H-pyrrole; and 1,2,3,4,5,6-hexahydro-7H-cyclopenta[b]pyridin-7-one. An increase in the concentration of carotenoids may also be indicative that the Maillard reaction has taken place.
The treated botanical material may, in some embodiments, contain a reduced level of nicotine compared with untreated botanical material, as shown in the Examples. Nicotine is known to have a bitter taste and therefore having reduced levels of this compound can have a positive effect on the taste and flavour of the treated botanical material.
The production of a botanical material with desirable organoleptic properties advantageously removes the requirement to add further substances to the botanical material to provide or enhance its organoleptic properties. Such substances include flavourants and/or aromatising ingredients.
As used herein, the terms "flavour" and "flavourant" refer to materials which, where local regulations permit, may be used to create a desired taste or aroma in a product for adult consumers. They may include extracts (e.g., licorice, hydrangea, Japanese white bark magnolia leaf, chamomile, fenugreek, clove, menthol, Japanese mint, aniseed, cinnamon, herb, wintergreen, cherry, berry, peach, apple, Drambuie, bourbon, scotch, whiskey, spearmint, peppermint, lavender, cardamon, celery, cascarilla, nutmeg, sandalwood, bergamot, geranium, honey essence, rose oil, vanilla, lemon oil, orange oil, cassia, caraway, cognac, jasmine, ylang-ylang, sage, fennel, piment, ginger, anise, coriander, coffee, or a mint oil from any species of the genus Mentha), flavour enhancers, bitterness receptor site blockers, sensorial receptor site activators or stimulators, sugars and/or sugar substitutes (e.g., sucralose, acesulfame potassium, aspartame, saccharine, cyclamates, lactose, sucrose, glucose, fructose, sorbitol, or mannitol), and other additives such as charcoal, chlorophyll, minerals, botanicals, or breath freshening agents. They may be imitation, synthetic or natural ingredients or blends thereof. They may be in any suitable form, for example, oil, liquid, or powder.

Dry ice expansion

The processes described herein comprise dry ice expansion of treated botanical material (that is, dry ice expansion of botanical material that has previously been treated according to the treatment process described herein). As set out above, the processes may comprise carrying out the treatment process to provide the treated botanical material and dry ice expansion of the treated botanical material.
The treatment process and the dry ice expansion may be carried out in different locations. There may also be a delay between the treatment process and dry ice expansion for example to allow the treated botanical material to be transported to the location where the dry ice expansion is to be carried out.
Methods of dry ice expansion of botanical materials, such as tobacco, are known in the art. For example, dry ice expansion may involve permeating (or impregnating) the botanical material with liquid carbon dioxide under pressure, for example by submerging and soaking the botanical material in liquid carbon dioxide. Excess liquid and/or gaseous carbon dioxide can be recovered for reuse, for example by draining the liquid. The process may comprise converting the liquid carbon dioxide within the botanical material into solid carbon dioxide (dry ice), for example by reducing the pressure. This phase change may occur at the triple point pressure for CO₂ (60.4 psig and minus 69.83 degrees F.). The solid carbon dioxide is then subjected to conditions under which the solid carbon dioxide vaporizes (or under which the solid carbon dioxide undergoes sublimation to form gaseous carbon dioxide), thereby causing the botanical material to expand. For example, the botanical material comprising the solid carbon dioxide can be rapidly heated as set out below.
Immediately prior to impregnation, the botanical material may have a moisture content of 10-40% such as 15-35%, or 20-30%. Thus, the processes described herein may involve adjusting the water content of the treated botanical material to a moisture content any of these ranges (for example by wetting the treated botanical material).
Typically, the botanical material that is impregnated is in cut form, such as cut tobacco. Suitable cut widths are disclosed below in the description of Figure 1.
A suitable method of dry ice expansion may comprise impregnating the cell structure of the botanical material with liquid carbon dioxide. Suitable conditions for this impregnation step may comprise contacting the botanical material in an impregnator vessel with liquid carbon dioxide at a temperature of -40 to -10 °C, such as -25 to -15 °C, for a period of around 1-10 minutes, such as 2-8 or 3-7 minutes, under pressure. The pressure may be for example 435 psig (3000 kPa). After the impregnation step, the process typically then comprises reducing the pressure within the impregnator vessel sufficiently to cause solidification of the liquid carbon dioxide within the cell structure of the botanical material. For example, the pressure may be reduced to atmospheric pressure (1 atm). The process may then involve rapidly heating the botanical material to sublime the solid carbon dioxide in the cells of the botanical material, thereby causing the botanical material to expand. This rapid heating may be carried out by introducing the botanical material comprising solid carbon dioxide into a gas stream having a temperature of from 250 to 400 °C, such as 300-360 °C, or about 330 °C.
Figure 1 depicts a suitable exemplary process for preparing dry ice expanded tobacco. Bales of tobacco material are sliced and then the bales are conditioned using water and steam. The tobacco material can be any of the tobacco materials described herein. Lamina tobacco, in particular lamina Virginia tobacco, is particularly preferred. One reason for this is that it exhibits desirable organoleptic properties and, compared with other tobacco varieties, relatively low levels of compounds considered to be undesirable. Another benefit of using Virginia tobacco is that it tends to readily expand during the expansion process. In some embodiments, stem tobacco may be used in addition to lamina. After conditioning, the conditioned tobacco material is blended with other conditioned tobacco materials or mixed before being fed into a cutter. Preferably, the cutter cuts the tobacco material at 25 to 28 cuts per inch (CPI). A cut width of 25 CPI is particularly preferred, although other cut widths could be used. Cutting the tobacco material increases its surface area and thus reduces the time it takes to become impregnated with liquid during the impregnation step. These cut widths may also increase the fill value of the final material.
After wetting the cut material and blending the wet cut material, the material has a moisture content of around 26%. This material is then fed into an impregnator vessel, which is subsequently charged with carbon dioxide at a temperature of -20 °C for around 6 minutes under pressure. These conditions ensure that the carbon dioxide stays in a liquid form and has enough time to penetrate and be absorbed into the tobacco material. Following on from this, the impregnated tobacco material is fed into a sublimator, the pressure is reduced to allow the liquid carbon dioxide to solidify, the impregnated tobacco material is then heated in a gas stream at a temperature of 330 °C. This results in rapid volatilisation of the moisture and carbon dioxide in the tobacco material, which causes it to expand.
Other gas temperatures may be used. For example, the gas temperature may be between about 250 °C and about 400 °C or more. The maximum temperature is preferably below the combustion temperature of the botanical material, such as tobacco. High temperatures may improve the rate of expansion and thus the efficiency of the process. The fill value of the botanical material may also be controlled by changing the temperature. Increasing the temperature may lead to more moisture being driven off from the material and thus a higher fill value of the final material. Conversely, using lower temperatures may decrease the fill value of the final material.
The high gas temperatures can be achieved by any suitable means (e.g. by heating air using a hot plate or burner). The botanical material at the end of the sublimation is relatively dry and has a moisture content of around 6%. The moisture content may be increased to around 12% to 14% (the target is often 13.6%) by hydrating it in a reordering cylinder to produce the final expanded botanical material. The expanded material may have a fill value of at least about 6 cm³/g.
When referring to "moisture" it is important to understand that there are widely varying and conflicting definitions and terminology in use. It is common for "moisture" or "moisture content" to be used to refer to water content of a material but in relation to the certain industries, such as the tobacco industry, it is necessary to differentiate between "moisture" as water content and "moisture" as oven volatiles. Water content is defined as the percentage of water contained in the total mass of a solid substance. Volatiles are defined as the percentage of volatile components contained in the total mass of a solid substance. This includes water and all other volatile compounds. Oven dry mass is the mass that remains after the volatile substances have been driven off by heating. It is expressed as a percentage of the total mass. Oven volatiles (OV) are the mass of volatile substances that were driven off.
Moisture content (oven volatiles) may be measured as the reduction in mass when a sample is dried in a forced draft oven at a temperature regulated to 110°C ± 1°C for three hours ± 0.5 minutes. After drying, the sample is cooled in a desiccator to room temperature for approximately 30 minutes, to allow the sample to cool.
Unless stated otherwise, references to moisture content herein are references to oven volatiles (OV).
Figure 2 shows a cross section through a tobacco leaf before (top) and after (bottom) dry ice expansion. The scale bar (centre, bottom) of each image corresponds to a distance of 100 microns. The expansion of the tobacco material during the dry ice expansion process can be seen from a comparison of these images.
Filling value (also referred to herein as fill value) is a measure of the volume occupied by a given mass of botanical material, such as tobacco, when a given pressure is applied at a given moisture content. That is, the fill value is a measure of the ability of a material to occupy a specific volume at a given moisture content. In this invention, filling value may be determined by Test Method A as disclosed in the Examples section below.
In some embodiments, the fill value of the dry ice expanded botanical material at 13.5% moisture content is at least 6 cm³/g, such as at least 6.5 cm³/g or at least 7 cm³/g. In some embodiments, the fill value of the dry ice expanded botanical material at 13.5% moisture content is 6 to 10 cm³/g, such as 6.5 to 9 cm³/g or 7 to 8 cm³/g. The dry ice expanded botanical material provided by the processes described herein may be incorporated into a non-combustible aerosol provision system. For example, the dry ice expanded botanical material may be incorporated into an aerosol-generating material for use in a non-combustible aerosol provision system or into a consumable for use a non-combustible aerosol provision system.
The treated DIET material may be incorporated into an aerosol-free delivery system.
As used herein, the term "delivery system" is intended to encompass systems that deliver at least one substance to a user, and includes non-combustible aerosol provision systems that release compounds from an aerosol-generating material without combusting the aerosol-generating material, such as electronic cigarettes, tobacco heating products, and hybrid systems to generate aerosol using a combination of aerosol-generating materials; and
aerosol-free delivery systems that deliver the at least one substance to a user orally, nasally, transdermally or in another way without forming an aerosol, including but not limited to, lozenges, gums, patches, articles comprising inhalable powders, and oral products such as oral tobacco which includes snus or moist snuff, wherein the at least one substance may or may not comprise nicotine.
According to the present disclosure, a "non-combustible" aerosol provision system is one where a constituent aerosol-generating material of the aerosol provision system (or component thereof) is not combusted or burned in order to facilitate delivery of at least one substance to a user.
In some embodiments, the delivery system is a non-combustible aerosol provision system, such as a powered non-combustible aerosol provision system.
In some embodiments, the non-combustible aerosol provision system is an electronic cigarette, also known as a vaping device or electronic nicotine delivery system (END), although it is noted that the presence of nicotine in the aerosol-generating material is not a requirement.
In some embodiments, the non-combustible aerosol provision system is an aerosol-generating material heating system, also known as a heat-not-burn system. An example of such a system is a tobacco heating system.
In some embodiments, the non-combustible aerosol provision system is a hybrid system to generate aerosol using a combination of aerosol-generating materials, one or a plurality of which may be heated. Each of the aerosol-generating materials may be, for example, in the form of a solid, liquid or gel and may or may not contain nicotine. In some embodiments, the hybrid system comprises a liquid or gel aerosol-generating material and a solid aerosol-generating material. The solid aerosol-generating material may comprise, for example, tobacco or a non-tobacco product.
Typically, the non-combustible aerosol provision system may comprise a non-combustible aerosol provision device and a consumable for use with the non-combustible aerosol provision device.
In some embodiments, the disclosure relates to consumables comprising aerosol-generating material and configured to be used with non-combustible aerosol provision devices. These consumables are sometimes referred to as articles throughout the disclosure.
In some embodiments, the non-combustible aerosol provision system, such as a non-combustible aerosol provision device thereof, may comprise a power source and a controller. The power source may, for example, be an electric power source or an exothermic power source. In some embodiments, the exothermic power source comprises a carbon substrate which may be energised so as to distribute power in the form of heat to an aerosol-generating material or to a heat transfer material in proximity to the exothermic power source.
In some embodiments, the non-combustible aerosol provision system may comprise an area for receiving the consumable, an aerosol generator, an aerosol generation area, a housing, a mouthpiece, a filter and/or an aerosol-modifying agent.
In some embodiments, the consumable for use with the non-combustible aerosol provision device may comprise aerosol-generating material, an aerosol-generating material storage area, an aerosol-generating material transfer component, an aerosol generator, an aerosol generation area, a housing, a wrapper, a filter, a mouthpiece, and/or an aerosol-modifying agent.
An aerosol-generating material is a material that is capable of generating aerosol, for example when heated, irradiated or energized in any other way. Aerosol-generating material may, for example, be in the form of a solid, liquid or semi-solid (such as a gel).
In addition to the expanded botanical material provided by the processes described herein, the aerosol-generating material may comprise one or more active substances and/or flavours, one or more aerosol-former materials, and optionally one or more other functional materials.
In some embodiments, the expanded botanical material provided by the processes described herein may be mixed with a further aerosol-generating material. That is, the expanded botanical material may be incorporated into an aerosol-generating composition (or a blend) comprising (i) the expanded botanical material or an aerosol-generating material comprising the expanded botanical material, and (ii) optionally one or more further aerosol-generating materials. The aerosol-generating material (i) comprising the expanded botanical material and/or the further aerosol-generating material (ii) may comprise one or more active substances and/or flavours, one or more aerosol-former materials, and optionally one or more other functional materials.
The aerosol-generating material may comprise a binder, such as a gelling agent, and an aerosol former. Optionally, a filler may also be present. Optionally, a solvent, such as water, is also present and one or more other components of the aerosol-generating material may or may not be soluble in the solvent.
The aerosol-generating material may comprise or be in the form of an aerosol-generating film. The aerosol-generating film may comprise a binder, such as a gelling agent, and an aerosol former. Optionally, a filler may also be present.
The aerosol-generating film may have a thickness of about 0.015 mm to about 1 mm. For example, the thickness may be in the range of about 0.05 mm, 0.1 mm or 0.15 mm to about 0.5 mm or 0.3 mm.
The aerosol-generating film may be continuous. For example, the film may comprise or be a continuous sheet of material. The sheet may be in the form of a wrapper, it may be gathered to form a gathered sheet or it may be shredded to form a shredded sheet. The shredded sheet may comprise one or more strands or strips of aerosol-generating material.
The aerosol-generating film may be discontinuous. For example, the aerosol-generating film may comprise one or more discrete portions or regions of aerosol-generating material, such as dots, stripes or lines, which may be supported on a support. In such embodiments, the support may be planar or non-planar.
The aerosol-generating film may be formed by combining the expanded botanical material with a binder, such as a gelling agent, a solvent, such as water, an aerosol-former and one or more other components, to form a slurry and then heating the slurry to volatilise at least some of the solvent to form the aerosol-generating film.
The slurry may be heated to remove at least about 60 wt%, 70 wt%, 80 wt%, 85 wt% or 90 wt% of the solvent.
The aerosol-generating material may comprise or be an "amorphous solid". In some embodiments, the aerosol-generating material comprises an aerosol-generating film that is an amorphous solid. The amorphous solid may be a "monolithic solid". The amorphous solid may be substantially non-fibrous. In some embodiments, the amorphous solid may be a dried gel. The amorphous solid is a solid material that may retain some fluid, such as liquid, within it. In some embodiments, the amorphous solid may, for example, comprise from about 50wt%, 60wt% or 70wt% of amorphous solid, to about 90wt%, 95wt% or 100wt% of amorphous solid.
The aerosol-former material may comprise one or more constituents capable of forming an aerosol. In some embodiments, the aerosol-former material may comprise one or more of glycerol, propylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1 ,3-butylene glycol, erythritol, meso-Erythritol, ethyl vanillate, ethyl laurate, a diethyl suberate, triethyl citrate, triacetin, a diacetin mixture, benzyl benzoate, benzyl phenyl acetate, tributyrin, lauryl acetate, lauric acid, myristic acid, and propylene carbonate.
Aerosol-generating materials for use in non-combustible aerosol provision systems may typically comprise higher amounts of aerosol-former materials than smokable materials for use in combustible aerosol provision systems. For example, an aerosol-generating material comprising the expanded botanical material may comprise aerosol former in a total amount of from 10 to 60 wt% calculated on a dry weight basis (DWB), such as from 10 to 50 wt% (DWB), 12 to 30 wt% (DWB), or 15 to 35 wt% (DWB). In these embodiments, dry weight basis (DWB) refers to the whole of the material, other than any water, and may include components which by themselves are liquid at room temperature and pressure, such as glycerol.
In some embodiments, an aerosol-generating composition (or a blend) comprises (i) the expanded botanical material, or an aerosol-generating material comprising the expanded botanical material, and (ii) optionally one or more further aerosol-generating materials, and the total amount of aerosol-former present in the aerosol generating composition (or blend) may be from 4 to 30 wt% (DWB), such as from 5 to 25 wt% (DWB), from 5 to 20 wt% (DWB) or from 10 to 20 wt% (DWB) of the composition (or blend) In these embodiments, dry weight basis (DWB) refers to the whole of the composition (or blend), other than any water, and may include components which by themselves are liquid at room temperature and pressure, such as glycerol.
The aerosol-generating material may be present on or in a support, to form a substrate. The support may, for example, be or comprise paper, card, paperboard, cardboard, reconstituted material, a plastics material, a ceramic material, a composite material, glass, a metal, or a metal alloy. In some embodiments, the support comprises a susceptor. In some embodiments, the susceptor is embedded within the material. In some alternative embodiments, the susceptor is on one or either side of the aerosol-generating material.
A susceptor is a material that is heatable by penetration with a varying magnetic field, such as an alternating magnetic field. The susceptor may be an electrically-conductive material, so that penetration thereof with a varying magnetic field causes induction heating of the heating material. The heating material may be magnetic material, so that penetration thereof with a varying magnetic field causes magnetic hysteresis heating of the heating material. The susceptor may be both electrically-conductive and magnetic, so that the susceptor is heatable by both heating mechanisms. The device that is configured to generate the varying magnetic field is referred to as a magnetic field generator, herein.
In some embodiments, the delivery system is an aerosol-free delivery system that delivers at least one substance to a user orally, nasally, transdermally or in another way without forming an aerosol, including but not limited to, lozenges, gums, patches, articles comprising inhalable powders, and oral products such as oral tobacco which includes snus or moist snuff, wherein the at least one substance may or may not comprise nicotine.
In some embodiments, extracts, such as tobacco extracts, may be created from dry ice expanded botanical material which has undergone the processing described herein. In some embodiments, the extract may be a liquid, for example it may be an aqueous extract. In other embodiments, the extract may be produced by supercritical fluid extraction.
In some embodiments, the extracts may be used in non-combustible aerosol provision systems or aerosol-free delivery systems. For example, the extracts may be heated to create an inhalable vapour in an electronic cigarette or similar device. Alternatively, the extracts may be added to tobacco or another material for heating, such as in a heat-not-burn product.
The favourable change in the organoleptic properties of the botanical material provided by the process herein means that the dry ice expanded botanical material can be added to blends (for example for use in a non-combustible aerosol provision system or aerosol-free delivery system), or to aerosol generating materials or consumables for use in non-combustible aerosol provision systems in higher quantities than untreated dry ice expanded botanical material without compromising the organoleptic properties of the blends, aerosol generating materials or consumables.
In some embodiments, a blend may comprise the expanded botanical material (such as tobacco) obtained by, or obtainable by, the process described herein in an amount of from 1 to 40 wt%, such as from 5 to 35 wt%, from 5 to 30 wt%, from 10 to 27, or from 12.5 to 25 wt%, or from 15 to 25 wt%, relative to the total weight of the blend.
When the expanded botanical material is dry ice expanded tobacco material, the blend may further comprise one or more other tobacco varieties, optionally including one or more Virginia tobaccos, one or more Burley tobaccos, one of more Oriental tobaccos and combinations thereof. Dry ice expanded tobacco obtained by, or obtainable by, the process described herein may contribute dark taste characteristics such that the blend can provided sufficient dark taste notes with lower inclusions of Burley tobacco varieties.
In particular embodiments, in addition to the dry ice expanded tobacco obtained by, or obtainable by, the process described herein, the blend may further comprise one or more Burley tobacco varieties in a total amount of 30 wt% or less, such as 25 wt% or less, 20 wt% or less, or 15 wt% or less, relative to the total weight of the blend. For example, the blend may further comprise one or more Burley tobacco varieties in a total amount of from 1 to 30 wt%, from 1 to 25 wt%, such as from 2 to 20 wt%, from 3 to 15 wt% or from 5 to 10 wt%. In addition to the dry ice expanded tobacco obtained by, or obtainable by, the process described herein, the blend may further comprise one or more Virginia tobacco varieties in a total amount of up to 55 wt%, such as from 1 to 55 wt%, from 1 to 50 wt%, from 10 to 40 wt%, or from 15 to 35 wt%, relative to the total weight of the blend. In addition to the dry ice expanded tobacco obtained by, or obtainable by, the process described herein, the blend may further comprise one or more Oriental tobacco varieties in a total amount of up to 35 wt%, such as from 1 to 35 wt%, from 1 to 30 wt%, from 2 to 25 wt% or from 5 to 20 wt%, relative to the total weight of the blend. These amounts do not include any Virginia, Burley or Oriental tobacco within the dry ice expanded tobacco itself.
In order to address various issues and advance the art, the entirety of this disclosure shows by way of illustration various embodiments in which the claimed invention(s) may be practiced and provide for superior dry ice expanded botanical material production processes. The advantages and features of the disclosure are of a representative sample of embodiments only, and are not exhaustive and/or exclusive. They are presented only to assist in understanding and teach the claimed features. It is to be understood that advantages, embodiments, examples, functions, features, structures, and/or other aspects of the disclosure are not to be considered limitations on the disclosure as defined by the claims or limitations on equivalents to the claims, and that other embodiments may be utilised and modifications may be made without departing from the scope and/or spirit of the disclosure. Various embodiments may suitably comprise, consist of, or consist essentially of, various combinations of the disclosed elements, components, features, parts, steps, means, etc. In addition, the disclosure includes other inventions not presently claimed, but which may be claimed in future.

Examples

Test Method A

In the below examples, the fill value of the tobacco was measured according to the following process. This method is applicable to other botanical materials as well as tobacco.
A 15 g sample of the tobacco material was deposited into a 60 mm diameter cylinder of a densimeter and then the tobacco material was compressed with a 2.90 ± 0.03 kg piston for 30 seconds. The height of the piston in the densimeter as well as the moisture content of the samples were measured. The fill values of the samples were calculated according to the following formulae.
The volume occupied by the tobacco material when compressed was determined using Formula 1: $Volume ({cm}^{3}) = π x r^{2} x \frac{h}{10}$

r = radius of cylinder (cm)
h = measured height (mm)

The fill value was then determined using the measured volume and mass of tobacco material according to Formula 2: $Fill value [\frac{{cm}^{3}}{10 g}] = 10 x \frac{Volume [{cm}^{3}]}{Mass [g]}$
The fill value was corrected to account for its moisture content using Formula 3: ${FV}_{0} = \frac{FV \times (100 - M_{0}) \times {(\frac{M}{M_{0}})}^{0.8}}{100 - M}$

FV₀= Fill value at moisture content M_o%
FV = Fill value determined at moisture content M% (cm³/10 g)
M_o= 13.5% (target moisture content)
M = Actual moisture content of tobacco material (%)
0.8 = constant

Moisture content (oven volatiles) is measured as the reduction in mass when a sample is dried in a forced draft oven at a temperature regulated to 110°C ± 1°C for three hours ± 0.5 minutes. After drying, the sample is cooled in a desiccator to room temperature for approximately 30 minutes, to allow the sample to cool.

Comparative Example 1

Dry ice expansion of untreated tobacco

Lamina Virginia and Burley tobacco were conditioned, mixed, cut and dried.
The tobacco material was then formed into dry ice expanded tobacco. The cut Virginia and cut Burley tobacco were wetted. For Sample R below, the Virginia and Burley tobacco were then blended. The wet and optionally blended tobacco material had a moisture content of around 26%. The tobacco material was then fed into an impregnator vessel, which was subsequently charged with carbon dioxide at a temperature of -20 °C for around 6 minutes under pressure. The impregnated tobacco material was fed into a sublimator and the pressure was then reduced to allow the liquid carbon dioxide to solidify. The impregnated tobacco material was then heated in a gas stream at a temperature of 330 °C which led to rapid volatilisation of the moisture and carbon dioxide in the tobacco material.
Sample A below is dry ice expanded of lamina Virginia tobacco. Sample R below is a 1:1 w/w blend of dry ice expanded lamina Virginia and Burley tobacco.

Production of expanded stem tobacco

Tobacco stems obtained by green-leaf threshing were wet to a moisture content of 25-35% and then cut to a cut width of 25-28 CPI. The cut stem was then expanded by steam treatment involving heating to a temperature of 180-250 °C for a period of 15 seconds to 3 minutes, leading to vaporisation of water within the tobacco cells and expansion of the tobacco. After the steam treatment the stem tobacco had a moisture content of 13-14%.

Treatment of Tobacco

80 kg of the DIET tobacco was packed in a single walled cardboard box having external dimensions of 0.835 m x 1.120 m x 0.765 m, wrapped with polyethylene liner (Polyliner^®), and was set to rest for a minimum period of 30 days before being exposed to the ambient processing conditions of 60°C and 60% relative humidity and a process time of 35, 37 or 39 days (for Sample A) or 35 days (for Sample R). The packing density of the tobacco before treatment was about 123 kg/m³.
70 kg of the expanded stem was packed in a C-48 box, wrapped with polyethylene liner (Polyliner^®), and was set to rest for a minimum period of 30 days before being exposed to the ambient processing conditions of 60°C and 60% relative humidity and a process time of 14, 21 or 28 days.

Taste evaluation

Cigarettes comprising the untreated DIET, untreated expanded stem, treated DIET, or treated expanded stem were produced. A blind smoking trial was then conducted by expert smokers. No significant difference in taste was observed for the treated expanded stem as compared to the untreated expanded stem. However, an increase in spicy taste notes was observed for the treated DIET (for both Sample A and Sample R) as compared to the untreated DIET. An increase in tannin taste notes was also observed for the treated Sample R DIET compared to the untreated control.
Thus, the taste properties of DIET tobacco were unexpectedly improved by the treatment, unlike other forms of expanded tobacco (expanded stem).

Comparative Example 2

Lamina Virginia tobacco was treated by the method set out in Example 1 for Sample A for a duration of 39 days. After the treatment, the temperature of the DIET tobacco was 64 °C. The temperature of the tobacco was then gradually reduced to 22 °C during a stabilisation period of 40 days. Large clumps of tobacco were observed within the treated DIET material. The properties of the tobacco after the stabilisation period are shown in the table below (Test 1)
After the stabilisation period, the DIET tobacco had a moisture content (OV) of 14% and a fill value of 6.8 cc/g. The proportion of the tobacco which did not pass through a mesh having a hole size of 2.5 cm x 2.5 cm was 40 wt%.

Example 3

3.1 Treatment of Tobacco

Virginia tobacco was green-leaf blended and threshed, conditioned and packed in a C-48 box at 200kg and 13% oven volatiles moisture (3 hours at 110°C), wrapped with polyethylene liner (Polyliner^®), and was set to rest for a minimum period of 30 days before being exposed to the ambient processing conditions of 60°C and 60% relative humidity and a process time of 30 days. No clumps of tobacco were observed after the treatment.
As compared to the tobacco material before treatment, the treated tobacco material contained: a reduced amount of nicotine; reduced amount of sugars; increased water content; increased content of Maillard reaction products including 2,5 deoxyfructosazine, 2,6 deoxyfructosazine, 5-acetyl-2,3-dihydro-1H-pyrrolizine, 2,3-dihydro-5-methyl-1H-pyrrolizine-7-carboxaldehyde, 1,2,3,4,5,6-hexahydro-5-(1-hydroxyethylidene)-7H-cyclopenta[b]pyridin-7-one, 1-(1-pyrrolidinyl)-2-butanone, 1-(2,3-dihydro-1H-pyrrolizin-5-yl)-1,4-pentanedione, 2,3,4,5,6,7-hexahydrocyclopent[b]azepin-8(1H)-one, 5-(2-furanyl)-1,2,3,4,5,6-hexahydro-7H-cyclopenta[b]pyridin-7-one, 4-(2-furanylmethylene)-3,4-dihydro-2H-pyrrole, and 1,2,3,4,5,6-hexahydro-7H-cyclopenta[b]pyridin-7-one; and increased content of oleic acid, linoleic acid and linolenic acid.
Microbial analysis of the treated tobacco was conducted by using Petrifilm^® Yeast and Mould Count Plates for moulds and yeasts, Petrifilm^® Aerobic Count Plates for total bacteria, and the most probable number (MPN) method for coliforms.
The results showed that the microbial content of the treated tobacco is very low, with no coliform CFUs observed in the treated tobacco after incubation at 35°C or 45°C, and very low numbers of CFUs observed for moulds and yeasts and in the aerobic plate count. This confirms that the treatment process described herein does not involve fermentation.

3.2 Dry-ice expansion

Treated tobacco material obtained in Example 3.1 was cut. The cut treated tobacco was then wetted to achieve a moisture content (OV) of around 26%. The tobacco material was then fed into an impregnator vessel, which was subsequently charged with carbon dioxide at a temperature of -20 °C for around 6 minutes under pressure. The impregnated tobacco material was fed into a sublimator and the pressure was then reduced to allow the liquid carbon dioxide to solidify. The impregnated tobacco material was then heated in a gas stream at a temperature of 330 °C which led to rapid volatilisation of the moisture and carbon dioxide in the tobacco material.

3.3 Properties evaluation

Fill value of the dry ice expanded tobacco produced in Example 3 was measured as 73.9 cm³/10 g. The fill value of dry ice expanded tobacco provided by an analogous process to Comparative Example 1 (Sample A) was measured as 73.1 cm³/10 g.
In a taste analysis, cigarettes comprising the dry ice expanded tobacco produced in Comparative Example 1 (Sample A) and the dry ice expanded tobacco produced in Example 3 were produced. The smokable material in the cigarettes was made up entirely of the dry ice expanded tobacco. A blind smoking trial was then conducted by expert smokers who evaluated the following taste attributes: impact, taste intensity, quality, dryness, sweetness, bitterness, aftertaste quality, mouth coating and off notes. No statistically significant differences between these attributes was observed when comparing the dry ice expanded tobaccos produced in Comparative Example 1 and Example 3.
Thus, despite the dry ice expansion process being carried out after the treatment process in Example 3 (rather than before the treatment process as in Comparative Example 1) the dry ice expanded botanical material provided in Example 3 still shows favourable taste/sensorial properties. Reversing the order of the treatment and dry ice expansion steps also does not significantly affect the fill value.
Aspects A1-A30 of the invention are set out below:

A1. A process for producing expanded botanical material for use in a non-combustible aerosol delivery system or an aerosol-free delivery system, the process comprising:
dry ice expansion of a treated botanical material, wherein the treated botanical material has previously been formed by a treatment process comprising:
heating a botanical material which is enclosed within a moisture-retaining material.
A2. The process of Aspect A1, wherein the botanical material is tobacco.
A3. The process of Aspect A1 or Aspect A2, wherein the dry ice expansion of the treated botanical material comprises:
1. (a) impregnating the treated botanical material with liquid carbon dioxide under pressure,
2. (b) converting the liquid carbon dioxide within the botanical material into solid carbon dioxide, and
3. (c) subjecting the solid carbon dioxide to conditions under which the solid carbon dioxide undergoes sublimation to form gaseous carbon dioxide.
A4. The process of Aspect A3, wherein step (c) comprises introducing the treated botanical material comprising solid carbon dioxide into a gas stream having a temperature of from 250 to 400 °C.
A5. The process of Aspect A3 or Aspect A4, wherein the treated botanical material in step (a) is in cut form.
A6. The process of Aspect A5 wherein the process comprises cutting the treated botanical material to provide the botanical material in cut form.
A7. The process of any of Aspects A1-A6, wherein the process comprises carrying out the treatment process to provide the treated botanical material.
A8. The process of any of Aspects A1-A7, wherein the moisture content of the botanical material before and during the treatment process is between about 10% and about 23%.
A9. The process of any of Aspects A1-A8, wherein the moisture content of the botanical material before and during the treatment process is between about 10% and about 15.5%.
A10. The process of any of Aspects A1-A9, wherein the botanical material has a packing density on a dry matter weight base of at least 200 kg/m³ at the start of the treatment process.
A11. The process of any of Aspects A1-A10, wherein the at the start of the treatment process the botanical material has a packing density on a dry matter weight base of up to about 500 kg/m³.
A12. The process of any of Aspects A1-A11, wherein the step of the treatment process of heating the botanical material increases the temperature of the botanical material to a temperature equal to or above a threshold temperature of 55°C, and/or wherein the temperature of the botanical material is raised during the treatment process to a temperature of from about 55°C to about 100°C.
A13. The process of any of Aspects A1-A12, wherein the step of the treatment process of heating the botanical material comprises exposing the botanical material to an ambient processing temperature of at least about 45°C.
A14. The process of any of Aspects A1-A13, wherein the botanical material comprises lamina tobacco.
A15. The process of any of Aspects A1-A14, wherein the botanical material comprises Virginia tobacco
A16. The process of Aspect A15, wherein the Virginia tobacco is lamina tobacco.
A17. The process of to any of Aspects A1-A16, wherein the botanical material is heated during the treatment process for between about 5 and 65 days.
A18. The process of Aspect A13, wherein the botanical material is exposed to the ambient processing temperature for between about 5 and 65 days.
A19. The process of any of Aspects A1-A18, wherein the dry ice expanded botanical material provided by the dry ice expansion has a fill value at 13.5% moisture of at least 6 cm³/g.
A20. The process of any of Aspects A1-A19, wherein the microbial content of the treated botanical material is lower than the microbial content of the botanical material at the start of the treatment process.
A21. The process of any of Aspects A1-A20, wherein the treatment process involves essentially no fermentation.
A22. A process according to any of Aspects A1-A21, wherein during the treatment process the botanical material is placed in a chamber to control the ambient processing temperature and/or ambient relative processing humidity.
A23. Expanded botanical material obtainable by the process of any one of Aspects A 1-A22.
A24. An aerosol-generating material for use in a non-combustible aerosol provision system, the aerosol-generating material comprising the expanded botanical material of Aspect A23.
A25. The aerosol-generating material of Aspect A24, further comprising one or more aerosol-formers in a total amount of from 10 to 60 wt% calculated on a dry weight basis (DWB), such as from 10 to 50 wt% (DWB), 12 to 30 wt% (DWB), or 15 to 35 wt% (DWB).
A26. An aerosol-generating composition comprising the expanded botanical material of Aspect A23, or the aerosol-generating material of Aspect A24 or A25, wherein the total amount of aerosol-former present in the aerosol generating composition is from 4 to 30 wt% of the composition by dry weight (DWB), such as from 5 to 25 wt% (DWB), from 5 to 20 wt% (DWB) or from 10 to 20 wt% (DWB).
A27. A consumable for use in a non-combustible aerosol provision system, the consumable comprising the expanded botanical material of Aspect A23 or the aerosol-generating material of any of Aspects A24-A25, or the aerosol-generating composition of Aspect A26.
A28. A non-combustible aerosol provision system comprising the expanded botanical material of Aspect A23, the aerosol-generating material of any of Aspects A24-A25, the aerosol-generating composition of Aspect A26, or the consumable of Aspect A27.
A29. Use of the expanded botanical material of Aspect A23 for the manufacture of: an aerosol-generating material for use in a non-combustible aerosol provision system or a consumable for use in a non-combustible aerosol provision system; or for the manufacture of an aerosol-free delivery system.
A30. An aerosol-free delivery system comprising the expanded botanical material Aspect A23.

Claims

A process for producing expanded botanical material for use in a non-combustible aerosol delivery system or an aerosol-free delivery system, the process comprising:
dry ice expansion of a treated botanical material, wherein the treated botanical material has previously been formed by a treatment process comprising:
heating a botanical material which is enclosed within a moisture-retaining material.
The process of claim 1, wherein the botanical material is tobacco.
The process of claim 1 or claim 2, wherein the dry ice expansion of the treated botanical material comprises:
(a) impregnating the treated botanical material with liquid carbon dioxide under pressure,

(b) converting the liquid carbon dioxide within the botanical material into solid carbon dioxide, and

(c) subjecting the solid carbon dioxide to conditions under which the solid carbon dioxide undergoes sublimation to form gaseous carbon dioxide.
The process of any preceding claim, wherein the process comprises carrying out the treatment process to provide the treated botanical material.
The process of any preceding claim, wherein the moisture content of the botanical material before and during the treatment process is between about 10% and about 23%, optionally between about 10% and about 15.5% before and during the treatment process.
The process of any preceding claim, wherein the botanical material has a packing density on a dry matter weight base of at least 200 kg/m³ at the start of the treatment process.
The process of any preceding claim, wherein the step of the treatment process of heating the botanical material increases the temperature of the botanical material to a temperature equal to or above a threshold temperature of 55°C, and/or wherein the temperature of the botanical material is raised during the treatment process to a temperature of from about 55°C to about 100°C.
The process of to any preceding claim, wherein the botanical material comprises lamina tobacco.
The process of to any preceding claim, wherein the botanical material is heated during the treatment process for between about 5 and 65 days.
Expanded botanical material obtainable by the process of any one of the preceding claims.
An aerosol-generating material for use in a non-combustible aerosol provision system, the aerosol-generating material comprising the expanded botanical material of claim 10.
A consumable for use in a non-combustible aerosol provision system, the consumable comprising the expanded botanical material of claim 10 or the aerosol-generating material of claim 11.
A non-combustible aerosol provision system comprising the expanded botanical material of claim 10, the aerosol-generating material of claim 11, or the consumable of claim 12.
Use of the expanded botanical material of claim 10 for the manufacture of: an aerosol-generating material for use in a non-combustible aerosol provision system or a consumable for use in a non-combustible aerosol provision system; or for the manufacture of an aerosol-free delivery system.
An aerosol-free delivery system comprising the expanded botanical material claim 10.