Classifications

• • A—HUMAN NECESSITIES
  • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
  • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
  • A24B3/00—Preparing tobacco in the factory
  • A24B3/18—Other treatment of leaves, e.g. puffing, crimpling, cleaning
  • A24B3/182—Puffing
  • A24B3/185—Puffing by impregnating with a liquid and subsequently freezing and evaporating this liquid
• • A—HUMAN NECESSITIES
  • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
  • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
  • A24B3/00—Preparing tobacco in the factory
  • A24B3/12—Steaming, curing, or flavouring tobacco

Definitions

• 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).
• DIET dry ice expanded tobacco
• tobacco material 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.
• 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.
• a process 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 botanical material that is treated in the treatment process may be tobacco.
• 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.
• a further aspect provides the use of the dry ice expanded botanical material of the third aspect for the manufacture of a component for use in a combustible aerosol provision 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.
• 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.
• treated botanical material refers to botanical material, such as tobacco, that has undergone the treatment process described herein.
• untreated botanical material refers to botanical material that has not undergone the treatment process.
• 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 combustible aerosol provision systems and/or components thereof. 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.
• 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.
• the formation of these clumps can be avoided by carrying out the dry ice expansion after the treatment process described herein.
• 180-200 kg of botanical material such as tobacco material
• 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.
• the temperature of the botanical material such as the tobacco material
• the botanical material, such as the tobacco material is incubated for a total of 25 to 35 days.
• the treated botanical material may have a different colour from untreated botanical material.
• the botanical material such as tobacco material, is darker than untreated botanical material.
• 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),
• extracts
• 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.
• 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 CO 2 (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.
• the botanical material comprising the solid carbon dioxide can be rapidly heated as set out below.
• the botanical material may have a moisture content of 10-40% such as 15-35%, or 20-30%.
• 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).
• 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).
• 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.
• 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.
• the 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.
• gas temperatures may be used.
• 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 cm 3 /g.
• moisture 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 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.
• 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 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.
• the treated dry ice expanded botanical material provided by the processes described herein may be incorporated into a combustible aerosol delivery system, which may also be referred to as a smoking article herein.
• delivery system is intended to encompass systems that deliver at least one substance to a user, and includes combustible aerosol provision systems, such as cigarettes, cigarillos, cigars, and tobacco for pipes or for roll-your-own or for make-your-own cigarettes (whether based on tobacco, tobacco derivatives, expanded tobacco, reconstituted tobacco, tobacco substitutes or other smokable material).
• a "combustible" aerosol provision system is one where a constituent aerosol-generating material of the aerosol provision system (or component thereof) is combusted or burned during use in order to facilitate delivery of at least one substance to a user.
• the combustible aerosol provision system is selected from the group consisting of a cigarette, a cigarillo and a cigar.
• the disclosure relates to a component for use in a combustible aerosol provision system, such as a filter, a filter rod, a filter segment, a tobacco rod, a spill, an aerosol-modifying agent release component such as a capsule, a thread, or a bead, or a paper such as a plug wrap, a tipping paper or a cigarette paper.
• a component for use in a combustible aerosol provision system such as a filter, a filter rod, a filter segment, a tobacco rod, a spill, an aerosol-modifying agent release component such as a capsule, a thread, or a bead, or a paper such as a plug wrap, a tipping paper or a cigarette paper.
• Dry ice expanded tobacco material provided by the processes described herein may be used for roll-your-own tobacco and/or pipe tobacco.
• Dry ice expanded botanical material provided by the processes described herein, such as dry ice expanded tobacco, may be blended with one or more (further) tobacco materials before being incorporated into a smoking article or smokeless tobacco product or used for roll-your-own or pipe tobacco.
• extracts such as tobacco extracts
• the extract may be created from dry ice expanded botanical material which has undergone the processing described herein.
• the extract may be a liquid, for example it may be an aqueous extract.
• the extract may be produced by supercritical fluid extraction.
• the extracts may be used in combustible aerosol provision systems.
• the extracts may be added to tobacco or another material for combustion.
• the favourable change in the organoleptic properties of the botanical material means that the dry ice expanded botanical material can be added to blends (for example for use in a smoking article), or to a combustible aerosol delivery system or to a component thereof, in higher quantities than untreated dry ice expanded botanical material without compromising the organoleptic properties of the blends, combustible aerosol delivery system or component thereof.
• a blend may comprise the dry ice expanded botanical material (such as tobacco) obtained by, or obtainable by, the process described herein in an amount of from 1 to 60 wt%, such as from 5 to 60 wt%, from 10 to 55 wt%, from 15 to 50, or from 20 to 45 wt %, relative to the total weight of the blend.
• dry ice expanded botanical material such as tobacco
• 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.
• the aerosol-former material may comprise one or more constituents capable of forming an aerosol.
• 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.
• Smokable materials for use in combustible aerosol provision systems may typically comprise lower amounts of aerosol-former materials than aerosol-generating materials for use in non-combustible aerosol provision systems.
• a smokable material comprising the expanded botanical material may comprise aerosol former in a total amount of from 0 to 20 wt% calculated on a dry weight basis (DWB), such as from 0.1 to 10 wt% (DWB), 0.25 to less than 10 wt% (DWB), such as 0.5 to 9 wt% (DWB) or 1 to 5 wt% (DWB).
• DWB dry weight basis
• the expanded botanical material provided by the processes described herein, or a smokable material comprising the expanded botanical material (for example in combination with an aerosol-former material), may be blended with further components to provide a blend, for example as set out above.
• the total amount of aerosol-former present in the blend may be from 0 to less than 4 wt% (DWB), such as 0.1 to 2 wt%.
• DWB dry weight basis
• DWB dry weight basis
• 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.
• volume cm 3 ⁇ ⁇ r 2 ⁇ h 10
• Moisture content 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.
• 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.
• 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/m 3 .
• 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.
• 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)
• 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.
• 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.

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Citations (5)

• 2024
  • 2024-01-16 EP EP24152239.0A patent/EP4588370A1/fr active Pending
• 2025
  • 2025-01-16 WO PCT/EP2025/051080 patent/WO2025153642A1/fr active Pending

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