WO2025076806A1

WO2025076806A1 - Method of making granular compositions comprising benefit agent

Info

Publication number: WO2025076806A1
Application number: PCT/CN2023/124458
Authority: WO
Inventors: Dan Xu; Yue Zhao; Yizhuo Zhang; Boon Ho NG; Kerui DING; Guojun NIE; Xiaobin CHU
Original assignee: Procter and Gamble Co
Current assignee: Procter and Gamble Co
Priority date: 2023-10-13
Filing date: 2023-10-13
Publication date: 2025-04-17
Anticipated expiration: 2026-04-13

Abstract

A process of making a granular composition is provided.

Description

METHOD OF MAKING GRANULAR COMPOSITIONS COMPRISING BENEFIT AGENT

FIELD OF THE INVENTION

The present invention is directed to methods of making granular compositions containing a benefit agent.

BACKGROUND OF THE INVENTION

Granular laundry detergent compositions are well known. Granular laundry detergent compositions comprise one or more surfactants which can provide a good fabric-cleaning performance. Genearlly, granular laundry detergent compositions can be prepared by using different processes including spray-drying and agglomerate. Spray-drying is the standard method for manufacturing laundry detergent base powder. Typically, detergent ingredients are mixed together to form an aqueous detergent slurry in a mixer, such as a crutcher mixer. This slurry is then transferred along a pipe through a first low pressure pump and then through a second high pressure pump to a spray nozzle, and the slurry is sprayed into a spray-drying tower, and spray-dried to form a spray-dried powder. Typically, a suitable agglomeration process comprises the step of contacting a detersive ingredient, such as a detersive surfactant, e.g. linear alkyl benzene sulphonate (LAS) and/or alkyl alkoxylated sulphate, with an inorganic material, such as sodium carbonate and/or silica, in a mixer.

Preferably, in addition to surfactants, a benefit agent (e.g. perfume) is often added in laundry detergents to delight consumers. For granular detergent products, the benefit agent is generally added by spraying onto base detergent particles, such as spray-dried base detergent particles and/or agglomerated base detergent particles. Typically, this spray-on step is carried out in a tumbling drum mixer.

However, the inventors of the present invention notice that the loss of spray-on benefit agent (e.g. perfume) is significant during the manufacturing of granular detergent products due to various causes, e.g. evaporation and discharging from dust removing devices. Currently, one of the solutions is to increase the level of the benefit agent so as to secure superiority of the final products to consumers, which apparently results in a higher cost.

Thus, there is a need in the art for a new approach to reduce the loss of benefit agent during the manufacturing of granular detergent products.

The inventors of the present invention have surprisingly found that when the nozzle for spraying benefit agent is configured to be positioned at an appropriate location, the loss of benefit agent is significantly reduced. As such, the total amount of benefit agent needed for the making of granular detergent products can be reduced, resulting in cost saving.

Furthermore, the inventors of the present invention have surprisingly found that when the spray of droplets has a specific range of median droplet size, the loss of benefit agent is also significantly reduced.

SUMMARY OF THE INVENTION

The present invention addresses the aforementioned needs by providing the following method of making a granular composition.

In one aspect, the present invention relates to a process of making a granular composition comprising the steps of: a) providing a plurality of particles in a rotating drum comprising a nozzle located inside said rotating drum as well as a liquid composition comprising a benefit agent; and b) spraying said liquid composition through said nozzle onto at least a portion of said plurality of particles so as to provide said granular composition, wherein said nozzle is configured to be positioned at a height of H_N from said plurality of particles when spraying, wherein H_N is from 12cm to 48cm. Particularly, the granular composition is a granular detergent composition, preferably a granular laundry detergent composition.

In another aspect, the present invention relates to a process of making a granular composition comprising the steps of: a) providing a plurality of particles in a rotating drum comprising a nozzle located inside said rotating drum as well as a liquid composition comprising a benefit agent; and b) spraying said liquid composition through said nozzle onto at least a portion of said plurality of particles so as to provide said granular composition, wherein said liquid composition is sprayed in the form of a spray of droplets having a median droplet size of from 10 μm to 1000 μm. In particular embodiments, the median droplet size is preferably from 10 μm to 1000 μm, preferably from 20 μm to 800 μm, more preferably from 25 μm to 600 μm, most preferably from 30 μm to 500 μm, e.g. 50 μm, 70 μm, 90 μm, 100 μm, 120 μm, 150 μm, 200 μm, 300 μm, 400 μm or any ranges therebetween.

In another aspect, the present invention relates to a system for making a granular composition, wherein said system comprises: i) a rotating drum comprising a nozzle, a flat panel and an air outlet which are located inside said rotating drum and above said plurality of particles, and wherein said flat panel is positioned between said nozzle and said air outlet, wherein said nozzle is configured to be positioned at a height of H_N from said plurality of particles when spraying which is from 12cm to 48cm, wherein the rotating drum has a diameter of D_R which is from 50 cm to 500 cm, ii) a static mixer which is in fluid communication with said nozzle, and iii) a first reservoir for containing a benefit agent and a second reservoir for containing a liquid protective agent, in which said first and second reservoirs are both in fluid communication with said static mixer.

It is an advantage of the process to reduce the loss of benefit agent during the manufacturing of granular products without resulting in a significant caking problem.

It is another advantage of the process to reduce the amount of benefit agent needed in the granular products.

It is another advantage of the process to save cost for making granular products.

These and other features, aspects and advantages of specific embodiments will become evident to those skilled in the art from a reading of the present disclosure.

BRIEF DESCRIPTION OF THE DRAWINGS

The embodiments set forth in the drawings are illustrative in nature and not intended to limit the invention defined by the claims. The following detailed description of the illustrative embodiments can be understood when read in conjunction with the following drawings, and in which:

Figure 1 illustrates an examlary system for making a granular detergent composition.

Figure 2 illustrates an experimental equipment set up for determining benefit agent (e.g. perfume) loss during the spray-on process.

Figure 3 illustrates a device for cake strength testing.

Figure 4 shows the results in Example 1 which proves the loss of benefit agent is significantly reduced without resulting in a significant caking problem when the nozzle for spraying benefit agent is configured to be positioned at an appropriate location.

DETAILED DESCRIPTION OF THE INVENTION

All percentages, parts and ratios are based upon the total weight of the composition of the present invention and all measurements made are at 25℃, unless otherwise specified. All such weights as they pertain to listed ingredients are based on the active level and therefore do not include carriers or by-products that may be included in commercially available materials, unless otherwise specified.

As used herein, the articles "a" and "an" when used in a claim, are understood to mean one or more of what is claimed or described.

As used herein, the term "laundry detergent" means a liquid or solid composition, and includes, unless otherwise indicated, granular or powder-form all-purpose or "heavy-duty" washing agents, especially cleaning detergents as well as cleaning auxiliaries such as bleach additives or pre-treat types. In one embodiment, the laundry detergent is a solid laundry detergent composition, and preferably a free-flowing particulate laundry detergent composition (i.e., a granular detergent product) .

As used herein, the term "liquid composition" means a composition that can flow freely but is of constant volume, which cover an aqueous solution, a non-aqueous solution, a suspension, a slurry, a paste and the like.

The term “height” of a nozzle from the plurality of detergent particles as used herein (i.e., H_N) refers to the minimum distance between the nozzle and the plurality of detergent particles. Usually, the plurality of detergent particles are arranged like a bed in a drum mixer as shown in Fig. 1, as such the plurality of detergent particles are also called as “powder bed” .

The term “spray angle” as used herein refers to the angle of spray shape, particularly the opening angle which the nozzle jet of droplets forms at the moment when it leaves the nozzle orifice.

Process of making

In one aspect, the present invention relates to a process of making a granular detergent composition comprising the steps of: a) providing a plurality of detergent particles in a rotating drum comprising a nozzle located inside said rotating drum as well as a liquid composition comprising a benefit agent; and b) spraying said liquid composition through said nozzle onto at least a portion of said plurality of detergent particles so as to provide said granular detergent composition, wherein said nozzle is configured to be positioned at a height of H_N from said plurality of detergent particles when spraying, wherein H_N is from 12cm to 48cm. Particularly, H_N is from 15cm to 45cm, preferably from 17cm to 43cm, more preferably from 19cm to 41cm, and most preferably from 20cm to 40cm.

In some embodiments, the rotating drum has a diameter of D_R which is from 50 cm to 500 cm, preferably from 70 cm to 400 cm, more preferably from 100 cm to 300 cm, and most preferably from 100 cm to 250 cm.

In some embodiments, said nozzle is configured to have a spray angle of from 30 degrees to 170 degrees, preferably from 60 degrees to 140 degrees, e.g. 60 degrees, 70 degrees, 80 degrees, 90 degrees, 100 degrees, 110 degrees, 120 degrees, 130 degrees or any ranges therebetween.

In some embodiments, said nozzle is configured to have a diameter of from 0.2 mm to 10 mm, preferably from 0.4 mm to 5 mm, more preferably from 0.6 mm to 3mm, e.g., 0.8 mm, 1 mm, 1.5 mm, 2 mm or any ranges therebetween.

In some embodiments, said nozzle is configured to have a flow rate of from 10kg/hr to 1500kg/hr, preferably from 120kg/hr to 1000kg/hr, e.g., 50kg/hr, 150kg/hr, 250kg/hr, 400kg/hr, 600kg/hr, 800kg/hr or any ranges therebetween.

In some embodiments, said nozzle is configured to have a pressure of from 0.05MPa to 0.5MPa, preferably from 0.1MPa to 0.4MPa, e.g., 0.1MPa, 0.2MPa, 0.3MPa, 0.4MPa or any ranges therebetween.

In some embodiments, said nozzle is a hydraulic spray nozzle (e.g., Full Cone Nozzles, Flat Spray Nozzles, Hollow Cone Nozzles, Fine Spray Nozzles) or an air atomizing nozzle.

In some embodiments, said nozzle is configured to be positioned within a middle zone of said rotating drum. As used herein, the term of “middle zone” of a rotating drum refers to a section of said rotating drum which is located around midpoint along the length of said rotating drum, preferably wherein said section covers around 50%, preferably around 40%, more preferably around 30%of the total length of said rotating drum.

In some embodiments, said rotating drum comprises a flat panel and an air outlet in which said flat panel and said air outlet are located inside said rotating drum and above said plurality of detergent particles, and wherein said flat panel is positioned between said nozzle and said air outlet.

Preferably, said flat panel is positioned in a direction which is substantially perpendicular to the rotating axis of said rotating drum, and/or wherein said flat panel has a shape of square, circle, oval, triangle and any combinations thereof, and/or wherein said flat panel comprises a surface having an area which is at least 20%of the cross-sectional area of said rotating drum. Particularly, said air outlet is configured for discharging air containing fine particles (e.g. fine particles having a particle size of less than 100 μm) to ensure a safe environment for operators and said flat panel is configured for at least partially preventing the sprayed liquid composition from discharging through said air outlet. The cross-sectional area of said rotating drum refers to the area of a cross-sectional plane along the rotating axis of said rotating drum. In some embodiments, said rotating drum comprises two flat panels and two air outlets.

In some embodiments, said liquid composition is sprayed in the form of a spray of droplets having a median droplet size of from 10 μm to 500 μm, preferably from 20 μm to 300 μm, more preferably from 25 μm to 200 μm, most preferably from 30 μm to 150 μm, e.g. 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 70 μm, 100 μm, 120 μm and any ranges therebetween.

In some embodiments, said benefit agent is selected from a group consisting of a polymer, perfumes, insect repellants, silicones, waxes, lubricants, vitamins, fabric softening agents, anti-bacterial agents, skin health agents and mixtures thereof.

Suitable polymers include, but are not limited to: polymeric carboxylate; polyester soil release agent; cellulosic polymer; a dye transfer inhibitor (DTI) polymer and mixtures thereof. Such DTI polymer may be selected from a group consisting of polyvinyl pyrrolidone (PVP) , poly (vinylpyridine-N-oxide) (PVNO) , polyvinylpyrrolidone-co-polyvinylimidazole (PVP/PVI) , poly (vinylpyrrolidone) co-poly (vinylpyridine-N-oxide) (PVP/PVNO) polymers, polyvinylpyrrolidone-polyalkyleneoxide-vinylester copolymer (e.g. PVP/PVAc-g-PEG) , and any combinations thereof.

In some embodiments, said liquid composition further comprises a liquid protective agent and said liquid composition is formed by mixing said liquid protective agent and said benefit agent in a mixer, preferably a static mixer. Preferably, wherein the liquid protective agent is selected from the group consisting of a non-ionic surfactant, an alkyl ester fatty acid sulphonate surfactant, a non-ionic polymer, α‐aryl esters and any combinations thereof. More preferably, the liquid protective agent is selected from the group consisting of alkyl alkoxylated alcohols, a methyl ester fatty acid sulphonate, polyethylene glycols, phenyl salicylate, and any combinations thereof. Most preferably, the liquid protective agent is selected from the group consisting of alkyl alkoxylated alcohols and/or a methyl ester fatty acid sulphonate.

In some embodiments, said plurality of detergent particles have a mean particle size of from about 200 to about 600 microns, preferably from about 300 to about 500 microns.

In some embodiments, said liquid composition has a viscosity of from about 0.1 cps to about 25,000 cps, preferably from about 0.3 cps to about 5,000 cps, more preferably from about 0.5 cps to about 1,000 cps, most preferably from about 0.7 cps to about 500 cps, e.g., 0.9 cps, 1 cps, 5 cps, 10 cps, 50 cps, 100 cps, 200 cps, 400 cps, or any ranges therebetween, as measured at about 20℃ and 1 s^-1.

In some embodiments, said rotating drum has a diameter of from about 0.3 m to about 5 m, preferably from about 0.5 m to about 3 m, preferably from about 0.8 m to about 2 m; and/or a length of from about 1 m to about 10 m, preferably from about 2 m to about 8 m, more preferably from about 2.5 m to about 6 m.

Particularly, the plurality of detergent particles are spray-dried, extruded or agglomerate particles.

Particularly, said plurality of detergent particles comprise a detersive surfactant preferably selected from the group consisting of alkyl benzene sulfonate, alkoxylated alkyl sulfate, alkyl sulfate, alkoxylated alcohol, and mixtures thereof.

In some embodiments, the process further comprises: c) mixing said granular detergent composition with at least one additional detergent ingredient preferably selected from the group consisting of polymeric carboxylate, chelant, starch, sodium carbonate, sodium chloride, sodium sulphate, citric acid, cellulosic polymer, suds suppressor, fluorescent whitening agent, hueing agent, flocculating agent, polyester soil release agent, and mixtures thereof.

In another aspect, the present invention relates to a process of making a granular detergent composition comprising the steps of: a) providing a plurality of detergent particles in a rotating drum comprising a nozzle located inside said rotating drum as well as a liquid composition comprising a benefit agent; and b) spraying said liquid composition through said nozzle onto at least a portion of said plurality of detergent particles so as to provide said granular detergent composition, wherein said liquid composition is sprayed in the form of a spray of droplets having a median droplet size of from 0.6 mm to 5 mm.. In particular embodiments, the median droplet size is preferably from 0.8 mm to 5 mm, more preferably from 0.9 mm to 4 mm, most preferably from 1 mm to 3 mm.

Typically, the spray drying process includes spraying an aqueous slurry comprising detergent ingredients into a spray-drying tower through which hot air flows. As it falls through the tower, the aqueous slurry forms droplets, the hot air causes water to evaporate from the droplets, and a plurality of spray-dried granules is formed. Preferably, the spray-drying tower is a counter-current spray-drying tower, although a co-current spray-drying tower may also be suitable. The resulting granules may form the finished granular detergent composition. Alternatively, the resulting granules may be further processed (such as via agglomeration) and/or further components (such as detergent adjuncts) may be added thereto.

Typically, the spray-dried powder is subjected to cooling, for example an air lift. Typically, the spray-drying powder is subjected to particle size classification, for example a sieve, to obtain the desired particle size distribution. Preferably, the spray-dried powder has a particle size distribution such that weight average particle size is in the range of from 300 micrometers to 500 micrometers, and less than 10wt%of the spray-dried particles have a particle size greater than 2360 micrometers.

It may be preferred to heat the aqueous slurry mixture to elevated temperatures prior to atomization into the spray-drying tower, such as described in WO2009/158162.

It may be preferred for anionic surfactant, such as linear alkyl benzene sulphonate, to be introduced into the spray-drying process after the step of forming the aqueous slurry mixture: for example, introducing an acid precursor to the aqueous slurry mixture after the pump, such as described in WO 09/158449.

It may be preferred for a gas, such as air, to be introduced into the spray-drying process after the step of forming the aqueous slurry, such as described in WO2013/181205.

It may be preferred for any inorganic ingredients, such as sodium sulphate and sodium carbonate, if present in the aqueous slurry mixture, to be micronized to a small particle size such as described in WO2012/134969.

Typically, a suitable agglomeration process comprises the step of contacting a detersive ingredient, such as a detersive surfactant, e.g. linear alkyl benzene sulphonate (LAS) and/or alkyl alkoxylated sulphate, with an inorganic material, such as sodium carbonate and/or silica, in a mixer. The agglomeration process may also be an in-situ neutralization agglomeration process wherein an acid precursor of a detersive surfactant, such as LAS, is contacted with an alkaline material, such as carbonate and/or sodium hydroxide, in a mixer, and wherein the acid precursor of a detersive surfactant is neutralized by the alkaline material to form a detersive surfactant during the agglomeration process.

Other suitable detergent ingredients that may be agglomerated include polymers, chelants, bleach activators, silicones and any combination thereof.

The agglomeration process may be a high, medium or low shear agglomeration process, wherein a high shear, medium shear or low shear mixer is used accordingly. The agglomeration process may be a multi-step agglomeration process wherein two or more mixers are used, such as a high shear mixer in combination with a medium or low shear mixer. The agglomeration process can be a continuous process or a batch process.

It may be preferred for the agglomerates to be subjected to a drying step, for example to a fluid bed drying step. It may also be preferred for the agglomerates to be subjected to a cooling step, for example a fluid bed cooling step.

Typically, the agglomerates are subjected to particle size classification, for example a fluid bed elutriation and/or a sieve, to obtain the desired particle size distribution. Preferably, the agglomerates have a particle size distribution such that weight average particle size is in the range of from 300 micrometers to 800 micrometers, and less than 10wt%of the agglomerates have a particle size less than 150 micrometers and less than 10wt%of the agglomerates have a particle size greater than 1200 micrometers.

It may be preferred for fines and over-sized agglomerates to be recycled back into the agglomeration process. Typically, over-sized particles are subjected to a size reduction step, such as grinding, and recycled back into an appropriate place in the agglomeration process, such as the mixer. Typically, fines are recycled back into an appropriate place in the agglomeration process, such as the mixer.

In some embodiments, the liquid protective agent is an alkyl alkoxylated alcohol having an average degree of alkoxylation of from 1 to 50, preferably a linear or branched, substituted or unsubstituted C_8-18 alkyl ethoxylated alcohol having an average degree of ethoxylation of from 1 to 12, more preferably from 5 to 10.

In some embodiments, the weight ratio of the liquid protective agent to the benefit agent in the liquid composition is from 0.05 to 50, preferably from 0.1 to 20, more preferably from 0.2 to 10.

Detersive Surfactant

Any suitable detersive surfactant is of use in the granular detergent composition.

Suitable detersive surfactants include, but are not limited to: anionic surfactants, non-ionic surfactants, cationic surfactants, zwitterionic surfactants, amphoteric surfactants and any mixtures thereof. Preferred surfactants include anionic surfactants, cationic surfactants, non-ionic surfactants and any mixtures thereof.

Suitable anionic surfactants can include alkyl benzene sulphonate. Preferably the anionic detersive surfactant comprises at least 50 wt%, at least 55 wt%, at least 60 wt%, at least 65 wt%, at least 70 wt%, at least 75 wt%, at least 80 wt%, at least 85 wt%, at least 90 wt%, or even at least 95 wt%, by weight of the anionic detersive surfactant, of alkyl benzene sulphonate. The alkyl benzene sulphonate is preferably a linear or branched, substituted or unsubstituted, C_8-18 alkyl benzene sulphonate. This is the optimal level of the C_8-18 alkyl benzene sulphonate to provide a good cleaning performance. The C_8-18 alkyl benzene sulphonate can be a modified alkylbenzene sulphonate (MLAS) as described in more detail in WO 99/05243, WO 99/05242, WO 99/05244, WO 99/05082, WO 99/05084, WO 99/05241, WO 99/07656, WO 00/23549, and WO 00/23548. Highly preferred C_8-18 alkyl benzene sulphonates are linear C_10-13 alkylbenzene sulphonates. Especially preferred are linear C_10-13 alkylbenzene sulphonates that are obtainable by sulphonating commercially available linear alkyl benzenes (LAB) ; suitable LAB include low 2-phenyl LAB, such as those supplied by Sasol under the trade nameor those supplied by Petresa under the trade nameOther suitable LAB include high 2-phenyl LAB, such as those supplied by Sasol under the trade name

The anionic detersive surfactant may preferably comprise other anionic detersive surfactants. A suitable anionic detersive surfactant is a non-alkoxylated anionic detersive surfactant. The non-alkoxylated anionic detersive surfactant can be an alkyl sulphate, an alkyl phosphate, an alkyl phosphonate, an alkyl carboxylate or any mixture thereof. The non-alkoxylated anionic surfactant can be selected from the group consisting of; C₁₀-C₂₀ primary, branched-chain, linear-chain and random-chain alkyl sulphates (AS) , typically having the following formula (I) :
CH₃ (CH₂) _xCH₂-OSO₃ ^-M⁺

wherein, M is hydrogen or a cation which provides charge neutrality, preferred cations are sodium and ammonium cations, wherein x is an integer of at least 7, preferably at least 9; C₁₀-C₁₈ secondary (2,3) alkyl sulphates, typically having the following formulae:

wherein, M is hydrogen or a cation which provides charge neutrality, preferred cations include sodium and ammonium cations, wherein x is an integer of at least 7, preferably at least 9, y is an integer of at least 8, preferably at least 9; C₁₀-C₁₈ alkyl carboxylates; mid-chain branched alkyl sulphates as described in more detail in US 6,020,303 and US 6,060,443; methyl ester sulphonate (MES) ; alpha-olefin sulphonate (AOS) ; and mixtures thereof.

Another preferred anionic detersive surfactant is an alkoxylated anionic detersive surfactant. The presence of an alkoxylated anionic detersive surfactant in the spray-dried powder provides good greasy soil cleaning performance, gives a good sudsing profile, and improves the hardness tolerance of the anionic detersive surfactant system. It may be preferred for the anionic detersive surfactant to comprise from 1%to 50%, or from 5%, or from 10%, or from 15%, or from 20%, and to 45%, or to 40%, or to 35%, or to 30%, by weight of the anionic detersive surfactant system, of an alkoxylated anionic detersive surfactant.

Preferably, the alkoxylated anionic detersive surfactant is a linear or branched, substituted or unsubstituted C_12-18 alkyl alkoxylated sulphate having an average degree of alkoxylation of from 0.5 to 30, preferably from 0.5 to 10, more preferably from 0.5 to 3. Preferably, the alkoxylated anionic detersive surfactant is a linear or branched, substituted or unsubstituted C_12-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 10, more preferably from 0.5 to 3. Most preferably, the alkoxylated anionic detersive surfactant is a linear unsubstituted C_12-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 7, more preferably from 0.5 to 3.

The alkoxylated anionic detersive surfactant, when present with an alkyl benzene sulphonate may also increase the activity of the alkyl benzene sulphonate by making the alkyl benzene sulphonate less likely to precipitate out of solution in the presence of free calcium cations. Preferably, the weight ratio of the alkyl benzene sulphonate to the alkoxylated anionic detersive surfactant is in the range of from 1: 1 to less than 5: 1, or to less than 3: 1, or to less than 1.7: 1, or even less than 1.5: 1. This ratio gives optimal whiteness maintenance performance combined with a good hardness tolerance profile and a good sudsing profile. However, it may be preferred that the weight ratio of the alkyl benzene sulphonate to the alkoxylated anionic detersive surfactant is greater than 5:1, or greater than 6: 1, or greater than 7: 1, or even greater than 10: 1. This ratio gives optimal greasy soil cleaning performance combined with a good hardness tolerance profile, and a good sudsing profile.

Additional Detergent Ingredients

The additional detergent ingredient may include a builder. Any suitable builder may be of use in the granular detergent composition. Suitable builders include, but are not limited to those selected from the group of: zeolite builder; phosphate builder; and mixtures thereof. Non-limiting examples of useful zeolite builders include: zeolite A; zeolite X; zeolite P; zeolite MAP; and combinations thereof. Sodium tripolyphosphate is a non-limiting example of a useful phosphate builder. The zeolite builder (s) may be present at from about 1 to about 20 %by weight of the detergent composition. It may also be especially preferred for the granular detergent composition to comprise low levels, or even be essentially free, of builder. By essentially free of it is typically meant herein to mean: “comprises no deliberately added” . In a preferred embodiment, the granular detergent composition is essentially free of zeolite, preferably has no zeolite. In a preferred embodiment, the granular detergent composition is essentially free of phosphate, preferably has no phosphate.

The additional detergent ingredient may include a polymer. Any suitable polymer may be of use in the granular detergent composition. Suitable polymers include, but are not limited to: polymeric carboxylate; polyester soil release agent; cellulosic polymer; and mixtures thereof. One preferred polymeric material is a polymeric carboxylate, such as a co-polymer of maleic acid and acrylic acid. However, other polymers may also be suitable, such as polyamines (including the ethoxylated variants thereof) , polyethylene glycol and polyesters. Polymeric soil suspending aids and polymeric soil release agents are also particularly suitable.

Another suitable polymer is cellulosic polymer, such as cellulosic polymer selected from the group of: alkyl alkoxy cellulose, preferably methyl hydroxyethyl cellulose (MHEC) ; alkyl cellulose, preferably methyl cellulose (MC) ; carboxy alkyl cellulose, preferably carboxymethylcellulose (CMC) ; and mixtures thereof.

Polymers may be present at from about 0.5 to about 20%or from about 1 to about 10%by weight of the detergent composition.

Other suitable detergent ingredients may be selected from the group of: chelants such as ethylene diamine disuccinic acid (EDDS) ; hydroxyethylene diphosphonic acid (HEDP) ; starch; sodium sulphate; carboxylic acids such as citric acid or salts thereof such as citrate; suds suppressor; fluorescent whitening agent; hueing agent; flocculating agent such as polyethylene oxide; and mixtures thereof. If the present detergent comprises masking agents and/or whiteners (e.g. Titanium dioxide) , they may be present at less than about 1 wt%or less.

In some embodiments, the additional detergent ingredient may be preferably selected from the group consisting of polymeric carboxylate, chelant, starch, sodium carbonate, sodium chloride, sodium sulphate, citric acid, cellulosic polymer, suds suppressor, fluorescent whitening agent, hueing agent, flocculating agent, polyester soil release agent, and mixtures thereof.

Liquid protective agent

Without wishing to be bound by theory, it is believed that the liquid protective agent may play a protective role for the benefit agent to prevent evaporation during the making (i.e. inside the rotating drum) and/or the storage. Preferably, the liquid protective agent is selected from a non-ionic surfactant, an alkyl ester fatty acid sulphonate surfactant, a non-ionic polymer, α‐aryl esters and any combinations thereof. More preferably, the liquid protective agent is selected from alkyl alkoxylated alcohols, polyethylene glycols, a methyl ester fatty acid sulphonate surfactant, phenyl salicylate, and any combinations thereof.

The non-ionic surfactant for use in the liquid composition could be an alkyl polyglucoside and/or an alkyl alkoxylated alcohol. Preferably the non-ionic surfactant is a linear or branched, substituted or unsubstituted C_8-18 alkyl ethoxylated alcohol having an average degree of ethoxylation of from 1 to 10.

Suitable non-ionic surfactants include alkyl polyglucoside and/or an alkyl alkoxylated alcohol. Preferred non-ionic alkyl alkoxylated alcohols include C_8-18 alkyl alkoxylated alcohol, preferably a C_8-18 alkyl ethoxylated alcohol, preferably the alkyl alkoxylated alcohol has an average degree of alkoxylation of from 1 to 50, preferably from 1 to 30, or from 1 to 20, or from 1 to 10, preferably the alkyl alkoxylated alcohol is a C_8-18 alkyl ethoxylated alcohol having an average degree of ethoxylation of from 1 to 20, preferably from 5 to 10. The alkyl alkoxylated alcohol can be linear or branched, and substituted or un-substituted. Suitable non-ionic surfactants can be selected from the group consisting of: C₈-C₁₈ alkyl ethoxylates, such as, non-ionic surfactants from Shell; C₆-C₁₂ alkyl phenol alkoxylates wherein preferably the alkoxylate units are ethyleneoxy units, propyleneoxy units or a mixture thereof; C₁₂-C₁₈ alcohol and C₆-C₁₂ alkyl phenol condensates with ethylene oxide/propylene oxide block polymers such as from BASF; C₁₄-C₂₂ mid-chain branched alcohols; C₁₄-C₂₂ mid-chain branched alkyl alkoxylates, preferably having an average degree of alkoxylation of from 1 to 30; alkylpolysaccharides, preferably alkylpolyglycosides; polyhydroxy fatty acid amides; ether capped poly (oxyalkylated) alcohol surfactants; and mixtures thereof.

Suitable non-ionic surfactants for use in the premix can be selected from the group of: C₈-C₁₈ alkyl ethoxylates, such as, non-ionic surfactants from Shell; C₆-C₁₂ alkyl phenol alkoxylates wherein the alkoxylate units are ethyleneoxy units, propyleneoxy units or a mixture thereof; C₁₂-C₁₈ alcohol and C₆-C₁₂ alkyl phenol condensates with ethylene oxide/propylene oxide block polymers such asfrom BASF; C₁₄-C₂₂ mid-chain branched alcohols, BA, as described in more detail in US 6, 150, 322; C₁₄-C₂₂ mid-chain branched alkyl alkoxylates, BAEx, wherein x = from 1 to 30, as described in more detail in US 6, 153, 577, US 6, 020, 303 and US 6,093, 856; alkylpolysaccharides as described in more detail in US 4, 565, 647, specifically alkylpolyglycosides as described in more detail in US 4, 483, 780 and US 4, 483, 779; polyhydroxy fatty acid amides as described in more detail in US 5,332,528, WO 92/06162, WO 93/19146, WO 93/19038, and WO 94/09099; ether capped poly (oxyalkylated) alcohol surfactants as described in more detail in US 6,482,994 and WO 01/42408; and mixtures thereof.

Suitable non-ionic polymers for use in the premix can be selected from the group consisting of polyethylene glycols, polypropylene glycols, and other polymers.

Suitable α‐aryl esters for use in the premix can be selected from the group consisting of benzoates, salicylates, and any combinations thereof, for example benzyl benzoate, phenyl salicylate.

The Granular Detergent Composition

The granular detergent composition is suitable for any laundry detergent application, for example: laundry, including automatic washing machine laundering and hand laundering, and even bleach and laundry additives.

The granular detergent composition can be a fully formulated detergent product, such as a fully formulated laundry detergent product, or it can be combined with other particles to form a fully formulated detergent product, such as a fully formulated laundry detergent product. The granular detergent composition may be combined with other particles such as: enzyme particles; perfume particles including agglomerates or extrudates of perfume microcapsules, and perfume encapsulates such as starch encapsulated perfume accord particles; surfactant particles, such as non-ionic detersive surfactant particles including agglomerates or extrudates, anionic detersive surfactant particles including agglomerates and extrudates, and cationic detersive surfactant particles including agglomerates and extrudates; polymer particles including soil release polymer particles, cellulosic polymer particles; buffer particles including carbonate salt and/or silicate salt particles, preferably a particle comprising carbonate salt and silicate salt such as a sodium carbonate and sodium silicate co-particle, and particles and sodium bicarbonate; other spray-dried particles; fluorescent whitening particles; aesthetic particles such as coloured noodles or needles or lamellae particles; bleaching particles such as percarbonate particles, especially coated percarbonate particles, including carbonate and/or sulphate coated percarbonate, silicate coated percarbonate, borosilicate coated percarbonate, sodium perborate coated percarbonate; bleach catalyst particles, such as transition metal catalyst bleach particles, and imine bleach boosting particles; performed peracid particles; hueing dye particles; and any mixture thereof.

The granular detergent composition according to the present invention may have a bulk density of from about 250 to about 550 grams per liter, or from about 400 to about 800 grams per liter. The granular detergent composition may have a mean particle granule size of from about 300 to about 550 microns, or from about 350 to about 450 microns.

Figure 1 illustrates an examlary system for making a granular detergent composition according to the present disclosure. Particularly, the system comprises a rotating drum 11 in which a plurality of detergent particles 13 (also called “powder bed” ) are mixing and a liquid composition containing perfume is sprayed onto the plurality of detergent particles 13 through a nozzle 12. The rotating drum 11 further comprises two air outlets 15 which are respectively located at two ends of the rotating drum 11 and two flat panels 14 which are respectively located between the nozzle 12 and one of the two air outlets 15. The nozzle 12 is configured to be positioned at a height of H_N from said plurality of detergent particles when spraying in which the H_N is from 12cm to 48cm.

Figure 2 illustrates an experimental equipment set up for determining perfume loss during the spray-on process. Particularly, a plastic box with no organic volatilization is used as an experimental sealing space in which a spray equipment (e.g. a spray gun or a synring) is arranged in the middle of the top and a lifting platform is arranged to control the distance between the spray equipment (e.g. from 5 cm to 100 cm) and the powder bed which is located on the lifting platform. Further, a VOC detector is arranged near the bottom of the plastic box (particularly, an extension tube extended from the VOC detector is located at 10 cm away from the bottom of the plastic box and 8 cm into the plastic box.

EXAMPLES

Example 1. Reduced loss of perfume when a liquid composition containing perfume and a protective agent

In order to explore the factors (including droplets size of spray, the position of nozzels, the formulation of spray, and the like) which may have an impact on the perfume loss, the inventors of the present invention have developed an experimental equipment set up as shown in Fig. 2. A spray gun and a syringe are respectively used as the spray equipment in which the spray gun is configured to have a droplet size<100 μm and the syringe is configured to have a droplet size of around 2 mm. The spray pressure maintained at 0.2MPa for the spray gun.

A sample of powder product (Powder Product Sample 1; amount: 1kg; thickness: 2cm) as shown in Table 1 was placed on the lifting platform. The powder product was preheated to 40℃ to simulate plant conditions. Samples of liquid composition containing perfume (Liquid Composition Samples A and B; Perfume amount: 2g) as shown in Table 1 was preheated to 40℃ as well and then fed into the spray equipment for spraying. For Sample A, a premixture of 2 g of perfume and 8 g of C₁₂-C₁₆ alkyl ethoxylate (viscosity at about 20℃ and 1 s^-1: 21.69 cps) were sprayed. For Sample B, 2 g of perfume (viscosity at about 20℃ and 1 s^-1: 0.89 cps) alone were sprayed, while 8 g of C₁₂-C₁₆ alkyl ethoxylate (i.e., which is the same amount with that in Sample A) was separately sprayed before the spraying of perfume so as to ensure the composition of finish products are the same between Liquid Composition Samples A and B. The spray pattern remained the substantially the same between different tests. Then, Volatile Organic Compounds (VOC) was determined by VOC detector at the distance of 40 cm between the spray equipment and the powder bed. Accordingly to previous experiences, the VOC level gradually increases since the spraying starts, and become steady after 1500 seconds. As such, the reading of VOC detector at 1500 seconds after the spraying was recorded as the VOC level (ppm) .

Table 1. Composition of the powder product and liquid composition

Table 2 as below shows the results of perfume loss as indicated by VOC, ppm. The results proves the loss of perfume is significantly reduced when a liquid composition contains both perfume and a liquid protective agent (e.g. C₁₂-C₁₆ alkyl ethoxylate) compared to a liquid composition containing perfume only.

Table 2

Example 2. Reduced loss of perfume when the spray of droplets has a specific range of median droplet size

The inventors of the present invention tested the impact of droplets size sprayed by the nozzle on perfume loss by using the equipment and the method in Example 1 as well as Powder Product Sample 1 and Liquid Composition Sample A. Volatile Organic Compounds (VOC) was determined by VOC detector at the distances of 40 cm and 60 cm between the spray equipment and the powder bed. Surprisingly, as shown in Table 3, VOC level for the bigger droplets is significantly lower compared to the smaller droplets which indicates the loss of perfume is significantly reduced when a spray having a relatively big droplet size is used. As such, the total amount of perfume needed for the making of granular detergent products can be reduced, resulting in cost saving.

Table 3

Example 3. Reduced loss of perfume when the nozzle for spraying perfume is configured to be positioned at an appropriate location

Although the bigger droplet size is favorable, spray having a smaller droplet size is also needed for some reasons, e.g. more even distribution. As such, the inventors of the present invention further explored the impact of nozzle position on the perfume loss for smaller droplet size, and surprisingly found that when the nozzle for spraying perfume is configured to be positioned at an appropriate location, the loss of perfume is significantly reduced. Further, the inventors of the present invention found that, when the nozzle is configured to be positioned at a more preferred location, another benefit (i.e. to prevent a compromised caking performance) can be provided.

Similarly as in Example 1, VOC level was determined at different distances from spray equipment to powder bed (e.g. 5 cm to 60 cm) by using the equipment and the method in Example 1 as well as Powder Product Sample 1 and Liquid Composition Sample A. Then, in order to understand if the caking performance is compromised, the cake strength was determined by the following method and the apparatus as shown in Figure 3 (Caking Strength Measurement Apparatus, available from Sichuan Machineary Institute) :

Cake strength test method

(1) Place the cylinder centrally under the force gauge.

(2) Ensure that the cylinder and sleeve are clean, and that sleeve moves freely along the cylinder.

(3) Place the locking pin into the hole in the cylinder and rest the sleeve, with the lugs at the bottom, onto the pin.

(4) Fill the space at the top of the cylinder with a sample of the agglomerates /powder.

(5) With a straightedge, level the powder with the top of sleeve.

(6) Place the lid centralized on top with the lugs facing down.

(7) Fasten the upper and lower lugs together with elastic bands.

(8) Place the 5kg weight carefully on top of the lid. Place the weight carefully on the cake former so as to not cause uneven pressure.

(9) Gently remove the metal pin.

(10) After 5 minutes note the height (in mm) sunk. This is cake compression. After noting the cake compression carefully remove the weight and elastic bands.

(11) Very gently slide the sleeve down to the base.

(12) Set the force gauge to 0 and switch on.

(13) Switch the motor on to direct the gauge at the center of the lid.

(14) Note the force (in kg) needed to break the cake. This is the cake strength.

(15) Repeat at least three times for each material and average the forces, this average is the mean cake strength for the material tested.

Apparatus

(a) Cake former

(b) Force recorder

Table 4 as below and Figure 4 shows the results of perfume loss as indicated by VOC, ppm and caking performance as indicated by cake strength. The results proves the loss of perfume is significantly reduced when the nozzle for spraying perfume is configured to be positioned at an appropriate location (i.e. <50 cm) . Further, if the distance from the spray equipment to the powder bed is kept being more than 10 cm, another benefit can be obtained, i.e., to prevent a significant caking problem. Thus, the inventors succesufully identified an optimal range of distances (i.e., >10 cm and <50 cm) from the spray equipment to the powder bed for balancing the perfume loss and the caking strength.

Table 4

The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as “40 mm” is intended to mean “about 40 mm. ”

Every document cited herein, including any cross referenced or related patent or application and any patent application or patent to which this application claims priority or benefit thereof, is hereby incorporated herein by reference in its entirety unless expressly excluded or otherwise limited. The citation of any document is not an admission that it is prior art with respect to any invention disclosed or claimed herein or that it alone, or in any combination with any other reference or references, teaches, suggests or discloses any such invention. Further, to the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this document shall govern.

While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims

A process of making a granular composition comprising the steps of:

a) providing a plurality of particles in a rotating drum comprising a nozzle located inside said rotating drum as well as a liquid composition comprising a benefit agent; and

b) spraying said liquid composition through said nozzle onto at least a portion of said plurality of particles so as to provide said granular composition, wherein said nozzle is configured to be positioned at a height of H_N from said plurality of particles when spraying,

wherein H_N is from 12cm to 48cm.
The process according to claim 1, wherein H_N is from 15cm to 45cm, preferably from 17cm to 43cm, more preferably from 19cm to 41cm, and most preferably from 20cm to 40cm.
The process according to claim 1 or 2, wherein said liquid composition is sprayed in the form of a spray of droplets having a median droplet size of from 10 μm to 1000 μm, preferably from 20 μm to 800 μm, more preferably from 25 μm to 600 μm, most preferably from 30 μm to 500 μm.
The process according to any one of preceding claims, wherein said rotating drum comprises a flat panel and an air outlet in which said flat panel and said air outlet are located inside said rotating drum and above said plurality of particles, and wherein said flat panel is positioned between said nozzle and said air outlet,

preferably, wherein said flat panel is positioned in a direction which is substantially perpendicular to the rotating axis of said rotating drum, and/or wherein said flat panel has a shape of square, circle, oval, triangle and any combinations thereof, and/or wherein said flat panel comprises a surface having an area which is at least 20%of the cross-sectional area of said rotating drum.
The process according to any one of preceding claims, wherein said benefit agent is selected from a group consisting of a polymer, perfumes, insect repellants, silicones, waxes, lubricants, vitamins, fabric softening agents, anti-bacterial agents, skin health agents and mixtures thereof.
The process according to any one of preceding claims, wherein said liquid composition further comprises a liquid protective agent and said liquid composition is formed by mixing said liquid protective agent and said benefit agent in a mixer, preferably a static mixer,

preferably, wherein the liquid protective agent is selected from the group consisting of a non-ionic surfactant, an alkyl ester fatty acid sulphonate surfactant, a non-ionic polymer, α‐aryl esters and any combinations thereof,

more preferably, the liquid protective agent is selected from the group consisting of alkyl alkoxylated alcohols, a methyl ester fatty acid sulphonate, polyethylene glycols, phenyl salicylate, and any combinations thereof, and

most preferably, the liquid protective agent is selected from the group consisting of alkyl alkoxylated alcohols and/or a methyl ester fatty acid sulphonate.
The process according to any one of preceding claims, wherein said plurality of particles are spray-dried, extruded or agglomerate particles.
The process according to any one of preceding claims, wherein said plurality of particles comprise a detersive surfactant preferably selected from the group consisting of alkyl benzene sulfonate, alkoxylated alkyl sulfate, alkyl sulfate, alkoxylated alcohol, and mixtures thereof.
The process according to any one of preceding claims, wherein said plurality of particles have a mean particle size of from about 200 to about 600 microns, preferably from about 300 to about 500 microns.
The process according to any one of preceding claims, wherein said liquid composition has a viscosity of from about 0.1 cps to about 25,000 cps, preferably from about 0.3 cps to about 5,000 cps, more preferably from about 0.5 cps to about 1,000 cps, most preferably from about 0.7 cps to about 500 cps, as measured at about 20℃ and 1 s^-1.
The process according to any one of preceding claims, wherein said rotating drum has a diameter of from about 0.3 m to about 5 m, preferably from about 0.5 m to about 3 m, preferably from about 0.8 m to about 2 m; and/or a length of from about 1 m to about 10 m, preferably from about 2 m to about 8 m, more preferably from about 2.5 m to about 6 m.
The process according to any one of preceding claims, wherein the process further comprises:

c) mixing said granular composition with at least one additional ingredient preferably selected from the group consisting of polymeric carboxylate, chelant, starch, sodium carbonate, sodium chloride, sodium sulphate, citric acid, cellulosic polymer, suds suppressor, fluorescent whitening agent, hueing agent, flocculating agent, polyester soil release agent, enzyme and mixtures thereof.
A process of making a granular composition comprising the steps of:

a) providing a plurality of particles in a rotating drum comprising a nozzle located inside said rotating drum as well as a liquid composition comprising a benefit agent; and

b) spraying said liquid composition through said nozzle onto at least a portion of said plurality of particles so as to provide said granular composition,

wherein said liquid composition is sprayed in the form of a spray of droplets having a median droplet size of from 0.6 mm to 5 mm.
The process according to claim 13, wherein the median droplet size is, preferably from 0.8 mm to 5 mm, more preferably from 0.9 mm to 4 mm, most preferably from 1 mm to 3 mm.
The process according to claim 13 or 14, wherein said nozzle is configured to be positioned at a height of H_N from said plurality of particles when spraying, and

wherein H_N is from 12cm to 48cm, preferably from 15cm to 45cm, more preferably from 17cm to 43cm, yet more preferably from 19cm to 41cm, and most preferably from 20cm to 40cm.
The process according to any one of claims 13 to 15, wherein said liquid composition further comprises a liquid protective agent, and wherein said liquid composition is formed by mixing said liquid protective agent and said benefit agent in a mixer, preferably a static mixer,

preferably, wherein the liquid protective agent is selected from the group consisting of a non-ionic surfactant, a non-ionic polymer, α‐aryl esters and any combinations thereof,

more preferably, the liquid protective agent is selected from the group consisting of alkyl alkoxylated alcohols, polyethylene glycols, benzyl benzoate, phenyl salicylate, and any combinations thereof, and

most preferably, the liquid protective agent is selected from the group consisting of alkyl alkoxylated alcohols.
The process according to any one of claims 13 to 16, wherein said plurality of particles are spray-dried, extruded or agglomerate particles.
The process according to any one of claims 13 to 17, wherein said plurality of particles comprise a detersive surfactant preferably selected from the group consisting of alkyl benzene sulfonate, alkoxylated alkyl sulfate, alkyl sulfate, alkoxylated alcohol, and mixtures thereof.
The process according to any one of claims 13 to 18, wherein the process further comprises:

c) mixing said granular composition with at least one additional ingredient preferably selected from the group consisting of polymeric carboxylate, chelant, starch, sodium carbonate, sodium chloride, sodium sulphate, citric acid, cellulosic polymer, suds suppressor, fluorescent whitening agent, hueing agent, flocculating agent, polyester soil release agent, enzyme and mixtures thereof.
A system for making a granular composition, wherein said system comprises:

i. a rotating drum comprising a nozzle, a flat panel and an air outlet which are located inside said rotating drum and above said plurality of particles, and wherein said flat panel is positioned between said nozzle and said air outlet,

wherein said nozzle is configured to be positioned at a height of H_N from said plurality of particles when spraying which is from 12cm to 48cm,

wherein the rotating drum has a diameter of D_R which is from 10 cm to 500 cm,

ii. a static mixer which is in fluid communication with said nozzle, and

iii. a first reservoir for containing a benefit agent and a second reservoir for containing a liquid protective agent, in which said first and second reservoirs are both in fluid communication with said static mixer.