Process for preparing particulate composition comprising benefit agent

Abstract

A method of preparing a particulate composition is provided.

Description

Technical Field

[0001] This invention relates to a method for preparing a particulate composition containing a beneficial agent. Background Technology

[0002] Granular laundry detergent compositions are well known. Granular laundry detergent compositions contain one or more surfactants that provide good fabric cleaning performance. Generally, granular laundry detergent compositions can be prepared using various methods, including spray drying and agglomeration. Spray drying is the standard method for manufacturing basic powders of laundry detergents. Typically, the detergent ingredients are mixed together in a mixer such as a spiral mixer to form an aqueous detergent slurry. This slurry is then transferred along pipes through a first low-pressure pump and then through a second high-pressure pump to nozzles, where it is sprayed into a spray drying tower and spray-dried to form a spray-dried powder. Typically, suitable agglomeration methods involve contacting detergency ingredients, such as detergency surfactants, like linear alkylbenzene sulfonates (LAS) and / or alkylalkoxylated sulfates, with inorganic materials, such as sodium carbonate and / or silica, in a mixer.

[0003] Preferably, in addition to surfactants, beneficial agents (such as fragrances) are often added to laundry detergents to please consumers. For granular detergent products, beneficial agents are typically added by spraying them onto base detergent particles (such as spray-dried base detergent particles and / or agglomerated base detergent particles). This spraying step is usually carried out in a tumbling drum mixer.

[0004] However, the inventors of this invention have noted that the loss of atomized beneficial agents (e.g., fragrances) during the manufacture of granular detergent products is significant due to various reasons (e.g., evaporation and discharge from dust removal devices). Currently, one solution is to increase the content of beneficial agents to ensure the superiority of the final product for consumers, which obviously leads to higher costs.

[0005] Therefore, there is a need in the art for a new method to reduce the loss of beneficial agents during the manufacturing of particulate detergent products.

[0006] The inventors of this invention have surprisingly discovered that when the nozzle used for spraying beneficial agents is configured to be positioned appropriately, the loss of beneficial agents is significantly reduced. Therefore, the total amount of beneficial agents required to prepare granular detergent products can be reduced, thereby saving costs.

[0007] Furthermore, the inventors of this invention have surprisingly discovered that when the droplet spray has a median droplet size within a specific range, the loss of beneficial agents is also significantly reduced. Summary of the Invention

[0008] The present invention satisfies the aforementioned needs by providing the following method for preparing particulate compositions.

[0009] In one aspect, the present invention relates to a method for preparing a particulate composition, the method comprising the steps of: a) providing a plurality of particles and a liquid composition comprising a beneficial agent in a rotating drum, the rotating drum including a nozzle located inside the rotating drum; and b) spraying the liquid composition through the nozzle onto at least a portion of the plurality of particles to provide the particulate composition, wherein the nozzle is configured to be positioned at a height H above the plurality of particles during spraying. N At, where H N The size ranges from 12cm to 48cm. Specifically, the granular composition is a granular detergent composition, preferably a granular laundry detergent composition.

[0010] On the other hand, the present invention relates to a method for preparing a particulate composition, the method comprising the steps of: a) providing a plurality of particles and a liquid composition comprising a beneficial agent in a rotating drum, the rotating drum including a nozzle located inside the rotating drum; and b) spraying the liquid composition through the nozzle onto at least a portion of the plurality of particles to provide the particulate composition, wherein the liquid composition is sprayed in the form of droplet spray having a median droplet size of 10 μm to 1000 μm. In a specific embodiment, the median droplet size is preferably 10 μm to 1000 μm, preferably 20 μm to 800 μm, more preferably 25 μm to 600 μm, and most preferably 30 μm to 500 μm, for example 50 μm, 70 μm, 90 μm, 100 μm, 120 μm, 150 μm, 200 μm, 300 μm, 400 μm, or any range therebetween.

[0011] On the other hand, the present invention relates to a system for preparing a particulate composition, wherein the system comprises: i) a rotating drum including a nozzle, a plate, and an outlet, the nozzle, plate, and outlet being positioned inside the rotating drum and above the plurality of particles, wherein the plate is positioned between the nozzle and the outlet, wherein the nozzle is configured to be positioned at a height H above the plurality of particles during spraying. N At this location, the height ranges from 12cm to 48cm, with the drum having a diameter D. R The nozzle has a diameter of 50 cm to 500 cm, ii) a static stirrer in fluid communication with the nozzle, and iii) a first reservoir for containing a beneficial agent and a second reservoir for containing a liquid preservative, wherein both the first reservoir and the second reservoir are in fluid communication with the static stirrer.

[0012] One advantage of this method is that it reduces the loss of beneficial agents during the manufacture of granular products without causing significant clumping problems.

[0013] Another advantage of this method is that it reduces the amount of beneficial agents required in granular products.

[0014] Another advantage of this method is that it saves on the cost of manufacturing granular products.

[0015] These and other features, aspects, and advantages of particular embodiments will become apparent to those skilled in the art upon reading this disclosure. Attached Figure Description

[0016] The embodiments shown in the figures are illustrative and are not intended to limit the invention as defined by the claims. A detailed description of the following illustrative embodiments will be understood when read in conjunction with the following figures, in which:

[0017] Figure 1 An exemplary system for preparing granular detergent compositions is shown.

[0018] Figure 2 An experimental setup for determining the loss of beneficial agents (e.g., fragrances) during a spraying process is shown.

[0019] Figure 3 An apparatus for testing agglomeration strength is shown.

[0020] Figure 4 The results of Example 1 are shown, which demonstrate that when the nozzle used for spraying beneficial agents is configured to be positioned in the proper place, the loss of beneficial agents is significantly reduced without causing significant clumping problems. Detailed Implementation

[0021] Unless otherwise stated, all percentages, parts and ratios are based on the total weight of the compositions of the present invention and all measurements were performed at 25°C. All such weights of the listed ingredients are based on the content of active substances and therefore, unless otherwise specified, do not include carriers or byproducts that may be included in commercially available raw materials.

[0022] As used herein, when used in claims, the articles “a” and “an” are understood to refer to one or more protected or described in the claims.

[0023] As used herein, the term "laundry detergent" refers to a liquid or solid composition and, unless otherwise specified, includes multipurpose or "heavy-duty" detergents in granular or powder form, particularly cleaning detergents and cleaning aids such as bleaching additives or pretreatment types. In one embodiment, the laundry detergent is a solid laundry detergent composition, and preferably a free-flowing granular laundry detergent composition (i.e., a granular detergent product).

[0024] As used herein, the term "liquid composition" means a composition that is free-flowing but has a constant volume, encompassing aqueous solutions, non-aqueous solutions, suspensions, slurries, pastes, etc.

[0025] As used herein, the term "height" of the nozzle from multiple detergent particles (i.e., H) N This refers to the minimum distance between the nozzle and multiple detergent particles. Typically, such as... Figure 1 As shown, multiple detergent particles are arranged like a bed in a rotary drum agitator, hence the term "powder bed".

[0026] As used in this article, the term "spray angle" refers to the angle of the spray shape, particularly the opening angle formed by a droplet nozzle jet as it leaves the nozzle orifice.

[0027] Preparation method

[0028] In one aspect, the present invention relates to a method for preparing a particulate detergent composition, the method comprising the steps of: a) providing a plurality of detergent particles and a liquid composition comprising a beneficial agent in a rotating drum, the rotating drum including a nozzle located inside the rotating drum; and b) spraying the liquid composition through the nozzle onto at least a portion of the plurality of detergent particles to provide the particulate detergent composition, wherein the nozzle is configured to be positioned at a height H above the plurality of detergent particles during spraying. N At, where H N It ranges from 12cm to 48cm. Specifically, H... N The length is 15cm to 45cm, preferably 17cm to 43cm, more preferably 19cm to 41cm, and most preferably 20cm to 40cm.

[0029] In some implementations, the drum has a diameter D R The diameter is 50cm to 500cm, preferably 70cm to 400cm, more preferably 100cm to 300cm, and most preferably 100cm to 250cm.

[0030] In some embodiments, the nozzle is configured to have a spray angle of 30 to 170 degrees, preferably 60 to 140 degrees, such as 60, 70, 80, 90, 100, 110, 120, 130 degrees or any range therebetween.

[0031] In some embodiments, the nozzle is configured to have a diameter of 0.2 mm to 10 mm, preferably 0.4 mm to 5 mm, more preferably 0.6 mm to 3 mm, such as 0.8 mm, 1 mm, 1.5 mm, 2 mm or any range therebetween.

[0032] In some embodiments, the nozzle is configured to have a flow rate of 10 kg / hr to 1500 kg / hr, preferably 120 kg / hr to 1000 kg / hr, such as 50 kg / hr, 150 kg / hr, 250 kg / hr, 400 kg / hr, 600 kg / hr, 800 kg / hr or any range therebetween.

[0033] In some embodiments, the nozzle is configured to have a pressure of 0.05 MPa to 0.5 MPa, preferably 0.1 MPa to 0.4 MPa, such as 0.1 MPa, 0.2 MPa, 0.3 MPa, 0.4 MPa or any range therebetween.

[0034] In some implementations, the nozzle is a hydraulic spray nozzle (e.g., a full cone nozzle, a flat spray nozzle, a hollow cone nozzle, a fine spray nozzle) or an air atomizing nozzle.

[0035] In some embodiments, the nozzle is configured to be positioned within the middle section of the drum. As used herein, the term "middle section" of the drum refers to the segment of the drum located around the midpoint along the length of the drum, preferably wherein the segment covers about 50%, preferably about 40%, and more preferably about 30% of the total length of the drum.

[0036] In some embodiments, the drum includes a plate and an air outlet, wherein the plate and the air outlet are positioned inside the drum and above the plurality of detergent particles, and wherein the plate is positioned between the nozzle and the air outlet.

[0037] Preferably, the plate is positioned substantially perpendicular to the axis of rotation of the drum, and / or the plate has a square, circular, elliptical, triangular, or any combination thereof shape, and / or the plate includes a surface having an area of ​​at least 20% of the cross-sectional area of ​​the drum. Specifically, the air outlet is configured to discharge air containing fine particles (e.g., fine particles with a particle size of less than 100 μm) to ensure a safe environment for the operator, and the plate is configured to at least partially prevent the sprayed liquid composition from being discharged through the air outlet. The cross-sectional area of ​​the drum refers to the area of ​​a cross section along the axis of rotation of the drum. In some embodiments, the drum includes two plates and two air outlets.

[0038] In some embodiments, the liquid composition is sprayed in the form of droplet spray having a median droplet size of 10 μm to 500 μm, preferably 20 μm to 300 μm, more preferably 25 μm to 200 μm, and most preferably 30 μm to 150 μm, such as 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 70 μm, 100 μm, 120 μm and any range between them.

[0039] In some embodiments, the beneficial agent is selected from the group consisting of polymers, fragrances, insect repellents, siloxanes, waxes, lubricants, vitamins, fabric softeners, antibacterial agents, skin health agents, and mixtures thereof.

[0040] Suitable polymers include, but are not limited to: polymeric carboxylates; polyester detergents; cellulose polymers; dye transfer inhibitor (DTI) polymers and mixtures thereof. Such DTI polymers may be selected from the group consisting of: polyvinylpyrrolidone (PVP), poly(vinylpyridine-N-oxide) (PVNO), polyvinylpyrrolidone-co-polyvinylimidazolium (PVP / PVI), poly(vinylpyrrolidone)-co-poly(vinylpyridine-N-oxide) (PVP / PVNO) polymers, polyvinylpyrrolidone-polyepoxyalkylene-vinyl ester copolymers (e.g., PVP / PVAc-g-PEG), and any combination thereof.

[0041] In some embodiments, the liquid composition further comprises a liquid protectant, and the liquid composition is formed by mixing the liquid protectant and the beneficial agent in a stirrer, preferably a static stirrer. Preferably, the liquid protectant is selected from the group consisting of: nonionic surfactants, fatty acid alkyl ester sulfonate surfactants, nonionic polymers, α-aryl esters, and any combination thereof. More preferably, the liquid protectant is selected from the group consisting of: alkylalkoxylated alcohols, fatty acid methyl ester sulfonates, polyethylene glycol, phenyl salicylate, and any combination thereof. Most preferably, the liquid protectant is selected from the group consisting of alkylalkoxylated alcohols and / or fatty acid methyl ester sulfonates.

[0042] In some embodiments, the plurality of detergent particles have an average particle size of about 200 micrometers to about 600 micrometers, preferably about 300 micrometers to about 500 micrometers.

[0043] In some embodiments, the liquid composition has properties such as at about 20°C and 1 second. -1 Viscosities measured below are approximately 0.1 cps to approximately 25,000 cps, preferably approximately 0.3 cps to approximately 5,000 cps, more preferably approximately 0.5 cps to approximately 1,000 cps, and most preferably approximately 0.7 cps to approximately 500 cps, for example, 0.9 cps, 1 cps, 5 cps, 10 cps, 50 cps, 100 cps, 200 cps, 400 cps, or any range thereof.

[0044] In some embodiments, the drum has a diameter of about 0.3m to about 5m, preferably about 0.5m to about 3m, preferably about 0.8m to about 2m; and / or a length of about 1m to about 10m, preferably about 2m to about 8m, more preferably about 2.5m to about 6m.

[0045] In some implementations, the multiple detergent particles are spray-dried, extruded, or agglomerated particles.

[0046] Specifically, the plurality of detergent particles contain a detergency surfactant, which is preferably selected from the group consisting of alkylbenzene sulfonates, alkoxylated alkyl sulfates, alkyl sulfates, alkoxylated alcohols, and mixtures thereof.

[0047] In some embodiments, the method further includes: c) mixing the particulate detergent composition with at least one additional detergent ingredient, preferably selected from the group consisting of: polymeric carboxylates, chelating agents, starch, sodium carbonate, sodium chloride, sodium sulfate, citric acid, cellulose polymers, defoamers, fluorescent whitening agents, colorants, flocculants, polyester detergents, and mixtures thereof.

[0048] On the other hand, the present invention relates to a method for preparing a particulate detergent composition, the method comprising the steps of: a) providing a plurality of detergent particles and a liquid composition comprising a beneficial agent in a rotating drum, the rotating drum including a nozzle located inside the rotating drum; and b) spraying the liquid composition through the nozzle onto at least a portion of the plurality of detergent particles to provide the particulate detergent composition, wherein the liquid composition is sprayed in the form of droplet spray having a median droplet size of 0.6 mm to 5 mm. In a specific embodiment, the median droplet size is preferably 0.8 mm to 5 mm, more preferably 0.9 mm to 4 mm, and most preferably 1 mm to 3 mm.

[0049] Typically, spray drying methods involve spraying an aqueous slurry containing detergent ingredients into a spray drying tower through which hot air flows. As it falls through the tower, the aqueous slurry forms droplets, and the hot air causes the water to evaporate from the droplets, forming multiple spray-dried particles. 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 particles can form a final granular detergent composition. Alternatively, the resulting particles can be further processed (e.g., via agglomeration) and / or additional components (such as detergent additives) can be added thereto.

[0050] Typically, spray-dried powders are cooled, for example, by air stripping. Typically, spray-dried powders are subjected to particle size classification, such as sieving, to obtain a desired particle size distribution. Preferably, the spray-dried powders have a particle size distribution such that the weight-average particle size is in the range of 300 to 500 micrometers, and less than 10% by weight of the spray-dried particles have a particle size greater than 2360 micrometers.

[0051] It is preferable to heat the aqueous slurry mixture to raise the temperature before atomizing it into a spray drying tower, as described in WO2009 / 158162.

[0052] For anionic surfactants, such as linear alkylbenzene sulfonates, it is preferable to introduce them into the spray drying method after the step of forming an aqueous slurry mixture: for example, after pumping, the acid precursor is introduced into the aqueous slurry mixture, as described in WO 09 / 158449.

[0053] For gases, such as air, it is preferable to introduce them into the spray drying method after the step of forming an aqueous slurry, as described in WO2013 / 181205.

[0054] For any inorganic component, such as sodium sulfate and sodium carbonate, it is preferable that if present in an aqueous slurry mixture, the sodium sulfate and sodium carbonate are micronized to a small particle size, as described in WO2012 / 134969.

[0055] Typically, suitable agglomeration methods involve contacting detergency components, such as detergency surfactants, for example linear alkylbenzene sulfonates (LAS) and / or alkylalkoxylated sulfates, with inorganic materials, such as sodium carbonate and / or silica, in a mixer. Agglomeration methods can also be in-situ neutralization agglomeration methods, wherein acidic precursors of the detergency surfactant, such as LAS, are contacted with alkaline materials, such as carbonates and / or sodium hydroxide, in a mixer, and wherein the acidic precursors of the detergency surfactant are neutralized by the alkaline material during the agglomeration process to form the detergency surfactant.

[0056] Other suitable detergent ingredients that can be agglomerated include polymers, chelating agents, bleaching activators, siloxanes, and any combination thereof.

[0057] Agglomeration methods can be high-, medium-, or low-shear agglomeration methods, wherein high-shear, medium-shear, or low-shear mixers are used accordingly. Agglomeration methods can be multi-step agglomeration methods, wherein two or more mixers are used, such as a combination of a high-shear mixer and a medium- or low-shear mixer. Agglomeration methods can be continuous or batch methods.

[0058] It is preferable to subject the agglomerates to a drying step, for example, a fluidized bed drying step. It is also preferable to subject the agglomerates to a cooling step, for example, a fluidized bed cooling step.

[0059] Typically, agglomerates undergo particle size classification, such as fluidized bed washing and / or sieving, to obtain a desired particle size distribution. Preferably, the agglomerates have a particle size distribution such that the weight average particle size is in the range of 300 micrometers to 800 micrometers, and less than 10% by weight of the agglomerates have a particle size of less than 150 micrometers, and less than 10% by weight of the agglomerates have a particle size of greater than 1200 micrometers.

[0060] For both fine and oversized agglomerates, recycling back into the agglomeration process is preferred. Typically, oversized particles undergo a crushing step, such as grinding, and are recycled back to the appropriate location within the agglomeration process, such as a mixer. Similarly, fine powder is typically recycled back to the appropriate location within the agglomeration process, such as a mixer.

[0061] In some embodiments, the liquid protective agent is an alkylalkoxylated alcohol with an average degree of alkoxylation of 1 to 50, preferably with an average degree of ethoxylation of 1 to 12, more preferably with a straight-chain or branched, substituted or unsubstituted C40 with a degree of ethoxylation of 5 to 10. 8-18 Alkyl ethoxylated alcohols.

[0062] In some embodiments, the weight ratio of the liquid protective agent to the beneficial agent in the liquid composition is 0.05 to 50, preferably 0.1 to 20, and more preferably 0.2 to 10.

[0063] Detergent surfactants

[0064] Any suitable detergency surfactant can be used in the granular detergent composition.

[0065] Suitable detergency surfactants include, but are not limited to, anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, and any mixtures thereof. Preferred surfactants include anionic surfactants, cationic surfactants, nonionic surfactants, and any mixtures thereof.

[0066] Suitable anionic surfactants may include alkylbenzene sulfonates. Preferably, the anionic detergency surfactant comprises at least 50%, at least 55%, at least 60%, at least 65%, at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, or even at least 95% alkylbenzene sulfonate by weight of the anionic detergency surfactant. The alkylbenzene sulfonate is preferably linear or branched, substituted or unsubstituted C42-C ... 8-18 Alkylbenzene sulfonates. These are C-type compounds that provide good cleaning properties. 8-18 The optimal content of alkylbenzene sulfonates. C 8-18 Alkylbenzene sulfonates may be modified alkylbenzene sulfonates (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 Alkylbenzene sulfonates are straight-chain C 10-13 Alkylbenzene sulfonates. Linear C-type alkylbenzene sulfonates are particularly preferred. 10-13 Alkylbenzene sulfonates, which can be obtained by sulfonating commercially available linear alkylbenzenes (LABs); suitable LABs include lower 2-phenyl LABs, such as those marketed under the trade name Isochem. ® Those supplied by Sasol, or under the trade name Petrelab ® Those supplied by Petresa. Other suitable LABs include advanced 2-phenyl LABs, such as those marketed under the trade name Hyblene. ® Those supplied by Sasol.

[0067] Anionic detergency surfactants may preferably include other anionic detergency surfactants. Suitable anionic detergency surfactants are non-alkoxylated anionic detergency surfactants. Non-alkoxylated anionic detergency surfactants may be alkyl sulfates, alkyl phosphates, alkyl phosphonates, alkyl carboxylates, or any mixture thereof. Non-alkoxylated anionic surfactants may be selected from; C 10 -C 20 Primary, branched, straight, and random alkyl sulfates (AS) typically have the following formula (I):

[0068] CH3(CH2) x CH2-OSO3 - M +

[0069] Wherein, M is hydrogen or an electrically neutral cation, preferably sodium and ammonium cations, and x is an integer of at least 7, preferably at least 9; C 10 -C 18 Secondary (2,3)alkyl sulfates typically have the following formula:

[0070]

[0071] Wherein, M is hydrogen or an electrically neutral cation, preferably including sodium and ammonium cations, and x is an integer of at least 7, preferably at least 9, and y is an integer of at least 8, preferably at least 9; C 10 -C 18 Alkyl carboxylic esters; medium-chain branched alkyl sulfates, as described in more detail in US 6,020,303 and US 6,060,443; methyl ester sulfonates (MES); α-olefin sulfonates (AOS); and mixtures thereof.

[0072] Another preferred anionic detergency surfactant is an alkoxylated anionic detergency surfactant. The presence of alkoxylated anionic detergency surfactants in spray-dried powders provides good cleaning performance against grease and grime, imparts good foaming properties, and improves the hardness tolerance of the anionic detergency surfactant system. The anionic detergency surfactant may preferably comprise 1% to 50%, or 5%, or 10%, or 15%, or 20%, or up to 45%, or up to 40%, or up to 35%, or up to 30% of the alkoxylated anionic detergency surfactant by weight of the anionic detergency surfactant system.

[0073] Preferably, the alkoxylated anionic detergency surfactant is a linear or branched, substituted or unsubstituted C44 with an average degree of alkoxylation of 0.5 to 30, preferably 0.5 to 10, and more preferably 0.5 to 3. 12-18Alkyl alkoxylated sulfates. Preferably, the alkoxylated anionic detergency surfactant is a straight-chain or branched, substituted or unsubstituted C-type surfactant with an average degree of ethoxylation of 0.5 to 10, more preferably 0.5 to 3. 12-18 Alkyl ethoxylated sulfates. Most preferably, the alkoxylated anionic detergency surfactant is a straight-chain unsubstituted C40 with an average degree of ethoxylation of 0.5 to 7, more preferably 0.5 to 3. 12-18 Alkyl ethoxylated sulfates.

[0074] When present in conjunction with alkylbenzene sulfonates, alkoxylated anionic detergency surfactants can further increase the activity of alkylbenzene sulfonates by making them less likely to precipitate from solution in the presence of free calcium cations. Preferably, the weight ratio of alkylbenzene sulfonate to alkoxylated anionic detergency surfactant is in the range of 1:1 to less than 5:1, or less than 3:1, or less than 1.7:1, or even less than 1.5:1. This ratio imparts optimal whiteness retention properties, as well as good hardness tolerance and good foaming properties. However, it is preferable that the weight ratio of alkylbenzene sulfonate to alkoxylated anionic detergency surfactant is greater than 5:1, or greater than 6:1, or greater than 7:1, or even greater than 10:1. This ratio imparts optimal cleaning performance against grease and grime, as well as good hardness tolerance and good foaming properties.

[0075] Additional detergent ingredients

[0076] Additional detergent ingredients may include builder agents. Any suitable builder agent may be used in the granular detergent composition. Suitable builder agents include, but are not limited to, those selected from: zeolite builder agents; phosphate builder agents; and mixtures thereof. Non-limiting examples of usable zeolite builder agents include: zeolite A; zeolite X; zeolite P; zeolite MAP; and combinations thereof. Sodium tripolyphosphate is a non-limiting example of a usable phosphate builder agent. The content of the zeolite builder agent is from about 1% to about 20% by weight of the detergent composition. It is also particularly preferred that the granular detergent composition contains a low content of builder agent, or even substantially no builder agent. "Substantially no" generally means herein: "does not contain any intentionally added." In a preferred embodiment, the granular detergent composition is substantially free of zeolite, preferably without zeolite. In a preferred embodiment, the granular detergent composition is substantially free of phosphate, preferably without phosphate.

[0077] Additional detergent components may include polymers. Any suitable polymer can be used in granular detergent compositions. Suitable polymers include, but are not limited to: polymeric carboxylates; polyester detergents; cellulose polymers; and mixtures thereof. A preferred polymeric material is a polymeric carboxylate, such as a copolymer of maleic acid and acrylic acid. However, other polymers may also be suitable, such as polyamines (including their ethoxylated variants), polyethylene glycol, and polyesters. Polymer dirt suspending agents and polymeric detergents are also particularly suitable.

[0078] Another suitable polymer is a cellulose polymer, such as a cellulose polymer selected from the following: alkylalkoxy cellulose, preferably methyl hydroxyethyl cellulose (MHEC); alkyl cellulose, preferably methyl cellulose (MC); carboxyl cellulose, preferably carboxymethyl cellulose (CMC); and mixtures thereof.

[0079] The polymer may be present in about 0.5% to about 20% or about 1% to about 10% by weight of the detergent composition.

[0080] Other suitable detergent ingredients may be selected from: chelating agents, such as ethylenediamine disuccinic acid (EDDS); hydroxyethylene diphosphonic acid (HEDP); starch; sodium sulfate; carboxylic acids, such as citric acid or its salts, such as citrate; defoamers; optical brighteners; toners; flocculants, such as polyethylene oxide; and mixtures thereof. If the detergent of the present invention contains masking agents and / or brighteners (e.g., titanium dioxide), they may be present in less than about 1% by weight or less.

[0081] In some embodiments, the additional detergent ingredients may preferably be selected from the group consisting of: polymeric carboxylates, chelating agents, starch, sodium carbonate, sodium chloride, sodium sulfate, citric acid, cellulose polymers, defoamers, optical brighteners, colorants, flocculants, polyester detergents, and mixtures thereof.

[0082] Liquid Protectant

[0083] Unbound by theory, it is believed that liquid protectants can protect beneficial agents from evaporation during preparation (i.e., inside the drum) and / or storage. Preferably, the liquid protectant is selected from nonionic surfactants, fatty acid alkyl ester sulfonate surfactants, nonionic polymers, α-aryl esters, and any combination thereof. More preferably, the liquid protectant is selected from alkylalkoxylated alcohols, polyethylene glycol, fatty acid methyl ester sulfonate surfactants, phenyl salicylate, and any combination thereof.

[0084] The nonionic surfactant used in the liquid composition may be an alkyl polyglucoside and / or an alkyl alkoxylated alcohol. Preferably, the nonionic surfactant is a linear or branched, substituted or unsubstituted C-type surfactant with an average degree of ethoxylation of 1 to 10. 8-18 Alkyl ethoxylated alcohols.

[0085] Suitable nonionic surfactants include alkyl polyglucosides and / or alkyl alkoxylated alcohols. Preferred nonionic alkyl alkoxylated alcohols include C 8-18 Alkyl alkoxylated alcohols, preferably C 8-18 Alkyl ethoxylated alcohols, preferably alkyl alkoxylated alcohols, have an average degree of alkoxylation of 1 to 50, preferably 1 to 30, or 1 to 20, or 1 to 10, and preferably alkyl alkoxylated alcohols are C 8-18 Alkyl ethoxylated alcohols having an average degree of ethoxylation of 1 to 20, preferably 5 to 10. Alkyl alkoxylated alcohols can be straight-chain or branched, and substituted or unsubstituted. Suitable nonionic surfactants can be selected from: C8-C 18 Alkyl ethoxylates, such as NEODOL from Shell ® Nonionic surfactant; C6-C 12 Alkylphenol alkoxylates, wherein preferably the alkoxyl unit is an ethyleneoxy unit, an propyleneoxy unit, or a mixture thereof; C 12 -C 18 Alcohols and C6-C 12 Condensations of alkylphenols with ethylene oxide / propylene oxide block polymers, such as Pluronic from BASF. ® C 14 -C 22 Medium-chain branched alcohols; C 14 To C 22 Medium-chain branched alkyl alkoxylates, preferably having an average degree of alkoxylation of 1 to 30; alkyl polysaccharides, preferably alkyl polysaccharide glycosides; polyhydroxy fatty acid amides; ether-terminated poly(alkoxylated) alcohol surfactants; and mixtures thereof.

[0086] Suitable nonionic surfactants for use in premixes can be selected from: C8-C 18 Alkyl ethoxylates, such as NEODOL from Shell ® Nonionic surfactant; C6-C 12 Alkylphenol alkoxylates, wherein the alkoxyl unit is an ethyleneoxy unit, an propyleneoxy unit, or a mixture thereof; C 12 -C 18 Alcohols and C6-C 12 Condensations of alkylphenols with ethylene oxide / propylene oxide block polymers, such as Pluronic from BASF. ®C 14 -C 22 Medium-chain branched alcohols, BA, as described in more detail in US 6,150,322; C 14 -C 22 Medium-chain branched alkyl alkoxylates, BAEx, wherein x = 1 to 30, as described in more detail in US 6,153,577, US 6,020,303 and US 6,093,856; alkyl polysaccharides, as described in more detail in US 4,565,647, particularly alkyl polyglycosides, 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-terminated poly(alkoxylated) alcohol surfactants, as described in more detail in US 6,482,994 and WO 01 / 42408; and mixtures thereof.

[0087] Suitable nonionic polymers for use in premixes can be selected from polyethylene glycol, polypropylene glycol, and other polymers.

[0088] Suitable α-aryl esters for use in premixes may be selected from the group consisting of benzoates, salicylates, and any combination thereof, such as benzyl benzoate and phenyl salicylate.

[0089] Granular Detergent Composition

[0090] This granular detergent composition is suitable for any laundry detergent application, such as laundry washing, including automatic washing machine washing and hand washing, and even bleaching and laundry detergent additives.

[0091] 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 granules to form a fully formulated detergent product, such as a fully formulated laundry detergent product. The granular detergent composition can be combined with other granules, such as: enzyme granules; fragrance granules, including agglomerates or extrudates of fragrance microcapsules, and fragrance encapsulations such as starch-encapsulated fragrance harmonizer granules; surfactant granules, such as nonionic detergency surfactant granules including agglomerates or extrudates, anionic detergency surfactant granules including agglomerates and extrudates, and cationic detergency surfactant granules including agglomerates and extrudates; polymer granules, including detergency polymer granules and cellulose polymer granules; buffer granules, including carbonate and / or silicate granules, preferably containing carbonates and... Silicate particles, such as sodium carbonate and sodium silicate co-particles, as well as particles and sodium bicarbonate; other spray-dried particles; fluorescent whitening particles; aesthetic particles, such as colored streaks or needle-like or layered particles; bleaching particles such as percarbonate particles, especially coated percarbonate particles, including carbonate and / or sulfate coated percarbonates, silicate coated percarbonates, borosilicate coated percarbonates, sodium perborate coated percarbonates; bleaching catalyst particles, such as transition metal catalyst bleaching particles and imine bleaching-enhancing particles; pre-formed peracid particles; tinting dye particles; and any mixtures thereof.

[0092] The particulate detergent composition according to the invention may have a bulk density of about 250 g / L to about 550 g / L, or about 400 g / L to about 800 g / L. The particulate detergent composition may have an average particle size of about 300 micrometers to about 550 micrometers, or about 350 micrometers to about 450 micrometers.

[0093] Figure 1 An exemplary system for preparing a particulate detergent composition according to the present disclosure is shown. Specifically, the system includes a rotating drum 11 in which a plurality of detergent particles 13 (also referred to as a “powder bed”) are mixed, and a liquid composition containing fragrance is sprayed through a nozzle 12 onto the plurality of detergent particles 13. The rotating drum 11 also includes two air outlets 15 located at opposite ends of the rotating drum 11 and two flat plates 14 located between the nozzle 12 and one of the two air outlets 15. The nozzle 12 is configured to be positioned at a height H above the plurality of detergent particles during spraying. N At, where H N It ranges from 12cm to 48cm.

[0094] Figure 2An experimental setup for determining fragrance loss during a spraying process is shown. Specifically, a plastic box containing non-volatile organic compounds (VOCs) is used as a sealed experimental space, with the spraying device (e.g., a spray gun or syringe) arranged at the top center, and a lifting platform configured to control the distance (e.g., 5 cm to 100 cm) between the spraying device and the powder bed located on the lifting platform. Furthermore, a VOC detector is positioned near the bottom of the plastic box (specifically, an extension tube extending from the VOC detector is located 10 cm from the bottom of the plastic box and 8 cm into the box).

[0095] Example

[0096] Example 1. Reduced fragrance loss when the liquid composition contains fragrance and preservative.

[0097] To explore factors that may affect fragrance loss (including droplet size of the spray, nozzle position, spray formulation, etc.), the inventors of this invention have developed, for example... Figure 2 The experimental setup is shown. A spray gun and a syringe were used as atomizing devices, with the spray gun configured to produce droplet sizes of <100 μm and the syringe configured to produce droplet sizes of approximately 2 mm. The spray pressure of the spray gun was maintained at 0.2 MPa.

[0098] Samples of the powdered products shown in Table 1 (Powdered Product Sample 1; Amount: 1 kg; Thickness: 2 cm) were placed on a lifting platform. The powdered products were preheated to 40°C to simulate factory conditions. Samples of liquid compositions containing fragrances as shown in Table 1 (Liquid Composition Samples A and B; Fragrance Amount: 2 g) were also preheated to 40°C and subsequently fed into a spraying device for spraying. For Sample A, 2 g of fragrance and 8 g of C were sprayed. 12 -C 16 Premix of alkyl ethoxylates (at about 20°C and 1s) -1 Viscosity at the specified temperature: 21.69 cps. For sample B, only 2 g of fragrance was sprayed (at approximately 20°C and 1 s). -1 The viscosity at the lower limit is 0.89 cps, while 8g of C is sprayed separately before spraying the fragrance. 12 -C 16 Alkyl ethoxylates (i.e., in the same amount as in sample A) were used to ensure that the composition of the final product was identical between liquid composition samples A and B. The spray patterns remained substantially the same across different tests. VOCs were then measured using a volatile organic compound (VOC) detector at a distance of 40 cm between the spray device and the powder bed. Based on prior experience, the VOC content gradually increased from the start of spraying and stabilized after 1500 seconds. Therefore, the VOC detector reading at 1500 seconds after spraying was recorded as the VOC content (ppm).

[0099] Table 1. Composition of Powder Products and Liquid Compositions

[0100]

[0101] Table 2 below shows the results of fragrance loss as indicated by VOC (ppm). The results demonstrate that, compared to liquid compositions containing only fragrance, when the liquid composition contains both fragrance and a liquid preservative (e.g., C... 12 -C 16 When both alkyl ethoxylates and alkyl ethoxylates are present, the loss of fragrance is significantly reduced.

[0102] Table 2

[0103]

[0104] Example 2. Fragrance loss is reduced when the droplet spray has a median droplet size within a specific range.

[0105] The inventors of this invention tested the effect of droplet size from a nozzle spray on fragrance loss using the equipment and method described in Example 1, along with powder product sample 1 and liquid composition sample A. Volatile organic compounds (VOCs) were measured at distances of 40 cm and 60 cm between the spraying device and the powder bed using a VOC detector. Surprisingly, as shown in Table 3, the VOC content of larger droplets was significantly lower than that of smaller droplets, indicating that fragrance loss is significantly reduced when using a spray with a relatively large droplet size. Therefore, the total amount of fragrance required to prepare granular detergent products can be reduced, thereby saving costs.

[0106] Table 3

[0107]

[0108] Example 3. Fragrance loss is reduced when the nozzle for spraying fragrance is configured to be positioned appropriately.

[0109] While larger droplet sizes are advantageous, sprays with smaller droplet sizes are also desired for various reasons (e.g., more uniform distribution). Therefore, the inventors of this invention further explored the effect of nozzle position on fragrance loss due to smaller droplet sizes and surprisingly found that fragrance loss was significantly reduced when the nozzle used for spraying fragrance was configured and positioned appropriately. Furthermore, the inventors of this invention discovered that when the nozzle is configured and positioned in a more preferred location, another benefit is provided (i.e., prevention of impaired clumping performance).

[0110] Similar to Example 1, VOC content was determined at different distances (e.g., 5 cm to 60 cm) from the spraying equipment to the powder bed using the equipment and methods of Example 1, along with powder product sample 1 and liquid composition sample A. Then, to understand whether agglomeration was impaired, the following methods and... Figure 3The apparatus shown (bulk strength measuring device, purchased from Sichuan Machineary Institute) is used to measure bulk strength:

[0111] Method for testing the strength of agglomerates

[0112] (1) Place the cylinder in the center of the force measuring instrument.

[0113] (2) Ensure that the cylinder and sleeve are clean and that the sleeve can move freely along the cylinder.

[0114] (3) Insert the locking pin into the hole of the cylinder and place the sleeve (with the lug at the bottom) on the pin.

[0115] (4) Fill the space at the top of the cylinder with a sample of agglomerates / powder.

[0116] (5) Use a ruler to make the powder level with the top of the sleeve.

[0117] (6) Place the lid in the center of the top, with the lugs facing down.

[0118] (7) Secure the upper lug and the lower lug together with an elastic band.

[0119] (8) Carefully place the 5kg weight on top of the lid. Carefully place the weight on the clumped coil holder to avoid uneven pressure.

[0120] (9) Gently remove the metal pin.

[0121] (10) Record the depth of the sinking (in mm) after 5 minutes. This is clumping compression. After noticing the clumping compression, carefully remove the weight and elastic band.

[0122] (11) Slide the sleeve down to the base very gently.

[0123] (12) Set the force gauge to 0 and turn it on.

[0124] (13) Turn on the motor to guide the force gauge to the center of the cover.

[0125] (14) Note the force (in kg) required to break up the agglomerate. This is the agglomerate strength.

[0126] (15) Repeat the test at least three times for each material and strive for an average value, which is the average agglomeration strength of the material being tested.

[0127] equipment

[0128] (a) Agglomerated coil frame

[0129]

[0130] (b) Force recorder

[0131]

[0132] Table 4 below and Figure 4 Results are shown for fragrance loss as indicated by VOC (ppm) and caking performance as indicated by caking strength. The results demonstrate that fragrance loss is significantly reduced when the nozzle used for spraying fragrance is configured and positioned appropriately (i.e., <50 cm). Furthermore, another benefit is obtained if the distance from the spraying device to the powder bed is maintained greater than 10 cm, namely, prevention of significant caking problems. Therefore, the inventors have successfully determined the optimal distance range from the spraying device to the powder bed (i.e., >10 cm and <50 cm) to balance fragrance loss and caking strength.

[0133] Table 4

[0134]

[0135] The dimensions and values ​​disclosed herein should not be construed as strictly limited to the precise numerical values ​​cited. Rather, unless otherwise specified, each such dimension is intended to represent the stated value and the range surrounding its functional equivalent. For example, a dimension disclosed as “40 mm” is intended to represent “approximately 40 mm”.

[0136] Unless expressly excluded or otherwise limited, every reference cited herein, including any cross-references or related patents or patent applications, and any patent application or patent claiming priority to or benefiting from it, is incorporated herein by reference in its entirety. Reference to any reference is not an endorsement of it as prior art to any disclosed or protected art herein, nor is it an endorsement of any such invention, either on its own or in combination with any one or more references. Furthermore, where any meaning or definition of a term in this invention conflicts with any meaning or definition of the same term in referenced documents, the meaning or definition given to that term in this invention shall prevail.

[0137] While specific embodiments of the invention have been illustrated and described by way of example, it will be apparent 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. Therefore, it is intended that all such changes and modifications falling within the scope of the invention be covered by the appended claims.

Claims

1. A method for preparing a particulate composition, the method comprising the following steps: a) Providing a plurality of particles and a liquid composition comprising a beneficial agent in a rotating drum, the rotating drum including a nozzle located inside the rotating drum; as well as b) Spraying the liquid composition through the nozzle onto at least a portion of the plurality of particles to provide the particulate composition, wherein the nozzle is configured to be positioned at a height H above the plurality of particles during spraying. N place, Where H N It ranges from 12cm to 48cm.

2. The method according to claim 1, wherein H N The length is 15cm to 45cm, preferably 17cm to 43cm, more preferably 19cm to 41cm, and most preferably 20cm to 40cm.

3. The method according to claim 1 or 2, wherein the liquid composition is sprayed in the form of droplet spray, the droplet spray having a median droplet size of 10 μm to 1000 μm, preferably 20 μm to 800 μm, more preferably 25 μm to 600 μm, and most preferably 30 μm to 500 μm.

4. The method according to any one of the preceding claims, wherein the drum comprises a flat plate and an air outlet, wherein the flat plate and the air outlet are positioned inside the drum and above the plurality of particles, and wherein the flat plate is positioned between the nozzle and the air outlet. Preferably, the plate is positioned in a direction substantially perpendicular to the axis of rotation of the drum, and / or the plate has a shape that is square, circular, elliptical, triangular, or any combination thereof, and / or the plate includes a surface having an area that is at least 20% of the cross-sectional area of ​​the drum.

5. The method according to any one of the preceding claims, wherein the beneficial agent is selected from the group consisting of polymers, fragrances, insect repellents, siloxanes, waxes, lubricants, vitamins, fabric softeners, antibacterial agents, skin health agents, and mixtures thereof.

6. The method according to any one of the preceding claims, wherein the liquid composition further comprises a liquid preservative, and the liquid composition is formed by mixing the liquid preservative and the beneficial agent in a stirrer, preferably a static stirrer. Preferably, the liquid protective agent is selected from the group consisting of: nonionic surfactants, fatty acid alkyl ester sulfonate surfactants, nonionic polymers, α-aryl esters, and any combination thereof. More preferably, the liquid protective agent is selected from the group consisting of: alkylalkoxylated alcohols, fatty acid methyl ester sulfonates, polyethylene glycol, phenyl salicylate, and any combination thereof, and Most preferably, the liquid protective agent is selected from the group consisting of alkyl alkoxylated alcohols and / or fatty acid methyl ester sulfonates.

7. The method according to any one of the preceding claims, wherein the plurality of particles are spray-dried, extruded, or agglomerated particles.

8. The method according to any one of the preceding claims, wherein the plurality of particles comprise a detergency surfactant, the detergency surfactant preferably being selected from the group consisting of alkylbenzene sulfonates, alkoxylated alkyl sulfates, alkyl sulfates, alkoxylated alcohols, and mixtures thereof.

9. The method according to any one of the preceding claims, wherein the plurality of particles have an average particle size of about 200 micrometers to about 600 micrometers, preferably about 300 micrometers to about 500 micrometers.

10. The method according to any one of the preceding claims, wherein the liquid composition has the following properties at about 20°C and 1 second. -1 The viscosity measured is 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, and most preferably from about 0.7 cps to about 500 cps.

11. The method according to any one of the preceding claims, wherein the drum has a diameter of about 0.3m to about 5m, preferably about 0.5m to about 3m, preferably about 0.8m to about 2m; and / or a length of about 1m to about 10m, preferably about 2m to about 8m, more preferably about 2.5m to about 6m.

12. The method according to any one of the preceding claims, wherein the method further comprises: c) Mixing the particulate composition with at least one additional ingredient, preferably selected from the group consisting of: polymeric carboxylates, chelating agents, starch, sodium carbonate, sodium chloride, sodium sulfate, citric acid, cellulose polymers, defoamers, fluorescent whitening agents, colorants, flocculants, polyester detergents, enzymes, and mixtures thereof.

13. A method for preparing a particulate composition, the method comprising the following steps: a) Providing a plurality of particles and a liquid composition comprising a beneficial agent in a rotating drum, the rotating drum including a nozzle located inside the rotating drum; as well as b) Spraying the liquid composition through the nozzle onto at least a portion of the plurality of particles to provide the particulate composition. The liquid composition is sprayed in the form of droplet spray, the droplet spray having a median droplet size of 0.6 mm to 5 mm.

14. The method according to claim 13, wherein the median droplet size is preferably 0.8 mm to 5 mm, more preferably 0.9 mm to 4 mm, and most preferably 1 mm to 3 mm.

15. The method of claim 13 or 14, wherein the nozzle is configured to be positioned at a height H from the plurality of particles during spraying. N place, and Where H N The length is 12cm to 48cm, preferably 15cm to 45cm, more preferably 17cm to 43cm, still more preferably 19cm to 41cm, and most preferably 20cm to 40cm.

16. The method according to any one of claims 13 to 15, wherein the liquid composition further comprises a liquid preservative, and wherein the liquid composition is formed by mixing the liquid preservative and the beneficial agent in a stirrer, preferably a static stirrer. Preferably, the liquid protective agent is selected from the group consisting of: nonionic surfactants, nonionic polymers, α-aryl esters, and any combination thereof. More preferably, the liquid protective agent is selected from the group consisting of alkylalkoxylated alcohols, polyethylene glycol, benzyl benzoate, phenyl salicylate, and any combination thereof. Most preferably, the liquid protective agent is selected from the group consisting of alkyl alkoxylated alcohols.

17. The method according to any one of claims 13 to 16, wherein the plurality of particles are spray-dried, extruded, or agglomerated particles.

18. The method according to any one of claims 13 to 17, wherein the plurality of particles comprise a detergency surfactant, the detergency surfactant preferably selected from the group consisting of alkylbenzene sulfonates, alkoxylated alkyl sulfates, alkyl sulfates, alkoxylated alcohols, and mixtures thereof.

19. The method according to any one of claims 13 to 18, wherein the method further comprises: c) Mixing the particulate composition with at least one additional ingredient, preferably selected from the group consisting of: polymeric carboxylates, chelating agents, starch, sodium carbonate, sodium chloride, sodium sulfate, citric acid, cellulose polymers, defoamers, fluorescent whitening agents, colorants, flocculants, polyester detergents, enzymes, and mixtures thereof.

20. A system for preparing a particulate composition, wherein the system comprises: i. A rotating drum, the rotating drum comprising a nozzle, a plate, and an air outlet, the nozzle, plate, and air outlet being positioned inside the rotating drum and above the plurality of particles, wherein the plate is positioned between the nozzle and the air outlet. The nozzle is configured to be positioned at a height H above the plurality of particles during spraying. N At this location, the height ranges from 12cm to 48cm. The drum described herein has a diameter D R The diameter ranges from 10cm to 500cm. ii. A static mixer, said static mixer being in fluid communication with said nozzle, and iii. A first reservoir for containing a beneficial agent and a second reservoir for containing a liquid preservative, wherein both the first reservoir and the second reservoir are in fluid communication with the static stirrer.

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