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WO2011074522A1 - Procédé de production de particules de détergent - Google Patents

Procédé de production de particules de détergent Download PDF

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Publication number
WO2011074522A1
WO2011074522A1 PCT/JP2010/072344 JP2010072344W WO2011074522A1 WO 2011074522 A1 WO2011074522 A1 WO 2011074522A1 JP 2010072344 W JP2010072344 W JP 2010072344W WO 2011074522 A1 WO2011074522 A1 WO 2011074522A1
Authority
WO
WIPO (PCT)
Prior art keywords
weight
group
detergent
anionic surfactant
base granule
Prior art date
Application number
PCT/JP2010/072344
Other languages
English (en)
Japanese (ja)
Inventor
将寛 山口
浩章 割田
Original Assignee
花王株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 花王株式会社 filed Critical 花王株式会社
Priority to CN201080057049.0A priority Critical patent/CN102686716B/zh
Priority to AU2010331312A priority patent/AU2010331312B2/en
Publication of WO2011074522A1 publication Critical patent/WO2011074522A1/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/83—Mixtures of non-ionic with anionic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2068—Ethers
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/72—Ethers of polyoxyalkylene glycols

Definitions

  • the present invention relates to a method for producing a detergent particle group and a detergent particle group obtained by the production method.
  • One method for producing detergent particles includes a method of mixing a powdery substance and a liquid surfactant composition. Among them, various methods for using an anionic surfactant in a paste state have been disclosed so far.
  • Patent Document 1 discloses a method for producing a granular detergent composition in which an alkyl ether sulfate paste is made to absorb oil in silica or silicate, and is granulated and dried.
  • a production method has an advantage that a high amount of an anionic surfactant can be incorporated, in order to facilitate the production of such a granular detergent composition, silica or silicate can be used.
  • An oil-absorbing carrier is required, and further, a drying step is required after the granulation step in order to remove moisture contained in the paste.
  • Patent Document 2 discloses a production method in which surface modification is performed by mixing a base granule produced by spray-drying and containing a water-soluble inorganic salt and having a support capacity of 20 mL / 100 g or more and an alkyl sulfate paste. Has been. However, in the case of such a production method, there are many aggregates, and dissatisfaction remains from the viewpoint of particle growth. Moreover, although this subject was improved by adding polyoxyethylene alkyl ether, it was necessary to mix in a large amount, and dissatisfaction remained from the viewpoint of composition flexibility.
  • a step of preparing a detergent particle group by mixing a base granule group having an oil absorption capacity of 0.2 mL / g or more And [2] a detergent particle group obtained by the production method according to [1] above.
  • the present invention does not require a drying step even when a surfactant composition having a high water content is used, has a particle size distribution that is sharp, has a sharp particle size distribution, and has good powder properties such as solubility. It relates to a manufacturing method.
  • a drying step for removing moisture after mixing the anionic surfactant composition and the base granules having an oil absorption capacity of 0.2 mL / g or more is not required.
  • By suppressing particle growth and sharpening the particle size distribution it is possible to obtain a detergent that not only improves the appearance but also has excellent solubility.
  • the coarse particle ratio of the manufactured detergent particle group can be suppressed.
  • Step (B) a step of preparing an anionic surfactant composition by mixing an anionic surfactant paste and an alkyl glyceryl ether
  • Step (C) a step of preparing a detergent particle group by mixing the anionic surfactant composition prepared in the step (B) and a base granule group having an oil absorption capacity of 0.2 mL / g or more
  • Step (B) is a step of preparing an anionic surfactant composition by mixing an anionic surfactant paste and an alkyl glyceryl ether.
  • an anionic surfactant paste is a mixture of an anionic surfactant and water.
  • the content of water in the anionic surfactant paste is preferably 15 to 50% by weight, more preferably 25% to 45% by weight, and further preferably 25 to 40% by weight.
  • % display of content of each component as described in this specification and a compounding quantity is weight% unless there is a prescription
  • alkyl sulfate ester salt polyoxyethylene alkyl sulfate ester salt, ⁇ -sulfo fatty acid ester salt, ⁇ -olefin sulfonate, alkyl or hydroxyalkyl ether carboxylate, N-acylated taurine, N-acylated methyl taurine N-acylated glycine, N-acylated aspartic acid, N-acylated sarcosine, N-acylated glutamic acid, higher fatty acid salt, alkylbenzene sulfonate, alkyl sulfate, monoalkyl phosphate ester salt, alkylamide ether sulfate
  • Examples include ester salts, fatty acid monoglyceride sulfates, and alkyliminodicarbox
  • anionic surfactants include alkyl sulfates, alkyl sulfate esters, ⁇ -sulfo fatty acid ester salts, ⁇ -olefin sulfonates, polyoxyethylene alkyl sulfate salts, and the like. . Alkyl sulfate is more preferable in that a remarkable effect can be obtained.
  • the content of the anionic surfactant in the anionic surfactant composition prepared in this step is preferably 40 to 80% by weight, more preferably 45 to 75% by weight, still more preferably 50 to 70% by weight. %.
  • the alkyl glyceryl ether used in this step has the following general formula (3): R—OCH 2 —CHOH—CH 2 OH (3) (Wherein R represents a linear or branched alkyl or alkenyl group having 1 to 24 carbon atoms, or a cycloalkyl group having 3 to 8 carbon atoms).
  • an anionic surfactant composition obtained by mixing this alkyl glyceryl ether and an anionic surfactant paste it is possible to obtain a detergent particle group with less aggregates and small particle growth.
  • R is a linear or branched alkyl group or alkenyl group having 1 to 24 carbon atoms, or a cycloalkyl group having 3 to 8 carbon atoms. 18 alkyl groups are preferred, and alkyl groups having 8 to 12 carbon atoms are more preferred.
  • R is a straight chain such as hexyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl, etc.
  • the blending amount of the alkyl glyceryl ether in this step is preferably 10 to 40 parts by weight, more preferably 15 to 40 parts by weight, and more preferably 20 to 40 parts by weight with respect to 100 parts by weight of the anionic surfactant in the anionic surfactant paste. Part is more preferred.
  • the blending amount is preferably 10 parts by weight or more, from the viewpoint of the effective amount of the anionic surfactant that can be supported on the base granule group and the cost of the alkyl glyceryl ether.
  • the blending amount is preferably 40 parts by weight or less.
  • the anionic surfactant composition in this step can be prepared by mixing a predetermined amount of anionic surfactant paste and a predetermined amount of alkyl glyceryl ether. You may add components other than these components as needed.
  • the viscosity of the anionic surfactant composition in this step is not particularly limited, but the surfactant composition was measured with MCR300 (manufactured by PHYSICA Messtechnik GmbH) at a temperature of 50 ° C. and a shear rate of 10 [1 / s].
  • MCR300 manufactured by PHYSICA Messtechnik GmbH
  • the range of 0.01 to 20 Pa ⁇ s is preferable and the range of 0.05 to 15 Pa ⁇ s is more preferable from the viewpoint of handling properties in the step of preparing the detergent particle group by mixing with the base granule group.
  • Specific operations for preparing the anionic surfactant composition include, for example, an operation of mixing a predetermined amount of an anionic surfactant paste and a predetermined amount of alkyl glyceryl ether. You may add and mix components other than these components as needed.
  • a mixer to be used a mixer generally used in the detergent field can be used, and as a condition during mixing, a condition generally employed in the detergent field can be employed.
  • Step (C) is a step of preparing a detergent particle group by mixing the anionic surfactant composition prepared in the above step (B) and a base granule group having an oil absorption capacity of 0.2 mL / g or more. is there.
  • Examples of the base granule group used in the step (C) include a granule group capable of supporting a surfactant. More specifically, the following spray-dried base granule group (a) and non-spray-dried base granule group (b) can be mentioned.
  • the spray-dried base granule group (a) is a granule group obtained by spray-drying a slurry containing a water-soluble inorganic salt.
  • the spray-dried base granule group (a) can be prepared by spray-drying a slurry containing the following components.
  • the water-soluble inorganic salt is not particularly limited, but for example, sodium carbonate, potassium carbonate, sodium sulfate, sodium sulfite and sodium chloride are preferable water-soluble inorganic salts.
  • a water-soluble inorganic salt one type can be used alone, or a plurality of types can be used in combination.
  • the following components can be further used.
  • builders generally used in laundry detergents for example, sequestering agents such as zeolite, citrate and sodium tripolyphosphate, and components having both sequestering ability and alkaline ability such as crystalline silicate And anti-staining agents such as acrylic acid polymer, acrylic acid maleic acid copolymer and carboxymethyl cellulose, and fluorescent brightening agents.
  • the amount of water in the slurry is not particularly limited, but, for example, 40 to 60% by weight of the slurry is preferable.
  • the conditions for spray drying the slurry may be any known condition and are not particularly limited.
  • the oil absorption capacity of the spray-dried base granule group (a) is preferably 0.2 mL / g or more, more preferably 0.3 mL / g or more. Moreover, as a preferable upper limit of oil absorption capacity, it is 0.7 mL / g or less. In this range, aggregation between the spray-dried base granule groups (a) is suppressed, which is suitable for suppressing particle growth of the particles in the detergent particle group. Therefore, the oil absorption capacity of the spray-dried base granule group (a) is preferably 0.2 to 0.7 mL / g, more preferably 0.3 to 0.7 mL / g, from the same viewpoint as described above.
  • the method for measuring the oil absorption capacity of the spray-dried base granule group (a) is as follows. 100 g of a sample (spray-dried base granule group (a)) is placed in a cylindrical mixing tank having an inner diameter of about 5 cm and a depth of about 15 cm equipped with a stirring blade inside. While stirring the stirring blade at 350 r / min, linseed oil at 25 ° C. is added at a rate of about 10 mL / min, and the change over time in the stirring power is measured. The amount of linseed oil input when the stirring power becomes the highest is the oil absorption capacity (mL / g).
  • the bulk density of the spray-dried base granule group (a) is preferably 200 to 1000 g / L, more preferably 300 to 1000 g / L, further preferably 400 to 1000 g / L, and more preferably 500 to 800 g / L.
  • the bulk density of the spray-dried base granule group (a) is measured by the method defined in JIS K3362 unless otherwise specified.
  • the average particle size of the spray-dried base granule group (a) is preferably 140 to 600 ⁇ m, more preferably 150 to 500 ⁇ m, still more preferably 180 to 300 ⁇ m.
  • the average particle diameter of the detergent particle group, the base granule group, and the like is obtained as follows using a sieve specified in JIS Z 8801 unless otherwise specified.
  • a 9-stage sieve and a saucer having openings of 2000 ⁇ m, 1400 ⁇ m, 1000 ⁇ m, 710 ⁇ m, 500 ⁇ m, 355 ⁇ m, 250 ⁇ m, 180 ⁇ m and 125 ⁇ m are prepared, and a low tap machine (Tanaka Chemical Machinery Co., Ltd., Tapping: 156 Times / minute, rolling: 290 times / minute).
  • a low tap machine Teanaka Chemical Machinery Co., Ltd., Tapping: 156 Times / minute, rolling: 290 times / minute.
  • the moisture content in the spray-dried base granule group (a) is measured by the following infrared moisture meter method. That is, 3 g of a sample (spray-dried base granule group (a)) is weighed on a sample pan of known weight, and the sample is heated and dried for 3 minutes with an infrared moisture meter (Infrared lamp 185W manufactured by Kett Science Laboratory Co., Ltd.). I do. After drying, weigh the sample pan and the dried sample. The difference between the weight of the sample pan and the sample obtained before and after drying obtained by such an operation is divided by the measured amount of the sample, and multiplied by 100 to calculate the amount (%) of moisture in the sample.
  • infrared moisture meter Infrared lamp 185W manufactured by Kett Science Laboratory Co., Ltd.
  • the content of the water-soluble inorganic salt in the spray-dried base granule group (a) is preferably 40 to 90% by weight of the granule group (a) from the viewpoint of washing performance and handling of the slurry before spray drying. More preferred is 50 to 90% by weight, and still more preferred is 55 to 90% by weight.
  • Non-spray-dried base granule group (b) is granulated in a container rotary granulator by adding a binder to a detergent powder raw material having an oil absorption capacity of 0.4 mL / g or more using a multi-fluid nozzle. It is a granule group obtained by.
  • the powder raw material for detergent include the following powder raw materials (referred to as “powder raw material (a)”).
  • the powder raw material (a) examples include soda ash (for example, light ash and dense ash) prepared by baking sodium bicarbonate, mirabilite, porous powder prepared by drying tripolyphosphate hydrate, clay mineral powder Etc. Light ash is preferable from the viewpoint of ease of handling and availability.
  • soda ash for example, light ash and dense ash
  • porous powder prepared by drying tripolyphosphate hydrate, clay mineral powder Etc.
  • Light ash is preferable from the viewpoint of ease of handling and availability.
  • the powder raw material (a) usually has fine pores of 10 ⁇ m or less inside, and a surfactant can be supported on the pores.
  • clay mineral powder examples include talc, pyrophyllite, smectite (saponite, hectorite, saconite, stevensite, montmorillonite, beidellite, nontronite, etc.), vermiculite, mica (phlogopite, biotite, chinwald mica, muscovite.
  • the average particle diameter of the powder raw material (a) excluding the clay mineral powder is preferably 10 to 250 ⁇ m, more preferably 50 to 200 ⁇ m, still more preferably 80 to 200 ⁇ m.
  • the particle size of the clay mineral powder is preferably 10 to 100 ⁇ m, more preferably 50 ⁇ m or less, and more preferably 30 ⁇ m or less.
  • the powder raw material (a) is preferably a water-soluble substance.
  • the oil absorption capacity of the powder raw material (a) used in this step is a value determined by the following evaluation method.
  • the upper limit of the oil absorption capacity of the powder raw material (a) is not particularly limited, but is preferably 1.0 mL / g or less, for example.
  • the content of the powder raw material (a) in the non-spray-dried base granule group (b) is preferably 40 to 95% by weight, more preferably 45 to 90% by weight of the granule group (b) from the viewpoint of oil absorption. 50 to 85% by weight is more preferable, and 50 to 80% by weight is more preferable.
  • the powder raw material (a) may be used alone as a powder raw material for detergent, or a plurality of types may be used.
  • non-spray-dried base granule group (b) can be obtained using the following other components. Specific examples include builders generally used for garment detergents, anti-staining agents and fluorescent whitening agents mentioned in the description of the spray-dried base granule group (a).
  • a method of granulating the detergent powder raw material and the binder with a container rotary granulator is employed.
  • a container rotating granulator a drum type mixer or a pan type mixer is preferable.
  • the drum-type mixer is not particularly limited as long as the drum-shaped cylinder rotates and performs processing.
  • the conical drum-type granulator is used. (Mixer), multi-stage conical drum granulator (mixer), etc. can also be used. These apparatuses can be used in both batch and continuous processes.
  • binder to be added examples include polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether and derivatives thereof, polyvinyl alcohol and derivatives thereof, water-soluble cellulose derivatives (these derivatives include ether compounds and the like). ), Organic polymers such as carboxylic acid polymers, starches and saccharides, inorganic polymers such as amorphous silicates, higher fatty acids, alkylbenzene sulfonic acids, general interfaces as described in the well-known collection of conventional techniques Examples include activators. From the viewpoint of caking property and detergency, water-soluble cellulose derivatives, saccharides and carboxylic acid polymers are preferred, and acrylic acid-maleic acid copolymer salts and polyacrylates are more preferred.
  • the salt is preferably a sodium salt, potassium salt or ammonium salt.
  • the weight average molecular weight of the carboxylic acid polymer is preferably from 1,000 to 100,000, more preferably from 2,000 to 80,000.
  • the added binder may be an aqueous solution.
  • the concentration when added as an aqueous solution is not particularly limited, but the particle size at the time of granulation of the non-spray-dried base granule group (b) is greatly influenced by the volume of the binder. What is necessary is just to determine a density
  • the concentration of the binder component when added as an aqueous solution is preferably 20 to 80% by weight.
  • the binder is added using a multi-fluid nozzle.
  • a multi-fluid nozzle is a nozzle that mixes and atomizes a liquid and atomizing gas (air, nitrogen, etc.) through an independent flow path to the vicinity of the nozzle tip.
  • a fluid nozzle or the like can be used.
  • the mixing part of the binder and atomizing gas may be either an internal mixing type that mixes within the nozzle tip or an external mixing type that mixes outside the nozzle tip.
  • an internal mixed type two-fluid nozzle such as manufactured by Spraying Systems Japan Co., Ltd., manufactured by Kyoritsu Alloy Manufacturing Co., Ltd., or manufactured by Ikeuchi Co., Ltd., manufactured by Spraying Systems Japan Co., Ltd.
  • an external mixing type two-fluid nozzle manufactured by Kyoritsu Alloy Mfg. Co., Ltd. and Atmax Co., Ltd. an external mixing type four-fluid nozzle manufactured by Fujisaki Electric Co., Ltd., and the like.
  • the atomizing gas atomizing pressure is 0.1 MPa (gauge pressure).
  • 1.0 MPa (gauge pressure) or less is preferable from the viewpoint of equipment load.
  • limiting in particular as the spraying pressure of a binder However, 1.0 MPa or less is preferable from a viewpoint of equipment load, for example.
  • the content of the binder in the non-spray-dried base granule group (b) is preferably 1 to 50% by weight in the non-spray-dried base granule group (b) from the viewpoints of caking property and oil absorption capacity. % By weight is more preferred, 8 to 40% by weight is still more preferred, and 10 to 35% by weight is more preferred.
  • the non-spray-dried base granule group (b) is, for example, a group of granules having a structure in which the powder raw material (a) is gently aggregated. In that case, it has (1) a large gap between granules, and (2) a small gap of 10 ⁇ m or less in the powder raw material (a) and two supporting sites between layers. By adjusting these two loading sites, a non-spray-dried base granule group (b) having a desired oil absorption capacity can be obtained.
  • the oil absorption capacity of the non-spray dried base granule group (b) is 0.2 mL / g or more, preferably 0.3 mL / g or more, and more preferably 0.4 mL / g or more.
  • the oil absorption capacity is preferably 0.7 mL / g or less. In such a range, aggregation of the non-spray-dried base granule group (b) is suppressed, which is preferable because the particle growth degree of the particles in the detergent particle group can be suppressed.
  • the oil absorption capacity of the non-spray dried base granule group (b) is preferably 0.2 to 0.7 mL / g, more preferably 0.3 to 0.7 mL / g, from the same viewpoint as described above.
  • the method for measuring the oil absorption capacity of the non-spray dried base granule group (b) is the same as the method for measuring the oil absorption capacity of the spray dried base granule group (a).
  • the bulk density of the non-spray-dried base granule group (b) is from 200 to 1000 g / from the viewpoint of securing the loading capacity of the surfactant composition and securing the high bulk density after loading the surfactant composition.
  • L is preferable, 300 to 1000 g / L is more preferable, 400 to 550 g / L is still more preferable, and 400 to 500 g / L is still more preferable.
  • the method for measuring the bulk density of the non-spray-dried base granule group (b) is the same as the method for measuring the bulk density of the spray-dried base granule group (a).
  • the average particle size of the non-spray-dried base granule group (b) is preferably 140 to 600 ⁇ m, more preferably 150 to 500 ⁇ m, still more preferably 200 to 500 ⁇ m.
  • the water content in the non-spray-dried base granule group (b) is preferably 30% by weight or less, more preferably 20% by weight or less, and further preferably 15% by weight or less from the viewpoints of handling properties and oil absorption.
  • the method for measuring the water content in the non-spray-dried base granule group (b) is the same as the method for measuring the water content in the spray-dried base granule group (a).
  • the ratio of the two components when mixing the anionic surfactant composition and the base granule group is not particularly limited as long as it can be uniformly mixed.
  • the anionic surfactant composition with respect to 100 parts by weight of the base granule group The amount of the product is preferably 5 to 100 parts by weight, more preferably 10 to 90 parts by weight, further preferably 20 to 70 parts by weight, and more preferably 25 to 50 parts by weight.
  • the anionic surfactant composition is preferably 5 parts by weight or more, more preferably 10 parts by weight or more, and 20 parts by weight or more with respect to 100 parts by weight of the granule group.
  • the anionic surfactant composition is preferably 100 parts by weight or less, more preferably 90 parts by weight or less, and more preferably 70 parts by weight with respect to 100 parts by weight of the granule group. More preferably, it is more preferably 50 parts by weight or less.
  • a mixing condition that substantially maintains the morphology of the base granule group that is, a mixing condition that does not cause the granule group to collapse may be selected.
  • a mixing condition that substantially maintains the morphology of the base granule group that is, a mixing condition that does not cause the granule group to collapse
  • it may be mixed manually using a spatula or the like, or when using a mixer equipped with a stirring blade, from the viewpoint of suppressing the collapse of the base granules and the efficiency of mixing
  • the shape of the mixing blade of the stirring blade provided in the paddle type is a paddle type
  • the fluid number of the stirring blade is preferably 0.5 to 8.0, more preferably 0.8 to 4.0, still more preferably 0. .5 to 2.0.
  • the fluid number of the stirring blade is preferably 0.1 to 4.0, more preferably 0.15 to 2.0.
  • the fluid number of the stirring blade is preferably 0.05 to 4.0, more preferably 0.1 to 2.0.
  • Fluid number V 2 / (R ⁇ g) (Here, V represents the peripheral speed [m / s] of the tip of the stirring blade, R represents the rotational radius [m] of the stirring blade, and g represents the acceleration of gravity [m / s 2 ].)
  • step (C) powder raw materials other than the base granule group can be blended if desired.
  • the blending amount is preferably 30 parts by weight or less with respect to 100 parts by weight of the base granule group from the viewpoint of solubility.
  • the powder raw material other than the base granule group referred to in this step means a powder cleaning strength enhancer or oil absorbent at room temperature.
  • bases showing sequestering ability such as zeolite and citrate
  • bases showing alkaline ability such as sodium carbonate and potassium carbonate
  • sequestering ability and alkaline ability such as crystalline silicate
  • bases having all of them include bases having all of them, amorphous silica and amorphous aluminosilicate having a high sequestering ability but a low sequestering ability.
  • this powder raw material in combination with the base granule group as desired, it is possible to achieve a high blending of the anionic surfactant composition and a reduction in the adhesion of the mixture into the mixer, and to improve the cleaning power. it can.
  • a powder raw material one type can be used alone, or a plurality of types can be used in combination.
  • polyethylene glycol (PEG) and / or fatty acid and / or soapy water is preferably added in an amount of 1 to 10 parts by weight with respect to 100 parts by weight of the base granule group.
  • the surface of the base granule group may be coated by mixing. This coating is preferred because the caking resistance of the detergent particles is improved.
  • PEG and / or fatty acid and / or soapy water it becomes possible to suppress aggregation and enhance dispersibility when dissolving the detergent particles, resulting in improved solubility of the detergent particles. This is preferable.
  • the detergent particle group obtained by the present invention may contain a nonionic surfactant.
  • the nonionic surfactant may be oil-absorbed and supported on the base granule group before and / or after the step (C), or may be mixed with the anionic surfactant composition used in the step (B) to form an anionic interface. Oil absorption and loading may be carried out simultaneously with the activator composition, but it is preferable to oil absorption and loading before the step (C) from the viewpoint of suppressing caking due to exudation of the nonionic surfactant.
  • content in the detergent particle group of this nonionic surfactant 20 weight% or less in a detergent particle group is preferable from a viewpoint of suppression of caking by oozing-out, and 15 weight% or less is more preferable. Moreover, 5 weight% or more is preferable from a viewpoint of detergency, and 10 weight% or more is more preferable.
  • the type of the nonionic surfactant is not particularly limited, and for example, the nonionic surfactant described in the well-known conventional technique collection (powder detergent for clothing) issued by the Japan Patent Office can be used.
  • the temperature in the mixer during mixing is preferably a temperature at which the anionic surfactant composition and the base granule group can be efficiently mixed while substantially suppressing the collapse of the base granule group.
  • a temperature equal to or higher than the pour point of the anionic surfactant composition to be mixed is preferable, a temperature equal to or higher than 10 ° C. of the pour point is more preferable, and a temperature equal to or higher than 20 ° C. is more preferable.
  • the mixing time during mixing is preferably about 2 to 20 minutes, more preferably about 2 to 10 minutes.
  • the temperature in the mixer can be adjusted by flowing cold water or hot water through a jacket or the like. Therefore, the apparatus used for mixing preferably has a structure with a jacket.
  • the mixing method of the anionic surfactant composition and the base granule group may be a batch type or a continuous type. When mixing batchwise, it is preferable to add the anionic surfactant composition after previously charging the base granule group into the mixer.
  • the temperature of the supplied anionic surfactant composition is preferably 70 ° C. or lower, more preferably 60 ° C. or lower, from the viewpoint of the stability of the anionic surfactant composition.
  • the mixer used for batch mixing is not particularly limited as long as it is a mixer generally used for batch mixing.
  • the mixing blade shape is a paddle type mixer, A mixer with a stirring shaft attached to this shaft and mixing the powder by attaching a stirring blade to this shaft: Henschel mixer (Mitsui Miike Chemical Co., Ltd.), high speed mixer (Fukae Kogyo Co., Ltd.), Vertical granulator (Powrec Co., Ltd.), Redige mixer (Matsubo Co., Ltd.), Proshare mixer (Pacific Kiko Co., Ltd.), TSK-MTI mixer (Tsukishima Kikai Co., Ltd.), JP 10 -296064 and Japanese Patent Laid-Open No. 10-296065, etc.
  • a mixer having a mixing blade shape of a ribbon type a cylindrical, semi-cylindrical or conical type solid mixer is used.
  • Mixer that mixes by rotating ribbon-shaped blades that form spirals in a container that has been formed Ribbon mixer (manufactured by Hiwa Machine Industry Co., Ltd.), batch kneader (manufactured by Satake Chemical Machinery Co., Ltd.) , Ribocorn (manufactured by Daishun Seisakusho Co., Ltd.), Julia mixer (manufactured by Tokuju Kosakusho Co., Ltd.), etc.
  • mixers that mix by revolving while rotating around an axis parallel to the wall of the wall: for example, Nauter mixer (manufactured by Hosokawa Micron Corporation), SV mixer (manufactured by Shinko Pantech Co., Ltd.), etc. .
  • a continuous mixer generally used for continuous mixing, but for example, the base granule group using a continuous device among the above mixers.
  • An anionic surfactant composition may be mixed.
  • ⁇ Surface modification> It is desirable to further modify the surface of the detergent particles obtained in the step (C). By performing the surface modification, it is possible to obtain a detergent particle group having improved fluidity and caking resistance. When performing surface modification, it is preferable to use fine powder. When the fine powder is used, surface modification can be performed by mixing the detergent particles obtained in the step (C) and the fine powder under predetermined conditions.
  • the fine powder is not particularly limited, but has an average primary particle size of 20 ⁇ m or less in terms of improving the coverage of the detergent particles and improving the fluidity and caking resistance of the detergent particles. Is preferred.
  • the average particle diameter is measured by a method using light scattering, for example, a particle analyzer (manufactured by Horiba, Ltd.) or microscopic observation.
  • the fine powder include inorganic fine powders such as silicate compounds such as crystalline silicate compounds, aluminosilicate, calcium silicate, silicon dioxide, bentonite, sodium tripolyphosphate, talc, clay, and amorphous silica derivatives. Body and metal soap with primary particles of 20 ⁇ m or less.
  • silicate compounds such as crystalline silicate compounds, aluminosilicate, calcium silicate, silicon dioxide, bentonite, sodium tripolyphosphate, talc, clay, and amorphous silica derivatives.
  • Body and metal soap with primary particles of 20 ⁇ m or less As such a fine powder, one kind can be used alone, or a plurality of kinds can be used in combination. Furthermore, it is preferable in terms of detergency that the fine powder has high ion exchange ability and alkali ability.
  • preferable fine powders include silicate compounds such as crystalline silicate compounds and aluminosilicates.
  • the amount of the fine powder used is preferably 0.5 to 40.0 parts by weight, more preferably 1 to 30 parts by weight, based on 100 parts by weight of the base granule group, from the viewpoint of fluidity and feeling of use.
  • a mixing condition capable of substantially maintaining the form of the base granule group carrying the anionic surfactant composition may be selected.
  • a mixing condition capable of substantially maintaining the form of the base granule group carrying the anionic surfactant composition
  • it may be mixed manually using a spatula or the like, or it is preferable to use a mixer equipped with both a stirring blade and a crushing blade.
  • the fluid number of the stirring blade provided in the machine is preferably 10 or less, more preferably 7 or less.
  • the fluid number is preferably 2 or more, more preferably 3 or more.
  • the fluid number of the crushing blade is preferably 8000 or less, and more preferably 5000 or less.
  • the fluid number is within this range, a detergent particle group having excellent fluidity can be obtained.
  • a preferable mixer in this step among the mixers used in the step (C), those equipped with both a stirring blade and a crushing blade can be mentioned. Further, by performing the step (C) and the surface modification using different mixers, it is easy to adjust the temperature of the substance to be mixed. For example, when a non-heat resistant component such as a fragrance or an enzyme is added during or after the surface modification, it is preferable to adjust the temperature of the mixture when the surface modification is performed. Such temperature adjustment can be performed by setting the jacket temperature or venting. In order to transfer the detergent particles obtained in the step (C) to an apparatus for efficiently modifying the surface, it is also a preferable aspect that a part of the fine powder is added to the detergent particles at the end of the step (C). .
  • the detergent particle group of the present invention can be obtained by the production method of the present invention as described above.
  • the detergent particle group is not particularly limited, but is a detergent particle group produced using the base granule group as a core, and substantially one base granule in one detergent particle.
  • a group of detergent particles having the characteristic of having as a core is preferred.
  • Particle growth degree [average particle size of detergent particles] / [average particle size of base granules] (1)
  • a detergent particle group having a particle growth degree of 1.25 or less is preferable, one having 1.20 or less is more preferable, and one having 1.15 or less is more preferable.
  • the lower limit of the degree of grain growth is not particularly limited, but is preferably 1.0 or more. Accordingly, the degree of particle growth is preferably 1.0 to 1.25, more preferably 1.0 to 1.20, and still more preferably 1.0 to 1.15 from the viewpoint of suppressing aggregation of the detergent particle group.
  • the detergent particles of the present invention are prevented from agglomerating between detergent particles, the amount of particles outside the desired particle size range (aggregated particles) is less, and the detergent particles have excellent solubility. And the particle size distribution of the detergent particles is sharp.
  • the average particle diameter of the detergent particle group of the present invention is preferably 150 ⁇ m or more, more preferably in the range of 150 to 500 ⁇ m, and still more preferably in the range of 180 to 350 ⁇ m.
  • the coarse particle ratio is defined by the weight percentage of the proportion of particles having a size of 500 ⁇ m or more in the base granule group or the detergent particle group.
  • the coarse particle ratio of the detergent particle group or the base granule group in the present invention is preferably 35% by weight or less, preferably 25% by weight or less, more preferably 15% by weight or less, and further preferably 10% by weight or less.
  • 5% by weight or less is even more preferable.
  • the coarse particle ratio of the detergent particle group to be produced does not increase greatly even when the base granule group having a relatively high coarse particle ratio is used.
  • This feature can be manifested by the “difference in the coarse particle rate of the detergent particles” defined below.
  • the increase in the coarse particle ratio of the detergent particle group is defined as the coarse particle ratio of the detergent particle group minus the coarse particle ratio of the base granule group.
  • the difference in increase in the coarse particle ratio of the detergent particle group of the present invention is preferably smaller, but is preferably 15% by weight or less, and more preferably 10% by weight or less.
  • the bulk density of the detergent particles is preferably 300 to 2000 g / L, more preferably 500 to 1500 g / L, and still more preferably 600 to 1000 g / L.
  • the method for measuring the bulk density of the detergent particles is the same as the method for measuring the bulk density of the spray-dried base granules (a).
  • the detergent particle group obtained by the production method of the present invention having the above-described structure has a suppressed particle growth and a sharp particle size distribution, which improves not only the appearance but also the solubility. It is an excellent detergent particle group.
  • the dissolution rate of the detergent particle group for 60 seconds can be used.
  • the dissolution rate for 60 seconds is preferably 80% or more, more preferably 90% or more.
  • the dissolution rate of the detergent particles for 60 seconds is calculated by the following method.
  • 1 liter of hard water (Ca / Mg molar ratio 7/3) corresponding to 71.2 mg CaCO 3 / liter cooled to 5 ° C. is a 1 liter beaker (inner diameter 105 mm, height 150 mm cylindrical type, for example, manufactured by Iwaki Glass Co., Ltd. 1 In a state where the water temperature of 5 ° C.
  • the stirring bar (length: 35 mm, diameter: 8 mm, for example, model: manufactured by ADVANTEC, trade name: Teflon (registered trademark))
  • SA round thin type
  • stirring is performed at a rotational speed (800 r / m) at which the spiral depth with respect to the water depth is approximately 1/3.
  • the detergent particles which have been reduced and weighed to 1.000 ⁇ 0.0010 g, are added and dispersed in water with stirring, and stirring is continued.
  • the detergent particle group dispersion in the beaker is filtered through a standard sieve (diameter: 100 mm) having an opening of 74 ⁇ m as defined in JISZ8801 of known weight, and the water-containing detergent particle groups remaining on the sieve are collected together with the sieve. Collect in an open container of known weight.
  • the operation time from the start of filtration until the sieve is collected is 10 ⁇ 2 seconds.
  • the collected residue of detergent particles is dried in an electric dryer heated to 105 ° C. for 1 hour, and then cooled in a desiccator (25 ° C.) containing silica gel for 30 minutes. After cooling, the total weight of the dissolved residue of the dried detergent, the sieve, and the collection container is measured, and the dissolution rate (%) of the detergent particle group is calculated by Equation (4).
  • Dissolution rate (%) ⁇ 1- (T / S) ⁇ ⁇ 100 (4)
  • the detergent particle group of the present invention is excellent in detergency. Unless otherwise specified, the following method is used as an index of detergency in the present specification.
  • An artificially contaminated cloth is prepared by attaching an artificially contaminated liquid having the following composition to the cloth.
  • the artificial contamination liquid is attached to the cloth by printing the artificial contamination liquid on the cloth using a gravure roll coater.
  • the process of making an artificially contaminated cloth by adhering an artificially contaminated liquid to the cloth is performed under the conditions of a gravure roll cell capacity of 58 cm 3 / cm 2 , a coating speed of 1.0 m / min, a drying temperature of 100 ° C., and a drying time of 1 minute.
  • a cotton gold cloth 2003 cloth manufactured by Tanigami Shoten
  • Sodium polyacrylate weight average molecular weight 10,000 (manufactured by Kao Corporation)
  • Zeolite Zeobuilder (type 4A, manufactured by Zeobuilder: median diameter: 3.0 ⁇ m)
  • Clay mineral powder Round rosyl DGA powder; Oil absorption capacity 0.44 mL / g (manufactured by Zude Chemi)
  • Light ash average particle size 100 ⁇ m; oil absorption capacity 0.45 mL / g (manufactured by Central Glass Co., Ltd.)
  • Crystalline silicate Pre-feed granule (manufactured by Tokuyama Siltech Co., Ltd.)
  • Polyoxyethylene alkyl ether Emulgen 106KH (manufactured by Kao Corporation)
  • Production Example 1 Production of spray-dried base granule group (a)
  • the spray-dried base granule group (a) was produced by the following procedure. ⁇ Process (A-1)> 405 kg of water was added to a 1 m 3 mixing tank equipped with a stirring blade, and after the water temperature reached 55 ° C., 110 kg of sodium sulfate, 123 kg of sodium carbonate, and 4.4 kg of sodium sulfite were added to this mixing tank. After stirring for 10 minutes, 137 kg of 40% by weight aqueous sodium polyacrylate was added to the mixing vessel. After further stirring for 10 minutes, 37 kg of sodium chloride and 120 kg of zeolite were added to this mixing tank, and further stirred for 30 minutes to obtain a homogeneous slurry. The final temperature of this slurry was 58 ° C.
  • the slurry was sprayed at a spray pressure of 2.5 MPa from a pressure spray nozzle installed near the top of the spray-drying tower to produce a spray-dried base granule group (a).
  • the hot gas supplied to the spray-drying tower was supplied at a temperature of 235 ° C. from the bottom of the tower and discharged at 119 ° C. from the top of the tower.
  • the water content of the obtained spray-dried base granule group (a) was 0.15% by weight.
  • the physical properties of the resulting spray-dried base granule group (a) were an average particle size of 257 ⁇ m, a bulk density of 538 g / L, a coarse particle ratio of 0.2% by weight, and an oil absorption capacity of 0.45 mL / g.
  • Production Example 2 Production of non-spray-dried base granule group (b-1) A non-spray-dried base granule group (b-1) was produced by the following procedure.
  • the physical properties of the obtained non-spray-dried base granule group (b-1) were as follows: the average particle size was 289 ⁇ m, the bulk density was 511 g / L, the coarse particle ratio was 12.2 wt%, and the oil absorption capacity was 0.51 mL / g. there were.
  • Production Example 3 Production of non-spray dried base granule group (b-2) A non-spray dried base granule group (b-2) was produced by the following procedure.
  • the physical properties of the non-spray-dried base granule group (b-2) obtained were as follows: the average particle size was 270 ⁇ m, the bulk density was 484 g / L, the coarse particle ratio was 20.4% by weight, and the oil absorption capacity was 0.52 mL / g. there were.
  • Examples 1-6 ⁇ Process (B)> 20 parts by weight (Example 1), 30 parts by weight (Example 2) or 40 parts by weight of 100 parts by weight of sodium alkyl sulfate in an anionic surfactant paste comprising 75% by weight of sodium alkyl sulfate and 25% by weight of water
  • the mixture of 90% by weight of 2-ethylhexyl glyceryl ether and 10% by weight of water was added and mixed at a temperature of 60 ° C. for 1 minute to obtain an anionic surfactant composition.
  • Example 1 The viscosity of the anionic surfactant composition of Example 1 and Example 4 was measured at a temperature of 50 ° C. and a shear rate of 10 [1 / s] using MCR300 (manufactured by PHYSICA Messtechnik GmbH). s (Example 1) 10.1 Pa ⁇ s (Example 4).
  • Each granulated product obtained by the above operation is placed in a plastic bag containing 4.2 parts by weight of crystalline silicate and 23.1 parts by weight of zeolite with respect to 100 parts by weight of spray-dried base granules (a). added.
  • the plastic bag was shaken 30 times up and down to modify the surface of the granulated product (mixture), and each detergent particle group was obtained.
  • Comparative Example 1 ⁇ Process (C)> 29.5 parts by weight of an anionic surfactant paste composed of 75% by weight of sodium alkyl sulfate and 25% by weight of water is added to 100 parts by weight (50g) of the spray-dried base granule group (a) produced in Production Example 1. And mixing for 10 minutes using a spatula to obtain a mixture. When the obtained mixture was observed, the presence of liquid was not observed, but many aggregates were observed.
  • the granulated product obtained by the above operation was added to a plastic bag containing 4.2 parts by weight of crystalline silicate and 23.1 parts by weight of zeolite with respect to 100 parts by weight of the spray-dried base granule group (a). .
  • the plastic bag was shaken up and down 30 times to carry out surface modification of the granulated product (mixture) to obtain detergent particles.
  • Comparative Example 2 ⁇ Process (B)> 25 parts by weight of polyoxyethylene alkyl ether with respect to 100 parts by weight of sodium alkyl sulfate was added to a mixture comprising 75% by weight of sodium alkyl sulfate and 25% by weight of water, and mixed for 1 minute at a temperature of 60 ° C. An activator composition was obtained. When the viscosity of the obtained anionic surfactant composition was measured at a temperature of 50 ° C. and a shear rate of 10 [1 / s] using MCR300 (manufactured by PHYSICA Messtechnik GmbH), it was 11.2 Pa ⁇ s.
  • the mixture obtained by the above operation was added to a plastic bag containing 4.2 parts by weight of crystalline silicate and 23.1 parts by weight of zeolite with respect to 100 parts by weight of the spray-dried base granule group (a).
  • the plastic bag was shaken up and down 30 times to carry out surface modification of the granulated product (mixture) to obtain detergent particles.
  • Table 1 shows the physical properties of the detergent particles obtained in Examples 1 to 6 and Comparative Examples 1 and 2.
  • Examples 7 to 10 ⁇ Process (B)>
  • an anionic surfactant paste comprising 75% by weight sodium alkyl sulfate and 25% by weight water, 20 parts by weight (Example 8) or 30 parts by weight (Example 7) of isodecylglyceryl per 100 parts by weight of sodium alkyl sulfate
  • a mixture consisting of 90% by weight of ether and 10% by weight of water or 20 parts by weight (Examples 9, 10) of 90% by weight of 2-ethylhexyl glyceryl ether and 10% by weight of water was added, and the temperature 60 The mixture was mixed at 1 ° C. for 1 minute to obtain an anionic surfactant composition.
  • Each granulated product obtained by the above operation is prepared by using 4.2 parts by weight of crystalline silicate and 23. It was added to a plastic bag containing 1 part by weight. The plastic bag was shaken 30 times up and down to modify the surface of the granulated product (mixture), and each detergent particle group was obtained.
  • Comparative Examples 3-5 Provides (C)> Anion comprising 75% by weight of sodium alkyl sulfate and 25% by weight of water with respect to 100 parts by weight (50 g) of the non-spray-dried base granules (b-1) or (b-2) produced in Production Example 2 or 3. 29.5 parts by weight of surfactant paste (Comparative Example 3), 31.5 parts by weight (Comparative Example 4) and 44.1 parts by weight (Comparative Example 5) were added and mixed for 10 minutes using a spatula. Each mixture was obtained. When the obtained mixture was observed, no liquid was observed in any of the mixtures, but many aggregates were observed.
  • Each granulated product obtained by the above operation is used with 100 parts by weight of the non-spray-dried base granule group (b-1) or (b-2), 4.2 parts by weight of crystalline silicate, and 23. of zeolite. It was added to a plastic bag containing 1 part by weight. The plastic bag was shaken 30 times up and down to modify the surface of the granulated product (mixture), and each detergent particle group was obtained.
  • Table 2 shows the physical properties and the like of the detergent particles obtained in Examples 7 to 10 and Comparative Examples 3 to 5.
  • Table 1 summarizes the results using the spray-dried base granule group (a). From Table 1, as compared with those of Comparative Examples 1 and 2, all of the detergent particle groups obtained in Examples 1 to 6, the coarse particle ratio, the difference in the coarse particle ratio of the detergent particle group, the degree of particle growth, It can be seen from the observation results of the obtained detergent particles that the solubility and detergency are good that the detergent particles having few aggregates can be produced by the production method of the present invention. From comparison between Examples 1 to 6 and Comparative Example 2, it was found that the predetermined effect was not exhibited simply by mixing nonionic surfactant (polyoxyethylene alkyl ether in Comparative Example 2) and anionic surfactant paste. It was found that a predetermined effect was exhibited for the first time by using an alkyl glyceryl ether as defined in the present application.
  • Table 2 summarizes the results using the non-spray-dried base granule group (b-1) or (b-2). From Table 2, the detergent particle groups obtained in Examples 7 to 10 were compared with those in Comparative Examples 3 to 5, all of the coarse particle ratio, the difference in the coarse particle ratio of the detergent particle group, the degree of particle growth, It can be seen from the observation results of the obtained detergent particles that the solubility and detergency are good that the detergent particles having few aggregates can be produced by the production method of the present invention.
  • the non-spray-dried base granule group (b-1) or (b-2) tended to have a higher coarse particle ratio than the spray-dried base granule group (a), but such (b-1) Or even if it was a case where (b-2) was used, it turned out that the coarse particle rate raise difference of a detergent particle group is small. From this, according to the manufacturing method of this invention, it was shown that the detergent particle group by which the raise of the coarse particle rate was suppressed irrespective of the difference in the coarse particle rate of the base granule group to be used can be manufactured.
  • the detergent particle group of the present invention has a sharp particle size distribution, few aggregates and excellent solubility, it can be suitably used, for example, for the production of clothing detergents and dishwasher detergents.

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Abstract

L'invention porte sur un procédé de production de particules de détergent qui comprend l'étape (B) consistant à mélanger une pâte de tensioactif anionique avec un oxyde d'alkyle et de glycéryle pour préparer une composition de tensioactif anionique et l'étape (C) consistant à mélanger la composition de tensioactif anionique préparée dans l'étape (B) avec des granulés de base ayant une absorption d'huile supérieure ou égale à 0,2 ml/g pour préparer les particules de détergent. L'utilisation du procédé a pour effet de permettre de produire des particules de détergent dont l'agglomération est empêchée et qui ont une étroite distribution du diamètre des particules, une solubilité élevée et un effet nettoyant élevé sans nécessiter une étape de séchage pour l'élimination d'eau après le mélange de la composition de tensioactif anionique avec les granulés de base ayant une absorption d'huile supérieure ou égale à 0,2 ml/g. En empêchant l'agglomération des particules et en conférant une étroite distribution de la taille des particules, on peut obtenir un détergent ayant non seulement un aspect amélioré mais également une excellente solubilité. En outre, la teneur des particules grossières dans les particules de détergent devant être produites peut être amenée à être faible indépendamment des différences de teneur en particules grossières dans les granulés de base.
PCT/JP2010/072344 2009-12-17 2010-12-13 Procédé de production de particules de détergent WO2011074522A1 (fr)

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WO2016191103A1 (fr) * 2015-05-22 2016-12-01 The Procter & Gamble Company Procédé de production de compositions tensioactives et de compositions détergentes comprenant de la glycérine alcoxylée en guise de solvant
US9932546B2 (en) 2015-05-22 2018-04-03 The Procter & Gamble Company Surfactant and detergent compositions containing propoxylated glycerine
US20180340136A1 (en) * 2015-05-22 2018-11-29 The Procter & Gamble Company Surfactant and detergent compositions containing ethoxylated glycerine

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JP5971753B2 (ja) * 2012-07-09 2016-08-17 花王株式会社 洗剤粒子の製造方法
JP2016069394A (ja) * 2014-09-26 2016-05-09 ライオン株式会社 粒状洗剤及びその製造方法並びに洗剤製品

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JP2009114395A (ja) * 2007-11-09 2009-05-28 Kao Corp 高嵩密度洗剤組成物
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JP4794946B2 (ja) * 2005-08-26 2011-10-19 花王株式会社 乳化液の製造方法
EP2277985A4 (fr) * 2008-05-19 2012-11-28 Kao Corp Amas de granulés portant un agent tensioactif
JP5326152B2 (ja) * 2008-05-27 2013-10-30 ライオン株式会社 粒状洗剤組成物

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JP2006137925A (ja) * 2004-10-14 2006-06-01 Kao Corp 単核性洗剤粒子群の製造方法
JP2009114395A (ja) * 2007-11-09 2009-05-28 Kao Corp 高嵩密度洗剤組成物
JP2010144045A (ja) * 2008-12-18 2010-07-01 Kao Corp 単核性洗剤粒子群の製造方法

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WO2016191103A1 (fr) * 2015-05-22 2016-12-01 The Procter & Gamble Company Procédé de production de compositions tensioactives et de compositions détergentes comprenant de la glycérine alcoxylée en guise de solvant
US9932546B2 (en) 2015-05-22 2018-04-03 The Procter & Gamble Company Surfactant and detergent compositions containing propoxylated glycerine
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US20180340136A1 (en) * 2015-05-22 2018-11-29 The Procter & Gamble Company Surfactant and detergent compositions containing ethoxylated glycerine
US20180340137A1 (en) * 2015-05-22 2018-11-29 The Procter & Gamble Company Surfactant and detergent compositions containing ethoxylated glycerine
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US10640733B2 (en) 2015-05-22 2020-05-05 The Procter & Gamble Company LLC Surfactant and detergent compositions containing ethoxylated glycerine

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JP5709302B2 (ja) 2015-04-30
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