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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
  • C11D17/065—High-density particulate detergent compositions
• • 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
  • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
  • C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
  • C11D1/146—Sulfuric acid esters
• • 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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/04—Water-soluble compounds
  • C11D3/10—Carbonates ; Bicarbonates

Definitions

• the present invention relates to a method for producing a high bulk density detergent particle group using a base granule group and a surfactant composition containing an anionic surfactant. Furthermore, this invention relates to the detergent composition formed by containing this detergent particle group.
• a production method including a step of supporting a liquid surfactant on a group of granules for supporting a surfactant.
• a group of granules for supporting a surfactant is required to have a high supporting ability for a liquid surfactant.
• the supporting ability required for the surfactant-supporting granule group is that a large amount of liquid surfactant can be supported (supporting capacity), and that the liquid surfactant once absorbed can be strongly retained inside the granules without causing stains ( It consists of two factors (bearing force).
• the loading capacity is required for blending a surfactant in an amount necessary for cleaning performance, and the loading capacity is used to suppress the liquid surfactant from causing stains, and the flowability of the powder detergent is reduced. And it is important in preventing the liquid surfactant from transferring to the container and its surface.
• powder detergents containing an anionic surfactant compound represented by the formula (1) as a surfactant have various disclosures so far with the aim of improving high cleaning activity and environmental friendliness.
• Patent Document 1 discloses detergent particles using a surfactant-supporting granule group for spray-drying a preparation containing a water-soluble inorganic salt and an anionic surfactant compound represented by the formula (1). The manufacturing method is disclosed. However, spray drying is essential for the production of this granule group, and a production method that does not use spray drying is required from the viewpoint of economy.
• Patent Document 2 discloses a method of continuously producing a detergent composition using a high-speed mixer / medium-speed mixer / dryer with a surfactant paste and a dried detergent material.
• Patent Document 3 discloses a method of continuously producing a detergent composition while recirculating fine particles of a surfactant paste and a dried detergent raw material with a high speed mixer / medium speed mixer / conditioning device.
• Patent Document 2 it is difficult to adjust the particle size in the production method of Patent Document 2, and the production method of Patent Document 3 uses a production method in which fine particles are recirculated in order to solve this problem, and is a production method with low productivity. . Therefore, there is a demand for a production method that can more easily obtain high-density detergent particles having a required particle size with a high yield.
• JP 2006-137925 A Japanese National Patent Publication No. 10-500716 Japanese National Patent Publication No. 10-506141
• the gist of the present invention is as follows.
• a method for producing detergent particles having a bulk density of 650 g / L or more including the following steps 1 to 3: Step 1: A step of mixing a powder raw material having an oil absorption capacity of 0.4 mL / g or more, Step 2: Adding water or an aqueous binder solution to the mixed powder obtained in Step 1, and preparing a base granule group with a low shear granulator, and Step 3: Base granule group obtained in Step 2, and A) component and b) component: a) The following formula (1): R—O—SO 3 M (1) (Wherein R represents an alkyl or alkenyl group having 10 to 18 carbon atoms, M represents an alkali metal atom or an amine), and b) 100 parts by weight of component a) above 25 to 70 parts by weight of water, Mixing with a surfactant composition containing [2] A detergent particle group obtained by the production method according to [1]; and
• the present invention uses a base granule group for supporting a surfactant composition obtained by a method not including spray drying, and a surfactant composition containing an anionic surfactant,
• the present invention relates to producing detergent particles having a high yield of high-density detergent particles having a required particle size. Furthermore, this invention relates to providing the detergent composition formed by containing this detergent particle group.
• the skin irritation is generally extremely high.
• a high-density detergent particle group having a small amount and a good biodegradability and a sharp particle size distribution with a high yield. Sharpening the particle size distribution not only improves the appearance, but also has an effect of efficiently obtaining a detergent that has good fluidity and excellent productivity.
• the base granule is a granule containing at least a powder raw material having an oil absorption capacity of 0.4 mL / g or more and water or an aqueous binder solution.
• it is a granule obtained by adding water or an aqueous binder solution to a powder mixture containing at least a powder raw material having an oil absorption capacity of 0.4 mL / g or more, and granulating with a low shear granulator, which has a liquid surface activity.
• It is a granule used for carrying an agent composition.
• the aggregate of the granules is called a base granule group.
• the detergent particles are particles containing a surfactant, a builder, and the like obtained by supporting a liquid surfactant composition on base granules, and the detergent particle group means an aggregate thereof.
• the detergent composition contains detergent particles and is optionally added separately from the detergent particles (for example, builder granules, fluorescent dyes, enzymes, fragrances, antifoams, bleaches, bleach activators) Etc.).
• Water-soluble means that the solubility in water at 25 ° C. is 0.5 g / 100 g or more, and water-insoluble means that the solubility in water at 25 ° C. is less than 0.5 g / 100 g.
• the liquid surfactant composition is a composition containing a surfactant that is liquid or pasty when supported on the base granule group, and contains an anionic surfactant represented by the formula (1). Things are also included.
• Powder raw material having an oil absorption capacity of 0.4 mL / g or more As an essential component in the present invention, a powder raw material having an oil absorption capacity of 0.4 mL / g or more can be mentioned.
• the oil absorption capacity of raw materials, base granule groups and the like is a value determined by the method described in the quality evaluation method described later.
• the powder raw material having an oil absorption capacity of 0.4 mL / g or more is an essentially porous substance having fine pores of 10 ⁇ m or less inside the powder, and a surfactant is supported on the pores. It is a substance that can.
• the upper limit of the oil absorption capacity is not particularly limited, but is desirably 1.0 mL / g or less, for example.
• a powder raw material may be composed of one component, or may be composed of a plurality of components.
• a mixed powder is prepared by carrying out step 1 of mixing such powder raw materials.
• the average particle size of the powder raw material is preferably 50 to 250 ⁇ m, more preferably 50 to 200 ⁇ m, still more preferably 80 to 200 ⁇ m.
• solubility it is preferably a water-soluble substance.
• powder raw materials include soda ash (for example, light ash or dense ash) prepared by baking sodium bicarbonate, sodium sulfate, porous powder prepared by drying trihydrate of sodium tripolyphosphate, and the like.
• soda ash for example, light ash or dense ash
• porous powder prepared by drying trihydrate of sodium tripolyphosphate, and the like.
• Light ash is preferable from the viewpoint of ease of handling and availability.
• the ability to support the surfactant can be further improved by adjusting the temperature during baking baking soda.
• the firing temperature is preferably 120 to 250 ° C, more preferably 150 to 220 ° C, and even more preferably 150 to 200 ° C.
• the content of the powder raw material is preferably 40 to 95% by weight, more preferably 45 to 90% by weight, still more preferably 50 to 85% by weight, and more preferably 50 to 80% by weight in the base granule group from the viewpoint of supporting ability. % Is more preferable.
• the granule group before the drying step is preferably 25 to 80% by weight, more preferably 30 to 77% by weight, still more preferably 32 to 77% by weight, More preferred is 32 to 73% by weight.
• Binder In the present invention, water or an aqueous binder solution is added to the mixed powder, and the mixed powder is granulated by using a low shear granulator to prepare a base granule group.
• a clay mineral As one component of the powder raw material, a mixture of the clay mineral and a powder raw material other than the clay mineral is granulated.
• the caking property generated by partly dissolving the powder raw material in water or the caking property of clay mineral is used for granulation.
• an aqueous binder solution since the caking property due to the binder can be further utilized, granulation becomes easier.
• a drying step when water is used, there is a concern that the particle strength may decrease with drying, but when an aqueous binder solution is used, the effect of the binder can be expected even after drying. Therefore, it is preferable to use a binder aqueous solution.
• the binder is not particularly limited as long as it has an ability to bind the components constituting the particles in the powder raw material and has a property of rapidly dissolving and / or dispersing in water.
• 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 1000 to 100,000, more preferably 2000 to 80000.
• the content of the binder in the base granule group is preferably 0 to 35% by weight, more preferably 5 to 30% by weight, and further preferably 8 to 20% by weight in the base granule group from the viewpoints of caking property and oil absorption capacity. Preferably, 10 to 20% by weight is more preferable.
• 0 to 30% by weight is preferable in the granule group before the drying step, more preferably 3 to 25% by weight, still more preferably 5 to 17% by weight, 7 to 17% by weight is more preferable.
• the concentration of the aqueous binder solution is not particularly limited, but the particle size at the time of granulation is greatly affected by the volume of the aqueous binder solution, so the concentration may be determined from the required binder amount and the desired granule particle size.
• Clay minerals have a layered structure and can carry a liquid surfactant between the layers. Therefore, by blending clay mineral as one component of the powder raw material, the carrying capacity of the liquid surfactant can be increased and at the same time the carrying power can be improved.
• the particle size of the base granule can be controlled by adjusting the blending amount.
• clay minerals examples include talc, pyrophyllite, smectite (saponite, hectorite, saconite, stevensite, montmorillonite, beidellite, nontronite, etc.), vermiculite, mica (phlogopite, biotite, chinwald mica, etc.) , Muscovite, paragonite, ceradonite, sea chlorite, etc.), chlorite (clinochlore, chamosite, nimite, pennite, sudowite, dombasite, etc.), brittle mica (clinentite, margarite, etc.), sulite, serpentine mineral ( Antigolite, lizardite, chrysotile, amicite, clonstedite, burcherin, greenerite, garnierite, etc.) and kaolin minerals (kaolinite, dickite, nacrite, halloysite, etc.).
• smectite saponite,
• talc talc
• smectite swellable mica
• vermiculite vermiculite
• chrysotile kaolin mineral, and the like
• smectite is more preferable
• montmorillonite is further preferable in terms of flexibility. These may be used alone or in appropriate combination of two or more.
• Examples of the clay mineral represented by the general formula (A) include “Round rosyl DGA212”, “Round rosyl PR414”, “Round rosyl DG214”, “Round rosyl DGA powder”, “EXM0242”, “Hulasoft-1” manufactured by Zude Chemi. Examples thereof include “powder”, “Detasoft A”, “Detasoft GIS”, “Detasoft GIB”, “Detasoft GISW” manufactured by Raviossa, and pure bentonite, standard bentonite, and premium bentonite manufactured by CSM.
• there are granulated granule types added with a binder component which may be added as long as the effects of the present invention are not impaired. .
• the clay minerals listed above are used in the present invention, those in the form of powder are preferable from the viewpoint of granulation, and in the case of a granulated product, it is preferable to crush in advance until a suitable particle size is obtained.
• the crusher that can be used for crushing include impact crushers such as hammer crushers, impact crushers such as atomizers and pin mills, and shear crushers such as flash mills. These may be a single-stage operation or a multi-stage operation of the same or different pulverizers.
• the average particle size of the clay mineral powder is preferably 100 ⁇ m or less, more preferably 50 ⁇ m or less, and even more preferably 30 ⁇ m or less.
• the clay mineral represented by the general formula (A) is composed of a total of alkali metal ions (Na ions, K ions, Li ions) and alkaline earth metal ions (Ca ions, Mg ions).
• Total molar ratio [(Na + K + Li) / (Ca + Mg)] is preferably 1.0 or more, more preferably 1.5 or more, and still more preferably 2.0 or more.
• a clay mineral having a high ratio of alkali metal ions it is only necessary to select a production area if it is a natural product, and it can also be prepared by adding an alkali metal salt when producing a clay granulated product. . Moreover, if it is a synthetic product, it can be arbitrarily prepared by a known method.
• the base granule group in the present invention contains an appropriate amount of moisture used in the production process.
• the water content measured with an infrared moisture meter is preferably smaller from the viewpoint of increasing the capacity of the granule group to carry the surfactant composition, preferably 15% by weight or less, more preferably 10% by weight or less, Preferably it is 5 weight% or less.
• the base granule group in the present invention even substances other than those listed in the above 1 to 4 can be appropriately blended as necessary.
• the blending amount of these substances is preferably 20% by weight or less, more preferably 10% by weight or less, and more preferably 5% by weight or less from the viewpoint of supporting ability. Examples of substances that can be blended are shown below.
• the water-soluble chelating agent is not particularly limited as long as it is a substance that retains sequestering ability, but crystalline silicate, tripolyphosphate, orthophosphate, pyrophosphate and the like can be used. Among these, crystalline silicate and tripolyphosphate are preferable.
• the water-insoluble chelating agent preferably has an average particle diameter of 0.1 to 20 ⁇ m from the viewpoint of dispersibility in water. Suitable water-insoluble chelating agents include crystalline aluminosilicates, such as A-type zeolite, P-type zeolite, and X-type zeolite. A-type zeolite is preferable in terms of sequestering ability and economy. .
• an alkali metal salt having a sulfate group and a sulfite group, an ammonium salt, and the like can be given.
• sodium sulfate, sodium sulfite, or potassium sulfate having a high degree of ion detachment is preferable.
• the combined use with magnesium sulfate is also preferable.
• Water-insoluble excipient No particular limitation is imposed on the substance as long as it has good dispersibility in water and does not adversely affect detergency. Examples thereof include crystalline or amorphous aluminosilicates, silicon dioxide, hydrated silicate compounds, and the like. From the viewpoint of dispersibility in water, the primary particles preferably have an average particle size of 0.1 to 20 ⁇ m.
• Fluorescent dyes, pigments, dyes, etc. are listed.
• the measurement of the average particle diameter of the said component can be measured by the method as described in the measuring method of the physical property mentioned later.
• the method for producing detergent particles of the present invention includes the following steps 1 to 3.
• a base granule group is prepared through Step 1 and Step 2, and a detergent particle group is prepared through Step 3.
• the base granule group in the present invention does not include a spray drying step, at least a step of stirring or mixing a powder raw material having an oil absorption capacity of 0.4 mL / g or more, and adding water or an aqueous binder solution to the obtained mixed powder, It can be prepared by a method including a step of granulating with a low shear granulator.
• Process 1 In the step of mixing powder raw materials having an oil absorption capacity of 0.4 mL / g or more, any method may be used as long as they can be mixed substantially uniformly.
• the low shear granulator used in step 2 may be used for mixing, or may be mixed in advance using another mixer and then transferred to the low shear granulator.
• the other mixer used for powder mixing include a drum mixer, a bread mixer, a ribbon mixer, a nauter mixer, a Shugi mixer, a Redige mixer, and a high speed mixer.
• the content of the clay mineral is preferably 0 to 45% by weight, more preferably 0 to 40% by weight, and further preferably 0 to 35% by weight in the base granule group from the viewpoint of supporting ability and particle size control.
• 0 to 30% by weight is more preferable.
• 0 to 40% by weight is preferable in the granule group before the drying step. Is more preferably from 35 to 35% by weight, still more preferably from 0 to 30% by weight, and even more preferably from 0 to 25% by weight.
• the weight ratio of the clay mineral to the powder raw material is preferably 0/1 to 0/30, more preferably 0/1 to 0/20, and still more preferably 0/2 to 0/20.
• Process 2 In this step, water or an aqueous binder solution is added to the mixed powder obtained in step 1, and a base granule group is prepared by a low shear granulator. In this process, granules having a structure in which powder raw materials are gradually aggregated are generated. Also, step 1 and step 2 can be performed simultaneously.
• the low-shear granulator used in this step may be an apparatus that gives strong shear to the granules and does not greatly compact.
• the granule of the present invention can be controlled by setting the number of rotations and the fluid number described below to a low level to suppress compaction.
• the low shear granulator is preferably a container rotary granulator in which granulation proceeds by rotation of the main body from the viewpoint of easy granulation and improved carrying ability, and among them, a bread granulator or drum A mold granulator is more preferable.
• These apparatuses can be used in both batch and continuous processes. From the viewpoint of powder mixing property and solid-liquid mixing property, it is preferable to provide a baffle plate for assisting mixing in the pan or drum.
• the fluid number of the granulator defined by the following formula is 1.0 or less from the viewpoint of supporting ability, and 0.8 or less. More preferably, 0.6 or less is still more preferable, and 0.4 or less is more preferable.
• Fr V 2 / (R ⁇ g)
• V Circumferential speed [m / s]
• R Radius from the center of rotation to the circumference of the rotating object [m]
• g Gravity acceleration [m / s 2 ]
• the fluid number of the granulator is 0.001 or more, more preferably 0.005 or more, still more preferably 0.01 or more, 0 .05 or more is even more preferable.
• V and R use the value of the main shaft, and a bread granulator or a drum granulator in which granulation proceeds by rotation of the body barrel.
• the values of the body trunk are used for V and R.
• V and R use values of the crushing blade.
• water or an aqueous binder solution with uniform dispersion it is preferable to add water or an aqueous binder solution with uniform dispersion.
• a method therefor for example, there is a method of refining such a liquid component using a multi-fluid nozzle such as a one-fluid nozzle or a two-fluid nozzle.
• a multi-fluid nozzle is a nozzle that circulates a liquid component and atomizing gas (air, nitrogen, etc.) to the vicinity of the nozzle tip through an independent flow path, and mixes and atomizes it.
• a liquid component and atomizing gas air, nitrogen, etc.
• a four-fluid nozzle or the like can be used.
• the mixing part of the liquid component and the 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.
• a multi-fluid nozzle for example, a wide-angle round type two-fluid nozzle (manufactured by Spraying Systems Japan Co., Ltd.), a full cone type two-fluid nozzle (manufactured by Atmax Co., Ltd.), a four-fluid nozzle ( Fujisaki Electric Co., Ltd.) can be used.
• an operation of drying the obtained base granule group may be further performed.
• voids in the particles constituting the base granule group are increased, and the carrying capacity of the base granule group can be further improved.
• a drying method that gives as much strong shearing force as possible is preferable.
• the batch type there are a method of putting in a container and drying with an electric dryer or a hot air dryer, a method of drying in a batch type fluidized bed, etc., and in a continuous type, a fluidized bed, a rotary dryer, a steam tube dryer, etc. Is mentioned.
• the drying temperature is preferably 80 ° C. or higher, more preferably 120 ° C. or higher, further preferably 150 ° C. or higher, and more preferably 180 ° C. or higher from the viewpoint of the drying speed.
• 300 degrees C or less is preferable, 250 degrees C or less is more preferable, and 220 degrees C or less is more preferable.
• the base granule group in the present invention is a granule group having a structure in which powder raw materials having an oil absorption capacity of 0.4 mL / g or more are gradually aggregated. Therefore, it has two supporting sites: (1) a large gap between powder raw materials, and (2) a small gap (for example, a gap of 10 ⁇ m or less) in the powder raw material. Of these, both (1) and (2) have a great influence on the carrying capacity and carrying force, and (1) has a great influence on the carrying speed, and a group of base granules having a desired carrying capacity by adjusting these two carrying sites. Can be obtained.
• liquid surfactant composition when a clay mineral is blended, the liquid surfactant composition can be supported between the layers, so that the supporting ability is expected to be improved.
• the bulk density of the base granule group in the present invention is 400 to 550 g / L from the viewpoint of securing the carrying capacity of the liquid surfactant composition and securing the high bulk density after loading the liquid surfactant composition. Is preferable, and 400 to 500 g / L is more preferable.
• the relatively low bulk density of the base granule group in the present invention is considered to be achieved by granulating with the low shear granulator described above.
• the average particle diameter of the base granule group is: 140 to 600 ⁇ m is preferable, 200 to 500 ⁇ m is more preferable, and 200 to 400 ⁇ m is still more preferable.
• the oil absorption capacity of the liquid surfactant composition of the base granule group is preferably 0.4 mL / g or more, more preferably 0.45 mL / g or more, from the viewpoint of increasing the allowable range of the liquid surfactant composition content. More preferably, it is 0.5 mL / g or more. It is considered that the relatively high oil absorption capacity of the base granule group in the present invention is achieved by granulating with the low shear granulator described above.
• the bulk density, average particle size, oil absorption capacity and water content of the liquid surfactant composition can be measured by the methods described in the physical property measurement method described later.
• R—O—SO 3 M In the formula of the anionic surfactant represented by the formula, R is an alkyl or alkenyl group having 10 to 18 carbon atoms, preferably 12 to 16 carbon atoms. M is preferably an alkali metal atom such as Na or K, or an amine such as monoethanolamine or diethanolamine, and Na or K is preferred from the viewpoint of improving the detergency of the detergent composition.
• a surfactant composition comprising an anionic surfactant represented by the formula (1) and a predetermined amount of water is used in the temperature range of use of the surfactant composition from the viewpoint of handling in production. It is desirable that the surfactant composition has a temperature range in which the viscosity is 10 Pa ⁇ s or less, preferably 5 Pa ⁇ s or less. Such a temperature range is preferably up to 70 ° C., more preferably up to 60 ° C., from the viewpoint of the stability of the surfactant composition.
• the viscosity is determined by measuring at a shear rate of 50 [1 / s] with a coaxial double cylindrical rotational viscometer (manufactured by HAAKE, sensor: SV-DIN).
• the viscosity of the surfactant composition used in Step 3 varies greatly depending on its water content.
• the water content of the alkali compound used is adjusted to have a desired moisture content, that is, a desired composition. It is preferable to prepare a surfactant composition having a viscosity.
• the surfactant composition contains 25 to 70 parts by weight of water (the water content of the surfactant composition is about 20 to 40%) with respect to 100 parts by weight of component a), the viscosity decreases.
• the range of the amount of water in the surfactant composition is preferably 30 to 70 parts by weight, more preferably 35 to 65 parts by weight with respect to 100 parts by weight of component a) from the viewpoint of handling.
• the acid precursor of component a) is very unstable and easily decomposes, it is preferably prepared so that the decomposition can be suppressed.
• the adjustment method is not particularly limited, and a known method can be used. For example, using a loop reactor, the heat of neutralization is removed by a heat exchanger or the like, and the temperature control of the component acid precursor and the surfactant composition may be performed carefully. The temperature range during production includes 30 to 60 ° C., and the storage temperature range after production includes 60 ° C. or less. In use, the surfactant composition may be used after raising the temperature as necessary.
• this obtained anionic surfactant composition has excess alkalinity from a viewpoint of suppressing decomposition
• the surfactant composition used in Step 3 includes a) an unreacted alcohol or unreacted polyoxyethylene alkyl ether when the acid precursor of component is produced, and mirabilite, which is a by-product during the neutralization reaction.
• a pH buffer, a decoloring agent, and the like that can be added during the neutralization reaction may be contained.
• the content of the component a) in the detergent particles obtained in the present invention is preferably in the range of 10 to 45% by weight and more preferably 15 to 40% by weight from the viewpoint of detergency and solubility.
• the component a) can be used alone as the surfactant, but a nonionic surfactant can also be mixed and used.
• a nonionic surfactant having a melting point of 30 ° C. or lower when used, a water-soluble nonionic organic substance having a melting point of 45 to 100 ° C. and a molecular weight of 1,000 to 30,000 has an effect of increasing the melting point of the surfactant. It is preferable to use a compound (hereinafter referred to as a melting point increasing agent) or an aqueous solution thereof together.
• Examples of the melting point raising agent that can be used in the present invention include polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether, and pluronic-type nonionic surfactant. Further, amphoteric surfactants and cationic surfactants can be used in combination for the purpose. Further, from the viewpoint of improving the dispersibility of the detergent particles in low-temperature water, anions other than the anionic surfactant represented by the formula (1), such as polyoxyethylene alkyl ether sulfate and alkylbenzene sulfonate The surfactant can be used in the detergent particle group in the range of 0 to 10% by weight, more preferably 0 to 5% by weight, still more preferably 0 to 3% by weight.
• the surfactant composition in Step 3 may contain a nonionic surfactant and / or an anionic surfactant other than the anionic surfactant represented by the formula (1).
• the amount of such component in the detergent particle group is preferably 0.1 to 10% by weight, more preferably 0.2 to 5% by weight, and further preferably 0.5 to 3% by weight.
• a fatty acid salt can be used in combination.
• nonionic surfactant examples include polyoxyethylene alkyl or alkenyl ether, polyoxyethylene alkyl or alkenyl phenyl ether, polyoxyethylene polyoxypropylene alkyl or alkenyl ether, and polyoxyethylene polyoxypropylene glycol represented by trademark Pluronic , Polyoxyethylene alkylamine, higher fatty acid alkanolamide, alkyl glucoside, alkyl glucose amide, alkyl amine oxide and the like. Among them, those having a high hydrophilicity and those having a low ability to form a liquid crystal produced when mixed with water or those which do not produce a liquid crystal are preferable, and polyoxyalkylene alkyl or alkenyl ether is more preferable.
• EO ethylene oxide
• PO propylene oxide
• PO propylene oxide
• R represents a hydrocarbon group, preferably an alkyl group or an alkenyl group
• EO represents an oxyethylene group
• PO represents an oxypropylene group
• X, Y and Z represent the average number of moles added, respectively.
• the more preferable average added mole number relationship is X> 0, Z> 0, X + Y +
• the blending amount of the nonionic surfactant in the detergent particle group is preferably 0 to 10% by weight in the detergent particle group from the viewpoints of improvement in detergency, improvement in caking resistance, and suppression of waste during powdering. %, More preferably 0 to 5% by weight, still more preferably 0 to 3% by weight.
• a powder raw material other than the powder raw material may be added as desired.
• the addition amount is 0 to 150 parts per 100 parts by weight of the granule group. Part by weight is preferred.
• the powder raw material include crystalline silicates such as aluminosilicate and prefeed (manufactured by Tokuyama Siltech Co., Ltd.).
• a detergent particle group having predetermined characteristics can be obtained by the production method of the present invention.
• the detergent particle group obtained by the production method of the present invention is also included in the present invention.
• Preferred physical properties of the detergent particles according to the present invention are as follows.
• Bulk density is 650 g / L or more, preferably 650 to 1000 g / L, more preferably 650 to 950 g / L, and further preferably 650 to 900 g / L.
• the average particle diameter is preferably 150 to 600 ⁇ m, more preferably 180 to 550 ⁇ m, and still more preferably 250 to 500 ⁇ m.
• the said bulk density and an average particle diameter can be measured by the method as described in the measuring method of the below-mentioned physical property.
• the Rosin-Rammler number can be used as an index of a preferable particle size distribution of the detergent particle group according to the present invention.
• the following formula is used to calculate the Rosin-Rammler number.
• n is preferably 1.0 or more, more preferably 1.3 or more, more preferably 1.5 or more, still more preferably 1.8 or more, and still more preferably 2.0 or more.
• the proportion of particles having a sieve opening of 250 to 500 ⁇ m is preferably 35% or more, more preferably 40% or more, more preferably 45% or more, and still more preferably. It is 50% or more, more preferably 60% or more.
• the ratio of the particles having a sieve opening of 125 to 500 ⁇ m is preferably 45% or more, more preferably 50% or more, more preferably 55% or more, still more preferably 60% or more, and still more preferably 70% or more. is there.
• the water content of the detergent particles in the present invention is preferably smaller from the viewpoint of high blending of the component a). Specifically, when the moisture content of the detergent particles is measured with an infrared moisture meter, the moisture content is preferably 20% by weight or less, more preferably 15% by weight or less, still more preferably 10% by weight or less, and more preferably 5% by weight. The following is even more preferable.
• a suitable production method for obtaining the detergent particle group includes the following step 3, and may further include step 4 or step 5 as necessary.
• Process 3 This step is a step of mixing the base granule group obtained in Step 2 with the surfactant composition containing the following components a) and b).
• component a) is an anionic surfactant represented by the formula (1)
• component b) is 25 to 70 parts by weight, preferably 100 parts by weight of component a). Is 25 to 65 parts by weight of water.
• the base granule group obtained by the process 2 should just be used at least. That is, in this step, other granule groups having the ability to carry a surfactant, for example, granule groups obtained by other methods such as spray drying may be used in combination with the base granule group. In addition, when using together, the mixture of the said base granule group and the granule group obtained by the other method can be handled as a base granule group.
• the ratio of the base granule group in the base granule group is preferably 50% by weight or more, more preferably 70% by weight or more, and still more preferably 90% by weight or more from the viewpoint of oil absorption.
• the surfactant composition is supported on the base granules by mixing the base granules and the surfactant composition.
• a method of mixing the base granule group and the surfactant composition using a batch type or continuous type mixer is as follows: (1) First, the base granule group is charged into the mixer, and then the surfactant composition is added. (2) The base is added to the mixer. Repeat the addition of the granule group and the surfactant composition little by little. (3) After charging a part of the base granule group into the mixer, the remaining base granule group and the surfactant composition are added in small quantities. A method such as repeating the addition can be employed.
• the rate of addition becomes more important as the amount of the surfactant composition is increased.
• the addition rate of the surfactant composition is not more than the oil absorption rate of the base granule group.
• the specific addition rate of the surfactant composition is preferably 35 parts by weight or less, more preferably 20 parts by weight or less, and still more preferably 10 parts by weight with respect to 100 parts by weight of the base granule group. / Min or less, more preferably 7.5 parts by weight / min or less.
• the amount of the surfactant composition added to the base granule group is preferably, for example, 30 to 100 parts by weight with respect to 100 parts by weight of the base granule group. From the viewpoint of detergency, it is preferably 30 parts by weight or more, more preferably 40 parts by weight or more, and still more preferably 50 parts by weight or more with respect to 100 parts by weight of the base granule group. Moreover, from a soluble viewpoint, 100 weight part or less is preferable with respect to 100 weight part of base granule groups, 80 weight part or less is more preferable, and 60 weight part or less is still more preferable.
• preferable mixing apparatuses include the following.
• the following (1) to (3) are preferable.
• Henschel mixer manufactured by Mitsui Miike Chemical Co., Ltd.
• high speed mixer manufactured by Fukae Kogyo Co., Ltd.
• vertical granulator manufactured by Paulek, Inc.
• Redige mixer manufactured by Matsuzaka Giken Co., Ltd.
• Proshear mixer manufactured by Taiheiyo Kiko Co., Ltd.
• the mixing apparatus described in JP-A-10-296064 and the mixing apparatus described in JP-A-10-296065 are preferable because the moisture and temperature of the mixture can be adjusted by aeration to suppress the collapse of the base granule group.
• a mixing device such as a Nauter mixer, SV mixer, or ribbon mixer that can mix powder and liquid without giving a strong shearing force is also preferable because it can suppress the collapse of the base granule group.
• the base granule group and the surfactant composition may be mixed using a continuous apparatus.
• the continuous apparatus include a flexographic type (manufactured by POWREC Co., Ltd.), a turbulator (manufactured by Hosokawa Micron Co., Ltd.), and the like.
• the melting point raising agent or this aqueous solution is added to the surfactant composition before the addition of the surfactant composition and simultaneously with the addition of the surfactant composition. It is preferable to add in the middle of the addition of the surfactant composition, after the addition of the surfactant composition, or in advance mixed with the surfactant composition.
• the melting point increasing agent it is possible to suppress the caking property of the detergent particle group and the bleed-out property of the surfactant in the detergent particle group.
• fusing point raising agents the same thing as what was illustrated in the melting point raising agent of the composition of the above-mentioned detergent particle group can be used.
• the amount of the melting point raising agent used is preferably 0.5 to 8 parts by weight, more preferably 0.5 to 5 parts by weight, and still more preferably 1 to 3 parts by weight with respect to 100 parts by weight of the base granule group. This range is preferable from the viewpoint of suppression of aggregation between detergent particles contained in the detergent particle group, high-speed solubility, and suppression of spotting and caking properties.
• As a method for adding the melting point increasing agent mixing with a surfactant in advance by an arbitrary method, or adding a melting point increasing agent after the addition of the surfactant is effective for the detergent particles to cause stains and caking properties. It is advantageous for suppression.
• the temperature in the mixer in this step is preferably adjusted so that the decomposition of the anionic surfactant can be suppressed.
• the temperature range during production is preferably 30 to 60 ° C.
• the storage temperature range after production is Is preferably 60 ° C. or lower.
• the batch mixing time for obtaining a suitable detergent particle group and the average residence time in continuous mixing are preferably 1 to 30 minutes, more preferably 2 to 25 minutes, and even more preferably 3 to 20 minutes.
• step 3 the base granule group and the surfactant composition may be mixed under aeration. More specifically, in step 3, an operation of blowing a gas such as air into the mixing tank of the mixing device during the addition and / or mixing of each raw material can be mentioned. By performing such an operation, the base granule group can further carry the surfactant composition, and the obtained detergent particle group has a higher composition of the surfactant composition.
• the temperature of the blown gas is preferably 10 to 65 ° C., more preferably 30 to 60 ° C., and further preferably 50 to 60 ° C.
• the blown amount is preferably 1 to 15 parts by weight / minute, more preferably 2 to 10 parts by weight / minute, and further preferably 3 to 8 parts by weight / minute with respect to 100 parts by weight of the detergent particles.
• a powdery surfactant and / or a powder builder before, simultaneously with, during or after the addition of the surfactant composition.
• a powder builder By adding a powder builder, the particle diameter of the detergent particles can be controlled, and the cleaning power can be improved.
• an acid precursor of an anionic surfactant it is more effective from the viewpoint of promoting the neutralization reaction to add an alkaline powder builder before adding the acid precursor.
• the term “powder builder” as used herein means a powder detergency enhancer other than a surfactant.
• a base that exhibits sequestering ability such as zeolite and citrate, and sodium carbonate.
• a base exhibiting alkaline ability such as potassium carbonate
• a base having both sequestering ability and alkaline ability such as crystalline silicate
• other bases such as sodium sulfate that enhance ionic strength.
• crystalline silicate JP-A-5-279013, column 3, line 17 (preferably baked and crystallized at 500 to 1000 ° C.), JP-A-7-89712, column 2.
• the crystalline silicate described in line 45, JP-A-60-227895, page 2, lower right column, line 18 (silicates in Table 2 are preferred) can be used as a preferred powder builder.
• the alkali metal silicate having SiO 2 / M 2 O (where M represents an alkali metal) is preferably 0.5 to 3.2, more preferably 1.5 to 2.6. Used.
• the amount of the powder builder used is preferably 0 to 12 parts by weight, more preferably 0 to 6 parts by weight with respect to 100 parts by weight of the base granule group.
• the detergent powder builder has good solubility in this range.
• Step 4 A step of modifying the surface of the detergent particles obtained in Step 3 with a surface coating agent. However, in step 3, crushing may proceed simultaneously.
• Process 5 The process of drying the detergent particle group obtained at the process 3 or the process 4.
• Step 4 the particle surface of the detergent particle group obtained in step 3 is modified.
• the following step 4 of adding various surface coating agents such as (1) fine powder and (2) liquid material is performed as the form at the time of addition.
• the number of times of Step 4 may be one or more times.
• the surface of the detergent particles is modified with a surface coating agent, the fluidity and caking resistance of the detergent particles tend to be improved. Therefore, it is preferable to provide a surface modification step in the production method of the present invention.
• a surface modification step As an apparatus used at the process 4, the thing which comprised both the stirring blade and the crushing blade among the mixers illustrated at the process 3 is mentioned as a preferable apparatus.
• Each surface coating agent will be described below.
• Fine powder preferably has an average primary particle size of 10 ⁇ m or less, more preferably 0.1 to 10 ⁇ m. When the average particle size is within this range, the coverage of the detergent particle group on the particle surface is improved, which is preferable from the viewpoint of improving the fluidity and caking resistance of the detergent particle group.
• the average particle diameter of the fine powder is measured by a method using light scattering, for example, a particle analyzer (manufactured by Horiba, Ltd.), or measurement by microscopic observation. Furthermore, it is preferable from the viewpoint of detergency that the fine powder has high ion exchange ability and high alkali ability.
• Such fine powder may be composed of one component or a plurality of components.
• the fine powder is preferably an aluminosilicate and may be crystalline or amorphous.
• fine powders such as sodium sulfate, calcium silicate, silicon dioxide, bentonite, talc, clay, amorphous silica derivatives, and crystalline silicate are also preferable.
• a metal soap having an average primary particle size of 0.1 to 10 ⁇ m, a powdered surfactant (such as an alkyl sulfate) and a water-soluble organic salt can be used in the same manner.
• crystalline silicate it is preferable to use it by mixing with fine powder other than crystalline silicate for the purpose of preventing deterioration due to moisture absorption or aggregation of crystalline silicate due to carbon dioxide.
• the amount of fine powder used is preferably 0.5 to 40 parts by weight, more preferably 1 to 30 parts by weight, and still more preferably 2 to 20 parts by weight with respect to 100 parts by weight of the detergent particles. When the amount of the fine powder used is within this range, the fluidity is improved and the consumer feels good.
• liquid material examples include water-soluble polymers and fatty acids, which can be added in an aqueous solution or in a molten state.
• a liquid material may be composed of one component or may be composed of a plurality of components.
• water-soluble polymer examples include carboxymethyl cellulose, polyethylene glycol, sodium polyacrylate, a polycarboxylic acid salt such as a copolymer of acrylic acid and maleic acid or a salt thereof, and the like.
• the amount of the water-soluble polymer used is preferably 0 to 10 parts by weight, more preferably 0 to 8 parts by weight, and still more preferably 0 to 6 parts by weight with respect to 100 parts by weight of the detergent particles. When the amount of the water-soluble polymer used is within this range, a detergent particle group exhibiting good solubility, good fluidity, and caking resistance can be obtained.
• (2-2) Fatty acid examples include fatty acids having 10 to 22 carbon atoms.
• the amount of the fatty acid used is preferably 0 to 5 parts by weight, more preferably 0 to 3 parts by weight with respect to 100 parts by weight of the detergent particles. In the case of a solid at room temperature, it is preferable to spray and supply after heating to a temperature showing fluidity.
• Process 5 In this step, an operation of drying the obtained detergent particle group may be further performed. By performing such an operation, water derived from the surfactant composition or the like can be removed from the detergent particle group.
• This step is an optional step of drying the detergent particle group obtained in step 3 or step 4. By removing the water, the activator component in the detergent particle group can be improved.
• a drying method that gives as little shearing force as possible is preferable.
• a method of drying in an electric dryer or hot air dryer in a container a method of drying in a batch type fluidized bed, and the like are mentioned.
• a continuous type a fluidized bed, a rotary dryer, a steam tube dryer, etc. Is mentioned.
• the drying temperature is preferably 40 to 110 ° C., more preferably 50 to 100 ° C., and still more preferably 60 to 90 ° C., from the viewpoint of inhibiting the decomposition of the anionic surfactant and the drying speed.
• the detergent composition of the present invention is a composition comprising the above-described detergent particle group, and further contains detergent components (for example, builder granules, fluorescent dyes, enzymes, perfumes, odorants, etc.) separately added to the detergent particle group.
• detergent components for example, builder granules, fluorescent dyes, enzymes, perfumes, odorants, etc.
• the content of the detergent particles in the detergent composition is preferably 50% by weight or more, more preferably 60% by weight or more, further preferably 70% by weight or more, 80% by weight or more, 100% by weight or less from the viewpoint of detergency. Is even more preferable.
• the content of detergent components other than the detergent particles in the detergent composition is preferably 50% by weight or less, more preferably 40% by weight or less, still more preferably 30% by weight or less, and still more preferably 20% by weight or less.
• the method for producing the detergent composition is not particularly limited, and examples thereof include a method of mixing the detergent particle group and a separately added detergent component.
• the detergent composition thus obtained contains detergent particles with a large carrying capacity of a surfactant, and therefore can exhibit a sufficient cleaning effect even with a small amount.
• the use of such a detergent composition is not particularly limited as long as it is a use using a powder detergent, and examples thereof include a powder detergent for clothing and a detergent for automatic tableware.
• the bulk density is measured by a method defined by JIS K 3362.
• the bulk density of the base granule group is the bulk density after removing granules of 2000 ⁇ m or more
• the bulk density of the detergent particle group is the bulk density after removing particles of 1180 ⁇ m or more.
• the bulk density increase degree defined by the following formula can be used as an index indicating the oil absorption of the detergent particle group.
• the degree of increase in the bulk density of the detergent particle group is preferably 1.2 to 1.7, more preferably 1.3 to 1.6.
• Increase in bulk density (bulk density of detergent particles) / (bulk density of base granules)
• Average particle diameter is measured by the following two methods. (1) For media with an average particle size of 80 ⁇ m or more, use a JIS K 8801 standard sieve (mesh 2000 to 125 ⁇ m) for 5 minutes, and then calculate the median diameter from the weight fraction of the sieve mesh size. To do. More specifically, using a 9-stage sieve and a tray with a mesh opening of 125 ⁇ m, 180 ⁇ m, 250 ⁇ m, 355 ⁇ m, 500 ⁇ m, 710 ⁇ m, 1000 ⁇ m, 1400 ⁇ m, and 2000 ⁇ m, the top of the top is stacked in order from the small sieve.
• the average particle size of the base granule group is the average particle size after removing granules of 2000 ⁇ m or more
• the average particle size of the detergent particle group is the average particle size of all the particles.
• Rosin-Rammler number By the same method as the measurement of the average particle diameter, the weight of the particles remaining on each sieve and the saucer was measured, and the weight ratio of the particles on each sieve (opening Dp [ ⁇ m]) (Cumulative rate R (Dp) [ ⁇ m]) is calculated. Then, the slope n of the least square approximation line when log (log (100 / R (Dp))) is plotted against each logDp is defined as the Rosin-Rammler number.
• Moisture Moisture measurement is performed by infrared moisture meter method. That is, 3 g of a sample is placed on a sample dish having a known weight, and the base granule group is heated at 200 ° C. using an infrared moisture meter (FD-240 manufactured by Kett Science Laboratory Co., Ltd.). Heating is performed at 105 ° C., and when the weight change disappears for 30 seconds, the drying is finished. Then, the water content is calculated from the weight after drying and the weight before drying.
• infrared moisture meter FD-240 manufactured by Kett Science Laboratory Co., Ltd.
• the flow time is defined as the time required for 100 mL of powder to flow out from the bulk density measurement hopper defined by JIS K 3362.
• the flow time is preferably 10 seconds or less, more preferably 8 seconds or less, and even more preferably 7 seconds or less.
• the fluidity of the base granule group is the fluidity after removing granules of 2000 ⁇ m or more
• the fluidity of the detergent particle group is the fluidity after removing particles of 1180 ⁇ m or more.
• Oil absorption capacity 30-35 g of powder was put into an absorption measuring device (AS410, manufactured by Asahi Research Institute), and the driving blade 200r. p. m. Rotate with A liquid nonionic surfactant (Emulgen 108 manufactured by Kao Co., Ltd.) is dropped at a liquid supply rate of 4 mL / min to determine the point at which the maximum torque is obtained. The liquid addition amount at the point where the torque becomes 70% of the point where the maximum torque is reached is divided by the powder input amount to obtain the oil absorption capacity.
• AS410 absorption measuring device
• a liquid nonionic surfactant Emgen 108 manufactured by Kao Co., Ltd.
• the granule yield in the present invention indicates the weight ratio of the base granule in a specific particle size range in the obtained base granule group.
• the detergent yield in the present invention refers to the weight ratio of the detergent particle group between 250 and 500 ⁇ m or the weight ratio of the detergent particle group between 125 and 500 ⁇ m in the obtained detergent particle group.
• Base granule group 1 used in Examples 1 to 7 was produced by the following procedure.
• the physical properties of the obtained granule group 1 were a granule group having an average particle size of 336 ⁇ m and a bulk density of 486 g / L, and an oil absorption capacity of 0.48 mL / g.
• the yield of granules less than 2000 ⁇ m was 96%.
• Base granule group 2 used in Examples 8 to 13 was produced by the following procedure.
• the physical properties of the obtained granule group 2 were a granule group having an average particle size of 305 ⁇ m and a bulk density of 487 g / L, and an oil absorption capacity of 0.56 mL / g.
• the yield of granules less than 2000 ⁇ m was 94%.
• the second preparation liquid was supplied to a spray drying tower (counterflow type) with a pump, and sprayed at a spray pressure of 2.5 MPa from a pressure spray nozzle installed near the top of the tower.
• the high temperature gas supplied to the spray drying tower was supplied at a temperature of 200 ° C. from the bottom of the tower, and was discharged at 90 ° C. from the top of the tower.
• the resulting spray-dried granule group had a moisture content of 4% by weight, an average particle size of 304 ⁇ m, and a bulk density of 494 g / L.
• the obtained detergent particle group 1 has a water content of 0.6%, an average particle size of 353 ⁇ m, a Rosin-Rammler number of 1.65, a 250-500 ⁇ m detergent yield of 52%, a 125-500 ⁇ m detergent yield of 73%, a bulk density of 755 g / L, fluidity was 6.0 s.
• Example 2 Composition A was brought to 60 ° C. Next, 100 parts by weight of the obtained base granule group 1 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started. In addition, 60 degreeC warm water was poured through the jacket at 10 L / min. Thereto, 60 parts by weight of the composition A was added in 8 minutes. Further, one minute after the start of charging the composition A, blowing was started in the mixer.
• a Redige mixer Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket
• the main shaft stirrring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s
• the blowing conditions were a temperature of 60 ° C., and the blowing rate was 7.3 parts by weight / min with respect to 100 parts by weight of the detergent particle group. After completion of the above composition A addition, the mixture was stirred for 3 minutes, and the detergent particle group 2 was discharged.
• the obtained detergent particle group 2 has a moisture content of 9.2%, an average particle size of 376 ⁇ m, a Rosin-Rammler number of 2.04, a 250-500 ⁇ m detergent yield 61%, a 125-500 ⁇ m detergent yield 76%, and a bulk density of 696 g / L, fluidity was 5.5 s.
• Example 3 Composition A was brought to 60 ° C. Next, 100 parts by weight of the obtained base granule group 1 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started. In addition, 60 degreeC warm water was poured through the jacket at 10 L / min. Thereto, 60 parts by weight of the composition A was added in 8 minutes. Further, one minute after the start of charging the composition A, blowing was started in the mixer.
• a Redige mixer Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket
• the main shaft stirrring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s
• the blowing conditions were a temperature of 60 ° C., and the blowing rate was 7.3 parts by weight / min with respect to 100 parts by weight of the detergent particle group. After completion of the above composition A addition, the mixture was stirred for 3 minutes to discharge the detergent particle group, and dried at 100 ° C. for 2 hours using an electric dryer to discharge the detergent particle group 3.
• the obtained detergent particle group 3 has a water content of 0.5%, an average particle size of 374 ⁇ m, a Rosin-Rammler number of 2.10, a 250-500 ⁇ m detergent yield 61%, a 125-500 ⁇ m detergent yield 76%, a bulk density of 688 g / L, fluidity 5.9 s.
• Example 4 Composition A was brought to 60 ° C. Next, 100 parts by weight of the obtained base granule group 1 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started. In addition, 60 degreeC warm water was poured through the jacket at 10 L / min. Thereto, 96.7 parts by weight of the composition A was charged in 13 minutes. Further, one minute after the start of charging the composition A, blowing was started in the mixer. The blowing conditions were a temperature of 60 ° C.
• the resulting detergent particle group 4 has a moisture content of 0.3%, an average particle size of 447 ⁇ m, a Rosin-Rammler number of 1.81, 250-500 ⁇ m, a detergent yield of 47%, a 125-500 ⁇ m detergent yield of 57%, a bulk density of 716 g / L, fluidity 6.2 s.
• the resulting detergent particle group 5 has a water content of 0.5%, an average particle size of 411 ⁇ m, a Rosin-Rammler number of 2.40, a 250-500 ⁇ m detergent yield of 58%, a 125-500 ⁇ m detergent yield of 69%, and a bulk density of 562 g / L, fluidity was 6.0 s.
• the obtained detergent particle group 6 has a water content of 10.6%, an average particle size of 423 ⁇ m, a Rosin-Rammler number of 2.51, 250-500 ⁇ m, a detergent yield of 58%, a 125-500 ⁇ m detergent yield of 67%, a bulk density of 559 g / L, fluidity was 5.5 s.
• the resulting detergent particle group 7 has a water content of 0.4%, an average particle size of 410 ⁇ m, a Rosin-Rammler number of 2.38, a 250-500 ⁇ m detergent yield of 59%, a 125-500 ⁇ m detergent yield of 70%, a bulk density of 544 g / L, fluidity 5.9 s.
• the obtained detergent particle group 8 has a water content of 0.4%, an average particle size of 454 ⁇ m, a Rosin-Rammler number of 2.57, a 250-500 ⁇ m detergent yield, 53%, a 125-500 ⁇ m detergent yield, a bulk density of 565 g / L, fluidity 6.2 s.
• Comparative Example 5 A detergent particle group 9 was obtained in the same manner as in Example 1 except that light ash was used in place of the base granule group 1.
• the resulting detergent particle group 9 has a water content of 0.5%, an average particle size of 321 ⁇ m, a Rosin-Rammler number of 1.40, a 250-500 ⁇ m detergent yield of 42%, a 125-500 ⁇ m detergent yield of 71%, a bulk density of 627 g / L, fluidity 6.1 s.
• Comparative Example 6 A detergent particle group 10 was obtained in the same manner as in Example 2 using light ash instead of the base granule group 1.
• the resulting detergent particle group 10 has a water content of 9.7%, an average particle size of 291 ⁇ m, a Rosin-Rammler number of 0.92, a 250-500 ⁇ m detergent yield of 17%, a 125-500 ⁇ m detergent yield of 49%, and a bulk density of 761 g / L, fluidity 5.6 s.
• Comparative Example 7 A detergent particle group 11 was obtained in the same manner as in Example 3 using light ash instead of the base granule group 1.
• the resulting detergent particle group 11 has a moisture content of 0.7%, an average particle size of 278 ⁇ m, a Rosin-Rammler number of 0.90, a 250-500 ⁇ m detergent yield of 17%, a 125-500 ⁇ m detergent yield of 49%, and a bulk density of 712 g / L, fluidity 6.4 s.
• Comparative Example 8 A detergent particle group 12 was obtained in the same manner as in Example 4 using light ash instead of the base granule group 1.
• the resulting detergent particle group 12 has a moisture content of 0.3%, an average particle size of 728 ⁇ m, a Rosin-Rammler number of 1.29, a 250-500 ⁇ m detergent yield of 20%, a 125-500 ⁇ m detergent yield of 32%, a bulk density of 655 g / L, fluidity 6.7 s.
• Example 5 Composition A was brought to 60 ° C. Next, 100 parts by weight of the obtained base granule group 1 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started. In addition, 60 degreeC warm water was poured through the jacket at 10 L / min. Thereto, 60 parts by weight of the above composition A is charged in 2 minutes, and then stirred for 3 minutes to discharge the detergent particles, and dried at 105 ° C. for 2 hours using an electric dryer to discharge the detergent particles 13. did.
• a Redige mixer Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket
• the main shaft stirrring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s
• the resulting detergent particle group 13 has a water content of 0.5%, an average particle size of 508 ⁇ m, a Rosin-Rammler number of 1.89, a 250-500 ⁇ m detergent yield of 38%, a 125-500 ⁇ m detergent yield of 48%, a bulk density of 663 g / L, fluidity 6.3 s.
• Example 6 Composition A was brought to 60 ° C. Next, 100 parts by weight of the obtained base granule group 1 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started. In addition, 60 degreeC warm water was poured through the jacket at 10 L / min. Thereto, 60 parts by weight of the above composition A is charged in 4 minutes, and then stirred for 3 minutes to discharge the detergent particles, and dried at 105 ° C. for 2 hours using an electric dryer to discharge the detergent particles 14. did.
• a Redige mixer Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket
• the main shaft stirrring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s
• the resulting detergent particle group 14 has a moisture content of 0.7%, an average particle size of 475 ⁇ m, a Rosin-Rammler number of 1.63, a 250-500 ⁇ m detergent yield of 38%, a 125-500 ⁇ m detergent yield of 51%, a bulk density of 679 g / L, fluidity 5.9 s.
• Example 7 Composition A was brought to 60 ° C. Next, 100 parts by weight of the obtained base granule group 1 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started. In addition, 60 degreeC warm water was poured through the jacket at 10 L / min. Thereto, 60 parts by weight of the composition A was charged in 4 minutes. Further, one minute after the start of charging the composition A, blowing was started in the mixer. The blowing conditions were a temperature of 60 ° C.
• the resulting detergent particle group 15 has a moisture content of 0.4%, an average particle size of 353 ⁇ m, a Rosin-Rammler number of 1.88, a 250-500 ⁇ m detergent yield of 57%, a 125-500 ⁇ m detergent yield of 75%, and a bulk density of 687 g / L, fluidity 5.9 s.
• blowing was started in the mixer.
• the blowing condition was a temperature of 60 ° C., and the blowing rate was 7.5 parts by weight / min with respect to 100 parts by weight of the detergent particle group.
• stirring was performed for 3 minutes, and the detergent particle group 16 was discharged.
• the resulting detergent particle group 16 has a moisture content of 9.7%, an average particle size of 358 ⁇ m, a Rosin-Rammler number of 1.74, a 250-500 ⁇ m detergent yield of 48%, a 125-500 ⁇ m detergent yield of 71%, a bulk density of 665 g / L, fluidity 5.6 s.
• Example 9 60 parts by weight of Composition B and 5 parts by weight of sodium polyoxyethylene lauryl ether sulfate (Emalgen 270J, manufactured by Kao Corporation) were mixed (hereinafter referred to as “Composition C”) to 60 ° C.
• Composition C sodium polyoxyethylene lauryl ether sulfate
• 100 parts by weight of the obtained base granule group 2 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started.
• 60 degreeC warm water was poured through the jacket at 10 L / min.
• 65 parts by weight of the composition C was added in 8.7 minutes.
• blowing was started in the mixer.
• the blowing conditions were a temperature of 60 ° C., and the blowing rate was 7.3 parts by weight / min with respect to 100 parts by weight of the detergent particle group.
• the mixture was stirred for 3 minutes, and the detergent particle group 17 was discharged.
• the resulting detergent particle group 17 had a water content of 9.7%, an average particle size of 429 ⁇ m, a Rosin-Rammler number of 1.93, a 250-500 ⁇ m detergent yield of 44%, a 125-500 ⁇ m detergent yield of 59%, and a bulk density of 706 g / L, fluidity 6.3 s.
• Example 10 Composition C was brought to 60 ° C. Next, 100 parts by weight of the obtained base granule group 2 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started. In addition, 60 degreeC warm water was poured through the jacket at 10 L / min. Thereto, 65 parts by weight of the composition C was added in 8.7 minutes. Further, 1 minute after the start of charging the composition C, blowing was started in the mixer.
• a Redige mixer Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket
• the main shaft stirrring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s
• the blowing conditions were a temperature of 60 ° C., and the blowing rate was 7.3 parts by weight / min with respect to 100 parts by weight of the detergent particle group. After completion of the addition of the composition C, the mixture was stirred for 3 minutes to discharge the detergent particle group, and dried at 105 ° C. for 2 hours using an electric dryer to discharge the detergent particle group 18.
• the resulting detergent particle group 18 has a water content of 0.5%, an average particle size of 380 ⁇ m, a Rosin-Rammler number of 1.54, a 250-500 ⁇ m detergent yield of 42%, a 125-500 ⁇ m detergent yield of 64%, a bulk density of 706 g / L, fluidity 5.9 s.
• Example 11 60 parts by weight of Composition B and 10 parts by weight of sodium polyoxyethylene lauryl ether sulfate (Emulgen 270J, manufactured by Kao Corporation) were mixed (hereinafter referred to as “Composition D”) to 60 ° C.
• Composition D sodium polyoxyethylene lauryl ether sulfate
• 100 parts by weight of the obtained base granule group 2 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started.
• 60 degreeC warm water was poured through the jacket at 10 L / min.
• 70 parts by weight of the above composition D was charged in 9.3 minutes.
• blowing was started in the mixer.
• the blowing conditions were a temperature of 60 ° C. and a blowing rate of 7.1 parts by weight / min with respect to 100 parts by weight of the detergent particle group.
• the mixture was stirred for 3 minutes to discharge the detergent particles, and dried at 105 ° C. for 2 hours using an electric dryer to discharge the detergent particles 19.
• the resulting detergent particle group 19 has a water content of 0.6%, an average particle size of 421 ⁇ m, a Rosin-Rammler number of 1.56, a 250-500 ⁇ m detergent yield of 40%, a 125-500 ⁇ m detergent yield of 58%, a bulk density of 728 g / L, fluidity 5.7 s.
• Example 12 60 parts by weight of Composition B and 5 parts of polyoxyethylene lauryl ether (Emulgen 106 manufactured by Kao Corporation) were mixed (hereinafter referred to as “Composition E”) to 60 ° C.
• Composition E polyoxyethylene lauryl ether
• 100 parts by weight of the obtained base granule group 2 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started.
• 60 degreeC warm water was poured through the jacket at 10 L / min. Thereto was added 65 parts by weight of the composition E in 8.7 minutes.
• blowing was started in the mixer.
• the blowing conditions were a temperature of 60 ° C., and the blowing rate was 7.3 parts by weight / min with respect to 100 parts by weight of the detergent particle group.
• the mixture was stirred for 3 minutes, and the detergent particle group 20 was discharged.
• the resulting detergent particle group 20 has a moisture content of 9.0%, an average particle size of 435 ⁇ m, a Rosin-Rammler number of 1.86, a 250-500 ⁇ m detergent yield of 40%, a 125-500 ⁇ m detergent yield of 58%, and a bulk density of 700 g / L, fluidity 7.1s.
• Example 13 Composition E was brought to 60 ° C. Next, 100 parts by weight of the obtained base granule group 2 was put into a Redige mixer (Matsuzaka Giken Co., Ltd., capacity 20 L, with jacket), and the main shaft (stirring blade, rotation speed: 60 rpm, peripheral speed: 0). .9 m / s) was started. In addition, 60 degreeC warm water was poured through the jacket at 10 L / min. Thereto was added 65 parts by weight of the composition E in 8.7 minutes. Further, 1 minute after the start of charging the composition E, blowing was started in the mixer. The blowing condition was 60 ° C. and the blowing rate was 7.3 parts by weight / min with respect to 100 parts by weight of the detergent particle group. After completion of the addition of the composition E, the mixture was stirred for 3 minutes to discharge the detergent particle group, and dried at 105 ° C. for 2 hours using an electric dryer to discharge the detergent particle group 21.
• a Redige mixer Matsuzaka Giken Co.
• the resulting detergent particle group 21 has a water content of 0.6%, an average particle size of 412 ⁇ m, a Rosin-Rammler number of 1.65, a 250-500 ⁇ m detergent yield of 41%, a 125-500 ⁇ m detergent yield of 60%, a bulk density of 697 g / L, fluidity 6.8 s.
• a high-density detergent particle having a required particle size is obtained using a group of base granules obtained by a method not including spray drying and a compound of an anionic surfactant represented by the formula (1). It can be produced with good yield.

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• 2010
  • 2010-06-29 WO PCT/JP2010/061038 patent/WO2011001966A1/ja active Application Filing
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