CN1119406C - Method for producing high-bulk density tetergent composition - Google Patents

Abstract

This manufacturing method of a high bulk density detergent composition having not less than 650g/L bulk density is, (a) a water soluble solid particle alkaline inorganic material which is not less than the amount necessary to neutralize a liquid acid precursor of an anionic detergent used in (b), a tripolyphosphate with an average particle diameter of 30&mu m, and at least another solid particle are mixed using a stirred pelletizer, and (b) adding the liquid acid precursor of the anionic detergent to the mixture obtd. in (a), the liquid acid precursor is neutralized with the alkaline inorganic material, while keeping the mixture in particle form, and pelletized.

Description

The production method of high-bulk density detergent compositions

The present invention relates to a kind of production method of detergent composition of high-bulk-density.Or rather, the present invention relates to a kind of production method of high-bulk density detergent compositions, wherein can obtain the granular detergent composition of the small grain size of high yield.

In detergent industry, have than high bulk density talking about recently, for example have 650g/L or＞production method of the powder detergent composition of 650g/L tap density.Like this contain anion surfactant, the powdered detergent of routine alkylbenzene sulfonate is to use alkali, for example sodium hydroxide, yellow soda ash etc., the acidic precursor of neutralize anionic surfactant makes on the spot.

For example, open NO.60-72999 of Japanese Patent and GB-2,166,452B discloses a kind of method that comprises the following steps: washing composition sulfonic acid, yellow soda ash and water are mixed with strong shear; The solid matter that produces is cooled to 40 ℃ or lower; The refrigerative product powder is broken; Then fine powder is formed granular substance.This method is one of typical method in those methods of usually being recommended, and wherein neutralization reaction product is a kind of dough shape material, and this method must be a kind of can provide the kneading unit of required very big energy, for example kneading machine for neutralization reaction.

GB-1369269 discloses a kind of method of producing cationic detergent, and this method comprises the mixing tank with the equipment shear, for example PLouGH SHARE mixing tank mixes washing composition sulfonic acid tempestuously with powdered sodium carbonate.In order to obtain granulous, rather than doughy product, adopt this method in above-mentioned two kinds of component mixtures, to blast gas, so that reactive material can flow, and the hybrid reaction mixture.In order to carry out this processing, what mixing tank must be special is especially complicated.In addition owing to needn't add the water that is used to quicken neutralization reaction, this reaction be appropriate so that form thicker product.In addition, the temperature during neutralization reaction rises to about 85 ℃ usually.When in and when temperature raises between the reaction period, but add the heat decomposition components, for example spices and volatile constituent are difficult to, and therefore, are difficult to contain heat decomposition components and volatile constituent in the said composition but make.

The open No.3-33199 of Japanese Patent discloses a kind of method of the production detergent composition that comprises the following steps; 55 ℃ or＜55 ℃ of temperature under, dry each component of neutralization adds fluid binder then and carries out granulation in super mixer/Fitz chilsonator.The open No.4-363398 of Japanese Patent discloses a kind of method of the production detergent composition that comprises the following steps; 55 ℃ or＞55 ℃ of temperature under, in super mixer/Fitz chilsonator, in the drying and component, then, fluid binder is added, to carry out granulation.The open No.3-146599 of Japanese Patent discloses a kind of production method of the detergent composition that comprises the following steps: in the successive super mixer in the drying and component, then, be increased to high-bulk-density with moderate-speed mixers, then will cool off and/or high-bulk-density product that exsiccant forms carries out granulation.

Comprise particle with the obtainable detergent composition of aforesaid method with small grain size.Yet for application aims, still needing changes the productive rate of the particulate detergent composition that contains desired particle size.

The open No.7-503750 of the Japanese Patent of unexamined discloses a kind of production method of detergent particles, this method is included in the high-shear mixer with the anion surfactant of granular neutralizing agent (yellow soda ash) neutralizing acid form, and the particle of 50% (volume) diameter less than 5 μ m arranged in the granular neutralizing agent.In the disclosure publication, do not have open or the relevant content of improving the productive rate of particulate detergent composition of proposition with needed granularity.

Therefore, purpose of the present invention provides a kind of method that comprises the particulate high-bulk density detergent compositions with suitably low scope granularity with high yield production.

From describe below, can obviously find out these and other purpose of the present invention.

The present invention is relevant with following content:

(1) a kind of tap density is 650g/L or greater than the production method of the high-bulk density detergent compositions of 650g/L, this method comprises the steps:

(a) in the stirring-type nodulizer, mix following component:

(i) granular solid-state water-soluble alkaline inorganic materials,

(ii) have mean particle size and be 1-30 μ m tri-polyphosphate and

(iii) except that component (i) with one or more granular solids (ii), wherein, the usage quantity of granular, solid-state water-soluble alkaline inorganics is equal to or greater than and is used for neutralizing the required amount of liquid anionic surfactant acid precursor in the step (b); With

(b) the acid precursor of liquid anion tensio-active agent is joined in the mixture that step (a) is obtained, with in the alkaline inorganic material and liquid anionic surfactant acid precursor, meanwhile, make mixture keep particle form, and make neutral mixture granulating, to obtain particulate mixtures;

(2) method described in above-mentioned (1) item, wherein resulting high-bulk density detergent compositions have 1000 μ m or＜mean particle size of 1000 μ m, 1400 μ m or＜the particulate weight percent of 1400 μ m is 55% or greater than 55%, wherein mean particle size is, to calculate with weight percent according to the screening size after 5 minutes according to JIS K 8801 vibration standards sieve.

(3) method described in above-mentioned (1) or (2), wherein said granular, solid-state water-soluble alkaline inorganics have 30 μ m or＞mean particle size of 30 μ m;

(4) go up the method for this (1) or (2), wherein, when step (b) N-process carries out, simultaneously the gas drum is sucked in the stirring-type nodulizer;

(5) method of above-mentioned (1) item or (2) item, wherein, in step (b), before adding the acid precursor of liquid anion tensio-active agent, earlier alkaline moisture solution is joined in the mixture of step (a) gained, and doubly mix with the 0.05-0.5 of the required amount of liquid anionic surfactant acid precursor that neutralizes;

(6) method of above-mentioned (5) item, wherein said aqueous based solution is an aqueous sodium hydroxide solution;

(7) above-mentioned (1) item or (2) described method also comprise the steps:

(c) surface modification is by the particulate mixtures of step (b) gained;

(8) above-mentioned (1) item or (2) described method, wherein said stirring-type granulation grain is equipped with stirring blade and is used for pulverizing and fractional knife mill;

(9) above-mentioned (7) described method, the surface-modifying agent that wherein is used for the surface modification step is that mean particle size is crystalline form or the amorphous alkali metal aluminosilicate of 1-30 μ m; With

(10) above-mentioned (1) item or (2) described method, wherein also adding mean particle size is crystalline form or the amorphous alkali metal aluminosilicate of 1-30 μ m, and mixes in step (a).1, step (a)

Step (a) is included in mixes following component in the stirring-type nodulizer:

(i) granular, solid-state water-soluble alkali inorganic substance,

(ii) have mean particle size and be 1-30 μ m tri-polyphosphate and

(iii) except that component (i) with one or more granular solids (ii), the consumption of wherein granular, solid-state water-soluble alkaline inorganics is equal to or greater than and is used for neutralizing the required amount of liquid anionic surfactant acid precursor in the step (b).

Granular, solid-state water-soluble alkaline inorganics can be usually any as the basifier of detergent composition, and its concrete example comprises yellow soda ash, sodium bicarbonate, water glass, salt of wormwood, lime carbonate etc.In granular, solid-state water-soluble alkaline inorganics, preferred yellow soda ash is because yellow soda ash can play detergent builder compound and basifier in final detergent composition.Therefore, by comprising the granular solid-state water-soluble alkaline inorganics component of yellow soda ash, add with the liquid anionic surfactant acid precursor of enough neutralization and the amount that can provide above-mentioned steps (a) function, and with its mixing, neutralization reaction can successfully be carried out.

In particular, add-on preferably granular, solid-state water-soluble alkaline inorganic materials is equal to or greater than the needed amount of neutralization, for example the 1-20 required amount of neutralization doubly, more preferably 2-10 neutralization required amount, the especially 3-8 doubly required amount of neutralization doubly.

In addition, mean particle size granular, solid-state water-soluble alkaline inorganic materials is not restricted especially.From the viewpoint of further increase productive rate and storage stability, the preferred 30 μ m of mean particle size or＞30 μ m, more preferably 40-200 μ m, preferred especially 50-100 μ m.At this, in the present invention, the mean particle size of granular, solid-state water-soluble alkaline inorganic materials is to adopt Laser Scattering Particle Size Distribution Analyzer (" LA-500 " made by HORIBALtd.), is that benchmark calculates with the volume.

The mean particle size that tri-polyphosphate has is 1-30 μ m, preferred 5-20 μ m, more preferably 6-15 μ m.In general, the mean particle size of tri-polyphosphate is more little, and productive rate is high more, reunites because can suppress the neutral particulate mixtures.On the other hand, from technical scale preparation comprise the productivity aspect of particulate tri-polyphosphate, the mean particle size of tri-polyphosphate with small grain size be preferably 1 μ m or＞1 μ m.From suppressing the aspect that the neutral particulate mixtures is reunited, mean particle size be preferably 30 μ m or＜30 μ m.Here, in the present invention, the mean particle size of tri-polyphosphate is to adopt Laser Scattering Particle Size Distribution Analyzer (" LA-500 " made by HORIBALtd.), is that benchmark calculates with the volume.

In addition, not restriction especially of the amount of tri-polyphosphate.The preferred content of tri-polyphosphate is 2-50% (weight) in final detergent composition product, and more preferably 10-40% (weight) is preferably 15-35% (weight) especially.From suppressing the aspect that the neutral particulate mixtures is reunited, the amount of tri-polyphosphate is preferably 2% (weight) or greater than 2% (weight).The composition degree of freedom aspect of the detergent composition product that collateral security generates sees, preferred amount is 50% (weight) or greater than 50% (weight).

The object lesson of one or more granular solids except granular, solid-state water-soluble alkaline inorganic materials and tri-polyphosphate is to be selected from the following material one or more: fluorescent agent; Spices; Anti-redeposition agent, for example sodium salt of polycarboxylate polymer and carboxymethyl cellulose; Granular surfactant, for example lipid acid and salt thereof, linear alkylbenzene sulfonate, alkyl-sulphate; Spray-dired powder, diatomite, calcite, kaolin, wilkinite, sodium sulfate, sodium sulphite etc.Granular solids can use separately or two or more mixes use.

Except the granular solid-state water-soluble alkaline inorganic materials and the not restriction especially of amount of the above-mentioned granular solids the tri-polyphosphate.In final detergent composition, the amount of this granular solids is preferably 2-80% (weight), more preferably 5-50% (weight), especially preferably 7-20% (weight).

In addition, in step (a), can add and have crystalline form or the amorphous alkali metal aluminosilicate that mean particle size is 1-30 μ m.By adding alkali metal aluminosilicate, can suppress undue reunion.In the knife mill of stirring-type nodulizer, alkali metal aluminosilicate also works to help to pulverize the product of reunion.The amount of above-mentioned alkali metal aluminosilicate is not restricted especially.In final detergent composition product, the amount of alkali metal aluminosilicate is preferably 1-8% (weight), and more preferably 2-5% (weight) in this scope, can obtain above-mentioned effect effectively.

Here, in the present invention, the mean particle size of silico-aluminate is to adopt Laser Scattering Particle Size Distribution Analyzer (" LA-500 " obtained by HORIBA Ltd.), by volume calculates.

In step (a), be to adopt the stirring-type nodulizer to mix above-mentioned each component.The stirring-type nodulizer is not restricted especially, and preferred stirring-type nodulizer should be equipped with stirring blade and be used for pulverizing and the dispersive knife mill.Here, paddle or pulverizer can adopt the suitable equipment replacement of function.

The object lesson that available of the present invention is used for the stirring-type nodulizer of intermittent process comprises vertical nodulizer (being made by Powrex Corp.); Super mixer (making) by Fukae Powtec Kogyo Corp.;

Mixing tank (by Matsubo Co., Ltd. makes); With PLOUGH SHARE mixing tank (by PACIFIC MACHINERY ﹠amp; ENGINEERING Co., LTD. makes); Gericke mixing tank (by Meiji Machine Co., Ltd. makes) etc.At this, preferred

Mixing tank and PLOUGH SHARE mixing tank.The object lesson that is applicable to the stirring-type nodulizer of successive processes comprises continous way Mixing tank (moderate speed's mixing tank: those of the long residence time are arranged; The CB circulator (by Make; Super mixer has those of the relatively short residence time); Turbilizer (making) by Hosokawa Micron Corporation; Shugi mixing tank (making) by Powrex Corp.; Flow Jet mixing tank (making) etc. by Funken Powtechs Inc..By the way, in the present invention, above-mentioned mixing tank can suitably be used in combination.

In addition, preferred stirring-type nodulizer is equipped with the chuck of adjustable joint nodulizer internal temperature and is used for advertising nozzle into gas to the stirring-type nodulizer.

The operational condition of stirring-type nodulizer is not restricted especially in the step (a).For example, mixing time preferably in 5 minutes, can determine adaptably according to the mixing tank kind that is adopted by the stirring velocity of main shaft and the speed that is used to pulverize with the dispersive knife mill.For example, under the situation of the mixing tank of intermittent process, the circumference stirring velocity of main shaft is 2-15m/s, is used for pulverizing and dispersive circumference chopper speed is preferably 20-60m/s.

By the way, between step (a) mixing period and after mixing, and/or when step (b) is added liquid anionic surfactant acid precursor, water can be added as reaction initiator.By adding reaction initiator, neutralization reaction can successfully be quickened.The add-on of water is restriction especially, and the add-on of water is preferably 0.2-3 part (weight), 0.5-1.5 part (weight) more preferably, and 100 parts (weight) being the mixture that obtains with step (a) serve as base calculating.From causing the viewpoint of neutralization reaction, the water yield is preferably 0.2 part (weight) or more, and from suppressing the viewpoint that detergent composition is reunited, the water yield is preferably 3 parts (weight) or still less.By the way, under the aqueous situation of the acid precursor of said mixture or liquid anion tensio-active agent or using under the situation of other aqueous solutions, the determining to take an examination of the add-on of water considered the water-content of these components.2, step (b)

Step (b) comprises the acid precursor of liquid anion tensio-active agent is joined in the mixture of gained in step (a); with the alkaline inorganics liquid anionic surfactant acid precursor that neutralizes; make mixture keep particle state simultaneously; granulation neutral mixture obtains particulate mixtures.In this step, form particulate mixtures, the particulate mixtures that produces is used as high-bulk density detergent compositions.

The acid precursor of liquid anion tensio-active agent refers in the anion surfactant of the sour form of liquid state, and it can form salt by neutralization reaction.Therefore, the acid precursor of liquid anion tensio-active agent can be any known anionic tensio-active agent of sour form, does not have restriction especially.Its object lesson comprises linear alkyl benzene sulphonic acid (LAS), the sulfonic acid of alpha-olefin sulfonic acid (AOS), alkylsurfuric acid (AS) and inner olefin sulfonic acid, fatty acid ester, alkyl oxide sulfuric acid, dialkyl sulfosuccinate succsinic acid, lipid acid etc.Liquid acidic precursor can use separately or two or more component is mixed use.

The amount of the acidic precursor of liquid anion tensio-active agent can be determined adaptably according to the composition of required detergent composition.In final detergent composition product, amount by the liquid anion tensio-active agent precursor that is the anion surfactant form that neutralization reaction produced is preferably 5-45% (weight), 10-40% (weight) more preferably, be preferably 20-40% (weight) especially, also 20-35% (weight) more preferably.By the way, even the major surfaces promoting agent that the present invention provides detergent composition to divide other form also can obtain same effect.

In step (b), liquid anionic surfactant acid precursor is joined in the mixture of step (a) gained, the mixture that step (a) is obtained keeps with granular form simultaneously.In order to make mixture keep granular form, liquid acidic precursor should be added in the mixture gradually.The acid required joining day of precursor of liquid anion tensio-active agent is depended on add-on, can not be generally speaking.Be at mixing tank under the situation of intermittent process, the required joining day is preferably 1 minute or more some more, and more preferably 1-10 minute, also more preferably 2-5 minute.Here, the required joining day is preferably more than 1 minute or one minute, therefore, when in the very short time, adding liquid anionic surfactant acid precursor, can since fast neutralization reaction produce heat, and elevate the temperature, to be explained below.

In addition, the acidic precursor of liquid anion tensio-active agent can add continuously, or adds with the multistage in batches.Remove in addition, the equipment of many interpolations can be provided.

By the way, in the adding stage of the acid precursor of liquid anion tensio-active agent, promptly in step (b), neutralization reaction and granulation can take place simultaneously, therefore form particulate mixtures.

After the acid precursor of liquid anion tensio-active agent adds, the stirring-type nodulizer was operated 30 seconds or more some more time again, preferred 1 minute or more than 1 minute.Owing to have this additional step, neutralization reaction can be finished smoothly.

In step (b), in preferably underway and when reaction, simultaneously, should in the stirring-type nodulizer, advertise into gas.Evaporate by gas being advertised in the stirring-type nodulizer, can be made the excess water that in neutralization reaction, produces, and use the gas cooling partical, prevent that thus partical from forming the face dough.Operable gas comprises N ₂Gas, air etc.The amount that gas is blown into (airshed) is not restricted especially.The speed that gas is blown into preferably is equal to or greater than 0.002 part of per minute (weight), more preferably is equal to or greater than 0.02 part of per minute (weight), and it serves as that base calculates with 100 parts of (weight) particals.

In step (b), because neutralization reaction produces reaction heat, the temperature of mixture may raise.If be difficult to add hot decomposable component because mixture temperature raise to make, for example spices and volatile constituent, then the mixture temperature in the step (b) preferably remains on 90 ℃ or lower, more preferably 80 ℃ or lower.In order to regulate mixture temperature in above-mentioned given scope, what meet the requirements is, for example, with cold water by stirring-type nodulizer chuck adoptable method in case above-mentioned gas advertise in the mixing tank.

In addition, in the present invention, in step (b), after the acidic precursor that adds the liquid anion tensio-active agent, should be with alkaline moisture solution, join in the mixture of step (a) gained and mix with the 0.05-0.5 amount doubly of the liquid anionic surfactant acid precursor aequum that neutralizes.

The alkaline moisture solution of specified quantitative should be added in the mixture of gained in step (a), tiny because the granularity of the detergent particles of the detergent composition product that formation generates can be made into, and the tap density height, and can quicken neutralization reaction.Aqueous based solution is preferably 0.05-0.5 times of the required amount of neutralising fluid anionic surfactant acid precursor, and more preferably 0.10-0.45 doubly is preferably 0.15-0.40 doubly especially.From causing the viewpoint of neutralization reaction and the desirable effect of acquisition, the amount of aqueous base preferably is equal to or greater than 0.05 times of the required amount of neutralization, from suppressing the viewpoint that detergent composition is reunited, preferred amount should be equal to or less than 0.5 times of the required amount of neutralization.By the way,, under the lower concentration situation, the aqueous base of excessive water with specified rate joined in the mixture, make detergent composition be easy to reunite though the concentration of aqueous base is not restricted especially.Therefore, the concentration of aqueous base is preferably 20-50% (weight), and more preferably 30-50% (weight) is preferably 40-50% (weight) especially.

In addition, it is not restricted especially to be used for the kind of aqueous base of the present invention.Its concrete example comprises aqueous NaOH, aqueous potassium hydroxide etc., and they are alkaline aqueous solutions, with the liquid anion tensio-active agent neutralization reaction take place easily.From reducing the viewpoint of cost, the aqueous NaOH among them is suitable for.Remove in addition, more preferably the PH that has of the aqueous solution of above-mentioned alkali should be 12 or greater than 12.

In addition, the mixing in this step can proceed to and can make the homodisperse degree of added aqueous base.

By the way, the adding of aqueous base can be undertaken by following concrete scheme:

(1) after the processing of step (a), can add; Or (2) add simultaneously with step (a).

Adding simultaneously under the situation of aqueous base with step (a), mixture can by as the following step of the embodiment of step (a) (a ') obtain: (a ') following component of mixing in the stirring-type nodulizer:

(i) granular, solid-state water-soluble alkaline inorganic materials,

(ii) mean particle size is the tri-polyphosphate of 1-30 μ m,

(iii) except component (i) and one or more granular solids (ii) and

(iv) aqueous base, aqueous base are that the 0.05-0.5 amount doubly with the required amount of the acidic precursor of the liquid anion surfactant that neutralizes adds.Wherein, the consumption of granular solid-state water-soluble alkaline inorganic materials should be equal to or greater than and be used for neutralizing the required amount of liquid anionic surfactant acid precursor in the step (b).

In this embodiment, importantly, at least in the preceding interpolation aqueous base of step (b).Therefore, in step (a ') stage afterwards, the interpolation step of aqueous base may not be restricted.More precisely, in embodiments, with granular, solid-state water-soluble alkaline inorganic materials with after aqueous base is mixed, can add other detergent components.When adding the component of alkali resistance difference, aforesaid method is efficiently.

By the way, from equably aqueous base being scattered in the viewpoint of mixture, preferred embodiment (1) wherein is after the processing of step (a), adds aqueous base.

Comprise the method for above-mentioned steps by utilization, might obtain to comprise to have the high-bulk density detergent compositions that bulk density is 650g/L or higher particulate mixtures.The high-bulk-density cleaning composition that obtains with the inventive method more preferably has following character.

(1) tap density is preferably 650-950g/L, more preferably 700-900g/L.In technical requirements of the present invention, tap density is to adopt the numerical value of the method calculating of JISK 3362 definition;

(2) from the dissolution rate aspect, mean particle size is preferably 1000 μ m or littler, 850 μ m or littler more preferably, and also 300-800 μ m more preferably is preferably 350-650 μ m especially; The particulate percentage ratio that 1400 μ m pass through be preferably 55% or＞55%, more preferably 60% or＞60%, also more preferably 65% or＞65%, preferred especially 70% or＞70%.In technical requirements of the present invention, mean particle size is counted by weight percentage, and depends on the size according to the screening of standard sieve vibration after 5 minutes of JIS K8801.Particulate percentage ratio that 1400 μ m the pass through meaning be 1400 μ m or＜weight percentage that 1400 μ m particles are occupied;

(3) free-flowing property with regard to flowing time preferred 8 seconds or＜8 seconds, more preferably 7 seconds or＜7 seconds.In technical requirements of the present invention, free-flowing property is defined as is measuring in the tap density 100ml powder from the used required time of loading hopper discharge according to JIS K 3362.3, step (c)

Method of the present invention also can comprise step (c), and this step is the particulate mixtures that surface modification is obtained in step (b).In order to obtain to the free-flowing property of the high-bulk density detergent compositions that obtains with the inventive method and the further improvement of storage stability, the desirable step (c) that provides.Specifically, by adding the following surface-modifying agent of specified rate, the particulate mixtures that will obtain in step (b) in the stirring-type nodulizer mixes simultaneously, can finish surface modification.

Surface-modifying agent can be any common known surface-modifying agent.Crystalline form or amorphous alkali metal aluminosilicate (zeolite), calcite, diatomite, silica etc. all are suitable for.It is 1-30 μ m, more preferably 1-10 μ m that above-mentioned silico-aluminate preferably has mean particle size.In addition, in final detergent composition product, the amount of surface-modifying agent is preferably 2-15% (weight), more preferably 4-12% (weight).By the way, the mean particle size of surface-modifying agent is to be that the basis adopts laser light scattering particle-size analyzer (" LA-500 " made by HORIBA Ltd.) to calculate with the volume.

In addition, under the situation of adding surface-modifying agent, the operating time of stirring-type nodulizer is not restricted especially, and the operating time can be preferably 1-5 minute.

By the way, in the method for the invention, liquid composition can add arbitrarily, depends on the composition of the detergent composition of gained.Can add liquid composition at step (a) and (b) and any one step (c).For example, preferably can before adding surface-modifying agent, add liquid composition.

The example of liquid composition comprises any given liquid composition that is generally used for detergent composition, comprises liquid non-ionic surfactant; Water-soluble polymers, for example polyoxyethylene glycol, vinylformic acid-maleic acid etc.; Lipid acid etc.Liquid composition can be used separately or two or more component is mixed use.From suppressing the viewpoint that detergent composition is reunited, the amount of liquid composition is preferably 15% (weight) of final detergent composition product or less, more preferably 10% (weight) or still less.

In addition, add surface-modifying agent in advance and add under the situation of liquid composition again, the operating time of stirring-type nodulizer is restriction especially not, and the operating time can be preferably 0.5-8 minute.

In the present invention, following component arbitrarily also can be included in the detergent composition.Component comprises for example enzyme, spices, SYNTHETIC OPTICAL WHITNER, pigment etc. arbitrarily.By the detergent composition that will obtain with the inventive method and component arbitrarily, by use mixing machine for example rotary blender mix, can allocate above-mentioned any component into.

Remove in addition, can be with the high-bulk density detergent compositions that the inventive method obtains as the component of other detergent composition of preparation.

Provide various embodiments of the present invention below.[1] tap density be 650g/L or＞production method of the high-bulk density detergent compositions of 650g/L comprises the steps:

(a ') the following component of mixing in the stirring-type nodulizer:

(i) granular, solid-state water-soluble alkaline inorganic materials,

(ii) have the tri-polyphosphate that mean particle size is 1-30 μ m,

(iii) except that component (i) and one or more granular solids (ii) and

(iv) aqueous base, aqueous base is the 0.05-0.5 amount adding doubly with the amount of the liquid anionic surfactant acid precursor needs that neutralize, the consumption of wherein granular, solid-state water-soluble alkaline inorganic materials is equal to or greater than and is used for neutralizing the required amount of liquid anionic surfactant acid precursor in the step (b); With

(b) acidic precursor with the liquid anion tensio-active agent joins in the mixture of step (a) gained, with in the alkaline inorganic material and the acidic precursor of liquid anion surfactant, make mixture keep granular form simultaneously, make the neutral mixture pelleting, obtain particulate mixtures.[2] in the method described in [1] item, wherein, in step (b), carry out N-process and simultaneously gas is blasted in the stirring-type nodulizer.

[3] in the method described in [2], wherein gas is to blast gas with the speed that is equal to or greater than per minute 0.002 part (weight), and it is serve as base calculating with 100 parts of (weight) particulate mixtures in the step (b).[4] in any one described method of [1] to [3], wherein the amount of tri-polyphosphate is the 5%-50% (weight) of the detergent composition amount that obtained.

[5] in any one described method of [1] to [3], wherein the mean particle size that has of tri-polyphosphate is 1-30 μ m.

[6] in any one described method of [1] to [3] item, the mean particle size that wherein resulting high-bulk-density cleaning composition has is 1000 μ m, or it is littler, 1400 μ m or＜1400 μ m particulate weight percents be 55% or＞55%, wherein mean particle size is counted by weight percentage, and depends on according to the screening size of JIS K8801 standard sieve vibration after 5 minutes.[7] in any one described method of [1] to [3] item, also comprise step: (c) particulate mixtures that obtains is done surperficial modification in step (b).[8] in [7] described method, wherein surface-modifying agent is crystalline form or amorphous alkali metal aluminosilicate.[9] in any one described method of [1]-[3] and [8], wherein the stirring-type nodulizer is equipped with stirring blade and is used for pulverizing and the dispersive knife mill.

High-bulk density detergent compositions with small grain size can be the tri-polyphosphate of 1-30 μ m by adopting mean particle size; with with granular, solid-state water-soluble alkaline inorganic materials; in the stirring-type nodulizer, the liquid anionic surfactant acid precursor that neutralizes obtains with high yield.

Embodiment

Adopt following work embodiment, the present invention will be described in more detail, and can not limit the scope of the invention.

Embodiment 1

Having shown in the table 1 detergent composition of forming is to adopt high-speed mixer " Loding mixing machine FKM-130D " (by Matsubo Co., Ltd. makes), press that the amount of per unit 35kg prepares.This mixing machine equipment stirring blade and shear, this shear is equivalent to be used for chopping and dispersive knife mill.

Here, detergent composition is to prepare with the following method of describing in detail below. Powder mixes

To comprise 7.7 parts of (weight) tripoly phosphate sodium STPP (STPP; 11.2 μ m), 11.94 parts of (weight) yellow soda ash (" LIGHT ASH " mean particle size:, by Central Glass Co., Ltd makes, 56.1 μ m) and the solid ingredient of 0.11 part of (weight) fluorescent agent mean particle size:, in agitator paddle speed of rotation is 130rpm (circumferential speed: be 2850rpm (circumferential speed: under condition 27m/S), mixed a minute with the shear speed of rotation 3.4m/S). Add reaction initiator

Water as reaction initiator, by the amount of 0.25 part (weight), is joined in the thing of mixing tank the inside.And under above-mentioned same mixing condition, mixed 1 minute and 30 seconds. Neutralization

When mixing tank is operated under above-mentioned similarity condition, 10.92 parts of (weight) linear alkyl benzene sulphonic acid (LAS) are joined in the thing of the inside of mixing tank, the joining day was with 4 minutes.During adding, allow water flow through the mixing tank chuck, cool off this batching down at 25 ℃.In this stage, temperature rises to 68.8 ℃.By the way, in the meantime, reaction mixture keeps particle form.By the way, above-mentioned LAS contains 0.16 part of sulfuric acid (weight).

After adding LAS, mixing tank continued to operate one minute under the same conditions. Add liquid ingredient and surface modification

When mixing tank was operated under above-mentioned similarity condition, neutralization reaction was finished, and at this moment, with the aqueous solution of 40% (weight) vinylformic acid-maleic acid, joined in the mixing tank with 0.18 part of (weight) multipolymer significant quantity, mixed 1 minute and 30 seconds.After, join as surface-modifying agent by the zeolite that is 4 μ m with 4.2 parts of (weight) mean particle sizes and to sneak in the device, make the mixture surface modification of generation, and mixture was operated 2 minutes again.By the way, zeolite contains 0.84 part of (weight) crystal water.

The detergent composition particle that produces has following character:

The percentage that 1400 μ m particles pass through: 73.9%;

Mean particle size: 577 μ m; With

Tap density: 818g/l; With

Free-flowing property: 6.2 seconds.

Therefore, this particle demonstrates good performance. Mix the back

Adopt impeller, 0.18 part of (weight) enzyme particle and the above-mentioned detergent composition that makes are mixed, after this, 0.07 part of (weight) spices is sprayed into the final powdered product that obtains high-bulk density detergent compositions.

By the way, in this embodiment, the amount of yellow soda ash be in and 6.7 times of the required amount of LAS.

Embodiment 2

Except being the tripoly phosphate sodium STPP of 8.3 μ m with mean particle size, use the method that is similar to embodiment 1, the composition with being similar to embodiment 1 makes detergent composition.

The particle of the detergent composition after the mixing step of back has following character:

The per-cent that 1400 μ m particles pass through: 77.0%;

Mean particle size: 530 μ m;

Tap density: 820g/L; With

Free-flowing property: 6.0 seconds.

Therefore, this particle demonstrates premium properties.

Embodiment 3

Except the LIGHTASH that uses among the embodiment 1 being ground into the LIGHTASH of mean particle size 6.9 μ m acquisition with hammer mill, use the composition that is similar to embodiment 1, the method with being similar to embodiment 1 obtains detergent composition.

The particle of the detergent composition after the mixing step of back has following performance:

The percentage that 1400 μ m particles pass through: 60.5%;

Mean particle size: 830 μ m;

Tap density: 831g/L; With

Free-flowing property: 7.4 seconds.Therefore, this particle demonstrates premium properties.

Embodiment 4

Except the flow velocity that divides with 500L/ air is advertised the mixing tank, carried out the process similar with embodiment 1.Air is that the speed with per minute 0.02 part (weight) blasts, and this speed is that the partical in neutralization and granulation step with 100 parts (weight) is a benchmark, obtains the detergent composition shown in the table 1.

The particle of the detergent composition after mix the back has following character:

The per-cent that 1400 μ m particles pass through: 76.2%;

Mean particle size: 542 μ m;

Tap density: 835g/L; With

Free-flowing property: 5.8 seconds.

Therefore, this particle demonstrates premium properties.By air is advertised into mixing tank, the mean particle size that the particulate mean particle size of generation obtains less than embodiment 1, thereby improved tap density and free-flowing property.

Embodiment 5

Adopt super mixer " Lodige mixing tank FKM-130D " (by Matsubo Co., Ltd. makes), have the detergent composition of the composition shown in the table 1 with the amount preparation of every unit 35kg.This mixing tank equipment stirring blade and shear, this shear is equivalent to be used for pulverize and the fractional knife mill.

Here, adopt the following process of following detailed description to come preparing washing agent composition. Powder mixes

Will be by 7.7 parts of (weight) tripoly phosphate sodium STPP (STPP; 11.2 μ m), 12.62 parts of (weight) yellow soda ash (" LIGHT ASH " mean particle size:, by Central Glass Co., Ltd. make, 56.1 μ m) and the solids fraction formed of 0.11 part of (weight) fluorescent agent mean particle size:, in the stirring blade speed of rotation is that 130rpm and shear speed of rotation are under the condition of 2850rpm, mixes 1 minute. Add reaction initiator

Water as reaction initiator, is joined in the thing of mixing tank the inside with the amount of 0.25 part (weight), and mixed under above-mentioned identical mixing condition 1 minute and 30 seconds. Neutralization

When mixing tank is operated, 10.92 parts of (weight) linear alkyl benzene sulphonic acid (LAS) are added in the thing of mixing tank the inside 4 minutes joining days under above-mentioned the same terms.During adding, allow water flow through the mixing tank chuck, cool off these components down at 25 ℃.In this stage, temperature rises to 61.8 ℃.By the way, during this stage, reaction mixture keeps particle form.By the way, above-mentioned LAS contains 0.16 part of (weight) sulfuric acid.In addition, under embodiment 4 the same terms, air is advertised in the mixing tank.

After adding LAS, mixing tank continues operation 1 minute under similarity condition.

The granular detergent composition that produces has following performance:

The particulate percentage that 1400 μ m-pass through: 84.7%;

Mean particle size: 578 μ m;

Tap density: 680g/L; With

Free-flowing property: 8.3 seconds. Surface modification

In addition, under the identical condition of embodiment 1, make the granular detergent composition surface modification of generation.The granular detergent composition that produces has following performance:

The percentage that 1400 μ m particles pass through: 90.1%;

Mean particle size: 462 μ m;

Tap density: 688g/L; With

Free-flowing property: 6.3 seconds.

Therefore, this particle demonstrates premium properties.By the way, in this embodiment, the amount of yellow soda ash be in and 7.0 times of the required amount of LAS.

Embodiment 6

The employing super mixer " Mixing tank FKM-130D " (by Matsubo Co., Ltd. makes), have the detergent composition of forming shown in the table 1 with the preparation of the amount of every unit 35kg.This mixing tank equipment stirring blade and shear, this shear is equivalent to be used for pulverize or the fractional knife mill.

Here, the following process preparing washing agent composition described in detail below of employing. Powder mixes

Will be by 7.7 parts of (weight) tripoly phosphate sodium STPP (STPP; 11.2 μ m), 13.74 parts of (weight) yellow soda ash (" LIGHTASH " mean particle size:, by Central Glass Co., Ltd. make, 56.1 μ m) and the solid ingredient formed of 0.11 part of (weight) fluorescent agent mean particle size:, in the stirring blade speed of rotation is that the speed of rotation of 130rpm and shear is under the condition of 2850rpm, mixes 1 minute. Add reaction initiator

Water as reaction initiator, is joined in the thing of mixing tank the inside with 0.25 part amount, under above-mentioned identical mixing condition, mixed 1 minute and 30 seconds. Neutralization

When mixing tank is operated under above-mentioned the same terms, 7.51 parts of (weight) linear alkyl benzene sulphonic acid (LAS), 0.48 part of (weight) lipid acid, 1.4 portions of (weight) nonionogenic tensides are sequentially joined in the thing of mixing tank the inside 4 minutes joining days.During adding, allow water flow through the mixing tank chuck, cool off these components down at 25 ℃.In this stage, temperature rises to 59.5 ℃.By the way, in this stage, reaction mixture remains on graininess.By the way, above-mentioned LAS contains 0.11 part of (weight) sulfuric acid.In addition, under embodiment 4 the same terms, air is advertised into mixing tank.

After adding LAS, mixing tank continued to operate 1 minute under the same conditions. Surface modification

When neutralization reaction is complete, by being that the zeolite of 4 μ m joins in the mixing tank as the mean particle size of surface-modifying agent, and mixture was operated 2 minutes again with 4.2 parts (weight), make the mixture surface modification of generation.By the way, above-mentioned zeolite contains 0.84 part of (weight) crystal water.

The granular detergent composition that produces has following performance:

The percentage that 1400 μ m particles pass through: 75.0%;

Mean particle size: 613 μ m;

Tap density: 871g/L; With

Free-flowing property: 5.4 seconds.

Therefore, this particle shows premium properties. Mix the back

Adopt impeller, 0.18 part of (weight) enzyme granulate and the above-mentioned detergent mixture that makes are mixed, then, spray into 0.07 part of (weight) spices, to produce the final powdered product of high-bulk density detergent compositions.

By the way, the amount of yellow soda ash be in and 10.7 times of the required amount of LAS and lipid acid. Comparative example 1

Except employing has the tripoly phosphate sodium STPP that mean particle size is 58.4 μ m, use embodiment 1 similarly to form the process similar to Example 1 of carrying out, obtain detergent composition.

Shape detergent composition after the mixing step of back has following character:

The percentage that 1400 μ m particles pass through: 34.2%;

Mean particle size: 1213 μ m;

Tap density 712g/L; With

Free-flowing property: 7.8 seconds.

Therefore, this particle has low bulk density, and coarse grained ratio is big, and productive rate is low. Comparative example 2

Except with having the tripoly phosphate sodium STPP that mean particle size is 36.5 μ m, use embodiment 1 similar composition to carry out process similar to Example 1, obtain detergent composition.

Granular detergent composition after the mixing step of back has following character:

The percentage that 1400 μ m particles pass through: 50.5%;

Mean particle size: 1087 μ m;

Tap density: 719g/L; With

Free-flowing property: 6.7 seconds.

Therefore, this particle has low bulk density, and coarse grained ratio is big, and productive rate is low. Comparative example 3

Except with to have granularity be the tripoly phosphate sodium STPP of 58.4 μ m and use that by hammer mill the LIGHTASH of embodiment 1 usefulness to be ground into mean particle size be the LIGHTASH that obtains of 6.9 μ m, use embodiment 1 similar composition to carry out process similar to Example 1, obtain detergent composition.

Granular detergent composition after the mixing step of back has following character:

The percentage that 1400 μ m particles pass through: 27.6%;

Mean particle size: 1670 μ m;

Tap density: 769g/L; With

Free-flowing property: 7.0 seconds.

Therefore, this particle has low bulk density, and coarse grained ratio is big, and yield is low.

By the way; The composition of the final powdered product of each detergent composition in table 1 expression the foregoing description and the comparative example.In addition; The character of table 2 and 3 detergent composition that after granulation, composition % (weight) comparative example 1-3 embodiment 4 embodiment 5 embodiment 6LAS-Na 32.00 32.00 32.00 22.00 soaps 0.00 0.00 0.00 1.50STPP 22.00 22.00 22.00 22.00 zeolites 12.00 12.00 12.00 12.00 sodium carbonate 28.67 29.32 30.62 35.23 sodium sulphate 0.68 0.68 0.68 0.47 acrylic acid maleic acid 0.50 0.50 0.00 0.00 non-ionic surface active agent 0.00 0.00 0.00 4.00 fluorescer 0.30 0.30 0.30 0.30 enzyme 0.50 0.50 0.00 0.50 spices 0.20 0.20 0.00 0.20 water 3.15 2.50 2.40 1.80 tables 2 of the whole powdered product of embodiment 1-3 of obtain of expression. table 1 composition of detergent

Embodiment

The highest powder temperature of particle mean size (μ m) 56.1 56.1 6.9 56.1 56.1 56.1 air capacities of passing through 000 500 500 500 (L/min) of the particle mean size of 12345 6STPP (μ m), 11.2 8.3 11.2 11.2 11.2 11.2LIGHTASH. (℃) particle 73.9 77.0 60.5 76.2 84.7 (90.1) that passes through of particle mean size (μ m) 577 530 830 542 578 (462) the 6131400 μ m of 68.8 69.0 74.7 61.0 61.8 59.5 final powdered product^*75.0 percentage (productive rate) is tap density (g/L) 818 820 831 835 680 (688) (%) ^*871 free-flowing properties (second) 6.2 6.0 7.4 5.8 8.3 (6.3) ^*5.4 annotate ^*: the value that obtains after the numeral surface modification in the bracket.Table 3

Comparative example

The particle mean size of 12 3STPP, the particle mean size of (μ m) 58.4 36.5 58.4LIGHTASH, the powder temperature that (μ m) 56.1 56.1 6.9 is the highest, (℃) particle mean size of 70.7 71.8 75.2 final powdered product, the particle percentage that (μ m) 1,213 1,087 16701400 μ m pass through, (productive rate), (%) 34.2 50.5 27.6 bulk densities, (g/L) 712 719 769 free mobilities, (second) 7.8 6.7 7.0

Find out that from The above results is clear confirm that the gathering or the coarse grained form of detergent composition can significantly be suppressed, because tri-polyphosphate has the mean particle size of 1-30 μ m, tri-polyphosphate and neutralization reaction do not have direct relation.

Embodiment 7

Use super mixer " Lodige mixing tank FKM-130D " (by Matsubo Co., Ltd. makes), have the detergent composition of composition shown in the table 4 with the amount preparation of every unit 35kg.This mixing tank equipment stirring blade and shear, this shear is equivalent to be used for pulverize and the dispersive knife mill.

Here, adopt following process preparing washing agent composition described in detail below. Powder mixes

Agitator paddle speed of rotation be 130rpm (circumferential speed: 3.4m/S) and the shear speed of rotation be 2850rpm (circumferential speed: under condition 27m/S), will be by 5.25 parts of (weight) tripoly phosphate sodium STPP (STPP; 11.2 μ m), (" LIGHT ASH ", by Central Glass Co., Ltd. makes, mean particle size: for 13.82 parts of (weight) yellow soda ash 56.1 μ m) and the solid ingredient mixing formed of 0.088 part of (weight) fluorescent agent 1 minute mean particle size:.By the way, the amount of yellow soda ash is in being used for and 7.8 times of the required amount of linear alkyl benzene sulphonic acid (LAS). Add alkaline aqueous solution

The aqueous sodium hydroxide solution of 0.56 part of (weight) 48% (weight) is joined in the thing of mixing tank the inside, and under above-mentioned identical mixing condition, mixed the mixture that produced 1 minute and 30 seconds.The amount of aqueous sodium hydroxide solution is in being used for and 0.2 times of the required amount of LAS. Neutralization

When mixing tank is operated under above-mentioned the same terms, with 11.26 parts of (weight) linear alkyl benzene sulphonic acid (LAS; Molecular weight: 322) join in the thing of mixing tank the inside 4 minutes joining days.During adding, allow water flow through the chuck of mixing tank, cool off these components at 25 ℃.In this stage, temperature rises to 72 ℃.By the way, in the meantime, reaction mixture keeps particle form.

After adding LAS, mixing tank continues operation 1 minute under the same conditions, to finish neutralization reaction and granulation process.

By the way, between neutralization and granulation stage, air is with 0.5m ³/ minute speed blast in the mixing tank. Add liquid ingredient and surface modification

When mixing tank is operated under above-mentioned the same terms, when neutralization reaction and granulation process are finished, the aqueous solution of 40% (weight) vinylformic acid-maleic acid significant quantity with 0.245 part of (weight) multipolymer is joined in the mixing tank, mixed 1 minute and 30 seconds.After this, zeolite joins in the mixing tank as surface-modifying agent by being 4 μ m with 4.2 parts of (weight) mean particle sizes, and mixture was operated 2 minutes again, makes the mixture surface modification of generation.By the way, this zeolite contains 0.84 part of (weight) crystal water.

The granular detergent composition that obtains has following character:

The percentage that 1400 μ m particles pass through: 76.5%;

Mean particle size: 578 μ m;

Tap density: 772g/L; With

Free-flowing property; 6.4 second.

Therefore, this saccharoid demonstrates good performance. Mix the back

Adopt impeller, 0.105 part of (weight) enzyme granulate and the above-mentioned detergent composition that makes are mixed, after this, 0.07 part of (weight) spices is sprayed into, obtain the final powdered product of high-bulk density detergent compositions.

Embodiment 8

Except the amount of 48% (weight) aqueous NaOH being changed into 1.12 parts (weight) (in being equivalent to and the required amount of LAS 0.4 times), adopt embodiment 7 similarly to form, the process with similar to Example 7 obtains detergent composition.

Granular detergent composition after the mixing step of back has following character:

The per-cent that 1400 μ m particles pass through: 79.0%;

Mean particle size: 550 μ m;

Tap density: 80gg/L; With

Free-flowing property: 6.2 seconds.

Therefore, this particle shows fabulous performance.

Embodiment 9

Except in whole neutralization reaction and granulation process, omitting air is blasted the mixing tank, adopt the composition similar, carry out and implement 7 similar processes, obtain detergent composition with embodiment 7.

Granular detergent composition after the mixing step of back has following character:

The percentage that 1400 μ m particles pass through: 70.0%;

Mean particle size: 630 μ m;

Tap density: 761g/L; With

Free-flowing property: 6.7 seconds.

Embodiment 10

Except not adding 48% (weight) aqueous sodium hydroxide solution, adopt the composition similar with embodiment 7, carry out the similar process of embodiment 7, obtain detergent composition.

At the back mixing step, granular detergent composition afterwards has following character:

The percentage that 1400 μ m particles pass through: 59.3%.

Mean particle size: 790 μ m;

Tap density: 678g/L; With

Free-flowing property: 7.2 seconds.

Embodiment 11

Except substituting with 0.25 part of (weight) water 48% (weight) aqueous sodium hydroxide solution, adopt embodiment 7 similar compositions to carry out the similar process of embodiment 7, obtain detergent composition.

Granular detergent composition after the mixing step of back has following character:

The percentage that 1400 μ m particles pass through: 67.5%;

Mean particle size: 660 μ m;

Tap density: 711g/L; With

Free-flowing property: 6.8 seconds.

Embodiment 12

Except between whole neutralization reaction process and granulation stage, not adding 48% (weight) aqueous sodium hydroxide solution and omitting air is not blasted the step of mixing tank, adopt embodiment 7 similar compositions to carry out the process similar, obtain detergent composition with embodiment 7.

Granular detergent composition after the mixing step of back has following character:

The percentage that 1400 μ m particles pass through: 58.6%;

Mean particle size: 813 μ m;

Tap density: 682g/L; With

Free-flowing property: 7.9 seconds.

Embodiment 13

Except the amount of 48% (weight) aqueous sodium hydroxide solution being changed into 1.96 parts (weight) (in being equivalent to and the required amount of LAS 0.7 times), adopt embodiment 7 similar compositions to carry out the process similar with embodiment 7, obtain detergent composition.

Granular detergent composition after the mixing step of back has following character:

The percentage that 1400 μ m particles pass through: 57.0%;

Mean particle size: 950 μ m;

Tap density: 721g/L; With

Free-flowing property: 8.0 seconds.

By the way; table 4 has been listed the composition of the final powdered product of every kind of detergent composition in an embodiment.In addition, table 5 has shown the performance of the detergent composition after reaction conditions and the granulation.4 ( ％ ( ) ) 78 9 10 11 12 13LAS-Na 33 33 33 33 33 33 33STPP 15 15 15 15 15 15 15 12 12 12 12 12 12 12 34.9 34.18 35.1 35.55 35 35.05 33.25 0.7 0.7 0.7 0.7 0.7 0.7 0.7- 0.7 0.7 0.7 0.7 0.7 0.7 0.7 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.2 0.2 0.2 0.2 0.2 0.2 0.2 2.95 3.67 2.75 2.3 2.85 2.8 4.65

Embodiment

The particle mean size of the powder temperature ℃ 72 75 79 69 69 71 82 final powdered product that amount L/min that 789 10 11 12 13 air pass through 500 500 0 500 500 0 500 is the highest, the percentage that (μ m) 578 550 630 790 660 831 9501400 μ m particles pass through, (productive rate), (%) 76.5 79.0 70.0 59.3 67.5 58.6 57.0 bulk densities, (g/L) 772 809 761 678 711 682 721 free mobilities, (second) 6.4 6.2 6.7 7.2 6.8 7.9 8.0

When those that embodiment 10 to embodiment 13 prepared detergent composition and embodiment 1 to embodiment 6 are made are compared, it demonstrates bad a little performance, is the tri-polyphosphate of 1-30 μ m because they contain the exhibiting high surface promoting agent and contain a small amount of mean particle size.Every kind of detergent composition that embodiment 7 to embodiment 9 makes contains the aqueous base of specified quantitative, so that the performance of the detergent composition that discovery is generated comprises the particle percentage that 1400 μ m pass through, mean particle size, tap density and free-flowing property all obtain significantly to improve.In addition, find out from embodiment 7 and embodiment 9 are clear, because air blasts mixing tank during neutralization and granulation process, so the performance of the detergent composition that is generated obtains further to improve.Remove in addition, know from embodiment 9,10,12 and find out that the aqueous base that adds specified quantitative greatly helps to make the detergent composition performance to be improved, wherein air blasts mixing tank.

The present invention has been done such description, obviously, can change by many modes for same content, such variation does not think to deviate from the spirit and scope of the present invention, all these, conspicuous for a person skilled in the art change all is included in the scope of following claim.

Claims (10)

1, a kind of tap density is 650g/L or greater than the production method of the high-bulk density detergent compositions of 650g/L, comprises step:

(a) in the stirring-type nodulizer, following component is mixed:

(i) granular solid-state water-soluble alkaline inorganic materials,

(ii) mean particle size be 1-30 μ m tri-polyphosphate and

(iii) one or more except that component (i) and (ii) are selected from the granular solids of fluorescent agent, spices, anti redeposition agent,

Wherein, the consumption of described granular solid-state water-soluble inorganic material is equal to or greater than the required amount of acidic precursor of the liquid anion surfactant that is used in the step (b) neutralizing; With

(b) acidic precursor with the liquid anion tensio-active agent joins in the mixture that is obtained by step (a), with in the alkaline inorganic material and the acidic precursor of liquid anion surfactant, described liquid acidic precursor is to add gradually in the mixture so that mixture keeps granular form, the neutral mixture pelleting, obtain particulate mixtures.

2, according to the method for claim 1, wherein the mean particle size that has of gained high-bulk density detergent compositions is 1000 μ m or less than 1000 μ m, 1400 μ m or be 55% or greater than 55% less than 1400 μ m particulate weight percents, wherein mean particle size is to be calculated by the weight percent according to the screening size of JIS K 8801 standard sieves vibration after 5 minutes.

3, according to the method for claim 1 or 2, the mean particle size of wherein said granular solid water dissolubility inorganic substance is 30 μ m or greater than 30 μ m.

4, according to the method for claim 1 or 2, wherein, when step (b) N-process carries out, blast gas to the stirring-type nodulizer simultaneously.

5, according to the method for claim 1 or 2, wherein, in step (b), before adding the acid precursor of liquid anion tensio-active agent, alkaline moisture solution is joined in the mixture of step (a) gained, and mix with the amount of the 0.05-0.5 of the required amount of liquid anionic surfactant acid precursor that neutralizes.

6, according to the method for claim 5, wherein said alkaline moisture solution is an aqueous sodium hydroxide solution.

7, according to the method for claim 1 or 2, also comprise step:

(c) particulate mixtures of surface modification gained in step (b).

8, according to the method for claim 1 or 2, wherein said stirring-type nodulizer has been equipped with stirring blade and has been used for pulverizing and the dispersive knife mill.

9, according to the method for claim 7, wherein, the surface-modifying agent that can be used for the surface modification step is to have the crystalline or amorphous alkali metal aluminosilicate that mean particle size is 1-30 μ m.

10, according to the method for claim 1 or 2, wherein, mean particle size is that the crystalline or amorphous alkali metal aluminosilicate of 1-30 μ m is further to add and blended in step (a).