CN102994258B - Preparation method of composition for alpha-sulfo-group fatty acid alkyl ester salt-containing detergent - Google Patents
Preparation method of composition for alpha-sulfo-group fatty acid alkyl ester salt-containing detergent Download PDFInfo
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- CN102994258B CN102994258B CN201210557785.3A CN201210557785A CN102994258B CN 102994258 B CN102994258 B CN 102994258B CN 201210557785 A CN201210557785 A CN 201210557785A CN 102994258 B CN102994258 B CN 102994258B
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- 239000000203 mixture Substances 0.000 title claims abstract description 65
- 239000000194 fatty acid Substances 0.000 title claims abstract description 50
- 239000003599 detergent Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 235000014113 dietary fatty acids Nutrition 0.000 title abstract 6
- 229930195729 fatty acid Natural products 0.000 title abstract 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 32
- 239000010457 zeolite Substances 0.000 claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 26
- 230000000694 effects Effects 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
- 239000011246 composite particle Substances 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 4
- 239000002563 ionic surfactant Substances 0.000 claims description 3
- 230000035515 penetration Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 11
- 238000005507 spraying Methods 0.000 abstract description 5
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 18
- 238000012360 testing method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000003860 storage Methods 0.000 description 5
- 238000000889 atomisation Methods 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 238000007046 ethoxylation reaction Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 3
- 238000010923 batch production Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000009686 powder production technique Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000008786 sensory perception of smell Effects 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical group [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Detergent Compositions (AREA)
Abstract
The invention discloses a preparation method of composition for alpha-sulfo-group fatty acid alkyl ester salt-containing detergent, and the preparation method comprises the following steps of: spraying a non-ionic surface active agent onto powdery alpha-sulfo-group fatty acid alkyl ester salt in the manner of spraying, spraying and stirring to be formed into a compound of the non-ionic surface active agent and the powdery alpha-sulfo-group fatty acid alkyl ester salt and formed into a layer of liquid non-ionic film-packed layer on a surface; and adding zeolite, and evenly mixing into the composition for detergent. The flowability of the composition for the detergent prepared by the method is obviously higher than that of the alpha-sulfo-group fatty acid alkyl ester salt per se, the detergent is hard to bond to be clustered, and is stable in property, the requirement of the stable discharge in a production technology can be met, and the generation of the bad smell when the alpha-sulfo-group fatty acid alkyl ester salt-containing powdery detergent is stored can be effectively restrained.
Description
Technical field
The present invention relates to a kind of preparation method of composition for detergent, be specifically related to a kind of preparation method of the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt (MES).
Background technology
Alpha-sulfo-fatty acid alkyl ester salt (MES), to adopt natural matter renewable resources Oleum Cocois, palm wet goods glyceride stock is through sulfonation, the product obtaining after neutralization, it is a kind of well behaved tensio-active agent, there is excellent lime soap dispersing power, low irritant and good biological degradability, compare and in cost performance, possess suitable advantage with the tensio-active agent of current use, and there is environment protection significance, be used for the Application and Development of petroleum replacing by product alkyl benzene sulphonate (ABS) at aspects such as washing composition and personal care articles, solving the industry, to rely on for a long time the common problem of oil significant, in washing sector application, have broad prospects.
At present, alpha-sulfo-fatty acid alkyl ester salt is applied to be needed in rear allotment of labor's skill of washing powder the alpha-sulfo-fatty acid alkyl ester salt of sheet through special disintegrating process, and forming could be composite in washing powder after powdery.But due to alpha-sulfo-fatty acid alkyl ester salt itself, to have easy bonding agglomerating, poor fluidity and 45 ℃ of above just characteristics in molten state, cause easily building bridge in feed bin, latch up phenomenon, be difficult to guarantee to reach the requirement of stable processing technique blanking.Powdery alpha-sulfo-fatty acid alkyl ester salt easily produces false caking after transportation and heap pressure, needs can use becoming crumby material powder to be broken into tiny particle through processing, if storage period is longer, there will be serious agglomeration problems.Have data to show, MES is applied in washing powder, and the product stock time has been grown and there will be offending smell.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt.The composition for detergent mobility making through the method is apparently higher than alpha-sulfo-fatty acid alkyl ester salt itself, and it is agglomerating to be difficult for bonding, stable in properties, meet the requirement of stable processing technique blanking, and the unhappy smell that can effectively suppress containing alpha-sulfo-fatty acid alkyl ester salt powdered detergent in storage process produces.
The object of the invention is to be achieved through the following technical solutions: a kind of preparation method of the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt, comprises the following steps:
(1) adopt spray pattern that nonionogenic tenside is evenly sprayed on powdery alpha-sulfo-fatty acid alkyl ester salt, stir to form the mixture that ionic surfactant pack is wrapped up in powdery alpha-sulfo-fatty acid alkyl ester salt on sprinkling limit, limit, a described nonionogenic tenside part is the internal penetration to MES particle by osmosis, another part has formed liquid nonionic film integument on composite particles surface, this nonionic film integument is kept apart MES and external environment, stop extraneous moisture to MES effect, and as the required binding agent of the attached polymer molding in subsequent handling,
(2) in the middle mixture forming of step (1), add zeolite, be mixed into composition for detergent, under the effect of the lip-deep liquid nonionic film integument of composite particles that described zeolite forms in step (1), there is the solid-state integument of mixture outside formation that nodulizing forms in step (1), the liquid nonionic of the composite surface forming in step (1) is adsorbed simultaneously, make composition not there is adhesive.The adsorption of zeolite has improved the mobility of the mixture forming in step (1).
The described zeolite of step of the present invention (2) is 4A zeolite.
The present invention also comprises step (3): the composition for detergent that described step (2) obtains, through the processing of sieving, obtains the composition for detergent powder of the particle diameter that meets production requirement.
The order number adopting when the composition for detergent in step of the present invention (3) sieves is sieve more than 16 orders, and preferably order number is sieve more than 20 orders.
The present invention can adopt drum tumbler to produce continuously, also can adopt batch production.And in batch production, for fear of occurring larger coarse particles, operation below concrete employing;
(1) to powdery alpha-sulfo-fatty acid alkyl ester salt, spray the nonionogenic tenside of 3 ~ 5 minutes, stir on sprinkling limit, limit, to form the mixture that ionic surfactant pack is wrapped up in powdery alpha-sulfo-fatty acid alkyl ester salt;
(2) add part zeolite, mix 10 ~ 15 minutes, to being uniformly dispersed;
(3) repeating step (1) and step (2), until the nonionogenic tenside in same batch and zeolite interpolation are complete, can obtain the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt.
The described zeolite of step of the present invention (2) is 4A zeolite.
The present invention also comprises step (4): the composition for detergent that described step (3) obtains, through the processing of sieving, obtains the composition for detergent powder of the particle diameter that meets production requirement.
The order number adopting when the composition for detergent in step of the present invention (4) sieves is sieve more than 16 orders, and preferably order number is sieve more than 20 orders.
the present invention compared with prior art has the following advantages:
The present invention forms the solid-state integument of one deck by using effect by liquid non-ionic surfactant to make the zeolite of dryness can nodulizing occur on the surface of MES particle, thereby reaches the object that MES is isolated from the outside.Be coated in MES particle surface liquid nonionogenic tenside some by osmosis, penetrate into MES granule interior, form mixture with MES, a part forms solid-state integument with the surface that zeolite acts on composite particles.By the MES composition of processing, be equivalent to MES surface again and established the protective layer of twice: outside be solid-state zeolite layer together, mainly play and improve liquidity, next plays and stops moisture, basic material to cause that to the effect of MES particle MES is hydrolyzed into the reaction of undesirable product disodium salt; The inside be nonionogenic tenside layer together, mainly utilize nonionogenic tenside and water directly to contact the character that easily forms gel, stop moisture to enter into by simple osmosis the hydrolysis that MES layer causes MES, the molecular sieve structure that moisture is entered zeolite by outer field zeolite adsorption under the obstruction of nonionogenic tenside layer is inner.
MES after treatment can effectively protect under the effect of protective layer the MES particle of the inside to avoid the impact of extraneous chemical substance outside, can effectively suppress alpha-sulfo-fatty acid alkyl ester salt and be applied in the generation of unpleasant peculiar smell in storage process after washing powder product; And agglomerating, the powdery alpha-sulfo-fatty acid alkyl ester salt false caking after transportation and heap are pressed of effectively avoiding boning between MES particle.
The mobility of composition prepared by the present invention occurs significantly to change, and mobility is significantly better than raw material powdery MES.Tiny MES(is mainly that particle diameter is less than 100 object MES particles) under the effect of nonionogenic tenside, there is the aggregate that nodulizing forms larger particles in particle, the dust that MES causes is reduced significantly, efficiently solve the dust problem existing in powdery MES use procedure; Within the shelf lives of short-term, reduce the tendency of material clumps, thereby solved the problem of material blanking difficulty in washing powder production process, improved the in-situ production environment of washing powder.
Embodiment
Below in conjunction with embodiment and test example, the present invention is set forth.
The preparation method of following examples 1 ~ 6 can adopt consecutive production mode, also can adopt the intermittent mode of production.
produce continuously:
(1) by proportioning, get nonionogenic tenside, powdery alpha-sulfo-fatty acid alkyl ester salt (MES) and zeolite.
(2) powdery MES by bin blanking to below conveying belt, after metering, be delivered in drum tumbler, nonionic spraying gun is arranged near drum tumbler feeding mouth place, nonionogenic tenside is piped to by the volumetric pump profit of pressurizeing the drop that forms atomization on the atomizing nozzle being arranged in drum tumbler, be dispersed in powdery MES particle, sprinkling limit, limit stirs into the mixture of nonionogenic tenside and powdery MES, a described nonionogenic tenside part is the internal penetration to MES particle by osmosis, another part has formed the liquid nonionic film of one deck integument on composite particles surface, this nonionic film integument is kept apart MES and external environment, stop extraneous moisture to MES effect, and as the required binding agent of the attached polymer molding in subsequent handling.
(3) from drum tumbler stage casing, add 4A zeolite, composite particles surface in the 4A zeolite agglomeration of the second half section of drum tumbler at MES and nonionogenic tenside, mix and obtain composition for detergent, under the effect of the lip-deep liquid nonionic film integument of composite particles that 4A zeolite forms in step (2), there is nodulizing and form solid-state integument, MES is wrapped up, make between composition grain, not there is adhesive.
(4) composition for detergent step (3) the being obtained processing of sieving, adopts 16 mesh sieves or 20 mesh sieves while sieving, obtain the composition for detergent powder of the particle diameter that meets production requirement.
batch production:
(1) by proportioning, get nonionogenic tenside, powdery alpha-sulfo-fatty acid alkyl ester salt (MES) and zeolite.
(2) powdery MES is placed in to mixing equipment, opening device, by atomisation unit by nonionogenic tenside atomization, nonionogenic tenside drop after atomization is dispersed in powdery MES particle, and at the liquid nonionic film of the surface of MES particle formation one deck, stir on sprinkling limit, limit, and this process exists tiny powdery MES that nodulizing phenomenon occurs and forms oarse-grained agglomerate.Nonionogenic tenside spraying time was controlled within the scope of 3 ~ 5 minutes.
(2) add part zeolite, mix 10 ~ 15 minutes, to being uniformly dispersed;
(3) repeating step (1) and step (2), until the nonionogenic tenside in same batch and zeolite interpolation are complete, can obtain the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt, part nonionogenic tenside and powdery alpha-sulfo-fatty acid alkyl ester salt form mixture, and form liquid nonionic film integument on powdery alpha-sulfo-fatty acid alkyl ester salt surface, zeolite and remainder nonionogenic tenside form solid-state integument on described composite particles surface, and powdery alpha-sulfo-fatty acid alkyl ester salt is isolated from the outside.
(4) composition for detergent that described step (3) obtains, through the processing of sieving, adopts 16 mesh sieves or 20 mesh sieves while sieving, obtain the composition for detergent powder of the particle diameter that meets production requirement.
Proportioning between nonionogenic tenside described in above-mentioned preparation, powdery alpha-sulfo-fatty acid alkyl ester salt and zeolite is:
Nonionogenic tenside 1.0 ~ 6.0%
Powdery alpha-sulfo-fatty acid alkyl ester salt 65 ~ 94%
Zeolite 5 ~ 34%;
Above-mentioned nonionogenic tenside adopts ethoxylated alcohol nonionic surfactant.Ethoxylated alcohol nonionic surfactant comprises that average degree of ethoxylation is the C of 3 ~ 10 ethoxylation
10 ~ 16alcohol, as: AEO7, AEO9, XL-80, SA-9, FMEE, TO-10 etc.The C of the ethoxylation that further, the preferred average degree of ethoxylation of the present invention is 7 ~ 9
10 ~ 16straight chain alcohol or branched-chain alcoho, as: AEO7, AEO9, XL-80 etc.
The general formula of above-mentioned alpha-sulfo-fatty acid alkyl ester salt is:
,
Wherein, R
1that average carbon atom number is 8~20 alkyl, R
2be that average carbon atom number is 1~4 alkyl, n=1 or 2, M are selected from Na
+, K
+, Li
+, NH
4 +, Ca
2+, Mg
2+or their mixture.Preferred R
1that average carbon atom number is 14~16 alkyl, R
2for methyl, M is Na
+.
For the index of balance mobility and solvability two aspects proposes granularity requirement.Particle size large fluidity is good, dust is few, but solvability is poor, otherwise solvability is good, dust is large, poor fluidity, easily conglomeration, be unfavorable for production operation.Therefore, the size of powdery alpha-sulfo-fatty acid alkyl ester salt of the present invention require be: 90%(weight) above alpha-sulfo-fatty acid alkyl ester salt particle size within the scope of 20 order ~ 100 orders.Further, the size of described powdery alpha-sulfo-fatty acid alkyl ester salt requires to be preferably: 90%(weight) above alpha-sulfo-fatty acid alkyl ester salt particle size within the scope of 30 order ~ 90 orders.
Adopt the benefit of 4A zeolite to be: 4A zeolite is current most widely used phosphorus-free adjuvant, itself there is water-insoluble characteristic, inner trickle cage structure can be limited in internal space by the part moisture of absorption, can effectively prevent composition in storage process because there is deliquescence in the moisture absorption, conglomeration, simultaneously, 4A zeolite also has stronger adsorptive liquid material (nonionogenic tenside, as AEO7, AEO9) ability, can make composition have dry and comfortable state, in above characteristic 4A zeolite, can make composition have with respect to the single good mobility of powdery MES.
testing method
2.1. fluidity testing method:
With reference to the measurement at GB 11986-89 surfactant powders and particle slope of repose (corresponding national standard number and title).Less according to the slope of repose of the definition powder at slope of repose, show that the frictional force between powder granule is less, also just the mobility of less powder is also just better for the resistance that powder runs in mobile process.It is generally acknowledged good fluidity when θ≤30 °, during θ≤40 °, can meet the need for liquidity in production process, result is referring to table 1.
2.2. improve washing powder finished product and store smell
In table 1, get the composition for detergent of embodiment 3 for the preparation of washing powder, comparative example 1 ~ 4 is the washing powder directly to prepare with 85% MES, and two kinds of washing powder carry out accelerated test, investigate the storage smell whether the present invention can improve washing powder.
1 ~ 7 starting material in the preparation method of washing powder: embodiment 7 ~ 10 and comparative example 1 ~ 4 are all prepared into washing powder base-material by the mode of high tower spray drying, 8 ~ 12 starting material all add in washing powder base-material in the rear allotment of labor's order stage by washing powder production technique, finally obtain washing powder finished product.
Accelerated test method: testing sample is installed by the PET clear vial of 80 milliliters of volumes, reach the effect of sealing by covering tightly lid, the amount of sample accounts for 2/3rds of bottle volumetric quantity.Sample is placed in to 45 ℃/60% humidity, under 48 ℃ of two different conditions, carries out the accelerated test of 4 weeks.Sample after test judges the character of smell by sense of smell, the results are shown in Table 2 and table 3.
Above embodiment is only for setting forth the present invention, and protection scope of the present invention is not only confined to above embodiment.Those skilled in the art, according to above content disclosed by the invention and scope that each parameter is got, all can realize object of the present invention.
Claims (2)
1. contain a preparation method for the composition for detergent of alpha-sulfo-fatty acid alkyl ester salt, it is characterized in that, comprise the following steps:
(1) adopt spray pattern that nonionogenic tenside is sprayed on powdery alpha-sulfo-fatty acid alkyl ester salt, stir to help form the mixture of nonionogenic tenside and powdery alpha-sulfo-fatty acid alkyl ester salt on sprinkling limit, limit, a described nonionogenic tenside part is the internal penetration to MES particle by osmosis, and another part has formed the liquid nonionic film of one deck integument on the surface of composite particles;
(2) in the mixture in step (1), add zeolite, be mixed into composition for detergent, described zeolite forms solid-state integument by there is nodulizing under the effect of the lip-deep liquid nonionic film integument of composite particles forming in step (1) on surface;
In described composition,
Nonionogenic tenside 1.0 ~ 6.0%
Powdery alpha-sulfo-fatty acid alkyl ester salt 65 ~ 94%
4A zeolite 5 ~ 34%.
2. the preparation method of the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt according to claim 1, it is characterized in that, also comprise step (3): the detergent composition that described step (2) the obtains processing of sieving, obtains the composition for detergent powder of the particle diameter that meets production requirement.
3. the preparation method of the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt according to claim 2, is characterized in that, the mixture in described step (3) adopts order number while sieving be sieves more than 16 orders.
4. contain a preparation method for the composition for detergent of alpha-sulfo-fatty acid alkyl ester salt, it is characterized in that, comprise the following steps:
(1) to powdery alpha-sulfo-fatty acid alkyl ester salt, spray the nonionogenic tenside of 3 ~ 5 minutes, stir on sprinkling limit, limit, to form the mixture that ionic surfactant pack is wrapped up in powdery alpha-sulfo-fatty acid alkyl ester salt;
(2) add part zeolite, mix 10 ~ 15 minutes, to being uniformly dispersed;
(3) repeating step (1) and step (2), until the nonionogenic tenside in same batch and zeolite interpolation are complete, can obtain the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt;
In described composition,
Nonionogenic tenside 1.0 ~ 6.0%
Powdery alpha-sulfo-fatty acid alkyl ester salt 65 ~ 94%
4A zeolite 5 ~ 34%.
5. the preparation method of the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt according to claim 4, it is characterized in that, also comprise step (4): the detergent composition that described step (3) the obtains processing of sieving, obtains the composition for detergent powder of the particle diameter that meets production requirement.
6. the preparation method of the composition for detergent containing alpha-sulfo-fatty acid alkyl ester salt according to claim 5, is characterized in that, the mixture in described step (3) adopts order number while sieving be sieves more than 16 orders.
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