CN1120228C - Process for making low density detergent compsn. by non-tower process - Google Patents
Process for making low density detergent compsn. by non-tower process Download PDFInfo
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- CN1120228C CN1120228C CN 96180525 CN96180525A CN1120228C CN 1120228 C CN1120228 C CN 1120228C CN 96180525 CN96180525 CN 96180525 CN 96180525 A CN96180525 A CN 96180525A CN 1120228 C CN1120228 C CN 1120228C
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Abstract
The present invention provides a non-tower method for continuously preparing a granulated detergent composition with low-density (optimising about 300 to 600 g/l). The method comprises the following steps: (a), firstly, dispersing an aqueous or a non-aqueous surfactant, and secondly, coating the surfactant by fine powder with the particle diameter of 0.1 to 500 mu m under certain condition in a mixer to obtain irregularly shaped granules and excessive fine powder; (b), spraying finely atomized liquid to the irregularly shaped granules and the excessive fine powder from the step (a) in another mixer under certain condition to stick the excessive fine powder onto the irregularly shaped granules.
Description
Invention field
The present invention relates to a kind of method of producing low density detergent composition by non-tower process.More particularly, the present invention relates to a kind of continuous production method, in the production process of this method, produce detergent agglomerate by adding tensio-active agent and coating in a series of mixing tanks.Method of the present invention can be produced free-pouring detergent composition, and its density can be in the regulated in wider range of consumer wants, and described product can carry out market sale.
Background of invention
In recent years, the product that receives much concern in the cloth-washing detergent industry is the concentrated type product with low dosage volume.For these so-called low dosage washing composition of favourable production, people have carried out multiple trial to produce the higher washing composition of volume density, and for example, density is 600g/l or higher.Because this low dosage washing composition can be saved resource and small packages form that can more convenient human consumer is sold, thereby its demand is increased day by day.Yet in fact, modern Betengent product answers " concentrating " to which kind of degree on earth, is still uncertain.In fact, many human consumers', particularly developing country human consumer still is a preference employing high dosage in each laundry operations.By the currently known methods of agglomeration process production modern detergent compositions, promptly the universals of Fei Tafa are, prepare its particulate apparent density through this method and are not less than 600g/l usually.Like this, the whole density that still need in agglomeration technique (as Fei Tafa), produce final composition have the modern washing composition, particularly low density detergent composition of certain handiness (as, density range is about 300-600g/l).
In general, the method for preparing washing agent particle or powder mainly comprises three types.First method relates in spray-drying tower carries out spraying drying to the aqueous detergent slurries, produces porous detergent particles (the tower method that for example, is used for low density detergent composition).Second method is included in the spray-drying tower carries out spray-dired step as first step to the aqueous detergent slurries, then, with particle and a kind of tackiness agent agglomeration such as nonionogenic tenside or anion surfactant that forms, at last, various detergent components are done mixed, produce detergent particles (for example, the tower method adds agglomeration technique, is used for high density detergent composition).In the third method, various detergent components do are mixed, after this, make itself and tackiness agent agglomeration such as nonionogenic tenside or anion surfactant, produce high density detergent composition (as, be used for the agglomeration technique of high density detergent composition).In above-mentioned three kinds of methods, the important factor of the detergent particles that control forms is described coating of particles, porosity and size distribution, the density of various raw materials, the shape of various raw materials and they chemical constitution separately.
Attempt to provide the method that can increase detergent particles or powder density in this area always.Particularly make spray-dired particle densification by the tower post treatment method.For example, one of means relate to carries out batch production, wherein, and at Marumerizer
In will comprise the spraying drying of tripoly phosphate sodium STPP and sodium sulfate or granulation detergent powder carry out densification and make ball-type.Described equipment comprises substantially horizontal, unsmooth and rotatable worktable, and this worktable is positioned at the housing of perpendicular and inner wall smooth.Yet,, be not suitable for the scale operation detergent powder because this method is a kind of periodical operation process.At last, people also attempt to provide the density of the detergent particles of a kind of continuation method to increase " behind the tower (post-tower) " or spraying drying and cross.Usually, these class methods need be pulverized or grind particulate first device and increase second of pulverizing back pellet density by agglomeration and install.Though these methods by handle or densification " behind the tower " or spraying drying after particle increased density, can not reach higher at the situation lower surface promoting agent activity level that does not apply subsequently, thereby be restricted.In addition, by " behind the tower " method handle or densification from considering economically and uneconomical (cost is very high), and production process complexity.And then all aforesaid methods all relate generally to and carry out densification or processing spray-dried granules.At present, there is quite a lot of dissimilar material in the washing composition production process, to be subject to spray-drying process.For example, in the detergent composition that forms, will be difficult to realize the tensio-active agent high-content, the high-content of tensio-active agent then is to impel the feature of producing washing composition in more effective mode.Therefore, still wish to find a kind of method that is not subjected to the production detergent composition of conventional spray drying technology restriction.
For this reason, also propose the various detergent composition that make in this area and carried out agglomerant method.For example, mix in mixing tank by making zeolite and/or layered silicate, and make the detergent builders agglomeration to form free-pouring agglomerate.Though this trial explanation, aforesaid method can be used for producing detergent agglomerate; But they do not provide a kind of mechanism, illustrate that pasty state, liquid and dry-matter shape detergent raw material are agglomerated into effectively has more low-density crisp, free-pouring detergent agglomerate.
Thereby, still need to seek a kind of agglomeration method (Fei Tafa) that is used for direct by detergent raw material continuous production low density detergent composition in this area, preferably its density can realize by regulating processing conditions.Equally, still wish to find a kind of more effective, have more adaptability and more economical method so that the scale operation washing composition, the final densities of washing composition final composition is answered the tool handiness.
Prior art
Following reference relates to the process that makes spray-dired particle densification: Appel etc., US5,33,924 (Lever); Bortolotti etc., US5,160,657 (Lever); Johnson etc., GB1,517,713 (Unilever); And Curtis, EP451,894.
Following reference relates to by agglomeration produces washing composition: Charles etc., US4,992,079 (FMC Corporation); Beujean etc., WO93/23,523 (Henkel); Beerse etc., US5,108,646 (Procter ﹠amp; Gamble); Capeci etc., US5,366,652 (Procter ﹠amp; Gamble); Hollingsworth etc., EP351,937 (Unilever); Swatling etc., US5,205,958.
For example, WO93/23,523 disclose a kind of method, and this method comprises by low speed mixer carries out pre-agglomeration, carries out agglomeration with high-speed mixer again, obtains high density detergent composition, and said composition has the following grain diameter of 25wt% to surpass 2mm.This method also discloses a kind of method, adopts this method, can regulate the density of last agglomerate by the consumption of regulating the liquid adhesive that adds in second mixing machine.But, from the document, can not be clear that the reason that density reduces.WO93/23, it is clearly for a person skilled in the art that 523 methods are different from method of the present invention.
US4,992,079 disclose a kind of agglomeration method that is used for the low density free phosphate detergent, and described washing composition is enhanced aspect oozing out at the antagonism nonionic.First procedure of processing is to make detergent component and the agglomeration of on-aqueous liquid tensio-active agent, second step then is to be carried on surfactant-dispersed on the particle in the rare gas element medium, the wetting dispersed particles of spray flow with the spray flow of sodium silicate aqueous solution or the water that separates concentrates water glass to form agglomerant washing composition.But it is that what reason causes producing low density on earth that the document does not clearly indicate.In addition, the document does not comprise aqueous surfactant and phosphorus-containing detergent yet.US4, it is clearly for a person skilled in the art that 992,079 method is different from method of the present invention.
Summary of the invention
The invention provides a kind of method of producing low-density particles shape detergent composition, can satisfy the demand of this area.The present invention also provides a kind of whole density of producing its final composition by agglomeration process (as Fei Tafa) that the method for the granular detergent composition of certain handiness is arranged, thereby satisfies the demand of this area.Method of the present invention can be by controlling the density that coating of particles is regulated composition grain.That is to say that method of the present invention can be used to obtain low-density granular detergent composition, and (for example, the density of irregularly shaped particles is about 300～600g/l).Described method does not adopt the conventional spray-drying tower of surfactant content in the meeting limit combination.In addition, consider and in described method, to produce various detergent composition that method of the present invention seems more effectively, more economical and have more handiness.And then because method of the present invention does not adopt and can discharge particulate matter and volatile organic compounds usually and enter spray-drying tower in the atmosphere, therefore, method of the present invention also is useful aspect environment protection.
Herein, term " agglomerate " is meant by with raw material and tackiness agent, carries out nodulizing and the particle that forms as tensio-active agent and/or inorganic solution/organic solvent and polymers soln.Herein, term " irregularly shaped particles " is meant by agglomeration raw material, fines and fine atomized liquid and forms under the low density principle condition to have erose particle.Except as otherwise noted, all herein percentage number averages are meant weight percentage.
According to one aspect of the present invention, a kind of method for preparing low-density granular detergent composition is provided, preferably its density is about 300-600g/l.This method comprises the steps:
(a) (i) disperse moisture or non-water surface promoting agent; With
In a mixing tank, be the fine powder coated surfaces promoting agent of 0.1～500 μ m with particle diameter (ii), obtain particle, described mixing tank is operated under the following conditions:
[mean residence time: about 5～30 seconds, upset tip velocity (Tip speed): about 5～10m/s, energy condition: about 0.15～4.20kj/kg]; Then
(b) in another mixing tank, little atomized liquid is sprayed to from the particle of step (a) and the excessive fine powder, described mixing tank is operated under the following conditions so that excessive fine powder is bonded on the erose particle.
[mean residence time: about 0.2～5 second, upset tip velocity: about 10～23m/s, energy condition: about 0.15～2.9kj/kg].
The present invention also provides the low-density particles shape detergent composition of being produced by any method embodiment of the present invention, and the density of preferred composition is about 300～600g/l.
Therefore, an object of the present invention is to provide a kind of method of continuous production detergent composition, in this method, energy input, residence time condition and upset tip velocity condition by the control mixing tank can make the density of finished product have more handiness.Another object of the present invention provide a kind of more effective, have more handiness and more economical method, to promote the washing composition of scale operation low dosage level and high dosage level.By reading the following preferred embodiment of the present invention and claims, these purposes of the present invention, characteristics and advantage will be clearly to one skilled in the art.
The accompanying drawing summary
Fig. 1 is after the method the first step of the present invention, has the low density (picture of 475～530g/l) irregularly shaped agglomerate.
Fig. 2 after the method the first step of the present invention and second goes on foot, has the low density (picture of 475～500g/l) irregularly shaped agglomerate.
Fig. 3 is after the method the first step of the present invention and second step and drying and the process of cooling, has the low density (picture of 450～475g/l) irregularly shaped agglomerate.
Fig. 4 for be used to obtain high-density (behind about 700～800g/l) the agglomeration process, the picture of circular agglomerate.
Detailed Description Of The Invention
The present invention relates to a kind of method of producing free-pouring low-density particles shape agglomerate, described The density of agglomerate is not less than about 300g/l, preferred about 300～600g/l. The method is by moisture Or non-water surface activating agent production detergent granules agglomerate, apply particle diameter at surfactant Be the fine powder of about 0.1～500 μ m, to obtain low-density particles.
Method The first step
In the first step of the inventive method, with Powdered, pasty state or liquid one or more Moisture or non-water surface activating agent and particle diameter are 0.1～500 μ m, preferred about 1～100 μ m's Fine powder will add in the blender (definition of surfactant and fine powder below will be described in detail).
In following another embodiment of the invention that will more be discussed in detail, before agglomeration, Can earlier surfactant be added blender or premixed device (such as screw extruder or other class of routine Like blender), after this, as described herein, in the blender that carries out the first step, add and mix The washing agent material carries out agglomeration.
In general, for reach low-density (about 300～600g/l), average in blender The time of staying should be about 5～30 seconds, and the upset tip (circumferential) velocity (speed) of blender should be about 5～10m/s, The energy of unit mass is about 0.15～4.20kj/kg, more preferably mean residence time in the blender Should be about 10～15 seconds, the upset tip (circumferential) velocity (speed) of blender should be about 6～8m/s, blender The energy of middle unit mass is about 0.15～2.5kj/kg, and most preferably mean residence time should be approximately 10～15 seconds, the upset tip (circumferential) velocity (speed) of blender should be about 6.5～7.5m/s, and is single in the blender The energy of position quality is about 0.15～1.30kj/kg.
The blender that is used for first step processing can be the blender of any type well known in the art, As long as blender can keep above-mentioned condition for the first step. Instantiation is by L dige The L dige CB blender that company (Germany) produces. The result of the first step is to obtain particle The particle (Fig. 1) that has fine powder on the surface.Second step
In the second step of the inventive method, the product that the first step is formed (particle and excessive thin Powder) adds in second blender, spray mist liquid on the particle in this blender then. For the excessive fine powder from the first step is bonded on the particle, can add in the second step about 0～10%, preferred about 2～5% the powder detergent component and/or other washing that are used for the first step The agent component.
In general, for reach low-density (about 300～600g/l), at the blender of second step In mean residence time should be about 0.2～5 second, the upset tip (circumferential) velocity (speed) of second step blender should Be about 10～23m/s, the energy of unit mass is about 0.15～2.9 in the second step blender Kj/kg, more preferably mean residence time should be about 0.5～2 second, the upset tip (circumferential) velocity (speed) of blender Should be about 13～20m/s, the energy of unit mass is about 0.15～1.9kj/kg in the blender, First-selected mean residence time should be about 0.5～2 second, and that the tip (circumferential) velocity (speed) of blender should be is about 15～17.5m/s the energy of unit mass is about 0.15～1.0kj/kg in the blender.
The blender that is used for second step processing can be the blender of any type well known in the art, As long as blender can keep above-mentioned condition for second step. Instantiation is by Schugi The Flexomic type blender that company (Holland) produces. The result of second step is, can obtain Granular detergent composition (Fig. 2).
With the method phase that well known to a person skilled in the art excessive circulation fine powder in the conventional agglomeration method Ratio, method of the present invention have reduced the excessive circulation fine powder from second step astoundingly. Exist Excessive fine powder can cause logistics excessively to circulate, and this can cause confusion to the method, thereby from economy Upper theory is non-remunerative.
According to the present invention, be generally about 10～40% of fine powder total amount in the first step from the circulation fine powder amount in second step.
Detergent raw material
Be used for tensio-active agent of the present invention and comprise following washing composition material, i.e. mist liquid and aucillary detergent composition, it is about 5～60% that its total amount accounts in the final product that obtains by the inventive method usually, preferred about 12～40%, and more preferably from about 15～30%.Should be included in above-mentioned tensio-active agent can be from arbitrary part of the inventive method, for example, and from the first step or from second step, perhaps from two steps of the present invention.
Detergent surfactant (moisture and/or non-water)
In the total amount by the final product that obtains of the inventive method, it is about 5～60% that the consumption of moisture or non-water surface promoting agent of the present invention can be, preferred about 12～40%, and more preferably 15～35%.
Moisture or the non-water surface promoting agent of the inventive method is as the detergent raw material of the above-mentioned the first step, and this tensio-active agent can be powder stock form or pasty state raw material form.
Tensio-active agent can be selected anion surfactant, nonionogenic tenside, zwitterionics, amphoterics, and their compatible mixtures.Adoptable detergent surfactant is disclosed in the following document: US3, and 664,961 (Norris, 1972.5.23 authorizes), US3,929,678 (Laughlin etc., 1975.12.30 authorizes), these two pieces of documents all are incorporated herein by reference.Adoptable cats product is disclosed in the following document: US4, and 222,905 (Cockrell, 1980.9.16 authorizes) and US4,239,659 (Murphy, 1980.12.16 authorizes), these two pieces of documents also are incorporated herein by reference.Described tensio-active agent preferably adopts anion surfactant and nonionogenic tenside and anion surfactant most preferably.
The non-limiting example that is preferred for anion surfactant of the present invention comprises: conventional C
11～C
18Alkylbenzene sulfonate (" LAS "), uncle's side chain and random C
10～C
20The C of alkyl-sulphate (" AS "), following formula
10～C
18Secondary (2,3) alkyl-sulphate: CH
3(CH
2)
x(CHOSO
3 -M
+) CH
3And CH
3(CH
2)
y(CHOSO
3 -M
+) CH
2CH
3, wherein, x and the integer that (y+1) is at least about 7, preferably at least about 9, M is water-soluble cationic, particularly sodium, unsaturated vitriol such as oleyl sulfate, C
10～C
18Alkyl alkoxy sulfate (" AE
xS ", EO1-7 ethoxy sulfate particularly).
Adoptable anion surfactant also comprises and contains 2～9 carbon atoms of having an appointment in the acyl group, and paraffin section contains the water-soluble salt of the 2-acyloxy-alkane-1-sulfonic acid of 9～23 carbon atoms of having an appointment; The water-soluble salt that contains the alkene sulfonic acid of about 12～24 carbon atoms; Moieties contains the β alkoxy alkane sulfonate that about 1～3 carbon atom and paraffin section contain about 8～20 carbon atoms.
Being used for optional other tensio-active agent example of the present invention comprises: C
10～C
18Alkyl alkoxy carboxylate salt (particularly EO1-5 ethoxy carboxylate), C
10～C
18Glyceryl ether, C
10～C
18Alkyl poly glucoside and corresponding sulfation glycan glycosides and C
12～C
18α-sulfonated fatty acid ester.If necessary, in composition, also can comprise conventional nonionogenic tenside and amphoterics, as: C
12～C
18Alkylethoxylate (" AE ") comprises so-called narrow peak value alkylethoxylate and C
6～C
12Alkyl phenolic alkoxy thing (the particularly mixture of ethoxylate and ethoxylate and propoxylated glycerine); C
10～C
18Amine oxides etc. also can be included in the final composition.Also can use C
10～C
18N-alkyl polyhydroxy fatty acid amide.Its representative instance comprises C
12～C
18The N-methyl glucose amide.Referring to WO9,206,154.Other comprises N-alkoxyl group polyhydroxy fatty acid amide by sugared deutero-tensio-active agent, as C
10～C
18N-(3-methoxy-propyl) glucamide.The N-propyl group is to N-hexyl C
12～C
18Glucamide can be used in the low-sudsing detergent.Also can adopt C
10～C
20Conventional soap.High if desired foam can use the C of side chain
10～C
16Soap.The preferred mixture that adopts anion surfactant and nonionogenic tenside.Other conventional tensio-active agent that adopts is listed in the standard textbook.
Cats product also can be used as detergent surfactant of the present invention, and suitable quaternary ammonium surfactant is selected from: single C
6～C
16, preferred C
6～C
10N-alkyl or alkenyl ammonium surfactant, wherein, remaining N position can be replaced by methyl, methylol or hydroxypropyl.
Amphoterics also can be used as detergent surfactant of the present invention, comprises the aliphatic derivatives of the heterocycle second month in a season and tertiary amine; Zwitterionics, can comprise aliphatic quaternary ammonium, quaternary phosphine and season sulfonium compound derivative; The water-soluble salt of α-sulfonated fatty acid ester; Sulfated alkyl ether; The water-soluble salt of alkene sulfonic acid; β-alkoxy alkane sulfonate; Formula R (R
1)
2N
+R
2COO
-Trimethyl-glycine, wherein, R is C
6～C
18Alkyl, preferred C
10～C
16Alkyl or C
10～C
16Amidoalkyl, each R
1Be generally C
1～C
3Alkyl, preferable methyl, R
2Be C
1～C
5Alkyl, preferred C
1～C
3Alkylidene group, more preferably C
1～C
2Alkylidene group.The example of suitable trimethyl-glycine comprises: coconut amido propyl-dimethyl trimethyl-glycine; The hexadecyldimethyl benzyl ammonium trimethyl-glycine; C
12～C
14Amido propyl betaine; C
8～C
14Amido hexyl diethyl betaines; 4[C
14～C
16Acyl group methyl amido diethyl ammonium]-1-carboxylic acid butane; C
16～C
18Acyl group amido dimethyl betaine; C
12～C
16Acyl group amido pentane diethyl betaines; C
12～C
16Acyl group methyl amido dimethyl betaine.Preferred trimethyl-glycine is C
12～C
18Dimethyl ammonium hexanoate and C
10～C
18Acyl group amido propane (or ethane) dimethyl (or diethyl) trimethyl-glycine; And formula R (R
1)
2N
+R
2SO
3 -Trimethyl-glycine, wherein, R is C
6～C
18Alkyl, preferred C
10～C
16Alkyl, more preferably C
12～C
13Alkyl, each R
1Be generally C
1～C
3Alkyl, preferable methyl, R
2Be C
1～C
6Alkyl, preferred C
1～C
3Alkylidene group, or preferred hydroxy alkylidene.The example of suitable trimethyl-glycine comprises C
12～C
14Dimethylammonio-2-hydroxypropyl sulfonate, C
12～C
14Amido propyl ammonium-2-hydroxypropyl trimethyl-glycine, C
12～C
14Dihydroxy ethyl ammonium propane sulfonate and C
16～C
18Dimethyl Ammonium hexane sulfonate, preferred C
12～C
14Amido propyl ammonium-2-hydroxypropyl trimethyl-glycine.
Fine powder
To be used for the first step raw material total amount, the fine powder amount that is used for the inventive method of the first step can be about 94～30%, preferred 86～54%.The raw material fine powder of the inventive method is preferably selected from anhydrous sodium carbonate, powdery tripoly phosphate sodium STPP (STPP), hydration tri-polyphosphate, powder sodium sulfate, silico-aluminate, crystalline layered silicate, nitrilotriacetic acid(NTA) (NTA), phosphoric acid salt, precipitated silicate, polymkeric substance, carbonate, Citrate trianion, Powdered tensio-active agent (as the powder alkane sulfonic acid) and from the recirculation fine powder of the inventive method, wherein, the median size of powder is 0.1～500 μ m, preferred 1～300 μ m, more preferably 5～100 μ m.When using hydration STPP as fine powder of the present invention, the hydration levels of preferred STPP should be not less than 50%.Silico-aluminate ion exchange material as washing assistant of the present invention preferably has high-calcium ionic exchange capacity and high switching speed simultaneously.Although be not bound by any theory, it is believed that this high-calcium ionic exchange velocity and ability are the functions of a plurality of interactional factors, described each factor derives from the method that produces the silico-aluminate ion exchange material.Like this, be used for silico-aluminate ion exchange material of the present invention, 605,509 (Corkill etc., Procter ﹠amp preferably according to US4; Gamble) produce, the document is incorporated herein by reference.
Because the high-exchange-capacity and the speed that can be provided by the sodium type all can not be provided for the potassium type and the Hydrogen of silico-aluminate, thereby, preferred " sodium " type silico-aluminate ion exchange material that adopts.In addition, the silico-aluminate ion exchange material is preferably the drying form, so that produce crisp as described in the present invention detergent agglomerate.Being used for silico-aluminate ion exchange material of the present invention preferably has and can optimize it as helping the particle diameter of washing composition effect.Herein, the median size of the described silico-aluminate ion exchange material of term " particle diameter " representative adopts the routine analysis technical measurement, for example microscope method of masurement and scanning electron microscope method (SEM).The particle diameter of silico-aluminate is preferably about 0.1～10 μ m, 0.5～9 μ m more preferably from about, first-selected about 1～8 μ m.
Preferably aluminosilicate salt ion exchange material has following formula
Na
z[(AlO
2)
z(SiO
2)
y]
xH
2O wherein, z and y are at least 6 integer, the mol ratio of z and y is about 1～5, x is about 10～264.More preferably silico-aluminate has following formula
Na
12[(AlO
2)
12(SiO
2)
12]
xH
2O wherein, x is about 20～30, preferred about 27.These preferred silico-aluminates are commercially available, for example are purchased with zeolite A, zeolite B and X zeolite.Perhaps, be applicable to that natural or synthetic silico-aluminate ion exchange material of the present invention can be according to US3, the described method preparation of 985,669 (Krummel etc.), the document is incorporated herein by reference.
The further feature that is used for silico-aluminate of the present invention is, their loading capacity is at least about 200 milligramequivalent calcium carbonate hardness/g (in dried state), and preferably this scope is about 300～352 milligramequivalent calcium carbonate hardness/g.In addition, another feature of silico-aluminate ion exchange material of the present invention is that their calcium ion exchange rate is at least about 2 grains (grain) Ca
++/ add human relations/minute/one restrain/add human relations, 6 grain Ca more preferably from about
++/ add human relations/minute/one restrain/add human relations.
Mist liquid
The total amount of the finished product that obtain in the inventive method, the little atomized liquid consumption that was used for for second step is about 1～10% (based on actives), preferred about 2～6% (based on activess).Little atomized liquid of the inventive method can be selected from liquid silicic acid salt, negatively charged ion or cats product, and it can be liquid form, moisture or non-aqueous polymer solution, water and its mixture.Other selectivity example that is used for the little atomized liquid of the present invention can be carboxymethylcellulose sodium solution, polyoxyethylene glycol (PEG) and dimethylene triamine pentamethyl-phosphonic acids (DETMP) solution.
The preferred embodiment that can be used as the anionic surfactant solution of the little atomized liquid of the present invention is about 88～97% active HLAS, about 30～50% active NaLAS, about 28% active A E3S solution, about 40～50% active liquid silicate etc.
The cats product and the suitable quaternary ammonium surfactant that can be used as the little atomized liquid of the present invention are selected from single C
6～C
16, preferred C
6～C
10N-alkyl or alkenyl ammonium surfactant, wherein, remaining N position is replaced by methyl, hydroxyethyl or hydroxypropyl.
The preferred embodiment that can be used as the moisture or non-aqueous polymer solution of the little atomized liquid of the present invention is a modified polyamine, and it comprises the polyamine backbone corresponding to following formula:
Has formula V
(n+1)W
mY
nThe modified polyamine of Z or corresponding to the polyamine backbone of following formula
Has formula V
(n-k+1)W
mY
nY '
kThe modified polyamine of Z, wherein, k is less than or equal to n, and the molecular weight of the polyamine backbone before the described modification is greater than about 200 dalton, wherein
I) the V unit is the terminal units with following formula:
Or
Or
Ii) the W unit is the skeleton unit with following formula:
Or
Or
Iii) the Y unit is the chain unit with following formula:
Or
Or
With
Iv) the Z unit is the terminal units with following formula:
Or
Wherein, the R unit of connection skeleton is selected from following radicals: C
2～C
12Alkylidene group, C
4～C
12Alkylene group, C
3～C
12Hydroxy alkylidene, C
4～C
12Alkyl sub-dihydroxy, C
8～C
12The dialkyl group arylidene ,-(R
1O)
xR
1-,-(R
1O)
xR
5(OR
1)
x-, (CH
2CH (OR
2) CH
2O)
z(R
1O)
yR
1(OCH
2CH (OR
2)-CH
2)
w-,-C (O) (R
4)
rC (O)-,-CH
2CH (OR
2) CH
2-and its mixture; Wherein, R
1Be C
2～C
6Alkylidene group and its mixture; R
2For hydrogen ,-(R
1O)
xB and its mixture; R
3Be C
1～C
18Alkyl, C
7～C
12Arylalkyl, C
7～C
12Aryl, C that alkyl replaces
6～C
12Aryl and its mixture; R
4Be C
1～C
12Alkylidene group, C
4～C
12Alkylene group, C
8～C
12Inferior aralkyl, C
6～C
10Arylidene and its mixture; R
5Be C
1～C
12Alkylidene group, C
3～C
12Hydroxy alkylidene, C
4～C
12Alkyl sub-dihydroxy, C
8～C
12The dialkyl group arylidene ,-C (O)-,-C (O) NHR
6NHC (O)-,-R
1(OR
1)-,-C (O) (R
4)
rC (O)-,-CH
2CH (OH) CH
2-,-CH
2CH (OH) CH
2O (R
1O)
yR
1OCH
2CH (OH) CH
2-and its mixture; R
6Be C
2～C
12Alkylidene group or C
6～C
12Arylidene; The E unit is selected from following radicals: hydrogen, C
1～C
22Alkyl, C
3～C
22Alkenyl, C
7～C
22Arylalkyl, C
2～C
22Hydroxyalkyl ,-(CH
2)
pCO
2M ,-(CH
2)
qSO
3M ,-CH (CH
2CO
2M) CO
2M ,-(CH
2)
pPO
3M ,-(R
1O)
xB ,-C (O) R
3And its mixture; Oxide compound; B is hydrogen, C
1～C
6Alkyl ,-(CH
2)
qSO
3M ,-(CH
2)
pCO
2M ,-(CH
2)
q(CHSO
3M) CH
2SO
3M ,-(CH
2)
q-(CHSO
2M) CH
2SO
3M ,-(CH
2)
pPO
3M ,-PO
3M and its mixture; M is hydrogen or water-soluble cationic, and its amount should be enough to satisfy charge balance; X is a water soluble anion; The m value is 4～about 400; The n value is 0～about 200; The p value is 1～6, and the q value is 0～6; The r value is 0 or 1; The w value is 0 or 1; The x value is 1～100; The y value is 0～100; The z value is 0 or 1.Most preferred polyethylene imine based example is that molecular weight is 1800 and polyethylene imine based by the further modification of ethoxylation, each nitrogen ethoxylation to about 7 ethylene oxide residues (PEI, 1800, E7).Preferred above-mentioned polymers soln and anion surfactant such as NaLAS premix.
Other preferred embodiment that can be used as the moisture or non-aqueous polymer solution of mist liquid of the present invention is the polycarboxylate dispersion liquid, can be by unsaturated monomer that will be suitable, and preferred acid shape unsaturated monomer carries out polymerization or copolymerization and prepares.The unsaturated monomer acid that can be aggregated to form suitable polycarboxylate comprises: vinylformic acid, toxilic acid (or maleic anhydride), fumaric acid, methylene-succinic acid, equisetic acid, methylfumaric acid, citraconic acid and methylene radical propanedioic acid.Having non-hydroxy-acid group in polycarboxylate is to suit as monomer fragments such as vinyl methyl ether, vinylbenzene, ethene, as long as this fragment is no more than about 40wt%.
The preferred molecular weight that adopts is for example preferably introduced below greater than 4000 homopolymerization polycarboxylate.Shi Yi homopolymerization polycarboxylate can be obtained by vinylformic acid especially.Thisly be used for the water-soluble salt that acrylic acid based polymer of the present invention is a polymeric acrylic acid.The molecular-weight average of this polymeric acid form preferred more than 4,000 to 10,000, preferred more than 4,000 to 7,000, first-selected more than 4,000 to 5,000.The water-soluble salt of this acrylate copolymer for example comprises the ammonium salt of an alkali metal salt, ammonium salt and replacement.
Also can use the copolymerization polycarboxylate, as vinylformic acid/maleic copolymer.This class material comprises the water-soluble salt of vinylformic acid and maleic acid.The molecular-weight average of this multipolymer acid form is preferably about 2,000～100,000, and more preferably from about 5,000～75,000, first-selected about 7,000～65,000.Vinylformic acid and the ratio of toxilic acid fragment in this multipolymer are generally about 30: 1～1: 1, more preferably from about 10: 1～2: 1.The example of the water-soluble salt of this vinylformic acid/maleic acid comprises the ammonium salt of its an alkali metal salt, ammonium salt and replacement.Above-mentioned polymers soln is preferably compound in advance with anion surfactant such as LAS.
The washing assistant composition
Can comprise in the detergent raw material of the inventive method other detergent ingredients and/or, in the subsequent step of the inventive method, can in detergent composition, mix various other compositions.These auxiliary components comprise other washing assistant, SYNTHETIC OPTICAL WHITNER, bleach-activating agent, suds suppressor or short infusion, anti-tarnishing agent, sanitas, soil-suspending agent, soil releasing agent, sterilant, pH regulator agent, non-washing assistant alkali source, sequestrant, terre verte, enzyme, enzyme stabilizers and spices.Referring to, US3,936,537 (1976.2.3 is issued to Baskerville, Jr etc.), the document is incorporated herein by reference.
Other washing assistant is selected from various water-soluble alkali metal salts, ammonium salt or the substituted ammonium salt of phosphoric acid, polyphosphoric acid, phosphonic acids, polyphosphonic acid, carbonic acid, boric acid, poly-hydroxy sulfonic acid, poly-acetate, carboxylic acid and poly carboxylic acid usually.An alkali metal salt of preferred above-mentioned acid, particularly sodium salt.That preferably use is phosphoric acid salt, carbonate, C
10～C
18Soap, polycarboxylate and its mixture.More preferably tripoly phosphate sodium STPP, tetrasodium pyrophosphate, Citrate trianion, tartrate, list and disuccinate and its mixture (stating as follows).
Compare with amorphous sodium silicate, the crystal type lamina sodium silicate obviously demonstrates calcium and the magnesium ion exchange capacity strengthens.In addition, lamina sodium silicate is preference magnesium ion but not calcium ion more, and this is the essential feature that guarantees that all basically " hard materials " are removed from washing water.Yet these crystal type lamina sodium silicates are more more expensive than amorphous silicate and other washing assistant usually.Thereby for economically viable laundry detergent is provided, the ratio of used crystal type lamina sodium silicate must careful selection.
Be applicable to that crystal type lamina sodium silicate of the present invention preferably has following formula
NaMSi
xO
2x+1YH
2O wherein, M is sodium or hydrogen, x is about 1.9～4, y is about 0～20.More preferably described crystal type lamina sodium silicate preferably has following formula
NaMSi
2O
5YH
2O wherein, M is sodium or hydrogen, y is about 0～20.These and other crystal type lamina sodium silicate is stated in following document: US4, and 605,509 (Corkill etc.), the document is incorporated herein by reference.
The specific examples of inorganic phosphate builders is that tripolyphosphate, tetra-sodium, the polymerization degree are about 6～21 polymerization metaphosphoric acid and ortho-phosphoric sodium and sylvite.The example of polyphosphonic acid washing assistant is the sodium of ethylidene diphosphonic acid and sylvite, ethane 1-hydroxyl-1, the sodium of 1-di 2 ethylhexyl phosphonic acid and sylvite and ethane, 1,1, the sodium of 2-tri methylene phosphonic acid and sylvite.Other phosphorus washing-aid compound is disclosed in the following document: US3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176 and 3,400,148; These documents all are incorporated herein by reference.
The example of without phosphorus inorganic builders is tetraborate decahydrate and SiO
2With alkali metal oxide weight ratio be about 0.5～4.0, preferred about 1.0～2.4 silicate.Be used for various an alkali metal salts, ammonium salt and substituted ammonium salt that water-soluble without phosphorus organic washing-assisting detergent of the present invention comprises poly-acetate, carboxylic acid, poly carboxylic acid and poly-hydroxy sulfonic acid.The example of poly-acetate and polycarboxylate washing assistant is sodium, potassium, lithium, ammonium and the substituted ammonium salt of ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), oxygen connection succsinic acid, mellic acid, benzene poly carboxylic acid and citric acid.
Polymer poly-carboxylate's washing assistant is stated in 308,067 (1967.3.7 is issued to Diehl) at US3, and the document is incorporated herein by reference.This class material comprises aliphatic carboxylic acid, as the homopolymer of toxilic acid, methylene-succinic acid, methylfumaric acid, fumaric acid, equisetic acid, citraconic acid and methylene radical propanedioic acid and the water-soluble salt of multipolymer.In these materials some can be used as the following stated water-soluble anionic polymer to be used, but only just can use when itself and non-soap type anion surfactant intimate mixture.
Other is suitable for polycarboxylate of the present invention and is the polyacetal carboxylation, as US4, and 144,226 (1979.3.13 is issued to Crtchfield etc.) and US4,246,495 (1979.3.27 is issued to Crtchfield etc.) are described, and these two pieces of documents all are incorporated herein by reference.These polyacetal carboxylations can be under polymerizing condition, and ester and a kind of polymerization starter of oxoethanoic acid placed the preparation of coming together.Formed polyacetal carboxylic acid ester is connected on the chemically stable end group again, makes polymeric acetal carboxylate stable, prevents its depolymerization rapidly in basic solution, changes into corresponding salt, and it is added in the detergent composition.Particularly preferred polycarboxylate washing assistant is the ether carboxylate lotion-aid combination, it comprises the combination of tartrate monosuccinic acid salt and tartrate disuccinate, and it is at US4, and 663, state in 071 (1987.5.5 is issued to Bush etc.), the document is incorporated herein by reference.
SYNTHETIC OPTICAL WHITNER and activator are at US4, and 412,934 (1983.11.1 is issued to Chung etc.) and US4 state in 483,781 (1984.11.20 is issued to Hartman), and two pieces of documents all are incorporated herein by reference.Sequestrant also is disclosed in US4, and the 17th hurdle the 54th of 663,071 (Bush etc.) walks to the 18th hurdle the 68th row, and the document is incorporated herein by reference.Foam properties-correcting agent also is optional member, is disclosed in US3,933,672 (1976.1.20 is issued to Bartoletta etc.) and US4, and in 136,045 (1979.1.23 is issued to Gault etc.), two pieces of documents all are incorporated herein by reference.
Be suitable for terre verte of the present invention at US4, state in 762,645 (1988.8.9 is issued to Tucker etc.), see that the 6th hurdle the 3rd walks to the 7th hurdle the 24th row, the document is incorporated herein by reference.Be applicable to that other decontamination lotion promoter of the present invention lists (the 13rd hurdle the 54th walks to 16 hurdles, 16 row) in the patent documentation of Baskerville, and, state in 663,071 (1987.5.5 is issued to Bush etc.) that the document is incorporated herein by reference at US4.
As with comparison of the present invention, by a series of mixing tanks, (mean density is that about 700～800g/l) picture is shown among Fig. 4 to the high-density agglomerate that obtains with operation under the condition different with the inventive method.Among Fig. 4, be used for agglomerant equipment and comprise L dige CB mixing tank (CB-30, under 500RPM, operate), be Schugi Flexomic mixing tank (under 2800RPM, operating) then, be L dige KM mixing tank (KM-600 adopts common plough formula mixer operations under 100RPM) at last.The material that is used to prepare Fig. 4 agglomerate is identical with material shown in Figure 2, all has a detailed description in following embodiment.
Optional procedure of processing
If wish to reduce the water content from the second step agglomerate, optional procedure of processing then of the present invention is a drying step.Drying step can adopt and well known to a person skilled in the art various drying plants.The preferred fluidized bed plant that adopts, this equipment will be discussed in the following discussion.
In another optional step of the present invention, will handle the detergent agglomerate of discharging by the process of cooling in cooling settings from fluidized-bed.Preferred equipment also is fluidized-bed.One or more stages that another optional procedure of processing is included in the following course of processing of giving an example add flowing property and/or the minimizing detergent composition excessive agglomeration of a kind of liniment to improve detergent composition: (1) can directly add liniment after fluidized bed cooler or moisture eliminator; (2) can between fluidized bed dryer and fluidized bed cooler, add liniment; (3) can and well known to a person skilled in the art at fluidized bed dryer and be used for adding liniment between the agglomerant moderate-speed mixers; And/or (4) can directly add to liniment and well known to a person skilled in the art and be used for agglomerant moderate-speed mixers and fluidized bed dryer.Liniment is preferably selected from silico-aluminate, silicate, carbonate and its mixture.Liniment not only can strengthen the free-flowing property of the detergent composition of formation, and can be by preventing or reducing excessive agglomeration and control agglomeration process, and is particularly all the more so when directly adding in the moderate-speed mixers.It is that the human consumer is desirable that washing composition has free-flowing property, and this makes that being easy to spoon in use gets washing composition.And those skilled in the art all knows, excessively the agglomeration meeting makes the flowing property and the aesthetic properties variation of final Betengent product.
Method of the present invention also can randomly comprise spray step, soon is being used for the present invention's first mixing tank and second mixing tank one or both of, or other tackiness agent in fluidized bed dryer and/or the fluidized bed cooler is sprayed.Add a kind of tackiness agent so that detergent component " bonding " or " adhesion " strengthen the agglomeration performance.Tackiness agent is preferably selected from water, anion surfactant, nonionogenic tenside, liquid silicon hydrochlorate, polyoxyethylene glycol, Polyvinylpyrolidone (PVP), polyacrylic ester, citric acid and its mixture.Other suitable binder substance comprises US5,108,646 (Beerse etc., Procter ﹠amp; Gamble Co.) described those, the document is incorporated herein by reference.
Other optional step of the inventive method is included in the detergent agglomerate that sieves oversize in the screening plant, and this screening plant can adopt various forms, includes, but is not limited to routine and is used for the selected sieve of the required particle diameter of final Betengent product.Other optional step comprises by the step of the further dry agglomerates of aforementioned device so that detergent agglomerate is nursed one's health.
Another optional step of the inventive method comprises that the whole bag of tricks that adopts sprinkling and/or mix other conventional detergent ingredients is to put in order the detergent agglomerate that forms.For example, described arrangement step comprises that sprinkling spices, whitening agent and enzyme are to the agglomerate of putting in order, so that more perfect detergent composition to be provided.This technology and used composition also well known to a person skilled in the art.
Below provide the representative example for preparing the serial mixing tank of granular detergent composition according to the inventive method and additional optional process:
(A) (1) carries out agglomeration in L dige CB type mixing tank, (2) in SchugiFlexomic type mixing tank, carry out agglomeration then, (3) in the Mogensens sifter, screen to remove particle greater than 4.5mm, (4) in fluidized bed dryer (Fluid Bed Dryer), carry out drying, (5) in fluidized bed cooler, cool off, (6) in the Mogensens sifter, screen to remove particle greater than 1.2mm, (7) carrying out crushing operation adds in fluidized bed dryer or fluidized bed cooler or the L dige CB mixing tank from the size of the excessive agglomerate of sifter and the agglomerate that (8) will pulverize with minimizing again;
(B) (1) carries out agglomeration in L dige CB type mixing tank, (2) in L dige KM type mixing tank, carry out agglomeration then, (3) in Schugi Flexomic type mixing tank, carry out agglomeration again, (4) in the Mogensens sifter, screen to remove particle greater than 4.5mm, (5) in fluidized bed dryer, carry out drying, (6) in fluidized bed cooler, cool off, (7) in the Mogensens sifter, screen to remove particle greater than 1.2mm, (8) carrying out crushing operation adds in fluidized bed dryer or fluidized bed cooler or the L dige CB mixing tank from the size of the excessive agglomerate of sifter and the agglomerate that (9) will pulverize with minimizing again.
Other basic step in described method comprises high reactivity paste construction process, as before the inventive method, by mix the cream hardening material with forcing machine moisture anion surfactant cream is carried out hardening treatment.The detailed description of high reactivity paste structured approach, referring to co-applications JA162F (1996.10.4 application), the document and the present invention are in application on the same day.
In order to make the present invention be easier to understand, with reference to following embodiment the present invention is described, but these embodiment only are used to illustrate the present invention, scope of the present invention are not had any restriction.
Embodiment
Embodiment 1:(is erose agglomerate after the first step of the present invention)
Present embodiment prepares agglomerate by following process: only adopt L dige CB type mixing tank (CB-30), adopt fluidized bed dryer (FBD), fluidized bed cooler (FBC) again, sieve then and pulverize.
By the pin type instrument (pin tools) of CB-30 mixing tank, the moisture coco group fatty alcohol sulphuric acid salt surfactant cream (71.5% activity) of 259kg/hr is disperseed with the micronization anhydrous sodium carbonate (median size 5～30 μ m) of powder STPP (median size 40～75 μ m), the 169kg/hr of 217kg/hr, micronization vitriol (median size 5～30 μ m) and the 288kg/hr recirculation fine powder of 103kg/hr.Tensio-active agent cream is added down at about 40～55 ℃, and powder at room temperature adds.The condition of CB-30 mixing tank is as follows:
Mean residence time: 14～20s
Upset tip velocity: 6.5～7.0m/s
Energy condition: 0.15～1.0kj/kg
After the agglomeration, the bed temperature of FBD remains on 40～60 ℃, and the bed speed of FBC remains on 15～30 ℃.
The particulate density that forms is 475～530g/l (Fig. 1).The content of fine powder is 30～50% behind the CB30 mixing tank, and target is 25%.
The embodiment 2:(the first step of the present invention and the erose agglomerate that obtains after second step)
Present embodiment prepares agglomerate by following process: adopt L dige CB type mixing tank (CB-30), adopt Schugi Flexomic mixing tank then, adopt fluidized bed dryer (FBD), fluidized bed cooler (FBC) again, (for example sieve then and pulverize, the course of processing is all identical with embodiment 1 with the raw material consumption, just increases the agglomeration step that Schugi Flexomic mixing tank carries out again after the agglomeration step that adopts L dige CB type mixing tank).
To add to Schugi Flexomic mixing tank from the agglomerate of CB-30 mixing tank.With the HLAS atomizing of 30kg/hr, and be sprayed in the Schugi Flexomic mixing tank.
The condition of Schugi Flexomic mixing tank is as follows:
Mean residence time: 0.5～2s
Upset tip velocity: 15～18m/s
Energy condition: 0.15～1.0kj/kg
The particulate density that forms behind Schugi Flexomic mixing tank is 475～530g/l (Fig. 2), and the particulate density that forms after screening and pulverizing is 450～475g/l (Fig. 3).Fine powder content from Schugi Flexomic mixing tank is 22～30%.
The erose agglomerate that embodiment 3:(is obtained by the inventive method)
Present embodiment prepares agglomerate by following process: adopt L dige CB type mixing tank (CB-30), adopt Schugi Flexomic mixing tank then, adopt fluidized bed cooler (FBC) again, sieve then and pulverize.
By the pin type instrument of CB-30 mixing tank, the anhydrous linear alkyl benzene sulphonic acid (94～96% activity) of 220kg/hr is disperseed with the micronization anhydrous sodium carbonate (median size 5～30 μ m) of powder STPP (median size 40～75 μ m), the 230kg/hr of 300kg/hr, the micronization vitriol (median size 5～30 μ m) of 100kg/hr, zeolite and the 100kg/hr recirculation fine powder of 90kg/hr.Tensio-active agent is added down at about 40～55 ℃, and powder at room temperature adds.The condition of CB-30 mixing tank is as follows:
Mean residence time: 10～18s
Upset tip velocity: 6～13m/s
Energy condition: 0.15～3.5kj/kg
To add to Schugi Flexomic mixing tank from the agglomerate of CB-30 mixing tank.With the HLAS atomizing of 30kg/hr, and be sprayed in the Schugi Flexomic mixing tank, in this mixing tank, add the carbonate of 20kg/hr.The condition of Schugi Flexomic mixing tank is as follows:
Mean residence time: 0.5～2s
Upset tip velocity: 15～18m/s
Energy condition: 0.15～1.0kj/kg
The particulate density that forms behind Schugi Flexomic mixing tank is 500～550g/l.
The erose agglomerate that embodiment 4:(is obtained by the inventive method)
Present embodiment prepares agglomerate by following process: adopt L dige CB type mixing tank (CB-30), adopt L dige KM mixing tank (KM-600) and Schugi Flexomic mixing tank then, adopt fluidized bed cooler (FBC) again, sieve then and pulverize.
By the pin type instrument of CB-30 mixing tank, the anhydrous linear alkyl benzene sulphonic acid (94～96% activity) of 220kg/hr is disperseed with the micronization anhydrous sodium carbonate (median size 5～30 μ m) of powder STPP (median size 40～75 μ m), the 230kg/hr of 300kg/hr, the micronization vitriol (median size 5～30 μ m) of 100kg/hr, zeolite and the 100kg/hr recirculation fine powder of 90kg/hr.Tensio-active agent is added down at about 40～55 ℃, and powder at room temperature adds.The condition of CB-30 mixing tank is as follows:
Mean residence time: 10～18s
Upset tip velocity: 6～13m/s
Energy condition: 0.15～3.5kj/kg
To add to from the agglomerate of CB mixing tank in the KM mixing tank, be about 40～60kgs at this retention value.Plough formula (ploW) RPM is 100, and axe formula (chopper) RPM is 1300 (three axe formula agitators are arranged on mixing tank).
To add to from the agglomerate of KM mixing tank in Schugi Flexomic (FX-160) mixing tank.With the HLAS atomizing of 30kg/hr, and be sprayed in the Schugi Flexomic mixing tank, in this mixing tank, add the carbonate of 20kg/hr.The condition of Schugi Flexomic mixing tank is as follows:
Mean residence time: 0.5～2s
Upset tip velocity: 15～18m/s
Energy condition: 0.15～1.0kj/kg
The particulate density that forms after the Schugi mixing tank sieves and pulverizes is about 600g/l.
Below at length invention has been described, and those skilled in the art can obviously find out, can carry out various improvement not deviating under the scope of the present invention, but the present invention is not subjected to the restriction of content as mentioned above.
Claims (11)
1, a kind ofly prepare the non-tower method that density is the granular detergent composition of 300～600g/l, this method comprises the steps:
(a) (i) disperse moisture or non-water surface promoting agent; (ii) in mixing tank, be that the fine powder of 0.1～500 μ m applies this tensio-active agent and obtains particle with particle diameter, described mixing tank is operated under the following conditions:
Mean residence time: 5～30 seconds, upset tip velocity: 5～10m/s, energy condition: 0.15～4.2kj/kg; Then
(b) in mixing tank, to from the particle of step (a) and the excessive fine powder, described mixing tank is operated under the following conditions so that excessive fine powder is bonded on the erose particle with the liquid spray of little atomizing:
Mean residence time: 0.2～5 second, upset tip velocity: 10～23m/s, energy condition: 0.15～2.9kj/kg.
2, according to the process of claim 1 wherein that described tensio-active agent is selected from anion surfactant, nonionogenic tenside, cats product, zwitterionics, amphoterics and its mixture.
3, according to the process of claim 1 wherein that described tensio-active agent is selected from alkylbenzene sulfonate, alkyl alkoxy sulfate, alkylethoxylate, alkyl-sulphate and its mixture.
4, according to the process of claim 1 wherein, step (a) (i) in described surfactant-dispersed moisture or non-aqueous polymer solution.
5, according to the method for claim 1, wherein, described fine powder is selected from anhydrous sodium carbonate, powdery tripoly phosphate sodium STPP, hydration tri-polyphosphate, sodium sulfate, silico-aluminate, crystalline layered silicate, phosphoric acid salt, precipitated silicate, polymkeric substance, carbonate, Citrate trianion, nitrilotriacetic acid(NTA) salt (NTA), Powdered tensio-active agent and from the recirculation fine powder of step (b), and composition thereof.
6, according to the process of claim 1 wherein that little atomized liquid is selected from liquid silicon hydrochlorate, anion surfactant, cats product, aqueous polymers solution, non-aqueous polymer solution, water and composition thereof.
7, according to the method for claim 1, wherein, the mean residence time of detergent agglomerate in the mixing tank of step (a) is 10～15 seconds, the upset tip velocity of detergent agglomerate in the mixing tank of step (a) is 6～8m/s, and energy condition is 0.15～2.5kj/kg in step (a) mixing tank.
8, according to the method for claim 5, wherein, the mean residence time of detergent agglomerate in the mixing tank of step (b) is 0.5～2 second, the upset tip velocity of detergent agglomerate in the mixing tank of step (b) is 13～20m/s, and energy condition is 0.15～1.9kj/kg in step (b) mixing tank.
9,, account for 10～40% of fine powder total amount in the step (a) from the total amount of the recirculation fine powder of step (b) according to the process of claim 1 wherein.
10, according to the process of claim 1 wherein that fine powder is the STPP of hydration, its hydration levels is not less than 50%.
11, according to the method for claim 1, the tensio-active agent total amount that is used for claim 1 method accounts for 5～60% of total composition that claim 1 method obtains.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96180525 CN1120228C (en) | 1996-10-04 | 1996-10-04 | Process for making low density detergent compsn. by non-tower process |
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|---|---|---|---|
| CN 96180525 CN1120228C (en) | 1996-10-04 | 1996-10-04 | Process for making low density detergent compsn. by non-tower process |
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| CN1120228C true CN1120228C (en) | 2003-09-03 |
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| ES2535580T3 (en) * | 2012-06-01 | 2015-05-12 | The Procter & Gamble Company | Spray drying process |
| US11109538B2 (en) * | 2017-12-29 | 2021-09-07 | Industrial Technology Research Institute | Method for producing galanthamine by a plant and electrical stimulation device |
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