CN1269824A - Process for making low density detergent composition by controlling nozzle height in fluid bed dryer - Google Patents

Process for making low density detergent composition by controlling nozzle height in fluid bed dryer Download PDF

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Publication number
CN1269824A
CN1269824A CN98808951.3A CN98808951A CN1269824A CN 1269824 A CN1269824 A CN 1269824A CN 98808951 A CN98808951 A CN 98808951A CN 1269824 A CN1269824 A CN 1269824A
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China
Prior art keywords
agglomerate
detergent
bed dryer
fluidized bed
speed mixer
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CN1170918C (en
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A·D·比尔
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Procter and Gamble Co
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Procter and Gamble Co
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets

Abstract

A process for preparing low density detergent agglomerates having a density in a range from about 300 g/l to about 550 g/l is provided. The process involves the steps of: (a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates; (b) mixing the agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding the built-up agglomerates into a fluid bed dryer in which a binder is sprayed via a nozzle having a height of from about 25 cm to about 60 cm from the distributor plate of the fluid bed dryer such that the built-up agglomerate are dried and agglomerated to form the desired low detergent agglomerates.

Description

The method for preparing low density detergent composition by nozzle height in the control fluidized bed dryer
Invention field
A kind of method for preparing low density detergent composition of relate generally to of the present invention.More particularly, the present invention relates to a kind of such method, by 2 high-speed mixers are advanced in the liquid acid precursor and the feeding sequentially of dry detergent raw material of surfactant paste or anion surfactant, then feeding advances to have to be used for the fluidized bed dryer of the optimal selection nozzle height of spray adhesive in the method.This method is produced free-pouring low density detergent composition, and it can be used as the mixture that conventional non-compact detergent compositions sells or can be used as in " densification " Betengent product of low dosage and uses.
Background of invention
Recently, people have had sizable interest to " densification " so detergent for washing clothes that have low dosage volume in the washing composition industry.For the ease of producing these so-called low dosage washing composition, carried out a lot of trials so that produce high bulk density and for example had 600g/l or more highdensity washing composition.The low dosage washing composition is in demand at present, because their save resource and can be with little packing and selling, this is more convenient to the human consumer., be that the desirability of " densification " property remains uncertain to modern Betengent product.In fact, a lot of human consumers, especially the human consumer in developing country still would rather use higher dosage in its laundry operations.Therefore, in preparation modern detergent compositions field, just need aspect the final densities of the finished product handiness arranged.
What 2 kinds of base types were arranged usually can preparing washing agent particle or the method for powder.The aqueous washing composition feed liquid of spraying drying prepares highly porous detergent particles in the spray-drying tower thereby first method is included in.In the second approach, various detergent components do are mixed, afterwards with them and for example nonionic or anion surfactant agglomeration of tackiness agent.In two kinds of methods, the greatest factor of the detergent particle granule density of control gained is density, porosity and surface-area, shape and their chemical constitutions separately of various raw materials., these parameters only can change in limited scope.Therefore, the handiness of true reactor density only can realize by the additional procedure of processing that causes lower detergent particle granule density.
In the prior art to providing the method that increases detergent particles or powder density that a lot of trials have been arranged.Attractive especially is by the spray-dired particulate density of tower aftertreatment.For example, a kind of trial comprises a kind of batch-wise method, and the detergent powder that will contain the spraying drying of tripoly phosphate sodium STPP and sodium sulfate or granulation in the method is at Marumerizer RMiddle increase density and balling-up.This device comprises substantially horizontal coarse rotatable, and it is placed in the cylinder that smooth wall is arranged of perpendicular and on its base., this method is the batch-wise method basically, therefore is not suitable for the scale operation detergent powder.Recently, carried out other trial so that provide a kind of successive method to increase " behind the tower " or spray-dried detergent particulate density.Such method generally need grind or abrasive grains first the device and by agglomeration increase this grind pellet density second the device.Although these methods are by handling or density " behind the tower " or spray-dired particle have reached needed density and increase, they do not provide, and the method that provides than the low-density particles handiness is provided.
In addition, all aforesaid methods all relate to density basically or handle spray-dired particle with other method.At present, material type that stands spray drying process in detergent particles production and relative quantity are restricted.For example, it is difficult to reach high-load tensio-active agent at the detergent composition that obtains, and it is a feature of being convenient to produce with more efficient methods washing composition.Therefore, need a kind of method, can preparing washing agent composition by this method and be not subjected to the restriction of conventional spray drying technology.
For this purpose, prior art also has been full of the disclosure that makes the agglomerant method of detergent composition.For example, thus carried out by zeolite and/or layered silicate are mixed the trial that the agglomerate detergent washing assistant forms free-pouring agglomerate in mixing machine.The trial of even now advises that its method can be used for preparing washing agent agglomerate, but they do not provide a kind of mechanism, can be by this mechanism with the conventional detergent raw material of surfactant paste or its precursor forms, liquid and dry substance agglomerate into effectively has low density rather than highdensity, crisp, free-pouring detergent agglomerate.In the past, the trial for preparing such low density agglomerate comprises unconventional detergent component, and it generally is expensive, has therefore increased the cost of Betengent product.One such example comprise with inorganic double salt for example the Burkeite agglomeration so that prepare the method for required low density agglomerate.
Therefore, still need in the art and a kind ofly directly do not need relatively costly extraordinary component to prepare the method for low density detergent composition from the detergent raw material component.In addition, still also need more effective, more flexible and more economical such method so that produce the washing composition of low dosage and high dosage on a large scale.
Background technology
Relate to spray-dired particle density below with reference to document: the US5133924 of Appel etc. (Lever), the US5160657 of Bortolotti etc. (Lever), the EP451894 of the GB1517713 of Johnson etc. (Unilever) and Curtis.Relate to by the agent of agglomeration preparing washing below with reference to document: the US5108646 of Beerse etc. (Procter ﹠amp; Gamble), US5366652 (the Procter ﹠amp of Capeci etc.; Gamble), the US5205958 of the EP351937 (Unilever) of Hollingsworth etc. and Swatling etc.Relate to inorganic double salt below with reference to document: the US4820441 of Evans etc. (Lever), the US4818424 of Evans etc. (Lever), the US4900466 of Atkinson etc. (Lever), the US5576285 of France etc. (Procter ﹠amp; Gamble) and the PCT WO 96/04359 (Unilever) of Dhalewadika etc.
Summary of the invention
The present invention has directly satisfied the above-mentioned needs of this area from surfactant paste and the method that the detergent raw material component of doing prepares low density (being lower than about 600g/l) detergent composition by providing a kind of.In fact, this method is included in the high-speed mixer and follows in the 2nd high-speed mixer the agglomeration of detergent raw material component.Afterwards, will be in this high-speed mixer the agglomeration and dry in fluidized bed dryer of agglomerant agglomerate, in moisture eliminator liquid adhesive is sprayed on the agglomerate from one or more nozzles, this nozzle is at the height through selecting apart from this fluidized bed dryer distribution plate.The spray-drying tower of the routine that this method need not be used at present, therefore more effective, more economical and more flexible aspect the kind of the detergent composition that can prepare with this method.In addition, this method is more suitable in the consideration of environment aspect, because it does not use generally particle and volatile organic compounds is not discharged into spray-drying tower in the atmosphere.
As used herein, term " agglomerate " expression is by the particle of agglomerate detergent granules or particle (it generally has than the littler median diameter of agglomerate that forms) formation.About " median diameter ", it refers to thereon that 50% particle has bigger particle diameter, its down particle of 50% have the more particle diameter value of small particle size.Except as otherwise noted, all percentage number averages used herein are in " weight percentage " expression by moisture-free basis.
According to an aspect of the present invention, provide a kind of method for preparing low density detergent agglomerates.This method comprises following step: thus (a) detergent surfactant lotion or its precursor are obtained agglomerate with detergent raw material agglomeration in the 1st high-speed mixer of doing; (b) thus in the 2nd high-speed mixer, mix the agglomerate that this agglomerate obtains compound (built-up); (c) with compound agglomerate feeding influent stream bed dryer, thereby in fluidized bed dryer, cause the low detergent agglomerate of the dry and agglomeration formation density of this compound agglomerate for the nozzle spray tackiness agent of about 25-60cm in about 300-550g/l scope by distance fluidized bed dryer distribution plate height.
According to another aspect of the present invention, provide the another kind of method for preparing low density detergent agglomerates.This method comprises following step: thus (a) detergent surfactant lotion or its precursor are obtained agglomerate with detergent raw material agglomeration in the 1st high-speed mixer of doing; (b) thus in the 2nd high-speed mixer, mix the agglomerate that this agglomerate obtains compound (built-up); (c) with compound agglomerate feeding influent stream bed dryer, thereby in fluidized bed dryer, cause the low detergent agglomerate of the dry and agglomeration formation density of this compound agglomerate for the nozzle spray tackiness agent of about 40-60cm in about 300-550g/l scope by distance fluidized bed dryer distribution plate height.The Betengent product of the described herein arbitrary method embodiment preparation of basis also is provided.
Therefore, the purpose of this invention is to provide a kind of method that directly prepares (this component does not comprise relatively costly extraordinary component) low density detergent composition from the detergent raw material component.A further object of the invention has provided a kind of like this method, and this method is more effective, thus the more flexible and more economical low washing composition that reaches high dosage of scale operation of being convenient to.By reading following detailed description of the preferred embodiments and appending claims, to those skilled in the art, these and other objects of the present invention, feature and bonus can become apparent.
Detailed description of the preferred embodiments
The present invention relates to a kind of method, prepare the low density agglomerate by 3 step method in the method, its final step comprises a fluidized bed dryer that contains one or more nozzles, and this nozzle is placed on the height place through selecting apart from this fluidized bed dryer distribution plate.Like this, this method forms free-pouring low density detergent agglomerates, it can be used as Betengent product and uses separately, and perhaps the mixture with conventional spray-dried detergent particle and/or high density detergent agglomerate uses in the Betengent product as selling final merchant.Should be appreciated that described method can operate continuously or with the batch-wise formal operations, this depends on the purposes of special requirement herein.Thereby the device that a major advantage of the inventive method is its to be used can be different from the parameter operation of the inventive method obtains high density detergent composition.Therefore, can make single large-scale industry production of detergents device so that produce high or low density detergent composition according to regional human consumer's needs and its inevitable change between fine and close and non-compact detergent product.
Method
In first step of present method, in a high-speed mixer, put into as hereinafter detergent surfactant lotion or its precursor and dried detergent raw material and agglomeration in greater detail.Different with the method for state of the art, this raw material of doing can only comprise the detergent materials that generally is used for modern granulated detergent product that those are relatively cheap.Such component includes but not limited to: washing assistant, filler, dried tensio-active agent and flow promotor.Washing assistant preferably includes silico-aluminate, crystalline layered silicate, and phosphoric acid salt, carbonate and their mixture, it is basic dry detergent feed composition in present method.For the required low-density agglomerate that reaches with present method preparation, relatively costly material is Burkeite (Na for example 2SO 4Na 2CO 3) and various silicon-dioxide optional.On the contrary, by tackiness agent and the nozzle height in the fluidized bed dryer (being sprayed on the agglomerate by this nozzle tackiness agent) selecting as hereinafter describe in detail, method of the present invention has obtained needed low density.In addition, in first step of method, also preferably include too small detergent particles or " fine powder " of about 40% weight of 1-.This can sieve median diameter by the detergent particles that will form and send back in first high-speed mixer in the scope of about 10-150 micron and with these " fine powders " and realize after fluidized bed dryer.
This high-speed mixer can be any mixing machine of Lodige CB 30 mixing machines or the similar trade mark for example of various commercially available mixing machines.The mixing machine of these types is formed by having the level, hollow, the immobilized cylinder that turning axle are housed the center basically, is connected with several shovels and clavate blade around turning axle, and its tip velocity is about 5-30m/s, more preferably from about 6-26m/s.This rotating speed is preferably about 100-2500rpm, more preferably from about 300-1600rpm.Preferably, the mean residence time of detergent component in this high-speed mixer be preferably in about 2-45 second, most preferably from about 5-15 second.This mean residence time is to be used in the flow (kg/h) that the weight of mixing machine under the steady state passes through divided by material easily to measure.Another suitable mixing machine is any of the various Flexomix type mixing machines that obtain from Schugi (Holland), and it is the vertical high-speed mixer of placing.This class mixing machine is preferably operated with the Froude index of about 13-32.Go through about this known Froude exponential, see people's such as Jacobs US5149455 (promulgation on September 22nd, 1992), it is can be by the zero dimension numerical value of those of ordinary skills' optimal selection.
In the preferred embodiment of present method invention, the liquid acid precursor of anion surfactant with comprise at least neutralizing agent for example the detergent raw material of doing of yellow soda ash put into.Preferred liquid acid tensio-active agent precursor is C 11-18Linear alkyl sulfonate surfactant (" HLAS "), but also can use any acid precursor of anion surfactant in the method.Preferred embodiment comprises C 12-14The liquid acid precursor and the C of linear alkyl sulfonate surfactant 10-18The vitriol of alkyl ethoxylated (" AS ") tensio-active agent feeding together advances first high-speed mixer, and preferably its weight ratio is about 5: 1-1: 5, and most preferably about 1: 1-3: 1 scope (HLAS: AS).The blended result is at HLAS and is included in " dry neutralization " reaction between the yellow soda ash in the dry detergent raw material like this, and they all form agglomerate.Preferably for example add HLAS before AS or alkyl ethoxylate sulfate (" the AES ") tensio-active agent and mix and neutralization adding other tensio-active agent so that guarantee the best of the HLAS in first high-speed mixer.In second step of present method, the detergent agglomerate that forms in a first step is sent in second high-speed mixer, this mixing machine can be with first step in the identical device that uses or can be with first step in dissimilar high-speed mixers.For example, can use Lodige CB mixing machine in a first step, and in second step, use the Schugi mixing machine.In this second method steps, agglomerate is mixed and further compound in the mode of control.In this step, can add the tackiness agent of q.s so that the agglomeration in mixing machine is compound.General tackiness agent comprises liquid sodium silicate, and the liquid acid precursor of anion surfactant is HLAS for example, nonionogenic tenside, polyoxyethylene glycol, or its mixture.
In the next procedure of present method, this compound agglomerate is sent in the fluidized bed dryer, in moisture eliminator that this agglomerate is dry and to agglomerate into median diameter be about 300-700 micron, 325-450 micron more preferably from about.The density of the agglomerate that forms is about 300-550g/l, more preferably from about 350-500g/l, most preferably from about 400-480g/l.All these density all are lower than the density of the general detergent composition that is formed by fine and close agglomerate or the most general spray-dried granules usually.
Above-mentioned tackiness agent preferably adds so that strengthen the formation of required agglomerate in this step.In this respect, particularly preferred tackiness agent is a liquid sodium silicate, and by final low-density compositions weight, its amount is about 0.1-20%.The height of nozzle (adding tackiness agent by this nozzle) is apart from the about 25-60cm of the distribution plate of fluidized bed dryer, 30-60cm more preferably from about, 40-60cm most preferably from about, even more preferably 40cm.All nozzles that use in this fluidized bed drying device preferably all have such height.Made us unexpectedly finding:, see all excellent low density agglomerate with having a process for preparing from low density and free-flowing property aspect by nozzle height being chosen in the above-mentioned scope.
In addition, maintain about 0.02-0.06kg/cm by mist flow with tackiness agent in the fluidized-bed 2/ h, more preferably from about 0.04-0.05kg/cm 2/ h can strengthen present method benefit in this respect.Preferably about 100-200 ℃ of inlet air temp in fluidized bed dryer, more preferably from about 110-130 ℃.In addition, the preferably about 5-20cm of not fluidized-bed layer height in fluidized bed dryer.Also find: by the fluidization air flow in the fluidized bed dryer is maintained about 0.6-0.8kg/m 2/ s can strengthen the benefit of present method.Also find: in one or more steps of present method, also be useful adding tackiness agent simultaneously more than one position.For example, 2 positions that can be in fluidized bed dryer for example or near the ingress or or add the liquid silicon hydrochlorate near the exit.In addition, the mid-diameter of adhesive droplets is about 20-150 micron, and it is to strengthen the parameter that forms required compound agglomerate.In addition, in this respect, the preferably about 0.1-0.6 of ratio of the mid-diameter of adhesive droplets and compound agglomerate (coming out) particle diameter from second high-speed mixer.
Randomly, present method can comprise tackiness agent is joined in second high-speed mixer and the fluidized bed dryer.Find also that in one or more steps of present method adding tackiness agent simultaneously more than one position also be useful.For example, 2 positions that can be in fluidized bed dryer for example or near the ingress or or add the liquid silicon hydrochlorate near the exit.First situation with second step as present method is the same, and agglomerate is combined into the large-size particle with height particle internal porosity from less size.The preferably about 20-40% of this particle internal porosity, most preferably from about 25-35%.Mercury porosimeter test by standard can be measured this particle internal porosity easily.
The inventive method estimates that other optional step that can comprise is included in the excessive detergent agglomerate of step sizing in the screening plant, and this screening plant can adopt various forms to include but not limited to the conventional sieve of selecting for the washing composition finished product that obtains required particle diameter.Other optional step comprises by make agglomerate stand other dry and/or cooling conditioning detergent agglomerate with said apparatus.
Another optional step of present method need in all sorts of ways and comprise spraying and/or mix the detergent agglomerate that other conventional detergent component processing obtains.For example, this procedure of processing comprises that with spices whitening agent and enzyme are sprayed on the final agglomerate so that detergent composition more completely is provided.Such technology and component are known in this area.
Detergent surfactant lotion or precursor
The liquid acid precursor of anion surfactant is used in first step of present method, in optional embodiments, is used as liquid adhesive in second of present method and/or the 3rd steps necessary.This liquid acid precursor is generally about 500-5000cps in the viscosity of 30 ℃ of mensuration.This liquid acid is the precursor of anion surfactant in greater detail hereinafter.The detergent surfactant lotion also can be used for the form of present method and preferably moisture thickness lotion, but the present invention also considers other form.This so-called thickness surfactant paste has about 5000-100000cps, and the viscosity of 10000-80000cps more preferably from about, and containing at least about 10% is more preferably at least about 20% water.This viscosity is to measure under the shearing rate of 70 ℃ and about 10-100/s.In addition, if you are using, this surfactant paste preferably contains detergent surfactant, and its amount is that above-mentioned specified amount and surplus are water and other conventional detergent component.
In this heavy-gravity surfactant paste, itself is preferably selected from negatively charged ion tensio-active agent, nonionic, zwitter-ion, the mixture that both sexes and cationic are compatible with it.Useful herein detergent surfactant is described in the US3664961 of the Norris of promulgation on May 23rd, 1972, and among the US3919678 of the Laughlin of promulgation on December 30th, 1975 etc., these 2 pieces of documents are incorporated herein by reference.Useful cats product is also included within those described in the US4239659 of Murphy of the US4222905 of Cockrell of on September 16th, 1980 promulgation and promulgation on December 16th, 1980, and these 2 pieces of documents are incorporated herein by reference.In these tensio-active agents, negatively charged ion and nonionogenic tenside are preferred, and anion surfactant is most preferred.
Useful in surfactant paste, perhaps comprise: conventional C from its non-limiting example that obtains the preferred anionic surfactants tensio-active agent of described liquid acid precursor herein 11-C 18Alkylbenzene sulfonate (" LAS "), primary, side chain and random C 10-C 20Alkyl-sulphate (" AS "), formula CH 3(CH 2) x(CHOSO 3 -M +) CH 3And CH 3(CH 2) y(CHOSO 3 -M +) CH 2CH 3C 10-C 18Secondary (2,3) alkyl-sulphate, x and (y+1) be to be at least approximately 7 wherein, preferably being at least about 9 integer and M is water-soluble cationic, sodium especially, unsaturated vitriol is oleyl sulfate for example, and C 10-C 18Alkyl alkoxy sulfate (" AE xS ", EO 1-7 ethoxy sulfate especially).
Randomly, other useful illustrative tensio-active agent comprises in lotion of the present invention: C 10-C 18Alkyl alkoxy carboxylate salt (especially EO 1-5 ethoxy carboxylate), C 10-C 18Glyceryl ether, C 10-C 18APG and its corresponding Sulfated polysaccharide glycosides, and C 12-C 18α-sulfonated fatty acid ester.If desired, Chang Gui nonionic and amphoterics for example comprise the C of so-called narrow peak alkylethoxylate 12-C 18Alkylethoxylate (" AE ") and C 6-C 12Alkyl phenolic alkoxy thing (especially ethoxylate and blended oxyethyl group/propoxylated glycerine), C 12-C 18Trimethyl-glycine and sultaine (" sultaine "), C 10-C 18Amine oxides etc. also can be included in the whole composition.Also can use C 10-C 18N-alkyl polyhydroxy fatty acid amide.General example comprises C 12-C 18N-methyl glucoside acid amides.See WO9206154.Other sugared deutero-tensio-active agent comprises N-alkoxyl group polyhydroxy fatty acid amide, for example C 10-C 18N-(3-methoxy-propyl) glucose amide.The N-propyl group is to N-hexyl C 12-C 18Glucamide can be used for low foaming.Also can use C 10-C 20Conventional soap class.High if desired whipability can be used the C of side chain 10-C 16Soap.The mixture of negatively charged ion and nonionogenic tenside is useful especially.Other conventional useful tensio-active agent is listed in the standard textbook.
The detergent materials of doing
The detergent raw material of doing of the inventive method preferably contains for example yellow soda ash of washing assistant and other standard wash agent component, especially when the liquid acid precursor of use tensio-active agent, need it in first step of the inventive method as neutralizing agent.Therefore, the preferred detergent raw material of doing comprises yellow soda ash and phosphoric acid salt or silico-aluminate washing assistant (it is called as aluminosilicate ion exchange material).Preferred washing assistant is selected from silico-aluminate, crystalline layered silicate, phosphoric acid salt, carbonate and its mixture.Preferred phosphate builders comprises tripoly phosphate sodium STPP, tetrasodium pyrophosphate and its mixture.The object lesson of other of inorganic phosphate builders is the tri-polyphosphate of sodium and potassium, pyrophosphate salt, and the polymerization degree is the polymeric metaphosphate of about 6-21, and orthophosphoric acid salt.The example of polyphosphonate 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 ethane 1,1, the sodium of 2-tri methylene phosphonic acid and sylvite.Other phosphorus washing-aid compound is disclosed in United States Patent (USP) 3159581,3213030,3422021,3422137,3400176 and 3400148, and these documents are incorporated by reference in this article.
Aluminosilicate ion exchange material as detergent builders preferably has high calcium ion exchange capacity and high rate of exchange herein.Do not plan to use one theory, it is believed that the function that such high-calcium ionic rate of exchange and ability are several mutual related factors, its method by this aluminosilicate ion exchange material of preparation draws.In this respect, aluminosilicate ion exchange material used herein is preferably according to US4605509 (the Procter ﹠amp of Corkill etc.; Gamble) prepare, the disclosed content of the document is incorporated by reference in this article.
This aluminosilicate ion exchange material is " sodium " form preferably because the potassium of this silico-aluminate and hydrogen form can not demonstrate resemble by na form provide high rate of exchange and ability.In addition, this aluminosilicate ion exchange material preferably the super-dry form so that help to produce described crisp detergent agglomerate herein.This aluminosilicate ion exchange material used herein has makes its grain diameter as the detergent builders optimum efficiency.The average grain particle diameter of the aluminosilicate ion exchange material that term used herein " grain diameter " expression is given, it is to measure by for example micro-mensuration of the analytical technology of routine and scanning electron microscope (SEM).The preferred grain diameter of this silico-aluminate is about 0.1-10 micron, more preferably from about 0.5-9 micron.Most preferably, this grain diameter is about 1-8 micron.
This aluminosilicate ion exchange material preferably has following formula:
Na z[(AlO 2) z(SiO 2) y] xH 2O wherein z and y is at least 6 integer, and the mol ratio of z and y is that about 1-5 and x are about 10-264.More preferably, this silico-aluminate has following formula:
Na 12[(AlO 2) 12(SiO 2) 12] xH 2O wherein x is 20-30, preferably about 27.These preferred silico-aluminates can be with for example title zeolite A, and zeolite B and X zeolite are buied.In addition, be applicable to that the naturally occurring or synthetic aluminosilicate ion exchange material that obtains herein can be according in preparing described in the US3985669 of Krummel etc., the disclosed content of the document is incorporated by reference in this article.
The feature of silico-aluminate used herein also is its ion-exchange capacity, and it is the normal CaCO of about 200mg at least 3Hardness per gram (calculating) by anhydrous base-material, and it is preferably at the normal CaCO of about 300-352mg 3Hardness per gram.In addition, the feature of this aluminosilicate ion exchange material also is its calcium ion exchange rate, and it is about 2 grain Ca at least ++/ gallon per minute/-Ke/gallon, more preferably at about 2-6 grain Ca ++/ gallon per minute/-scope of Ke/gallon.
Additional detergent component
Dry detergent raw material in the methods of the invention can comprise additional detergent component and/or can be in the inventive method step afterwards the annexing ingredient of any amount be joined in the detergent composition.These additional components comprise other clean washing assistant, SYNTHETIC OPTICAL WHITNER, bleach-activating agent, profoamer or suds suppressor, rust-preventive agent and corrosion inhibitor, soil-suspending agent, dirt release agent, sterilant, pH regulator agent, non-washing assistant alkali source, sequestrant, terre verte, enzyme, enzyme stabilizers and spices.See the Baskerville of promulgation on February 3rd, 1976, the US3936537 of Jr. etc., the document is incorporated by reference in this article.
Other washing assistant can be selected from various borates usually, polyhydroxy sulfonate, poly-acetate, carboxylate salt, Citrate trianion, tartrate list and disuccinate and its mixture.An alkali metal salt of above-mentioned acid sodium salt especially preferably.Compare with unformed water glass, crystalline layered sodium silicate demonstrates the calcium and the magnesium ion exchange capacity of obvious raising.In addition, lamina sodium silicate exchange magnesium ion energy force rate exchange calcium ion is strong, and this is to guarantee to remove from washing water all " hardness " necessary characteristics basically.Yet these crystalline layered sodium silicates are more expensive than amorphous silicic salt and other washing assistant usually.Therefore, for economically viable detergent for washing clothes is provided, must determine the ratio of crystalline layered sodium silicate carefully.
Be applicable to that crystalline layered sodium silicate herein preferably has following formula:
NaMSi xO 2x+1YH 2O wherein M is sodium or hydrogen, and x is that about 1.9-4 and y are about 0-20.More preferably, this crystalline layered sodium silicate has following formula:
NaMSi 2O 5.yH 2O wherein M is that sodium or hydrogen and y are about 0-20.The crystalline layered sodium silicate of these and other has been discussed in the US4605509 of Cotkill etc., and the document is incorporated herein by reference in front.
The example of non-phosphorus inorganic builders is tetraborate decahydrate and SiO 2With the weight ratio of alkalimetal oxide be about 0.5-4.0, the preferred silicate of about 1.0-2.4.Useful in this article water miscible non-phosphorus organic washing-assisting detergent comprises the poly-acetate of various basic metal, ammonium and replacement ammonium, carboxylate salt, multi-carboxylate and polyhydroxy sulfonate.Poly-acetate and multi-carboxy acid salt washing agent's example is an ethylenediamine tetraacetic acid (EDTA), triglycollamic acid, oxygen di-succsinic acid, mellitic acid, the sodium of benzene polycarboxylic acid and citric acid, potassium, lithium, ammonium and substituted ammonium salt.
The polymeric multi-carboxy acid salt washing agent is described in the US3308067 of the Diehl of promulgation on March 7th, 1967, and the disclosed content of the document is incorporated by reference in this article.Such material comprises for example toxilic acid of aliphatic carboxylic acid, methylene-succinic acid, methylfumaric acid, fumaric acid, equisetic acid, the homopolymer of citraconic acid and methylene radical propanedioic acid and the water-soluble salt of multipolymer.As mentioned below, some these material is useful as water-soluble anionic polymer, but have only when with the intimate mixture of non-soap anionic surfactant in the time.
Be used for the US4246495 that herein other suitable multi-carboxylate is described in the US4144226 of Crutchfield etc. of promulgation on March 13rd, 1979 and the Crutchfield of promulgation on March 27th, 1979 etc., these 2 pieces of documents are incorporated by reference in this article.Can prepare these polyacetal carboxylations by under polymerizing condition, the ester of Glyoxylic acid hydrate and polymerization starter being put together.The polyacetal carboxylic acid ester who obtains is connected on the chemically stable end group then and prevents that depolymerization can be transformed into corresponding salt in basic solution, and it is joined in the detergent composition so that stablize this polyacetal carboxylic acid ester.Particularly preferred multi-carboxy acid salt washing agent is the ether carboxylate lotion-aid combination, comprise the tartrate monosuccinic acid salt described among the US4663071 of the Bush that is described on May 5th, 1987 promulgation etc. and the combination of tartrate disuccinate, the disclosure of the document is incorporated by reference in this article.
SYNTHETIC OPTICAL WHITNER and activator are described among the US4483781 of Hartman of the US4412934 of the Chung of November 1 nineteen eighty-three promulgation etc. and promulgation on November 20th, 1984, and these 2 pieces of documents are incorporated by reference in this article.Sequestrant also is described in 54 row-18 hurdles, 17 hurdles, 68 row of US4663071 of Bush etc., and it is incorporated by reference in this article.Foaming regulator also is that these 2 pieces of documents are incorporated by reference in this article among the US4136045 of the US3933672 of component of choosing wantonly and the Bartoletta that is described in promulgation on January 20th, 1976 etc. and the Gault of promulgation on January 23rd, 1979 etc.
Be used for 3 row-7 hurdles, 6 hurdles, 24 row of US4762645 that herein suitable terre verte is described in the Tucker etc. of promulgation on August 9th, 1988, the document is incorporated by reference in this article.Those that are used for herein suitable additional clean washing assistant and are enumerating at 13 hurdles, 54 row-16 hurdles 16 row of the patent of Baskerville with at the US4663071 of the Bush of promulgation on May 5th, 1987 etc., these 2 pieces of documents are incorporated by reference in this article.
For the present invention is more readily understood, with reference to following embodiment, these embodiment only be used for illustrating rather than be used for limited field.
Embodiment
This embodiment has illustrated present method invention, has wherein prepared low-density agglomerant detergent composition.With powder is that yellow soda ash (median diameter is 15 microns) and median diameter are that the mixture of 25 microns tripoly phosphate sodium STPP (" STPP ") is charged in Lodige CB 30 high-speed mixers.Liquid acid precursor (the C of sodium alkylphenylsulfonateas as surfactant 12H 25-C 6H 4-SO 3-H or as middle finger " HLAS " that go out hereinafter) and the moisture C of 70% active ingredient 10-18The sulfate surfactant of alkyl ethoxylated (EO=3, " AES ") lotion also is delivered in these LodigeCB 30 high-speed mixers, wherein adds HLAS earlier.Under 1600rpm this mixing machine of running and in these Lodige CB 30 high-speed mixers mean residence time this yellow soda ash about 5 seconds after, STPP, HLAS and AES formation median diameter are about 110 microns agglomerate.Then this agglomerate feeding is advanced in Schugi (the Model # FX160) high-speed mixer, this mixing machine turns round under 2800rpm, and its mean residence time is about 2 seconds.In this step the HLAS tackiness agent is delivered in Schugi (the Model # FX160) high-speed mixer, this causes forming median diameter is about 180 microns compound agglomerate.Afterwards, make this compound agglomerate by 4 district fluidized bed dryers, this moisture eliminator is operated under the air themperature height of distribution plate that is about 125 ℃ times and nozzle in fluidized-bed the 1st and the 4th district is the condition of 40cm.The mist flow of water glass is 0.046kg/cm 2/ h, fluidized bed height are 10cm, and the flow of fluidization air is 0.6kg/m 2/ s.When amount of pointing out below and particle diameter, also fine powder is joined in this Lodige CB30 mixing machine.In the 1st and the 4th district of fluidized bed dryer, liquid sodium silicate sent to the result forms about 485g/l of density and the about 360 microns final detergent agglomerate of median diameter in this fluidized bed dryer.Unexpectedly be, this final agglomerate has fabulous physical properties, because go out by its excellent cake strength grade is shown, they are free-pouring.
Provided the composition of this agglomerate below in the Table I.
Table I (% weight)
Component I
LAS(Na) 15.8
AES(EO＝3) 4.7
Yellow soda ash 48.0
STPP 22.7
Water glass 5.5
Water 3.3
100.0
This agglomerate comprises about 14% fine powder (being lower than 150 microns), and it is from fluidized bed circulation Lodige CB 30, and this has improved the productivity for preparing agglomerate with this method.
So describe the present invention in detail, obviously can in not departing from the scope of the present invention, carry out various changes for a person skilled in the art, and the invention is not restricted to the content described in the specification sheets.

Claims (10)

1, a kind of method for preparing low density detergent composition is characterized in that following step:
(a) thus detergent surfactant lotion or its precursor and detergent raw material agglomeration in the 1st high-speed mixer of doing are obtained agglomerate;
(b) thus mixing this agglomerate in the 2nd high-speed mixer obtains compound (built-up) agglomerate; With
(c), be the described low detergent agglomerate of 300-550g/l thereby the nozzle spray tackiness agent that is 25-60cm by the described fluidized bed dryer distribution plate height of distance in fluidized bed dryer causes the dry also agglomeration of this compound agglomerate to form density with described compound agglomerate feeding influent stream bed dryer.
2, the process of claim 1 wherein that described tackiness agent is a water glass.
3, the process of claim 1 wherein that the mist flow of described tackiness agent is 0.02-0.06kg/cm 2/ h.
4, the process of claim 1 wherein that the temperature of inlet air of described fluidized bed dryer is 110-130 ℃.
5, the process of claim 1 wherein that described tackiness agent has the drop mid-diameter of 20-100 micron.
6, the process of claim 1 wherein that the fluidizing air flow quantity is 0.6-0.8kg/m in the described fluidized bed dryer 2/ s.
7, the process of claim 1 wherein that described step (a) comprises agglomeration C 11-18The liquid acid precursor and the C of linear alkyl sulfonate surfactant 10-18Alkyl ethoxylated sulphate surfactants.
8, the process of claim 1 wherein and add described tackiness agent in the import and the exit of described fluidized bed dryer.
9, the process of claim 1 wherein that described nozzle height is 35-45cm.
10, a kind of method for preparing low density detergent composition is characterized in that following step:
(a) thus detergent surfactant lotion or its precursor and detergent raw material agglomeration in the 1st high-speed mixer of doing are obtained agglomerate;
(b) thus mixing this agglomerate in the 2nd high-speed mixer obtains the compound agglomerate; With
(c), be the described low detergent agglomerate of 300～550g/l thereby the nozzle spray water glass that is 40-60cm by the described fluidized bed dryer distribution plate height of distance in fluidized bed dryer causes the dry also agglomeration of this compound agglomerate to form density with described compound agglomerate feeding influent stream bed dryer.
CNB988089513A 1997-07-14 1998-07-08 Process for making low density detergent composition by controlling nozzle height in fluid bed dryer Expired - Fee Related CN1170918C (en)

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