CN1120230C - Process for making high density detergent - Google Patents

Process for making high density detergent Download PDF

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Publication number
CN1120230C
CN1120230C CN97198597.9A CN97198597A CN1120230C CN 1120230 C CN1120230 C CN 1120230C CN 97198597 A CN97198597 A CN 97198597A CN 1120230 C CN1120230 C CN 1120230C
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China
Prior art keywords
thickener
detergent
moderate
rotating shaft
speed mixers
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CN97198597.9A
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CN1232494A (en
Inventor
P·A·扎菲罗
W·G·哈尔沃森
S·W·卡佩斯
A·威廉斯
L·V·达尔顿
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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
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C11D17/065—High-density particulate detergent compositions

Abstract

A process for producing high density detergent compositions is provided. The process is a continuous process during which high density detergent agglomerates are produced by feeding a surfactant paste and dry starting detergent material into a mixer/densifier having a centrally positioned rotating shaft which experiences minimal vibration via the use of tuned dampers mounted on the shaft. The process produces a free flowing, high density detergent composition which can be commercially sold as a low dosage or ''compact'' detergent composition.

Description

Process for making high density detergent
Invention field
The present invention relates generally to produce the method for high density detergent composition.Especially, it is that tensio-active agent mashed prod and exsiccant detergent raw material are sent in mixing tank/thickener that the present invention points to the continuation method of producing the high density detergent granule, and this mixing tank/thickener has the rotating shaft of the minimum positioned centrally of vibration.This method is produced free-pouring highdensity detergent composition, and this detergent composition can be sold with the detergent composition form of low consumption or " closely knit " commercial.
Background of invention
Detergent industry has sizable interest for the cloth-washing detergent that therefore has low consumption of " closely knit " recently.In order to promote the production of these so-called low consumption washing composition, people are many-sided by every means to produce high bulk density, for example have 600 grams per liters or more highdensity washing composition.The demand of at present low consumption washing composition is very high, because low consumption washing composition is saved resource, can feel that the small packages form is sold easily with the human consumer.
The production method that two kinds of main types are generally arranged can preparing washing agent particle or detergent powder according to these two kinds of methods.First type method is included in and makes the aqueous detergent slurries carry out spraying drying in the spray-drying tower, to produce the high porosity detergent particles.In the method for second type, different detergent components is done and is mixed, and does to mix the different detergent components in back for example nonionic or anion surfactant carry out agglomeration with binding agent.In these two class methods, the greatest factor of controlling resulting detergent particle granule density is the density of different material, porosity and surface-area, and their chemical constitutions separately.These parameters are merely able to change in certain scope.Therefore, can only utilize other procedure of processing to realize that bulk density increases significantly, these other steps have caused the densification of detergent particles.
For carrying out many trials in this area, working method aspect that the density that increases detergent particles or powder is provided always.Special concern utilizes the tower aftertreatment to make the spray-dried granules densification.For example, a kind of trial is intermittently legislation, and in the method for having a rest during this time, the detergent powder that contains the spraying drying of tripoly phosphate sodium STPP and sodium sulfate or granulation is at nodularization device Maramerizer _In densification and agglomerate into spherical.This equipment comprises the rolling disc of the substantially horizontal roughening that is positioned at cylinder perpendicular, that slick wall surrounds and cylinder bottom.This method comes down to method intermittently, therefore is not suitable for the scale operation detergent powder very much.Other trial has been proposed recently, so that the continuation method of increase " behind the tower " or spray-dried detergent pellet density to be provided.In typical case, such method needs the first kind of equipment and second equipment, and first kind of equipment makes particle pulverize or grind, and second kind of equipment utilization nodulizing increases the density of pulverized particles.The increase that these methods obtain desired density by processing or densification to " behind the tower " or spray-dried granules.
All above-mentioned methods mainly all are spray-dired particle densifications or with other method processing treatment.Recently, in the production of detergent particles, the relative quantity and the type that stand the spraying drying material processed have been made restriction.For example, in resulting detergent composition, be difficult to obtain high-grade tensio-active agent, these characteristics have promoted the production of low consumption washing composition.Therefore, need a kind of method, utilize this method not having producing detergent composition under traditional restricted condition that spray drying technology applied.Be full of with making detergent composition that agglomerant method take place open in the art for this reason.For example, attempt to make the agglomeration of washing composition buider, its method is that zeolite and/or lamellated silicate are mixed in mixing tank, to form free-pouring.
, in above-mentioned all methods, successive scale operation tends to have any problem, and particularly is related to consistently and the qualified product of acquisition under the minimum situation of producing apparatus wearing and tearing.For example, when some mixing tank/thickener laboratory scale or even situation at pilot-scale under operation when fabulous, in the continuous manufacturing site location of large-scale industry, the function of mixing tank/thickener does not always have reproducibility.
A problem that has occurred relates to plant-scale mixing tank/thickener shaft the over-drastic vibration, and this over-drastic vibration may have injurious effects for the detergent composition of being produced and mixing tank/thickener with the close producing apparatus in other position.This problem also can cause making the structural failure of buildings, for this damage, may need considerable repair expense.Therefore, still need a kind of method, the plant-scale mixing tank/thickener that is used to produce low consumption high density detergent composition by this method can operate continuously, and the damage that does not have tangible mechanical vibration and cause by mechanical vibration.
In view of the above, in the method that still needs a kind of continuous production high density detergent composition in the art, this method relates to the mixing tank/thickener with minimum mechanical vibration.Also need so a kind of method, this method is more effective and more economical for the large-scale production that promotes low consumption or closely knit washing composition.
Background technology
Following reference is to point to make spray-dired particle densification: people such as Appel, United States Patent (USP) 5,133,924 (Lever); People such as Bortolotti, United States Patent (USP) 5,160,657 (Lever); People such as Johnson, English Patent 1,517,713 (UniLever) and Curtis, european patent application 451,894.Following reference is to point to utilize nodulizing to produce washing composition: people such as Capeci, United States Patent (USP) 5,366,652; People such as Capeci, United States Patent (USP) 5,486,303; People such as Capeci, United States Patent (USP) 5,489,392; People such as Capeci, United States Patent (USP) 5,516,448; People such as Beerse, United States Patent (USP) 5,108,646 (Procter ﹠amp; Gamble); Ho1lings worth et al, european patent application 351,937 (Unilever); With people such as Swatling, United States Patent (USP) 5,205,958.
Summary of the invention
The present invention satisfies above-mentioned requirements in this area, and a kind of continuous production high density detergent composition method is provided.In this method tensio-active agent mashed prod and dry detergent raw material sent into and produce the high density detergent granule in mixing tank/thickener, this mixing tank/thickener has the minimum rotating shaft of positioned centrally vibration.In this method, on the central rotating shaft of mixing tank/thickener tuned damper has been installed, this causes a kind of method unexpectedly, and this method can produce high density detergent composition, and the mechanical vibration minimum generally has the repair expense that links also minimum with such vibration.This method can be produced free-pouring high density detergent composition, and said composition can be sold with the detergent composition of low consumption or " closely knit " commercial.
Term as used herein " granule " is meant the particle that the agglomeration of detergent raw material composition is formed, and the mean particle size of detergent raw material composition is less than formed.If not indicated otherwise, employed here all percentage ratios and ratio are all represented with weight percentage (butt).Above-mentioned all documents are included into as a reference here in the lump.The viscosity that this paper quoted all is in 70 ℃ (± 5 ℃) and the about 10-100 of velocity of shear second -1Condition under record.
According to an aspect of the present invention, provide the method for preparing crisp free-pouring high density detergent composition firmly.These method following steps: (a) detergent surfactant mashed prod and exsiccant detergent raw material are mixed in adding super mixer/thickener continuously, to obtain the washing composition granule; (b) the washing composition granule is mixed in moderate-speed mixers/thickener, so that further densification of washing composition granule and agglomeration, wherein moderate-speed mixers/thickener comprises central rotating shaft, tuned damper is housed in the rotating shaft so that under the situation of medium axle span in about 10 hertz-Yue 20 hertz range of frequency the maximum vibration of rotating shaft be about-1.0G to 1.0G; (c) make washing composition granule drying, so that form detergent composition.
According to a further aspect in the invention, the method that provides another successive to produce high density detergent composition.This method comprises the steps: that (a) mixes in adding moderate-speed mixers/thickener the spray-dried detergent particle continuously, wherein moderate-speed mixers/thickener comprises a central rotating shaft, a tuned damper equipment is housed on the central rotating shaft so that under the situation of medium axle span in about 10 hertz-20 hertz range of frequency the maximum vibration of axle be approximately-1.0G to 1.0G; (b) make washing composition granule drying, so that form detergent composition.In addition, the present invention also provides the detergent composition that utilizes above-mentioned any method manufacturing.
In view of the above, the purpose of this invention is to provide the method for continuous production high density detergent composition, this method relates to the mixing tank/thickener with minimum mechanical vibration.Another object of the present invention provides a such method, and this method is more effective or more economical for the large-scale production that promotes low consumption or closely knit washing composition.These purposes of the present invention and other purpose, characteristics and bonus can be very clearly for those by the those skilled in the art that read following detailed description of preferred embodiments, accompanying drawing and claims.
Brief Description Of Drawings
Fig. 1 is the schema of explanation preferred method, according to most preferred embodiment of the present invention, has disposed two mixing tank/thickeners, fluidized bed dryer, fluidized bed cooler and screening plant in this flow process successively;
Fig. 2 is the local sectility skeleton view of the employed mixing tank/thickener of the inventive method, and this figure has illustrated the tuned damper that is contained on the central rotating shaft;
Fig. 3 is the sectional side view of central rotating shaft, and central rotating shaft is equipped with tuned damper on it; With
Fig. 4 is the end view of moderate-speed mixers/thickener shaft, illustrates the tuned damper with four damping devices, and four damping devices are installed in around the axle by union lever and clamper.
The detailed description of preferred embodiments method
The inventive method can be used for producing the low consumption high density detergent composition and the composition that contains the conventional spray-dried granules that carries out " behind the tower " densification that contains by the granule of washing composition original composition direct production.The implication of " spray-dried granules " is meant porous particle, and this porous particle is to make by the aqueous slurries that drying comprises the detergent ingredients of tensio-active agent, buider and other standard additional detergent composition.In typical case, aqueous slurries is sprayed in the tower with refluent heat airflow to finish this drying.The implication of " behind the tower " densification refers to those detergent particles that has passed through traditional spray-drying tower or similar devices and after this passed through mixing tank/thickener as herein described.
Referring now to Fig. 1, Fig. 1 has provided schema, and this schema illustration has illustrated the various embodiment of simple and direct method and this method.In first step of this method, the present invention sneaks into the plurality of washing agent material composition logistics that comprises tensio-active agent pasty state logistics 12 and dry detergent raw material stream 14 in super mixer/thickener 10 continuously.It is about 65% that the tensio-active agent mashed prod preferably contains the 25%-that has an appointment, and preferably contains the 35%-that has an appointment about 55% and most preferably contain the detergent surfactant of the moisture pasty state form of the 38%-that has an appointment about 44%.The detergent raw material of doing 14 preferably contains the 20%-that has an appointment about 50%, preferably contain the 25%-that has an appointment about 45%, most preferably contain aluminosilicate or the zeolite buider of the 30%-40% that has an appointment and preferably contain the 10%-40% that has an appointment, preferably contain 15%-30% approximately and most preferably contain the yellow soda ash of about 15%-25%.Mix continuously in tensio-active agent mashed prod 12 and the described herein proportional range of detergent raw material 14 done, so that guarantee to produce needed free-pouring hard crisp high density detergent composition.The ratio preferably about 1 of tensio-active agent mashed prod 12 and the detergent raw material of doing 14: 10-10: 1, preferably be about 1: 4-4: 1, most preferably be about 2: 1-2: 3.
Should be appreciated that additional detergent raw material composition also can be sneaked in super mixer/thickener 10, and can not deviate from scope of the present invention, the back narration of several appearances is arranged in the additional detergent material composition.Have been found that under the described herein processing parameter condition, in super mixer/thickener 10, can successfully finish first procedure of processing, super mixer/thickener 10 is the mixing tank of L_dige CB mixing tank or similar brand preferably.The mixing tank of these types is made up of the static cylinder of the hollow with the level of the center being installed by rotating shaft basically, has several Plow shape blades around the rotating shaft.Rotating shaft is preferably with about 100 rev/mins-2500 rev/mins speed rotation, preferably with about 300 rev/mins-1600 rev/mins rotating speed rotation.The mean residence time of detergent ingredients in super mixer/thickening material 10 in about 2 seconds-45 seconds scope, most preferably is in about 5 seconds-15 seconds scope preferably.
The final washing composition granule that forms in super mixer/thickener 10 is sent in the mixing tank/thickener 16 of low speed or middling speed then, further carries out agglomeration in this process.In another embodiment, single spray-dried granules (not shown) stream is directly imported in moderate-speed mixers/thickener, and here super mixer/thickener 10 is strict selected for this specific embodiment of the present invention.Employed moderate-speed mixers/the thickener 16 of this method should comprise liquid distribution and agglomeration instrument, so that these two kinds of technology can be carried out simultaneously.Having for example is L_dige KM (Plow shape) mixing tank, and the moderate-speed mixers/thickener 16 of DraisK-T160 mixing tank or similar brand mixing tank is preferred.Preferably about 0.5 minute-Yue 15 minutes the residence time in moderate-speed mixers/thickener 16, most preferably the residence time is about 1 minute-Yue 10 minutes.
Referring now to Fig. 2, Fig. 2 has provided the local sectility skeleton view of moderate-speed mixers/thickener 16.As being seen by Fig. 2, central shaft 18 rotates in moderate-speed mixers/thickener 16 (for example L_dige KM (Plow shape) mixing tank).According to the present invention, a tuned damper 20 has been installed at least in the rotating shaft 18.Moderate-speed mixers/thickener 16 is realized liquid distribution by the bite 22 that is installed on mixing tank/thickener 16 inwalls and size is generally less than rotating shaft 18 sizes again.Be to move with about 3600 rev/mins rotating speed at least under the typical situation of bite.Moderate-speed mixers/thickener 16 also has Plow 24 and two inlets 21 and 23 that are installed on the central shaft 18, and Plow 24 can operate in the mixing/thickening of promotion process, the inlet 21 and 23 washing composition materials that can receive from super mixer/thickener 10.
As previously mentioned, rotating shaft 18 has the tendency that stands suitable intensive mechanical vibration, and this intensive mechanical vibration meeting affects operational process nocuously.Have been found that in this respect along the length direction of rotating shaft 18, one or more tuned dampers 20 are installed in different positions can reduce or eliminate so unwanted mechanical vibration.Synthetically turn to Fig. 3 and Fig. 4 now, wherein Fig. 3 has disclosed the local side figure of tuned damper 20, and Fig. 4 has represented to be equipped with on it end view of the rotating shaft 18 of tuned damper 20.Can see that by Fig. 3 and Fig. 4 tuned damper 20 comprises four columnarly can be reduced to minimal damping equipment 26 to the mechanical vibration of rotating shaft 18.Tuned damper 20 comprises two at least, preferably includes four these so-called columnar damping devices 26, and damping device 26 is installed in the rotating shaft 18, and per two are mutually 90 °, are connected by union lever 23.Damping device 26 can utilize any known mechanical means easily for example the split ring device link to each other with rotating shaft 18, the split ring device is then by the sleeve closure shown in Fig. 2,3 and 4.The outer tube 21 of the damping device of tuned damper 20 preferably make by bearing by material that it is exposed to environment wherein.In the method, environment is meant the detergent ingredients that it can allow outer tube 21 to be made by plastics.
Damping device 26 comprises a pair of tuning key 28 and 30, and tuning key is installed and is adjacent to member 32 two flexibilities or spring-like and 34.Flexible member 32 and 34 can be by for example resilient material manufacturing of any flexible materials, resilient material comprises paracril, natural rubber or synthetic isoprene-isobutylene rubber (for example available from llene industrial), perhaps flexible member 32 and 34 can be molded into final shape (for example Forsheda AB, Sweden) by the supplier.Flexible member 32 and 34 contacts with counterweight 35, and counterweight 35 is helpful aspect the mechanical vibration that cause at the continuous rotating speed that weakens by rotating shaft 18.
Tuned damper 20 is preferably regulated by the manipulation and the installation site of damping device 26, so that the maximum vibration of rotating shaft 18 is in the selected scope.Under the particular case, tuned damper 20 is regulated by the size of flexible member 32 and 34, in order to obtain tuned damper 20 needed natural frequencies.Tuned damper 20 preferably carries out tuning, so that its natural frequency is the natural frequency 95% of axle 18 approximately.If use more than one tuned damper 20, each natural frequency that is installed in the tuned damper 20 of axle on 18 can be distributed in the several frequencies place in 10 hertz of-20 hertz of scopes so, perhaps can both be tuned to identical frequency.
When tuned damper 20 suitably, in medium range of frequency of striding dead axle 18 measured about 10 hertz-Yue 20 hertz, the preferred maximum vibration of axle 18 is the about 1.0G of pact-1.0G-, and even more preferably about-about 0.5G of 0.5G-most preferably is pact-0.25G-0.25G.The maximum vibration that such maximum vibration stands commercial size manufacturing site location typical case demonstrates surprising improvement, such maximum vibration may be in ± order of magnitude scope of 3.5G in.Maximum vibration preferably uses 90 second timed interval to record.One skilled in the art will appreciate that such maximum vibration measure use conventional jerkmeter (from New York. Buffalo, PCB 308B ICP company obtains) be to be easy to finish.
For example, during present method operate continuously, the jerkmeter that axle 18 vibration use and propulsion source (for example, the digital tape recorder operated of PCB 480E 090 of ICP company and series of cells for example the TCD-D3 of Sony DAT register) link to each other carries out record.Register and propulsion source are contained in waterproof, the shockproof casing (for example Carlon CJ1085 casing).Transmitter utilizes dental bonding agent or other hard binding agent to link to each other with axle 18 and locatees, so that the radial vibration of measuring shaft.Vibration record at least 2 hours, preferably 4 hours.Operation one is finished, just from casing taking-up magnetic tape recorder and play.In 90 seconds the timed interval, make map device (for example Hewlett-Packard 3560A or 35670A analyzer) in digital or simulation and upward data are mapped.For example Excel or Matlab can measure vibration peak and root-mean-square value by PC base software program.
Do not plan bound by theory, but aggravated especially, on the internal surface of mixing tank/thickener 16, speckle with this moment on so-called " washing composition wall " with moderate-speed mixers/thickener 16 associated negative value maximum vibrations.In this process, have at least about 1 millimeter washing composition coating or a part of internal surface of the topped moderate-speed mixers/thickener 16 of washing composition wall.By this topped inner surface portion of very small thickness with 1 millimeter may be most (about 100% internal surface is by topped) or only be that 50% internal surface may be by topped.The existence of this washing composition coating provides irregular surface profile, during the axle 18 of moderate-speed mixers/thickener 16 rotates multitude 24 therewith surface profile contact.This irregular surface finally causes axle 18 to be subjected to the effect of irregular power, has therefore strengthened comprehensive mechanical vibration further.Tuned damper 20 also can be eliminated this additional mechanical vibration or make this additional mechanical vibration be reduced to minimum.
Again synthetically with reference to Fig. 1-4, the preferred density of the washing composition granule of discharging from moderate-speed mixers/thickener 16 that obtains or the spraying granule of another embodiment is 650 grams per liters at least, even more preferably about 700 grams per liters-Yue 800 grams per liters.The particle porosity of resulting this detergent composition granule preferably in the scope of about 5%-about 20%, preferably is about 10%.When the washing composition granule of discharging or spray-dired particle is prepared to pack at this moment and when selling with the closely knit Betengent product of low consumption, these washing composition granules or spray-dired particle can stand the processing of one or more optional procedure of processings from moderate-speed mixers/thickener 16.
Optional procedure of processing
The washing composition granule can randomly carry out drying in the equipment in fluidized bed dryer 36 or similarly.In the other optional step of present method, the washing composition granule of discharging from fluidized bed dryer 36 cools off fluidized bed cooler 36 or similar equipment known in the art by agglomeration and regulates further.
Following one or more positions that another optional procedure of processing is included in this flow process add coating, and to improve the mobile of detergent composition and/or to make the excessive nodulizing of detergent composition be reduced to minimum: (1) coated agent can be according to coated agent logistics 40 represented directly adding (preferably) after fluidized bed cooler 38 like that; (2) the coated agent can be according to coating logistics 42 represented adding between fluidized bed dryer 36 and fluidized bed cooler 38 like that; (3) coating can be by logistics 44 represented being added between fluidized bed dryer 36 and the moderate-speed mixers/thickener 16 like that; And/or (4) coating can be by represented such directly being added in moderate-speed mixers/thickener 16 of logistics 46.Should understand that the coated agent can be by the array mode of any one or they of logistics shown in Figure 1 40, logistics 42, logistics 44 and logistics 46 and added.In the method, coated agent logistics 40 is most preferred.
The coated agent preferably is selected from one group of material being made up of silico-aluminate, silicate, carbonate and their mixture.The coated agent has not only strengthened the free-flowing property of resulting detergent composition, and particularly when the coated agent directly is added in moderate-speed mixers/thickener 16, also by preventing excessive agglomeration or make excessive nodulizing be reduced to minimum to be used to control nodulizing, this resulting detergent composition is that the human consumer is needed, because this detergent composition can dip washing composition during use at an easy rate.As those skilled in the art known to fully like that, excessive agglomeration meeting causes final washing composition product very poor flowability and aesthetic feeling.
Present method can randomly be included in the step of the other binding agent of spraying in the middle of any or two among mixing tank/thickener 10 and 16.Adding " binding agent " is in order to strengthen nodulizing, to provide " bonding " or " adhesion " agent to detergent component.One group of material that binding agent preferably selects free water, anion surfactant, nonionogenic tenside, polyoxyethylene glycol, polyacrylic acid polyvinylpyrrolidone ester, citric acid and their mixture to form.People's such as Beerse United States Patent (USP) 5,108,646 (Procter and Gamble company) has been narrated other the suitable binder material that comprises these materials of listing here, and this U.S. Patent Publication is incorporated herein by reference document in the lump at this paper.
The optional step of other that the inventive method is considered is included in and screens out granularity excessive washing composition granule or spray-dried granules in the screening plant 48; screening plant 48 can be taked various forms, includes but not limited to for the selected traditional mesh screen of the washing composition finished product of required granularity.Other optional step comprises makes granule stand other drying and regular washing composition granule.
The other optional step of present method need be utilized various methods, synthetically with reference to the final procedure of processing 50 of Fig. 1, processes resulting washing composition granule at last, and these methods comprise that the common detergent ingredients that makes other sprays and/or mix.For example, final procedure of processing comprises spices, whitening agent and enzyme is sprayed on the finished product granule, so that detergent composition more completely to be provided.Such technology and batching are well-known in the present technique field.
The detergent surfactant mashed prod
Though the present invention also considered several forms, the employed detergent surfactant mashed prod of present method preferably is in aqueous viscous batter form.This so-called viscous surface promoting agent mashed prod has the viscosity of about 5,000 centipoises-Yue 100,000 centipoises, preferably is the viscosity of about 10,000 centipoises-Yue 80,000 centipoises, contains about 10% water at least, preferably contains about 20% water at least.Viscosity is to be about under the 10-100/ situation of second 70 ℃ and velocity of shear to measure.In addition, the tensio-active agent mashed prod if you are using, preferably should contain detergent surfactant, equilibrium water and other the common detergent ingredients of front specified amount.
It preferably is selected from anionic, non-ionic, zwitterionic, amphoteric and cationic species and their compatible mixtures the tensio-active agent of the tensio-active agent mashed prod of viscosity itself.The United States Patent (USP) 3 of the Norris of issue on May 23rd, 1972, the people's such as Laughlin of issue on December 30th, 664,961 and 1975 United States Patent (USP) 3,919,678 have all narrated detergent surfactant used herein, and these two pieces of patent this paper all are incorporated herein by reference document in the lump.Useful cats product also comprises the United States Patent (USP) 4 of the Cockrell of issue on September 16th, 1980,222, the United States Patent (USP) 4 of the Murphy of issue on December 16th, 905 and 1980,239,659 those tensio-active agents of being narrated, these two pieces of patent this paper also are incorporated herein by reference document in the lump.Among these tensio-active agents, anion surfactant and nonionogenic tenside are preferred, and anion surfactant is most preferred.
The infinite example of useful preferred anionic surfactants tensio-active agent comprises common C in the tensio-active agent mashed prod 11-C 18Alkylbenzene sulfonate (" LAS "), one-level side chain and random C 10-C 20Alkyl-sulphate (" AS "), chemical formula is 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 7 integer in the formula preferably is at least 9 integer, and M is a water-soluble cationic, particularly sodium.Unsaturated vitriol is oleoyl vitriol and C for example 10-C 18Alkyl alkoxy sulfate (" AE xS ", EO1-7 ethoxy sulfate particularly).
The optional exemplary surfactants of useful other comprises: C in the mashed prod of the present invention 10-C 18Alkyl alkoxy carboxylate salt (particularly EO1-5 ethoxy carboxylate), C 10-C 18Glyceryl ether, C 10-C 18Alkyl polyglycoside and their the many glycosides of corresponding sulfation, and C 12-C 18α-sulfonated fatty acid ester.If necessary, common non-ionic and amphoterics for example comprises so-called narrow peak alkylethoxylate and C 6-C 12The C of alkylphenol alcoxyl hydrochlorate (particularly ethoxy hydrochlorate and blended ethoxy/third oxygen hydrochlorate) 12-C 18Alkyl ethoxy hydrochlorate (" AE "), C 12-C 18Trimethyl-glycine and sultaine, C 10-C 18Amine oxide or the like also can be included in whole compositions.Also can use C 10-C 18N-alkyl polyhydroxy fatty acid amide.Typical example comprises C 12-C 18N-methyl grape sugar acid amides.Ask for an interview WO9,206,154.Other sugared deutero-tensio-active agent comprises N-alkoxyl group polyhydroxy fatty acid amide, for example C 10-C 18N-(3-methoxy-propyl) glucamide.The N-propyl group is to the C of N-hexyl 12-C 18Glucamide can both be used for low pore forming material.Also can use C 10-C 20Soap commonly used.High if desired foaming can be used side chain C 10-C 16Soap.The mixture of negatively charged ion and nonionogenic tenside is useful especially.Listed other common useful tensio-active agent in the standard textbook.
The dry detergent material
The inventive method detergent raw material preferably comprises the washing composition aluminosilicate and helps washing composition and yellow soda ash, and washing assistant is called the aluminosilicate ion exchange material.Here the aluminosilicate ion exchange material as detergent builders preferably has high-calcium ionic exchange capacity and high switching speed.Under the situation that is not intended to bound by theory, it is believed that high like this calcium ion exchange rate and high-exchange-capacity are the functions of several mutual related factors, these factors are to be drawn by the method for producing the aluminosilicate ion exchange material.In this respect, employed here aluminosilicate ion exchange material is preferably according to people's such as Corkill United States Patent (USP) 4,605,509 (Procter ﹠amp; Gamble) produce, open this paper of this patent introduces in the lump as document.
The aluminosilicate ion exchange material is preferably " sodium " type because the potassium type of this aluminosilicate and Hydrogen do not demonstrate resemble that the sodium type provides high ion-exchange speed and capacity.In addition, the aluminosilicate ion exchange material is preferably the form of complete drying, so that promote the production of crisp as described herein hard detergent granule.Here employed aluminosilicate ion exchange material preferably has makes their efficiency optimizationization and grain diameters as detergent builders.The average grain particle diameter with the given aluminium sulfate ion exchange material of routine analysis technical measurement, for example micro-mensuration of routine analysis technology and scanning electron microscope (SEM) represented in the term of employed here " grain diameter ".Preferred aluminium silicate particles particle diameter is about 0.1 micron-Yue 10 microns, preferably is about 0.5 micron-Yue 9 microns.Grain diameter most preferably is about 1 micron-Yue 8 microns.
The aluminosilicate ion exchange material preferably has chemical formula
Na z[(AlO 2) z.(SiO 2) y]xH 2O
Z and y are at least 6 integer in the formula, and z is about 1-5 to the mol ratio of y, and x is about 10-264.Aluminosilicate preferably has chemical formula
Na 12[(AlO 2) 12.(SiO 2) 12]xH 2O
X is about 20-30 in the formula, preferably about 27.These aluminosilicates are commercial to be bought, and for example label is zeolite A, zeolite B and X zeolite.In addition, the manually synthetic aluminosilicate ion exchange material that is suitable for herein using that obtains of naturally occurring or people can be by the method manufacturing of people's such as Krummel United States Patent (USP) 3,985,669 narrations, and this patent disclosure this paper is incorporated herein by reference document in the lump.
Aluminosilicate used herein is further characterized by their loading capacity, calculates according to butt, and loading capacity is 200 milligramequivalent CaCO at least 3Hardness per gram, loading capacity are preferably at about 300-352 milligramequivalent CaCO 3In the hardness per gram scope.In addition, this aluminosilicate ion exchange material is further characterized by their calcium ion exchange rate, and calcium ion exchange rate is at least about being 2grain Ca ++/ gpm/-Ke/gallon, preferably at about 2grain Ca ++/ gpm/-Ke/gallon-Yue 6grain/ gpm/-scope of Ke/gallon in.
Help detergent ingredients
The dry detergent raw material of present method can comprise auxiliary washing composition composition and/or can add any amount of auxiliary composition during the later step of present method in detergent composition.These additional compositions comprise other detergent builder compound, SYNTHETIC OPTICAL WHITNER, bleach-activating agent, short infusion, froth suppressor, rust-preventive agent and resist, dirt suspension agent, dirt releasing agent, sterilant, pH regulator agent, non-washing assistant alkali source, sequestrant, polynite, enzyme, enzyme stabilizers and spices.Referring to Baskerville, the United States Patent (USP) 3,936,537 that people such as Jr. issued on February 3rd, 1976, this patent this paper is incorporated herein by reference document.
Other washing assistant generally can be selected from ammonium phosphate, polyphosphate, phosphonate, polyphosphonic acid salt, carbonate, borate, polyhydroxy sulfonate, many acetate, carboxylate salt and the multi-carboxylate of various water-soluble basic metal, ammonium or replacements.Basic metal, particularly above-mentioned sodium salt are preferred.Here that preferred use is phosphoric acid salt, carbonate, C 10-C 18Lipid acid, multi-carboxylate and their mixture.Tripoly phosphate sodium STPP, tetrasodium pyrophosphate, Citrate trianion, tartrate, list-and two-butyrates and their mixture (vide infra) even more preferably.
Compare with unbodied water glass, the crystalline lamina sodium silicate demonstrates the obvious increase of calcium ion and magnesium ion exchange capacity.In addition, lamina sodium silicate affinity magnesium ion and be better than calcium ion, this is to guarantee whole " hardness " removed from washing water and a feature needing.The crystalline lamina sodium silicate is generally than amorphous sodium silicate costliness, also than other washing assistant expensive price.In addition, for the washing composition of practical economically washing usefulness is provided, must determine the ratio of employed crystalline lamina sodium silicate carefully.
The crystalline lamina sodium silicate that is fit to herein use preferably has following chemical formula
NaMSi xO 2x+1·yH 2O
M is sodium or hydrogen in the formula, and x is about 1.9-4, and y is 0-20.The crystalline lamina sodium silicate more preferably has following chemical formula
NaMSi 2O 5·yH 2O
M is sodium or hydrogen in the formula, and y is 0-20 approximately.The crystalline lamina sodium silicate of these and other carried out discussion in people's such as Corkill United States Patent (USP) 4,605,509, this patent also is incorporated herein by reference document at this paper.
The object lesson of inorganic phosphate builders is tri-polyphosphate, the pyrophosphate salt of sodium and potassium, has polymer metaphosphate and orthophosphoric acid salt that the polymerization degree is about 6-21.The example of polyphosphonic acid salt washing assistant is the sodium of ethylidene diphosphonic acid and sylvite, ethane 1-carboxyl-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.United States Patent (USP) 3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176 and 3,400,148 disclose other phosphorus washing-aid compound, and these patents this paper is incorporated herein by reference document.
The example of non-phosphorus inorganic builders is ten hydrates of tetraborate and has SiO 2To the about 0.5-4.0 of the weight ratio of alkalimetal oxide, the preferably silicate of about 1.0-2.4.Here useful water miscible non-phosphorus inorganic builders comprises many acetate, carboxylate salt, multi-carboxylate and the polyhydroxy sulfonate of various basic metal, ammonium and replacement ammonium.Many acetate and multi-carboxy acid salt washing agent's example is sodium, potassium, lithium, ammonium and the substituted ammonium salt of ethylene dinitrilotetra-acetic acid, triglycollamic acid, hydroxyl disuccinic acid, mellitic acid, benzene polycarboxylic acid and citric acid.
The polymeric multi-carboxy acid salt washing agent is that the Diehl United States Patent (USP) 3,308,067 of issue on March 7th, 1967 proposes, and open this paper of this patent is incorporated herein by reference document.Such material comprises the aliphatic carboxylic acid for example homopolymer of toxilic acid, methylene-succinic acid, methylfumaric acid, fumaric acid, aconic acid, citraconic acid and methylene radical propanedioic acid and the water-soluble salt of multipolymer.Some water-soluble anionic polymers of in these materials certain as description, and only when being in intimate mixture, be only useful with non-soap anionic surfactant.
Other suitable multi-carboxylate used herein is the United States Patent (USP) 4 of people's such as Crutchfield issue in 13 days March in 1979,144,226 and the United States Patent (USP) 4 issued on March 27th, 1979 of people such as Crutchfield, 246, the polyacetal carboxylation of 495 narrations, these two pieces of patents are incorporated herein by reference document here in the lump.Under polymerizing condition, glyoxylic esters and polymerization starter are put together can prepare these polyacetal carboxylations.Resulting polyacetal carboxylic acid ester links to each other with chemically stable end group then, makes the polyacetal carboxylation for depolymerization is stable rapidly in basic solution, is converted into corresponding salt, and adds in the detergent composition.Particularly preferred multi-carboxy acid salt washing agent is an ether carboxylate salt lotion-aid combination, said composition contains the United States Patent (USP) 4 that people such as Bush issued on May 5th, 1987,663, the tartrate monosuccinic acid salt of 071 narration and the composition of tartrate disuccinate, open this paper of this patent also is incorporated herein by reference document.
The United States Patent (USP) 4,483,781 that United States Patent (USP) 4,412,934 that people such as Chung issue on November nineteen eighty-three 1 and Hartman1984 delivered at November 20 has been narrated SYNTHETIC OPTICAL WHITNER and activator, and these two pieces of patents also are incorporated herein by reference document here.People's such as Bush United States Patent (USP) 4,663,071 has also been narrated SYNTHETIC OPTICAL WHITNER from 17 hurdles, 54 row to 18 hurdles, 68 row, and this patent this paper also is incorporated herein by reference document.Foam properties-correcting agent also is optional ingredients, the United States Patent (USP) 3 that people such as Bartoletta issued on January 20th, 1970,933,672 and the United States Patent (USP) 4 issued on January 23rd, 1979 of people such as Gault, 136,045 narrates these foam properties-correcting agent, and these two pieces of patent this paper also are incorporated herein by reference document.
The United States Patent (USP) 4,762 that people such as Tucker issued on August 9th, 1988,645 the 6th hurdle the third lines to the, 7 hurdles the 24th row has been narrated suitable polynite, and this patent also is incorporated herein by reference document in this article.Baskerville patent the 13rd hurdle 54 row have been enumerated the other detergent builder compound used herein that is suitable for to the United States Patent (USP) 4,663,071 of people's such as 16 hurdles, 16 row and Bush issue in 5 days Mays in 1987, and these two pieces of patent this paper also are incorporated herein by reference document.
For the present invention is easier to understand, be illustrated below with reference to following example, the purpose of these examples just illustrates, and is not limited in this scope.
Example I
This example has illustrated method of the present invention, and this method is produced free-pouring crisp hard high density detergent composition.The feed stream of two different washing composition original compositions is sent in L_dige CB-30 mixing tank/thickener continuously with 2800 kilograms/hour speed, a feed stream contains the tensio-active agent mashed prod, mashed prod contains tensio-active agent and water, another feed stream contains the dry detergent raw material, and this detergent raw material contains aluminosilicate and yellow soda ash.The rotating speed of L_dige CB-30 mixing tank/thickener shaft is 1400 rev/mins approximately, and mean residence time was 10 seconds approximately.The inclusion of L_dige CB-30 mixing tank/thickener is sent into continuously and is supplied further agglomeration in L_dige KM600 mixing tank/thickener, and the agglomeration period average residence time is 6 minutes approximately.L_dige KM 600 mixing tanks/thickener comprises four tuned dampers that connect with central rings.Tuned damper is arranged in the below of mixer length, and the position is partitioned into 90 ° around rotating shaft.Each quality or wt pts weigh 30 pounds, and the flexible member of tuned damper is arranged by size, and be tuned to about 25 hertz.Four tuned dampers all are encapsulated in the sleeve pipe.Resulting washing composition granule is sent to fluidized bed dryer then, then is sent to fluidized bed cooler again, and mean residence time is about 10 minutes respectively and 15 minutes.The coated agent, aluminosilicate is sent into about the middle below of moderate-speed mixers/thickener 16 greatly, to control and to prevent excessive agglomeration.The washing composition granule sieves with the common sieve apparatus of crossing then, finally obtains uniform grain sizes and distributes.Following table 1 has been listed from the composition of the washing composition granule of fluidized bed cooler discharge:
Table I Component The weight percent % of combined feed total feedC 14- 15Alkyl-sulphate/alkyl ethoxy sulfate 29.1 aluminosilicate 34.4 yellow soda ash, 17.5 polyoxyethylene glycol (molecular weight 4000) 1.3 mishmashes (water etc.) 16.7
100.0
The additional washing composition batching that contains spices, enzyme and other submember is being sprayed on above-mentioned in final procedure of processing, the detergent composition made from final formation.
Following Table II has been listed the relative proportion of whole washing composition compositions of making of the flow process generation that utilizes present method:
Table II Component (weight percent %)
AC 14- 15Alkyl-sulphate/C 14- 15Alkyl ethoxy sulfate 16.3Neodol 23-6.5 13.0C 12- 14N-methyl glucose amide 0.9 polyacrylate (molecular weight=4500) 3.0 polyethylene glycol (molecular weight=4000) 1.2 sodium sulphate 8.9 aluminosilicates 26.3 sodium carbonate 27.2 proteinase-10 .4 amylase 0.1 lipase, 0.2 cellulase, 0.1 submembers (water, spices etc.)12.4
100.0
1By the commercial C that buys of the Shell Oil Co. 12- 13Alkyl ethoxy compound (EO=6.5).
The density of resulting detergent composition is 796 grams per liters, and mean particle size is 613 microns.
Example II
This example has illustrated that this method at first makes the particle spraying drying, mixes then according to another method of the present invention in moderate-speed mixers/thickener.The detergent composition of following Table III is 300 ℃ of temperature, 2800 pounds of speed/time, make in the counter-flow air spray-drying tower that diameter is 10 feet.Particle is sent in L_dige KM-600 mixing tank/thickener, about 12 minutes of the residence time.L_dige KM-600 mixing tank/thickener comprises four tuned dampers that connected by central rings.This tuned damper is positioned the middle below of this mixer length, places around the rotating shaft 90 ° at interval.Each quality or wt pts weigh 30 pounds, flexible member configuration size dimension and be tuned to about 25 hertz.All four tuned dampers are adorned then and are enclosed in the sleeve pipe.
Table III Component The weight percent % of combined feed total feedC 14- 15Alkyl-sulphate/alkyl ethoxy sulfate 10.2C 12- 13Linear alkyl benzene sulfonate 10.2 aluminosilicates, 27.0 sodium carbonate, 21.9 polyethylene glycol (molecular weight 400) 1.4 polyacrylate (molecular weight=4500) 4.0 sodium sulphate 13.0 brightening agents, 0.3 sodium metasilicate (1.6r), 1.0 impurityes (water, spices etc.)11.0
100.0
The additional detergent composition that comprises spices and enzyme is sprayed on the above-mentioned particle in final procedure of processing, finally to obtain making detergent composition.Following Table IV has been listed the relative proportion of whole detergent composition of making of the flow process generation that utilizes present method:
Table IV Component % weight
AC 12- 16Linear alkyl benzene sulfonate 9.0C 14- 15Alkyl-sulphate/C 14- 15Alkyl ethoxy sulfate 9.0Neodol 23-6.5 12.0 polyacrylate (molecular weight=4500) 3.5 polyethylene glycol (molecular weight=4000) 1.2 sodium sulphate, 11.4 sodium metasilicate (1.6r) 0.9 aluminosilicate 23.8 brightening agents 0.3 sodium carbonate 28.4 proteinase-10 .4 amylase 0.1 lipase, 0.2 cellulase, 0.1 submembers (water, spices etc.)9.7
100.0
1The commercial C that can buy from the Shell Oil Co. 12- 13Alkylethoxylate (EO=6.5).
The density of final resulting detergent composition is 822 grams per liters.
Because the present invention at length narrates, and knows so those skilled in the art will know, can make different changes in not deviating from scope of the present invention, can't think that the present invention is confined to the described content of specification sheets herein.

Claims (18)

1. continuous preparing washing agent method for compositions comprises the steps:
(a) detergent surfactant mashed prod and dried detergent raw material are sneaked in super mixer/thickener continuously, to obtain the washing composition granule;
(b) described washing composition granule is mixed in moderate-speed mixers/thickener, so that make further densification of described washing composition granule and agglomeration, wherein said moderate-speed mixers/thickener comprises central rotating shaft, tuned damper equipment is housed, so that described rotating shaft at the maximum vibration in the rotating shaft of middle span is-1.0G to 1.0G on the central rotating shaft in 10 hertz-20 hertz range of frequency;
(c) dry described washing composition granule is so that form described detergent composition.
2. the process of claim 1 wherein that described moderate-speed mixers/thickener comprises that the part of described moderate-speed mixers/thickener inner wall surface has the washing composition coating of at least 1 mm thick.
3. the process of claim 1 wherein that the density of described detergent composition is 650 grams per liters at least.
4. the process of claim 1 wherein that the maximum vibration of described central shaft is-0.5G to 0.5G approximately.
5. the process of claim 1 wherein that the maximum vibration of described central shaft is-0.25G to 0.25G approximately.
6. the method for claim 1 also comprises adding the step that applies agent after described super mixer/thickener, and wherein said coating agent is selected from this group material of being made up of aluminosilicate, carbonate, silicate and their mixture.
7. the method for claim 1, this method also comprises the step of cooling off described washing composition granule.
8. the process of claim 1 wherein that the mean residence time of described washing composition granule in described super mixer/thickener is in about 2 seconds-Yue 45 seconds scope.
9. the process of claim 1 wherein that the mean residence time of described washing composition granule in described moderate-speed mixers/thickener is in about 0.5 minute-Yue 15 minutes scope.
10. continuous preparing washing agent method for compositions, this method comprises the following steps:
(a) sneak into the spray-dried detergent particle in moderate-speed mixers/thickener continuously, wherein said moderate-speed mixers/thickener comprises central rotating shaft, tuned damper equipment is housed, so that described rotating shaft is pact-1.0G about 1.0G extremely at the maximum vibration in the rotating shaft of middle span in about 10 hertz-Yue 20 hertz range of frequency on the central rotating shaft;
(b) dry described washing composition granule is so that form described detergent composition.
11. the method for claim 10, wherein said moderate-speed mixers/thickener are included in have an appointment at least 1 millimeter washing composition coating of the part of described moderate-speed mixers/thickener inner wall surface.
12. the method for claim 10, the maximum vibration of wherein said rotating shaft are that pact-0.5G is to about 0.5G.
13. the method for claim 10, the maximum vibration of wherein said rotating shaft are that pact-0.25G is to about 0.25G.
14. the method for claim 10, this method make described spray-dried granules sneak into the interior step of super mixer/thickener before also being included in described moderate-speed mixers/thickener.
15. the method for claim 14, this method add the step that applies agent after also being included in described super mixer/thickener, wherein said coating agent is selected from one group of material being made up of aluminosilicate, carbonate, silicate and their mixture.
The method of 16 claims 14, the mean residence time of wherein said spray-dried granules in described super mixer/thickener are in about 2 seconds-Yue 45 seconds scope.
17. the method for claim 10, this method also comprises the step of cooling off described spray-dried granules.
18. the method for claim 10, the mean residence time of wherein said spray-dried granules in described moderate-speed mixers/thickener is in the about 15 minutes scope of about 0.5-.
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