CN1110542C - High active granular detergent compositions and process for making them - Google Patents
High active granular detergent compositions and process for making them Download PDFInfo
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- CN1110542C CN1110542C CN95196314A CN95196314A CN1110542C CN 1110542 C CN1110542 C CN 1110542C CN 95196314 A CN95196314 A CN 95196314A CN 95196314 A CN95196314 A CN 95196314A CN 1110542 C CN1110542 C CN 1110542C
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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
- 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
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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
Abstract
Process for making a detergent composition having at least 40 % by weight of surfactant and a bulk density of at least 650 g/l, the process comprising the single step of high shear mixing until granular at a temperature from ambient to 60 DEG C, a binder component comprising said surfactant and less than 20 % water, with a particulate solid component, of initial particle size from 0.1 to about 500 microns, said particulate solid component having at least about 15 % by weight of particles with a particle size of at least about 50 microns and a sufficient amount of smaller particles so that the average surface area of the particulate component is at least about 9 m<2>/g as measured by the BET method, and wherein the binder maintains the mixture in a particulate state throughout the process.
Description
The application is the common pending application S/N 08/083 that submitted on June 25th, 1993,115 part continues, S/N 08/083,115 is submission on November 24th, 1992, existing resigned application S/N 07/980,856 part continues, S/N 07/980,856 submitted to the part of existing resigned common pending application S/N 07/816,408 to continue on December 31st, 1991.
Technical field
The present invention relates to a kind of production high active granular detergent composition, the method of high-bulk-density granular detergent composition particularly, be a kind of tap density more than 600 grams per liters, preferably be at least 650 grams per liters, and comprise the detergent composition of at least 40% (weight) tensio-active agent.Preferred this granular detergent composition has good powder property.More specifically, the present invention relates to a kind of preparation granular detergent composition, particularly contain the method for surfactant composition at high proportion.
Background and prior art
Surfactant content is up to about 40% (weight) or above granular detergent composition, than the composition of lower concentration content advantage arranged, particularly in water consumption less work environment.In addition, the granular detergent composition of high-bulk-density is more favourable than the composition of low bulk density.Reducing of saccharoid packaging volume promptly because packing diminishes, helps storing the transportation with product.The factor of decision detergent particles tap density is that dry mix is produced the tap density of the used starting raw material of particle and the chemical constitution that spray-drying process is produced the used slurry of particle.Adopt one of these two kinds of influence factors to change tap density if limit the preparation effective composition, then in most of the cases, the growth that tap density is very big can only realize by mechanical workout.
From enhanced environmental protection viewpoint day by day, the consumption that preferably can reduce water is with conserve water and be used for heating its energy.By this, be applicable to that the high reactivity powdered detergent of low water consumption is very favourable.
Generally speaking, machinery is fine and close to be realized the particle of commercial high-bulk-density by spray-dried powders is carried out.The method power consumption of this production high-bulk-density detergent particles is high, investment is big.Be used to carry out spray-dired equipment price costliness, and this method itself to be removed the water of 30～40% (weight) and be consumed big energy from slurry.Because spraying drying is a thermal process, so limited the component that adds preparation, particularly can produce nonionogenic tenside and some sensitivities or the volatile component of undesirable smog, as enzyme and spices, can be degraded or lose.After the spraying drying, also need other equipment and energy is used for further mechanical workout so that the powder densification.
European application EP-A-337,330 (Henkel) relate to a kind of continuous production and contain method a large amount of negatively charged ion and nonionogenic tenside, the high-bulk-density detergent powder, said method is included in the super mixer, add the nonionogenic tenside material processing spray-dried detergent materials, the mean residence time of washing composition material in mixing tank is 10～60 seconds.
United States Patent (USP) 4,923,636 and be issued to people's such as Blackburn United States Patent (USP) 4,826,632 and the United States Patent (USP) 5,324 that is issued to people such as Dumas, 455 disclose to improving tap density, can be sprayed to the liquid surfactant composition on the spray-dired powder.Although the fine and close ＂ of these ＂ spray-dried powders do not produce by mechanical compaction, begin to produce with spray-dried powders and still exist shortcoming.In addition, if want not destroy the character of powder, only have limited amount liquid surfactant can supply to spray, and spray method depend on the absorption powder-base.
Many prior aries of producing detergent particles without spraying drying are arranged.These technology all have shortcoming.Most of technology are to form dough earlier in the first step, and going on foot again second, discrete (deagglomerated) becomes particle.Generally speaking, then particle is coated, and in the step afterwards it is carried out drying.An embodiment of this method is disclosed in the U.S. Patent No. 5,045,238 of Jolicoeur.This multistep processes need be carried out the granulation operation respectively more than one mixing tank.Other method need use the acid tensio-active agent just can produce.Some in addition need high temperature, this can cause starting raw material to be degraded.
U.S. Patent No. 4 that authorize May 15 nineteen ninety, people such as Strauss, 925,585 disclose surfactant paste and detergent builder compound subtly dispersing and mixing become a dough sticking, similar intermediate, prepare the method for high-bulk density detergent compositions.For this dough is made particle, must be cooled to it to be low to moderate-25 ℃ temperature, for example use dry ice, further mix then, make macrobead.In order to reach the ideal water content, particle is carried out drying, for example fluidized bed dryer with independent drying step.This method comprises three steps at least, because need cooling and dry, so length consuming time, cost height.
The U.S. Patent No. 4,666,740 that licensed to Wixon on May 19th, 1987 discloses by liquid or paste nonionic detergent being sprayed onto the method on ready-made carbonate-supercarbonate bead, prepares some high-bulk-density detergent particles.Subsequently bead is coated with zeolite and make free-pouring particle.
The european patent application No.420 317 of Appel discloses and has passed through the liquid acid precursor of neutralize anionic surfactant on the spot, the three-step approach of preparation high-bulk-density granular detergent composition.Usually, in these class methods, need excessive carbonate to guarantee that suitable conversion is carried out in acid.And the rising that excessive carbonate can cause the pH of product to make us not expecting.Owing to use the acid precursor, also need the careful operation of granulation process, keep properly and conscientiously coordinate.
People's such as Beerse United States Patent (USP) 5,108,646 discloses a kind of preparation granular detergent detergent builders, rather than the prilling process of detergent composition completely.Gravely, in addition applicant's invention need, also describe the granulation route of a complete washing composition of preparation at least about the active surfactant of 40% (weight).Contain detergent solids in applicant's the particle, as washing assistant and weighting agent, and as the granulation process tackiness agent, the low-down mixed surfactant activator of water content.People such as Beerse disclose a kind of method of carrying out granulation with moisture mixed active lotion, but for preparing Betengent product completely, particle must mix with at least 1.3 times of spraying drying basal granule to its weight.The solid detergent part of Beerse must be selected from zeolite or silicate, and the solid particle diameter is limited to 0.1～10 micron.The present invention allows any detergent solids composition, comprises that soda powder or sodium sulfate that particle diameter is relatively large exist.In addition, be different from and of the present inventionly be, the anion surfactant of Beesre is limited to 3: 1 to the ratio of nonionogenic tenside or is bigger.In the additive particles of Beerse, washing assistant is 1.75: 1～3.5: 1 to the weight ratio of tackiness agent.So the maximum of tensio-active agent is about 36% in the additive.
People need a kind of method of preparation granular detergent composition, particularly high-bulk density detergent compositions, and this method is made starting raw material without spray-dried powders, so reduced the shortcoming and the complicacy of art methods.
We find that with the raw material that is easy to get, the granular detergent composition of producing high reactivity, high-bulk-density with method simple, less energy-consumption is possible.We find that also it also is possible using the granular detergent composition that the method environment friendliness, that power consumption is low is produced high reactivity, high-bulk-density, preferably produces the high detergent composition of surfactant content.
Especially, we find now, if when handling starting raw material with super mixer/fine and close device, the surfactant system that one mobile is contained anion surfactant and alkoxy-based non-ionic surface active agent joins in the granulous starting raw material and goes, and can realize these targets and other preferred target.Anion surfactant can be linear alkylbenzene sulfonate, alkyl-sulphate etc.Have been found that, by solid detergent composition and tackiness agent granulation together, can produce the high super detergent powder of surfactant content, said tackiness agent is by low anion surfactant and the nonionogenic tenside liquid mixture of water content and have high surface area, constitute as the small-particle component of granulation aid.Whole particulate mixtures has high surface area, or selects component of mixture to obtain high surface area by operation.Active (tensio-active agent) content can be at least the tensio-active agent of 40% (weight) up to 60% (weight).Compare with the granulation process that does not add the high surface area component, the advantage of this law has been to improve the active quantities that is incorporated in the particle.
Summary of the invention
So, the invention provides a kind of be used to the produce method of high reactivity, high-bulk density detergent compositions and the product for preparing with this method, this method may further comprise the steps: be that about 0.1～about 500 microns granular solids component high shear mixing is granular until forming with a kind of binder ingredients and a kind of initial particle, said binder ingredients comprises through neutralization or part neutral tensio-active agent, wherein, in whole process mixture to be remained granular for tackiness agent.For crystal seed is provided, have at least the particle diameter of 15% (weight) granular solids to be necessary at least 50 microns, preferred about 50～400 microns.The applicant finds, if add the particle with suitable particle diameter and surface-area of q.s, make the average surface area of all particles that record with the BET method, use at least more than 9 meters squared per gram, preferably more than at least 15 meters squared per gram, then can use high-load especially active substance, theoretically, consumption can reach 60%.
The advantage of present method and product is simple to operate, need only a mixing tank with finishing once going on foot, production cost is low, and operation at room temperature.Therefore, environmental problem is arranged seldom, institute's energy requirement is also few.For most of preparations, do not need drying step.This law is flexible, promptly sensitive ingredients can be when process begins and solid and binder ingredients add together, do not need the later stage feed in raw material (postdosing).
This law comes down to a kind of agglomeration technique, wherein solid ingredient is passed through the binder ingredients agglomeration, forms to comprise solid ingredient and tensio-active agent detergent granules mutually.Q.s high surface area solid makes the solid of unit weight can adsorb more surfactant.
This agglomeration technique than the advantage that the mobile surfactant composition method in the granular starting raw material that absorbs is had is, by nodulizing, can make more that the flow surface promoting agent material of volume is incorporated in the composition, keeps good powder property simultaneously.
This agglomeration technique can use the operate continuously method or carry out with intermittent process.But preferred continuous processing.
Detailed Description Of The Invention
The present invention relates to a kind of method for preparing high reactivity, high-bulk density detergent compositions and composition itself, this method comprises the steps: that (i) is a tackiness agent that contains through neutralization or part neutral tensio-active agent, thereby to be submicron to about 500 microns solid ingredient join makes particulate mixtures in the high speed shear mixing tank with an initial particle, (ii) said mixture is carried out high speed shear and mix, thereby the component granulation with the formation particle diameter is 1～1200 micron particle.The preferred back of mixing as zeolite, joins coating in the mixing tank.
Detergent composition suitably is a kind of detergent composition completely.The used complete ＂ of term ＂ is meant a kind of detergent composition that can play tensio-active agent effective washing powder effect, that comprise q.s, washing assistant and alkaline source.Alkaline source is meant soda powder or phosphoric acid salt.The complete ＂ of term ＂ does not limit with traditional amount and adds some minor component, for example is less than 5% (weight).This class minor component comprises enzyme, SYNTHETIC OPTICAL WHITNER, spices, anti redeposition agent or dyestuff, to strengthen the performance of washing powder.
If be ready, can be granular detergent composition as the raw material in the washing composition production process.For example, can be sprayed onto a kind of tensio-active agent of liquid ingredient such as nonionogenic tenside on the composition, then coated with coating, as coated with zeolite.If with the detergent composition is raw material, then preferably use the direct product of the inventive method.Promptly before they are used as raw material, the interpolation component is not mixed in the detergent granules.But,, can carry out premix to detergent granules and the independent particle that contains other material respectively if be ready.Its advantage is, allow in the somewhere with single stage method produce detergent composition and randomly with independent particles mixture, be transported to place far away then and store or further process on request.
For as raw material, suitable detergent composition is pure state basically.Our said ＂ ＂ of pure state basically is meant the composition that may contain up to other particulate material of 10% (weight), but preferably is substantially free of the composition of any other this material.
The particle of solid ingredient must contain at least 15%, particle diameter is 50 microns solid, the solid average surface area must be at least 9 meters squared per gram.
An important feature of present method is that mixture remains particle or granular in whole process.Not forming dough promptly means and does not need discrete step.Just because of this reason, this law is just simple, and can a step produce end product.
＂ particle diameter ＂ in the context of the invention is meant the median size of measuring with the Rosin-Rammler computing method.
Importantly this law is a kind of improving method that is easy to control, and has ideal particle size range and powder property with its detergent powder of producing, can compare with detergent powder in the market.For obtaining detergent powder with good powder performance, except that adding tackiness agent, it is useful adding one or more components with this composition that the viscosity that makes the whole tackiness agents that finally obtained significantly improves again.The viscosity that the interpolation of these components generally can make above and be mentioned raises 5 at least, preferably raises 10 at least, and (is 0.1～20 revolutions per second of (s with the Haake viscometer in shearing rate most preferably to raise 100 at least
-1) time measure).
Because viscosity increases, this method seems more easy to control, and this can cause the better powder property of detergent composition.
This example that can improve the component of viscosity comprise water, particularly with certain stoichiometry, be enough in and the alkaline matter (as caustic soda) of lipid acid blended lipid acid mutually, their final soap that obviously generates.
In process of production, solid ingredient and binder ingredients to be mixed, solid ingredient comprises detergent builder compound, as water-soluble alkaline inorganic material (as being the yellow soda ash of crystal seed with lime carbonate), zeolite, tripoly phosphate sodium STPP and other water-soluble inorganic material, as sodium bicarbonate or silicate, white dyes, polycarboxylate polymer, anti redeposition agent, weighting agent; Binder ingredients also comprises water, silicate solutions, liquid polymers component, polyoxyethylene glycol, spices, lipid acid and other material except that through neutralization or part neutral tensio-active agent.In the context of the present invention, under the condition that the term adhesive component is meant in this production process to be run into, any component of plastically deformable.
The present invention allows to add the tensio-active agent of high level in the detergent powder that granulation produces.Beyond thought is that the particle that interpolation has enough high surface areas on a small quantity just can make the average surface area of granular solids be at least about 9 meters squared per gram, preferably is at least about 15 meters squared per gram, has greatly improved the amount of surfactant that can add.For a place is provided to seeding, to there be the particle diameter of the granular solids of 15% (weight) to be not less than 50 microns at least, preferred 50 microns～400 microns.In addition, the high surface area solid preferably has a mean diameter that is different from other standard solid component.This can cause the remarkable increase of tensio-active agent to the solids weight ratio.Particularly, add additional, high surface area, can make long-pending 9 meters squared per gram that surpass of total solid surface, preferred at least 12 meters squared per gram, most preferably the granular component of 15 meters squared per gram can make accessible tensio-active agent weight reach 60% (weight).
High surface area can realize by using the porous particle, as using zeolite MAP, Sipernat, or uses the particle of very little (submicron), as Cabot Cab-O-Sil.Also can use other porous granule.The high surface area of the particles mixture that is obtained makes the more liquid actives of the solid absorption of unit weight subsequently.In addition, the multi-modal distribution that comes from the particle of different components mixture has given particle bigger intensity.The effect of the small-particle in the distribution is the viscosity that increases yielding stress and liquid active bond agent composition, promotes effective nodulizing of bigger granular component thus.The multi-modal of particle distributes and also enables solids is carried out more effective packing, thereby has strengthened particle.Though more effective packing has reduced the gap in the agglomerate that the liquid actives can fill, this loss can be more by using the gap that porous granule obtained remedy.
Can add (postdosed) later on and comprise enzyme, SYNTHETIC OPTICAL WHITNER, bleach precursor, bleaching stibilizer, froth suppressor, spices and dyestuff to the examples of substances in the composition.Liquid or paste components can be adsorbed onto on the solid porous particle expediently, generally speaking, inorganics can be joined subsequently in the prepared composition of the inventive method.
With regard to the chemical composition of starting raw material, present method is very flexible.Can prepare the composite composition of phosphoric acid salt and zeolite.Present method also is suitable for preparing the composition that comprises calcite/carbonate.
The initial particle diameter of granular solids component is 0.1～500 micron, preferred 1～350 micron, and more preferably 0.1～300 micron.Solid ingredient preferably comprises 5～95% detergent builders, and more preferably 10～80%, 20～60% (weight) most preferably.
Can comprise negatively charged ion, nonionic or zwitterionics through neutralization or part neutral tensio-active agent.In the ＂ part and ＂ be meant a kind of tensio-active agent, it is selected from straight chained alkyl phenylsulfate or sulfonate, C
12～C
18The water-soluble salt of straight chained alkyl phenylsulfate, alpha-olefin vitriol or sulfonate, internal olefin vitriol or sulfonate, fatty acid ester vitriol or sulfonate, primary alkyl sulphates or sulfonate, primary alconol and secondary alcohol sulfate or sulfonate and lipid acid, for example tallow soap or coconut soap.
Nonionogenic tenside can be selected from alkylene oxide group and hydrophobic organic compound through the compound that condensation produced, hydrophobic organic compound such as alkylphenol or alcohol.Preferred nonionic is to contain the fatty alcohol of 8～30 carbon atoms and the water-soluble condensation product of every mol of alcohol 3～15 moles of ethylene oxide condensations in the molecule.Other ionic surfactant pack is drawn together the moieties that contains about 10～18 carbon atoms and two and is selected from the alkyl that contains 1～3 carbon atom or the water-soluble amine oxides of hydroxyalkyl part, derive by sugar and next nonionogenic tenside with those, for example alkyl polyglycoside.
Zwitterionics comprise aliphatic quaternary ammonium phosphorus drone and the derivative of sulphur drone compound, one of them aliphatics substituting group contains an anionic water-soluble group.
Binder ingredients comprises said tensio-active agent, and the water that is less than 20%, preferably contains to be less than 10% water.The preferred adhesive component comprises through neutralization or part neutral surfactant mixture, for example contains the straight chain of 11～14 carbon atoms or primary alkyl benzene sulfonate and the every mol of alcohol C with 3～7 moles of ethylene oxide ethoxyquins
12～C
15The mixture of primary alconol, wherein anion surfactant is 3: 1 to the weight ratio of nonionogenic tenside, or C
14～C
17Primary alconol or secondary alcohol sulfate and every mol of alcohol are with the C of 3～7 moles of ethylene oxide ethoxyquins
12～C
15The mixture of primary alconol, its weight ratio are 2: 1.
Preferably comprise the water that is less than 20% (weight),, most preferably be less than the water of 5% (weight) more preferably less than 10% (weight) through the neutral tensio-active agent, and can be according to the United States Patent (USP) 4,923,636 and 4 that licenses to Blackburn, 826,632, or license to the United States Patent (USP) 4 of Fernley, 052,342, or license to people's such as Dumas United States Patent (USP) 5,324, method preparation described in 455 is incorporated herein by reference herein.
The surfactant content of tackiness agent is preferred 50%～100%, and more preferably 55%～90%, most preferably 60%～80%.The preferred surfactants mixture comprises the anion surfactant of 20～80% (weight), the nonionogenic tenside of 20～80% (weight) and not moisture.
The preferred adhesive component comprises the water that is less than 30% (weight), and more preferably 0.5%～25%, most preferably 5%～15%.
In one embodiment, binder ingredients comprises:
(a) sodium salt or the sylvite of a kind of alkyl-sulphate or sulfonate (Sulfanate), its amount are 20～80% (weight);
(b) a kind of oxyalkylated nonionogenic tenside, its amount are 20～80% (weight);
(c) water surplus, its amount are 0 to being less than 20% (weight).
Help being used to carry out the preferred Littleford of high speed shear mixing tank of production operation
(TM)Board FM 130D mixing tank.This instrument mainly is made of one big, immobilized hollow cylinder, and its longitudinal axis is horizontal.Along this axis is one the turning axle of several dissimilar blades to be installed.When being used to carry out operation of the present invention, the tip speed of preferred this axle is 1 meter per second～20 meter per seconds, more preferably 1 meter per second～12 meter per seconds.Mixing tank can be equipped with one or more high speed cutters, and preferred tip speed is 15 meter per seconds～80 meter per seconds during operation, more preferably 20 meter per seconds～70 meter per seconds.Other type mixer that is applicable to the inventive method has Lodige
(TM), Eirich
(TM)RVO2, Powrex
(TM)VG100, Zanchetta
(TM), Schugi
(TM)And Fukae
(TM)
In the method according to the invention, solid ingredient is packed into mixing tank, then with binder ingredients or be sprayed onto on the solid ingredient, or pump suction mixing tank.Component is mixed preferred 0.2～8 minute of blended total residence time, more preferably 0.25～5 minute.After being preferably in this mixing time and finishing, with coating, as zeolite, add in the mixing tank, a rotating spindle then allows mixing tank work 20～60 seconds.By preferred 600 grams per liters of the prepared particulate tap density of present method～1150 grams per liters, particle diameter (measuring with the Rosin-Rammler method) is 300～1200 microns, more preferably 400～800 microns.
Preferred 3: 2～2: 3 of the ratio of binder ingredients and solid ingredient (weight ratio), more preferably 1: 1～2: 3.
Present method is preferably carried out under the temperature of room temperature to 60 ℃, more preferably room temperature to 40 ℃.
The present invention has done to further specify with following indefiniteness embodiment, unless dated especially among the embodiment, umber and percentage are all represented with weight.
Among the embodiment, use following shortenings to replace employed title material.
Zeolite: zeolite 4A (Wessalith, Degussa produces)
And zeolite MAP (Crosfield product)
Carbonate: yellow soda ash G100 (FMC product)
LAS: linear alkylbenzene sulfonate
Non-ionic: the alcohol of nonionogenic tenside, ethoxylation,
Neodol 25-7, Shell produces
SiL90: the pyrogenic silica by Cabot produces is described in detail in communique
CGEN-82/90
Sip 50s: a kind of silicate by Degussa produces is described in detail in communique PT
71-16-1-391-HC
Table 1
| 1 | 1/1 HAM (1) | 3 | 4 | |
| Adhesive type | 1/1 HAM (1) | 1/1 HAM (1) | 2/1 HAM (2) | 2/1 HAM |
| The granulation aid type | siL90 | sip50s | siP50s | siP50s |
Solid matter mixing %
| Zeolite 4A | 30 | 0 | 0 | 0 |
| Zeolite MAP | 0 | 60 | 58 | 58 |
| The G100 soda powder | 40 | 40 | 39 | 38 |
| Granulation aid | 30 | 0 | 3 | 4 |
| Surface-area (meters squared per gram) | 32.2 | 7.2 | 20.5 | 25.0 |
| Actives in the product, % | 48 | 38 | 41 | 45 |
| Equipment | FP (3) | BL (4) | BL | FP |
(1) 1/1 HAM:1 part LAS and 1 part of 7E.OC
12-15The composition of alcohol (non-ionic type) high reactivity mixture
(2) 2/1 HAM:2 part LAS and 1 part of 7E.OC
12-15The composition of alcohol (non-ionic type) high reactivity mixture
(3) FP: food processing machinery
(4) BL: intermittent type Lodige mixing tank
Embodiment 1～4th, in a high-speed intermittent Lodige (Littleford FM 130D) mixing tank with 45 kilograms of (100 1b) scales or in universal VC-4 food processing machinery with the less macro preparation of 300～500gm.Before the beginning granulation and between granulation stage 30 seconds to 2 minutes during this period of time in, in mixing tank, add solids and tackiness agent.When the diameter of most of particles seems between 100～500 microns, stop granulation.But prepared powder unrestricted flow.
Embodiment 1,3 and 4 explanations be that wherein the particulate surfactant content surpasses the preparation of 40% (weight).The amount of actives is recorded in table 1 in used solid mixture, resulting specific surface area and the product.Specific surface area square metre is measured with every gram particle, and the specific surface area value of given mixture is to calculate on the weighted average basis of the surface-area of measuring with the BET method.The BET surface-area of used various components is listed in the table below in 2.
Embodiment 2 has illustrated that as a reference examples used amount of surfactant is lower than 40% when solid mixture has a less relatively specific surface area.
Other mixing tank also is suitable for.
Table 2
The character of solids
| BET area (meters squared per gram) | Mean diameter (micron) | |
| The G100 soda powder | 0.00157 | 300 |
| Zeolite 4A | 7.4 | 4 |
| Zeolite MAP | 35 | 1.6 |
| siL90 | 100 | ＞1 |
| siP50s | 450 | ～4 |
Claims (8)
1. a production contains 40% (weight) tensio-active agent at least, tap density is at least the method for the detergent composition of 650 grams per liters, this method comprises following one step: under the condition of room temperature to 60 ℃, a kind of binder ingredients and a kind of initial particle are 0.1～about 500 microns granular solids component high shear mixing is until forming particle, this binder ingredients comprises said tensio-active agent and is less than 20% water, said granular solids component comprises at least about 15% (weight), particle diameter is at least the more small-particle of about 50 microns particle and q.s, the average surface area that adopts the granular component that the BET method measured is reached is at least about 9 meters squared per gram, and wherein tackiness agent in whole process of production mixture to be remained granular.
2. according to the process of claim 1 wherein that tackiness agent comprises 20～80% anion surfactant and 20～80% nonionogenic tenside.
3. according to the method for claim 1 or 2, wherein binder ingredients comprises:
(a) sodium salt or the sylvite of a kind of alkyl-sulphate or sulfonate (Sulfanate), its amount are 20～80% (weight);
(b) a kind of oxyalkylated nonionogenic tenside, its amount are 20～80% (weight);
(c) water surplus, its amount are 0 to being less than 20% (weight).
4. according to the method for above-mentioned any one claim, wherein tackiness agent comprises and is less than 10% water.
According to the process of claim 1 wherein tackiness agent comprise with certain stoichiometry, be enough in and the alkaline matter of lipid acid blended lipid acid mutually.
6. according to the method for above-mentioned any claim, wherein solid ingredient comprises the detergency washing assistant of 5～95% (weight).
7. according to the method for above-mentioned any claim, wherein tackiness agent and solid ingredient being mixed, is 300～1200 microns particle up to the formation particle diameter.
8. according to the method for above-mentioned any claim, wherein composition comprises tackiness agent and solid ingredient, and the weight ratio of tackiness agent and solid ingredient is 3: 2～2: 3.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US31498294A | 1994-09-29 | 1994-09-29 | |
| US08/314,982 | 1994-09-29 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1164257A CN1164257A (en) | 1997-11-05 |
| CN1110542C true CN1110542C (en) | 2003-06-04 |
Family
ID=23222342
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95196314A Expired - Fee Related CN1110542C (en) | 1994-09-29 | 1995-09-21 | High active granular detergent compositions and process for making them |
Country Status (10)
| Country | Link |
|---|---|
| EP (1) | EP0783562B1 (en) |
| CN (1) | CN1110542C (en) |
| AU (1) | AU701791B2 (en) |
| BR (1) | BR9509051A (en) |
| CA (1) | CA2200856C (en) |
| DE (1) | DE69510074T2 (en) |
| ES (1) | ES2132716T3 (en) |
| MY (1) | MY113791A (en) |
| WO (1) | WO1996010071A1 (en) |
| ZA (1) | ZA958129B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992007932A1 (en) * | 1990-10-26 | 1992-05-14 | The Procter & Gamble Company | Process for agglomerating aluminosilicate or layered silicate detergent builders |
| EP0544365A1 (en) * | 1991-11-26 | 1993-06-02 | Unilever N.V. | Detergent compositions and process for preparing them |
| CN1074705A (en) * | 1992-01-17 | 1993-07-28 | 尤尼利弗公司 | Detergent composition |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4828721A (en) * | 1988-04-28 | 1989-05-09 | Colgate-Palmolive Co. | Particulate detergent compositions and manufacturing processes |
| KR0170424B1 (en) * | 1990-07-05 | 1999-01-15 | 호르스트 헤를레,요한 글라슬 | Process for making washing and cleaning active tensile granulates |
| CA2083331C (en) * | 1991-11-26 | 1998-08-11 | Johannes H. M. Akkermans | Detergent compositions |
-
1995
- 1995-09-21 AU AU36514/95A patent/AU701791B2/en not_active Ceased
- 1995-09-21 EP EP95934088A patent/EP0783562B1/en not_active Expired - Lifetime
- 1995-09-21 ES ES95934088T patent/ES2132716T3/en not_active Expired - Lifetime
- 1995-09-21 CN CN95196314A patent/CN1110542C/en not_active Expired - Fee Related
- 1995-09-21 WO PCT/EP1995/003723 patent/WO1996010071A1/en active IP Right Grant
- 1995-09-21 BR BR9509051A patent/BR9509051A/en not_active IP Right Cessation
- 1995-09-21 CA CA002200856A patent/CA2200856C/en not_active Expired - Fee Related
- 1995-09-21 DE DE69510074T patent/DE69510074T2/en not_active Expired - Lifetime
- 1995-09-27 ZA ZA958129A patent/ZA958129B/en unknown
- 1995-09-28 MY MYPI95002904A patent/MY113791A/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992007932A1 (en) * | 1990-10-26 | 1992-05-14 | The Procter & Gamble Company | Process for agglomerating aluminosilicate or layered silicate detergent builders |
| EP0544365A1 (en) * | 1991-11-26 | 1993-06-02 | Unilever N.V. | Detergent compositions and process for preparing them |
| CN1074705A (en) * | 1992-01-17 | 1993-07-28 | 尤尼利弗公司 | Detergent composition |
Also Published As
| Publication number | Publication date |
|---|---|
| DE69510074T2 (en) | 1999-10-21 |
| CN1164257A (en) | 1997-11-05 |
| EP0783562B1 (en) | 1999-06-02 |
| MX9702347A (en) | 1997-10-31 |
| MY113791A (en) | 2002-05-31 |
| BR9509051A (en) | 1998-06-23 |
| CA2200856C (en) | 2005-06-07 |
| WO1996010071A1 (en) | 1996-04-04 |
| CA2200856A1 (en) | 1996-04-04 |
| AU701791B2 (en) | 1999-02-04 |
| ZA958129B (en) | 1997-03-27 |
| EP0783562A1 (en) | 1997-07-16 |
| AU3651495A (en) | 1996-04-19 |
| ES2132716T3 (en) | 1999-08-16 |
| DE69510074D1 (en) | 1999-07-08 |
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