CN1188505C - Process for production of detergent composition - Google Patents
Process for production of detergent composition Download PDFInfo
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- CN1188505C CN1188505C CNB971816093A CN97181609A CN1188505C CN 1188505 C CN1188505 C CN 1188505C CN B971816093 A CNB971816093 A CN B971816093A CN 97181609 A CN97181609 A CN 97181609A CN 1188505 C CN1188505 C CN 1188505C
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- 239000000203 mixture Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000003599 detergent Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title abstract description 12
- 230000008569 process Effects 0.000 title abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 71
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 34
- 238000005520 cutting process Methods 0.000 claims abstract description 14
- 239000011149 active material Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 21
- 239000011236 particulate material Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 17
- 238000005507 spraying Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 230000009471 action Effects 0.000 abstract description 2
- 239000007858 starting material Substances 0.000 abstract 3
- 229910021536 Zeolite Inorganic materials 0.000 description 17
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 17
- 239000010457 zeolite Substances 0.000 description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 238000004140 cleaning Methods 0.000 description 13
- 238000009826 distribution Methods 0.000 description 13
- 238000005406 washing Methods 0.000 description 13
- 101710108306 Bifunctional dihydroflavonol 4-reductase/flavanone 4-reductase Proteins 0.000 description 12
- 101710170824 Dihydroflavonol 4-reductase Proteins 0.000 description 12
- 239000002253 acid Substances 0.000 description 11
- 235000019832 sodium triphosphate Nutrition 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 101710194948 Protein phosphatase PhpP Proteins 0.000 description 8
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 7
- 238000000280 densification Methods 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 238000005469 granulation Methods 0.000 description 7
- 230000003179 granulation Effects 0.000 description 7
- 229910052700 potassium Inorganic materials 0.000 description 7
- 239000011591 potassium Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 6
- 238000001694 spray drying Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 150000002632 lipids Chemical class 0.000 description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000002671 adjuvant Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000013517 stratification Methods 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 235000010724 Wisteria floribunda Nutrition 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- -1 for example Chemical compound 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- VJAGHZLYXAKQID-UHFFFAOYSA-N benzenesulfonic acid;potassium Chemical compound [K].OS(=O)(=O)C1=CC=CC=C1 VJAGHZLYXAKQID-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- RBNPOMFGQQGHHO-UHFFFAOYSA-N glyceric acid Chemical compound OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- VSXGXPNADZQTGQ-UHFFFAOYSA-N oxirane;phenol Chemical compound C1CO1.OC1=CC=CC=C1 VSXGXPNADZQTGQ-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- NFIYTPYOYDDLGO-UHFFFAOYSA-N phosphoric acid;sodium Chemical compound [Na].OP(O)(O)=O NFIYTPYOYDDLGO-UHFFFAOYSA-N 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001444 polymaleic acid Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- ABDKAPXRBAPSQN-UHFFFAOYSA-N veratrole Chemical compound COC1=CC=CC=C1OC ABDKAPXRBAPSQN-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
- Glanulating (AREA)
Abstract
A process for the production of a detergent powder composition having a bulk density of no more than 750 g/l, e.g. no more than 700 or 650 g/1, the process comprising mixing a particulate starting material which contains no more than 10 % by weight of the starting material of detergent active material and which starting material has a d50 average particle diameter of from 100 mu m to 1000 mu m and a particle porosity of at least 0.4, together with a liquid component comprising a detergent active material or a precursor therefor in a mixer/granulator having both a stirring and a cutting action.
Description
Technical field
The present invention relates to a kind of method of producing cleaning composition.Specifically, the present invention relates to the method that a kind of production has the cleaning composition of medium or low bulk density, also relate to the cleaning composition of producing by this method.
Background of the present invention
Usually, cleaning composition is produced by spray drying process, wherein, the composition and the water of said composition are mixed into water mediation slurry, then this slurry is sprayed onto in the spray-drying tower, and contacts, anhydrate so that remove with warm air, thereby acquisition detergent particles, this particle are commonly referred to as " basis " powder.Thus obtained particle has highly porous.The powder of being produced has the tap density of 300-550g/l usually in this way, and this density reaches as high as 650g/l.
Spray-drying powder can produce good powder transportation performance usually, as good distribution and solubility property.But, the investment of spray-drying process and cost are higher.However, still have this low-density washing powder of a large amount of consumer wants.
In recent years, produced washing powder by the mechanically mixing method already with high-bulk-density.700-900g/l even higher tap density had been obtained already.Usually, this washing powder is produced like this: the spray-dired basic powder of densification in one or several mechanical mixer, optionally choose wantonly and add other composition, or mix the composition of described composition, and do not use the spraying drying step by continuous or batch mixed technology.
Powder with high-bulk-density and low packaging volume helps storing and distributing operation, uses but also help the human consumer.In addition, if do not use the spraying drying step, its investment and production cost usually can be lower, and such method also can make energy consumption reduction, thereby the benefit of environmental protection aspect is provided.Therefore, wish usually to avoid in the washing composition production technique, using spray drying technology.
But, described highdensity powder has the porosity lower than conventional spray-dried powders usually, and this can hinder this powder to carry in washing liq.In addition, up to now, under the prerequisite of not using the spraying drying step, also be not easy to realize having the production of low bulk density, for example make the tap density of this powder be lower than about 700g/l to medium tap density powder with commercial size.
EP-A-367 339 has disclosed the method that a kind of production has the cleaning composition of high-bulk-density, wherein, handle feed particulate material with super mixer, form or keep the yielding state of this mixture with a moderate-speed mixers, dry then and/or cool off.Described raw material can be a kind of spray-dired basic powder, maybe can use the composition of composition not carry out spraying drying step in advance in the washing composition production process.
Disclose (Unilever: the right of priority in the application is unexposed before the date) according to WO97/02338, if described composition is prepared with a kind of composition with low bulk density, can for example obtain to be lower than the low bulk density of 700g/l by the method for not using the spraying drying step.But, this method is not suitable for using the raw material of selling with the high density granular form comparatively speaking, or this material itself is produced (latter can produce the bigger particle of porosity usually) by spraying drying.
We have found that, can obtain the powder of medium or low bulk density by a kind of new method, this method is such: with a kind of powder and a kind of liquid component mechanically mixing that contains detergent active material or its precursor, described powder contains seldom or does not contain the detergent active material, and this powder is by the granulometric composition with predetermined mean particle size and particle porosity.
The present invention defines
Therefore; first aspect of the present invention provides a kind of production tap density to be no more than 750g/l; for example be no more than 700 or the cleaning composition of 650g/l; this method comprises that a kind of feed particulate material is put into the mixing tank/tablets press with stirring and cutting function with a kind of liquid component that contains detergent active material or its precursor mixes; described feed particulate material contains the detergent active thing of not enough this raw material 10% of weight percent, the d of this raw material
50Median size is 100-1000 μ m, and the particle porosity is at least 0.4.
The invention still further relates to a kind of cleaning composition with the inventive method preparation.
The detailed description of the invention
The present invention results from unexpected a discovery, and promptly the tap density of product depends on the speed of rotation when mixing.This also is the function of selected given mixer, and but, the speed of mixing tank is low more basically, and the tap density of product is also low more.
Described novel method have two outstanding and be advantage independently.First advantage is by selecting to have had the powder raw material of needed mean particle size and porosity, can prepare medium or the low bulk density powder.
Second advantage is that the working condition that possesses spraying drying and mechanically mixing aggregation equipment at the same time obtains down.By give with the possibility of spraying drying goods as the raw material of mechanical aggregation process, the invention provides described combined method in the further handiness of producing aspect the washing powder goods.In this article, shortenings " NTR " is meant " non-tower approach ", promptly powder is by mix producing, rather than produces with spray-drying tower, even raw material itself is that what to produce by spraying drying also is like this.
Be advisable with 400-650g/l with its tap density of cleaning composition that the inventive method is produced, be preferably 450-650g/l, more preferably 500-600g/l.Further its particle porosity of the preferred cleaning composition of producing is at least 0.2, and more preferably at least 0.25.
Described feed particulate material shared weight percent in the composition of being produced by described mechanically mixing method is preferably 20-40% and is advisable with 10-75%.
Except with median size (d for example
50) represent beyond the size-grade distribution, if can being suitable for Rosin-Rammler, it distributes, can also represent size-grade distribution with the Rosin-Rammler number.This number calculates n power distribution of the following formula of described size-grade distribution substitution:
Wherein, R is the cumulative percentage that surpasses the powder of certain particle size D.D
rBe mean particle size, and n is a size-grade distribution tolerance.D
rWith n be the Rosin-Rammler number that is fit to the tolerance size-grade distribution.High n value means to have narrow size-grade distribution, and low n value means to have wide size-grade distribution.
Described method can be a continuation method, or carries out with the batch form.
One type the setting that is suitable for finishing described mechanically mixing comprises a super mixer/compactor, and described raw material and described liquid component are dropped in this device, forms the particulate state detergent.In a kind of preferred embodiment; this device also comprises a middling speed tablets press/compactor; particulate state detergent from described super mixer/compactor is devoted in this middling speed device; form thus or keep a kind of yielding state, subsequently resulting product is carried out drying and/or cooling.
An example of described super mixer/compactor is L ǒ dige (trade mark) CB30Recyzler.This device mainly is made up of a large-scale static hollow cylinder, and this is a horizontal positioned, and its diameter is about 30cm.Have a turning axle at this middle part, on this axle, paddle is installed.This device can rotate under the speed of 100-2500rpm according to needed densification degree and granularity.The paddle that is installed on the described axle can be to producing sufficient mixing effect at this stage blended solid and liquid.Its average residence time depends on speed of rotation, the position of paddle and the cofferdam of outlet opening of axle to a certain extent.
Can also use the super mixer compactor that washing powder is had other type of similar action.For example, can use Shugi (trade mark) tablets press and Drais (trade mark) K-TTP80.
Composition to described raw material in super mixer/compactor carries out thorough mixing, preferably carries out the mixing of the short period of about 5-30 second.
After mixing the above-mentioned first time, described detergent still keeps suitable porosity, and this may be that the low density goods are needed.But; the further words of densification if desired; just can not be chosen in to use in super mixer/compactor and reside permanently the further raising that the mode of staying the time realizes tap density; preferably in a middling speed tablets press/compactor, described detergent was carried out about 1-10 minute second treatment step of preferred 2-5 minute.In this second treatment step, its treatment condition are for making described powder and become or keeping yielding state.The described particle porosity of result can further reduce.With the key distinction of first step be lower mixing velocity and general long residence time, residence time was at least 30 seconds, for example 1-10 minute, and must make this powder yielding.
Second mixing step can realize that successfully this mixing tank is also called L ǒ dige Ploughshare by L ǒ dige (trade mark) KM300 mixing tank.This device mainly is made up of a hollow static tube, and a turning axle is arranged in the middle.Various plow-shape paddles are installed on this axle.This energy rotates with the speed of 40-160rpm.Optionally use one or several high-speed knife to prevent undue gathering.Other the mechanical example that is applicable to this step is Drais (trade mark) K-T160.
In order to use, to process and storing, the washing powder of densification must no longer be yielding state.Therefore, after second mixing step, carry out drying and/or cooling to the powder of densification.This step can be finished in a known way, for example, finishes in a fluidizer (dry, cooling) or an air lift (cooling).This powder preferably only needs a cooling step, because devices needed is fairly simple and less expensive.
When using two-step mixing process mentioned above, to second mixing step, preferred first mixing step importantly obtains the yielding state of described washing powder, to obtain best densification effect.Then, described super mixer/compactor and/or middling speed tablets press/compactor just can effectively make described granulate material distortion, so that its particle porosity reduces, and therefore improve its tap density.
Mixing tank/the tablets press that is applicable to the another kind of type of the inventive method is a flute profile, and preferably has a vertical substantially agitator axis.The agitator of preferred especially Fukae (trade mark) SSOG series, this serial agitator are that the Fukae Powtech Kogyo company by Japan produces; This device is the trough-shaped container form basically, can enter this container by a upper member, and its bottom is provided with an agitator, and this agitator has vertical substantially axle, and its sidewall is provided with cutting unit.Described agitator and cutting unit can be worked independently of one another, and with independently, the operation of variable speed.
Other the similar mixing tank that is applicable to the inventive method has Diosna (trade mark) V series, and this series is by the Dierks﹠amp of Germany; S ǒ hne produces; With the Pharma Matrix (trade mark) that produces by the T K Fielder company limited of Britain.Other the similar mixing tank that is applicable to the inventive method comprises the CVG-C of Fuji's (trade mark) series that the Sanyo of Fuji by Japan produces; With by gondola Zanchetta﹠amp; The Roto (trade mark) that Co srl produces.
Granulation is preferably finished by starting described agitator and cutting unit simultaneously; Usually short residence time (for example, dividing clock time with 5-8 for the batch material of 35Kg) is just enough.Can control final tap density by selecting residence time and stirring velocity.
Described agitator operates to suitable with the speed of 25-250rpm, for example, and 100-200rpm or be low to moderate 30-50rpm.But, this speed depends on device size.Described cutting unit itself is fit to the speed operation with 200-3500rpm, preferred 300-3000rpm.For example, this cutting unit is suitable for the speed operation with 200-2500, preferred 300-2200rpm.Pre-mixing, interpolation liquid, granulation, interpolation optionally that batch process is usually directed to solids component are suitable for controlling the layer composite of granulation terminal point, and the discharge of product.Production phase according to this method is suitably regulated stirring and/or cutting speed in feet per minute.Described mixing step preferably be controlled a little more than the temperature of envrionment temperature under carry out, preferably be higher than 30 ℃.Suitable temperature range is 30-45 ℃.
The amount of the detergent active material in the described feed particulate material is no more than 10% of this raw material weight.But, the amount of the detergent active material in the described feed particulate material is advisable to be no more than this raw material weight 5%, preferably is no more than 1% of its weight.Described feed particulate material can be substantially free of or not contain any detergent active material fully.Described feed particulate material is more suitable by the spraying drying preparation.But, the raw material with desired parameters also can obtain by other method, for example, comprises granulation.
The d of described feed particulate material
50Median size is 100-1000 μ m.This size-grade distribution for the control finished product is important.But, preferably this median size is 150-800 μ m, particularly 200-700 μ m.Described particle in the preferred described raw material has 90% per-cent, and its particle diameter is 100-1000 μ m.
The particle porosity of described feed particulate material is at least 0.4, but is preferably at least 0.45, for example 0.45-0.55.Most preferably at least 0.50.Under any circumstance, described feed particulate material can comprise a kind of spray-dried materials, and in other words, some or all described raw materials are produced by drying process with atomizing.
The mensuration of particle porosity is based on well-known air and flows through that the Kozeny-Carman relation of piling up powder bed measures;
Wherein: φ ν=air flow quantity
Δ P=falls by the pressure of bed
D
BedThe diameter of=bed
The h=height of bed
D
p=particle diameter
ε
BedThe porosity of=bed
η=gas viscosity
The k=empirical constant equals 180 for particulate solid
The tap density of powder can be used following formulate: tap density=r
Solid(1-ε
Bed) (1-ε
Particle)
Wherein: r
SolidSolid density in the=described particle
ε
Particle=particle porosity
According to above formula, can obtain its particle porosity by following experiment:
Filling diameter with the powder (granularity is 355-710 μ m) of known quantity is the Glass tubing of 16.3mm, and the supporter of a glass filter (aperture is 40-90 μ m) as powder is housed in this pipe.The height of record powder bed.Allow the speed be 375cm
3/ minute air flow through described powder bed.Mensuration is fallen by this pressure.To be determined at also that the pressure by empty Glass tubing falls under the special air flow.
Repeating above mensuration with the powder of same amount, but, this time is to obtain closeer stacking bed by patting the Glass tubing that this powder is housed gently.Measuring its pressure equally under the special air flow falls.
In order to derive its particle porosity by above mensuration, need know particulate solid density (formula 2).More than measure and carry out, for example, measure by the penta specific gravity hydrometer that provides by Quantachrome is provided with the helium hydrometer method.
According to said determination and formula, can derive the particle porosity easily.
For the purpose of the present invention, powder mass flow is to be dynamic flow (DFR) expression of unit with ml/s, and this flow is measured by the following method.Employed device is made up of a tubular Glass tubing, and the internal diameter of this Glass tubing is 35mm, and length is 600mm.This Glass tubing is fixed, made its longitudinal center line keep vertical.The slick conically shaped that its lower end is made by polyvinyl chloride is as the end, and the interior angle of this conically shaped is 15 °, and the lower part outlet hole that to have a diameter be 22.5mm.First beam sensor is installed in 150mm place, described outlet top, second beam sensor is installed in 250mm place, first sensor top.
In order to measure the DFR of pulverized specimen, with described outlet opening temporary close, for example, cover described outlet, and pour powder into described top by funnel with a plate, exceed about 10cm up to the described upper sensor of the aspect ratio of this powder; Guarantee the homogeneity of this filling by a pad between described funnel and described pipe.Then described outlet is opened, and drop to the used time t of lower sensor (second) from upper sensor by the described powder height of electronic device records.Said determination will repeat 2 or 3 times usually, and averages.If being the volume (ml) of the pipe between upper sensor and lower sensor then DFR (ml/s), V can provide by following formula:
Average and computation process is carried out the DFR value that can obtain directly to read by electronic method.
Described feed particulate material preferably includes washing assistant, most preferably is silico-aluminate, for example zeolite 4A and zeolite A24 or salt, preferably inorganic salt.Salt preferably phosphoric acid sodium, for example, tripoly phosphate sodium STPP (STP), carbonate, supercarbonate and vitriol also can use.
Also other solid material (if necessary) can be mixed in the described feed particulate material, and can these materials alternately or additionally be added wherein at any suitable stage of described mechanically mixing.
Described liquid component preferably contains at least a liquid nonionic type tensio-active agent.It can also contain the acid precursor and/or the lipid acid of one or more aniorfic surfactant.Then described acid precursor is neutralized, generating corresponding aniorfic surfactant, and add one or more suitable basic materials with described fatty acid saponification by suitable stage in described mechanically mixing technology.Suitable basic material comprises alkaline carbonate, for example Na
2CO
3And oxyhydroxide, for example NaOH.Described basic material can solid form or the adding of aqueous solution form.Can also be before described mechanically mixing step precursor or lipid acid in the described liquid component of part neutralization/saponification.Described cleaning composition suitably contains the anionic detergent active.This promoting agent can the pre-neutralization material forms adds, and preferably as a kind of composition of feed particulate material, or neutralizes in position.Under latter event, the acid precursor of described promoting agent preferably neutralizes with a kind of solid neutralizing agent, carbonate for example, and this neutralizing agent is a kind of composition of described feed particulate material preferably.
Be present in detergent active material in the described composition and can be selected from anionic, cationic, amphoteric, amphoteric ion type or non-ionic type detergent active material or its mixture.The example of suitable synthetic anionic washing compound is benzene sulfonic acid sodium salt and Phenylsulfonic acid potassium (C
9-C
20), linear secondary alkyl (C particularly
10-C
15) benzene sulfonic acid sodium salt (LAS); Sodium alkyl sulfate or potassium (PAS); With the alkyl glycerol ether sodium sulfate, particularly come from the higher alcohols and the ether that comes from the synthol of oil of tallow or Oleum Cocois.Operable suitable nonionic surface active agent comprises the reaction product that has compound and alkylene oxide, particularly oxyethane or the oxyethane and the propylene oxide of a hydrophobic grouping and an active hydrogen atom such as fatty alcohol, aliphatic acid, aliphatic amine or alkylphenol etc.Concrete non-ionic type washing compound has alkyl (C
6-C
22) the phenol ethylene oxide condenses, generally have 5-25 EO, promptly each molecule has 5-25 ethylene oxide unit(s), and aliphatic series (C
8-C
18) condensation product of uncle or secondary straight or branched alcohol and oxyethane, be generally 5-50EO.
Purposes according to hope, the consumption of detergent active material can account for the 1-50% of its weight in the described composition, the consumption of non-ionic type material in feed particulate material is lower than 10% of its weight, more preferably less than 5% of its weight, and/or in described mixing process, use as liquid-containing binder, optionally, use together as water with other liquid component.
The 30-70% that accounts for described cleaning composition with described feed particulate material is advisable.
Can in described mixing step, optionally use a kind of layer composite, form and weaken or prevent excessive polymerization with the control particle.Suitable material comprises silico-aluminate, for example zeolite 4A.This layer composite is suitable for using with the per-cent of 1-4%.
Described composition can be used as the complete combination thing form of being made up of itself and uses, or mixes use with other composition or mixture, therefore, can constitute the major portion or the less important part of the finished product.Said composition can be mixed with the composition such as the powder of spraying drying basis.Can as required common added ingredients such as enzyme, SYNTHETIC OPTICAL WHITNER and perfume compound be mixed with said composition, to make the full formula goods.
Below will the present invention is further illustrated by following indefiniteness embodiment.
Embodiment
All embodiment use following equipment: a Fukae FS30 is used for NTR experiment in batches, and a L ǒ dige Recycler CB30+Ploughshare KM300 is used for N continuous TR experiment.In the present invention, except other has explanation, all consumptions of representing with the per-cent form are based on weight, and are to drop into the gross weight of cleaning composition before the composition or composition to add any back.
Produce zeolite of the present invention-NTR powder
Following slurry is carried out spraying drying, to produce the powder of highly porous and low bulk density (BD):
Slurry 1 (weight %) slurry 2 (weight %)
Zeolite A24 40.0 43.8
LAS 0.0 1.3
Sokalan?CP5 10.0 5.0
Water 50.0 49.9
Resulting powder has following characteristic:
Characteristic basis powder 1 basic powder 2
BD，[g/l] 629 370
DFR，[ml/s] 115 88
d
50[μm] 210 279
RRd[μm] 242 299
RRn[-] 2.7 2.4
Water content [%] 5-7 7
Particle porosity 0.51 0.70
RRd=Rosin Rammler diameter
RRn=Rosin Rammler number
Sokalan CP5 is a kind of polyacrylate/polymaleic acid salt copolymer.
This spray-dired zeolite based porous support is used as basic powder subsequently in the NTR method, described in routine 1-8.
Example 1﹠amp; 2
Two kinds of basic powder are used for the batch NTR experiment that Fukae carries out.And basic powder 2 also is used for N continuous TR experiment.
2 contrasts of Formulation Example 1 example
(weight %) (weight %) (weight %)
Basis powder 1 43.4
Basis powder 2 46.4
Zeolite A24 46.4
PAS adjuvant 31.9 33.8 33.9
Non-ionic type 7EO 9.4 10.0 10.0
Non-ionic type 3EO 6.3 6.6 6.6
Lipid acid 2.5 2.6 2.6
NaOH 0.6 0.7 0.7
Zeolite A24 stratification thing 5.6 0.0 0.0
Premixture
Agitator rpm 200
Cutting unit rpm 3000
[second] 10
Granulation
Agitator rpm 100
Cutting unit rpm 3000
Time [minute] 1-0.5 11
Stratification [second] 10
Powder characteristics
DFR[ml/s] 140 90 55
RRd[μm] 492-574 366 1015
RRn 2.6 1.9 1.6
The PAS adjuvant that is used for described test has following prescription: PAS 45wt%
Zeolite 38wt%
Carbonate 9wt%
Water+other composition 8wt%
Example 3
Basic powder 2 can also be used for N continuous TR method, to replace zeolite A24.Following material is imported Recycler CB30:
Basis powder 2 46.3%
PAS adjuvant 33.6
Non-ionic type 7EO 10.0
Non-ionic type 3EO 6.6
Lipid acid 2.2
50%NaOH solution 1.2
When using Ploughshare KM300, do not have further densification steps, and under some occasion, be delivered directly in the fluidized-bed and cool off from the product of Recycler CB30.According to the speed of described circulator, can obtain BDs and DFRs by Recycler CB30:
Circulator speed [rpm] 1,500 1,200 1,000 800 500
BD[g/l] 620 570 544 502 436
Above result shows, circulator speed can be controlled the final BD of product as useful instrument.
Example 4-8
With N continuous TR method with the powder granulation of porous zeolite basis.
Example 45678 contrasts
Prescription (Kg/h)
Basis powder 2 459 458 458 458 457
Control vector 422
(zeolite A24)
PAS adjuvant 330 332 331 331 330 331
Non-ionic type/lipid acid 184 185 184 183 184 184
Mixture
50%NaOH solution 12 12 12 12 12 8.5
Processing parameter
RPM(CB30) 1800 1500 1200 1000 300 1500
RPM(KM300) 120 120 120 120 120 120
The result who draws with Recycler CB30
BD[g/l] 652 792 648 612 528 806
DFR[ml/s] 89 61 115 114 106 111
The result who draws with Ploughshare KM300
BD[g/l] 748 689 687 670 457 908
DFR[ml/s] 77 81 85 90 130 124
Speed by Recycler CB30 produces impact effect.Can utilize its speed that the BD of powder is adjusted to desirable value.Meanwhile, still can produce good size-grade distribution.Use the standard zeolite of mean particle size, can not produce powder with extremely low Recycler CB30 speed, because can not obtain suitable size-grade distribution as 0.5-30 μ m.
Produce STP-NTR powder of the present invention
Following slurry is carried out spraying drying, has the powder of highly porous and low BD with production:
Prescription wt%
STP(Rhodiaphos?H5) 38.8
LAS 1.1
50%NaOH solution 0.3
45% alkaline silicate solution 12.0
Water 47.9
Resulting powder has following characteristic:
Characteristic
BD，[g/l] 404
DFR，[ml/s] 111
d
50[μm] 303
RRd[μm] 349
RRn[-] 2.9
Water content [%] 5.9
Particle porosity 0.67
The powder that spray-dired STP-base carrier is used for preparation example 9-13.
Example 9﹠amp; 10
A Fukae FS30 mixing tank is used for the batch NTR method of STP-base carrier, and the prescription of described carrier is as follows:
10 contrasts of example 9 examples
(kg) (kg)
Standard STP 00 4.7
Spray-dired STP carrier 4.7 4.7 0
Yellow soda ash 5.25.2 5.2
Zeolite 4A (Wessalith P) 1.0 1.0 1.0
LAS acid 3.3 3.3 3.3
Zeolite 4A stratification thing 0 0.3 0
Premixture
The pre-mixing time (second) 10 10 10
RPM (agitator/cutting unit) 10,0/3,000 10,0/3,000 100/3000
Mix
RPM (agitator) 100 200 100
RPM (cutting unit) 3,000 3,000 3000
Mixing time [second] 120 120 120
Powder characteristics
BD[g/l] 576 688 846
DFR[ml/s] 110 119 132
RRd[μm] 486 373 680
RRn[-] 1.72 1.70 1.19
Powder by porous support production has lower BD and narrower size-grade distribution equally, as indicated by higher RRn value.
Example 11-13:STP carrier carries out N continuous TR granulation
Recycler CB30/Ploughshare KM300 is used for the N continuous TR method of STP base carrier, and it is as follows to fill a prescription:
Prescription (kg/h)
Example 11 examples 12 examples 13
(Kg) (Kg) (Kg)
Spray-dired STP carrier 316 316 316
Yellow soda ash 340,340 340
Zeolite 4A 1019999
LAS acid/water 249 249 249
Recycler?CB30
RMP 1500 1000 1800
Ploughshare?KM300
Zeolite 4A stratification thing [Kg/h] 30 5050
RPM120 120 120
Powder characteristics
After Ploughshare handles 481 522 649
BD[g/l]
Claims (7)
1. produce the method that tap density is no more than the detergent powder composition of 750g/l for one kind; this method comprises: feed particulate material is put into the mixing tank/tablets press with stirring and cutting function with the liquid component that contains detergent active material or its precursor mix; 10% weight of not enough this raw material of contained detergent active material in the described feed particulate material is characterized in that the d of this raw material
50Median size is 100-1000 μ m; the particle porosity is at least 0.4; and make by the travelling speed of setting described mixing tank/tablets press and to stir, the tap density of detergent powder composition product is controlled at preset value with the speed operation of 25-250rpm and cutting speed operation with 200-3500rpm.
2. according to the method for claim 1, it is characterized in that the d of described raw material
50Median size is 150-800 μ m.
3. according to the method for claim 1, it is characterized in that the d of described raw material
50Median size is 200-700 μ m.
4. according to the method for claim 1, it is characterized in that described raw material comprises a kind of material of producing by spraying drying.
5. according to the method for claim 1; it is characterized in that described mixing tank/tablets press comprises a trough-shaped container and an agitator; this agitator rotates around vertical stirrer shaft, or comprises that keeps flat a hollow cylinder, at this hollow cylinder middle part a turning axle that paddle is housed is arranged.
6. according to the method for claim 1, it is characterized in that the particle porosity of described raw material is at least 0.45.
7. according to the method for claim 1, it is characterized in that the particle porosity of described raw material is at least 0.50.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB9625066.7 | 1996-12-02 | ||
| GBGB9625066.7A GB9625066D0 (en) | 1996-12-02 | 1996-12-02 | Process for the production of a detergent composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1245530A CN1245530A (en) | 2000-02-23 |
| CN1188505C true CN1188505C (en) | 2005-02-09 |
Family
ID=10803825
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB971816093A Expired - Fee Related CN1188505C (en) | 1996-12-02 | 1997-10-29 | Process for production of detergent composition |
Country Status (14)
| Country | Link |
|---|---|
| EP (1) | EP0942958B2 (en) |
| CN (1) | CN1188505C (en) |
| AR (1) | AR009644A1 (en) |
| AU (1) | AU721831B2 (en) |
| BR (1) | BR9714494A (en) |
| CA (1) | CA2273849C (en) |
| DE (1) | DE69709398T3 (en) |
| EA (1) | EA001453B1 (en) |
| ES (1) | ES2169882T3 (en) |
| GB (1) | GB9625066D0 (en) |
| ID (1) | ID22478A (en) |
| TR (1) | TR199901756T2 (en) |
| WO (1) | WO1998024876A1 (en) |
| ZA (1) | ZA979825B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE69932827T2 (en) | 1998-08-20 | 2007-03-15 | The Procter & Gamble Company, Cincinnati | METHOD FOR PRODUCING DETERGENTS USING A MEDIUM-FAST MIXER / COMPRESSOR |
| US6794354B1 (en) | 1998-09-18 | 2004-09-21 | The Procter & Gamble Company | Continuous process for making detergent composition |
| ATE295409T1 (en) * | 1998-09-18 | 2005-05-15 | Procter & Gamble | CONTINUOUS PRODUCTION PROCESS FOR DETERGENT |
| AU9585098A (en) * | 1998-09-25 | 2000-04-17 | Procter & Gamble Company, The | Granular detergent composition having improved appearance and solubility |
| CA2343810A1 (en) * | 1998-09-25 | 2000-04-06 | Jacqueline Westfield | Granular detergent composition having improved appearance and solubility |
| JP2002528600A (en) | 1998-10-26 | 2002-09-03 | ザ、プロクター、エンド、ギャンブル、カンパニー | Method for producing a granular detergent composition having improved appearance and solubility |
| US6767882B1 (en) | 1999-06-21 | 2004-07-27 | The Procter & Gamble Company | Process for producing coated detergent particles |
| CA2375416A1 (en) * | 1999-06-21 | 2000-12-28 | Kenji Shindo | Process for producing coated detergent particles |
| US6951837B1 (en) | 1999-06-21 | 2005-10-04 | The Procter & Gamble Company | Process for making a granular detergent composition |
| WO2020222996A1 (en) * | 2019-04-29 | 2020-11-05 | The Procter & Gamble Company | A process for making a laundry detergent composition |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8626082D0 (en) * | 1986-10-31 | 1986-12-03 | Unilever Plc | Detergent powders |
| CA2001535C (en) * | 1988-11-02 | 1995-01-31 | Peter Willem Appel | Process for preparing a high bulk density granular detergent composition |
| GB9125035D0 (en) * | 1991-11-26 | 1992-01-22 | Unilever Plc | Detergent compositions and process for preparing them |
| GB9513327D0 (en) * | 1995-06-30 | 1995-09-06 | Uniliver Plc | Process for the production of a detergent composition |
-
1996
- 1996-12-02 GB GBGB9625066.7A patent/GB9625066D0/en active Pending
-
1997
- 1997-10-29 CN CNB971816093A patent/CN1188505C/en not_active Expired - Fee Related
- 1997-10-29 AU AU53168/98A patent/AU721831B2/en not_active Ceased
- 1997-10-29 BR BR9714494A patent/BR9714494A/en not_active IP Right Cessation
- 1997-10-29 ID IDW990449A patent/ID22478A/en unknown
- 1997-10-29 EA EA199900516A patent/EA001453B1/en not_active IP Right Cessation
- 1997-10-29 DE DE69709398T patent/DE69709398T3/en not_active Expired - Lifetime
- 1997-10-29 ES ES97950085T patent/ES2169882T3/en not_active Expired - Lifetime
- 1997-10-29 CA CA002273849A patent/CA2273849C/en not_active Expired - Fee Related
- 1997-10-29 WO PCT/EP1997/006073 patent/WO1998024876A1/en active IP Right Grant
- 1997-10-29 EP EP97950085A patent/EP0942958B2/en not_active Expired - Lifetime
- 1997-10-29 TR TR1999/01756T patent/TR199901756T2/en unknown
- 1997-10-31 ZA ZA979825A patent/ZA979825B/en unknown
- 1997-11-28 AR ARP970105599A patent/AR009644A1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CA2273849A1 (en) | 1998-06-11 |
| DE69709398D1 (en) | 2002-01-31 |
| EP0942958A1 (en) | 1999-09-22 |
| WO1998024876A1 (en) | 1998-06-11 |
| DE69709398T3 (en) | 2007-04-19 |
| AU5316898A (en) | 1998-06-29 |
| EA001453B1 (en) | 2001-04-23 |
| EA199900516A1 (en) | 2000-02-28 |
| TR199901756T2 (en) | 1999-11-22 |
| CA2273849C (en) | 2007-04-10 |
| ZA979825B (en) | 1999-04-30 |
| EP0942958B1 (en) | 2001-12-19 |
| ID22478A (en) | 1999-10-21 |
| DE69709398T2 (en) | 2002-06-20 |
| BR9714494A (en) | 2000-03-21 |
| GB9625066D0 (en) | 1997-01-22 |
| ES2169882T3 (en) | 2002-07-16 |
| CN1245530A (en) | 2000-02-23 |
| AR009644A1 (en) | 2000-04-26 |
| AU721831B2 (en) | 2000-07-13 |
| EP0942958B2 (en) | 2006-12-13 |
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