CN102712884B - Method for producing detergent granules - Google Patents
Method for producing detergent granules Download PDFInfo
- Publication number
- CN102712884B CN102712884B CN201080061447.XA CN201080061447A CN102712884B CN 102712884 B CN102712884 B CN 102712884B CN 201080061447 A CN201080061447 A CN 201080061447A CN 102712884 B CN102712884 B CN 102712884B
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- China
- Prior art keywords
- detergent particles
- particles group
- paste
- tensio
- weight parts
- Prior art date
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- 239000003599 detergent Substances 0.000 title claims abstract description 287
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 84
- 239000008187 granular material Substances 0.000 title abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 262
- 238000000034 method Methods 0.000 claims abstract description 101
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims description 177
- 239000000843 powder Substances 0.000 claims description 92
- 239000013543 active substance Substances 0.000 claims description 89
- 239000002994 raw material Substances 0.000 claims description 89
- 238000005406 washing Methods 0.000 claims description 78
- 239000007788 liquid Substances 0.000 claims description 61
- 238000002156 mixing Methods 0.000 claims description 59
- 239000012530 fluid Substances 0.000 claims description 57
- 239000003795 chemical substances by application Substances 0.000 claims description 47
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 28
- 239000007921 spray Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 18
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 13
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 150000001340 alkali metals Chemical group 0.000 claims description 3
- 125000003342 alkenyl group Chemical group 0.000 claims description 3
- 150000001412 amines Chemical group 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 17
- 230000000694 effects Effects 0.000 abstract description 13
- 238000001694 spray drying Methods 0.000 abstract description 2
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 49
- 238000003756 stirring Methods 0.000 description 44
- 238000010521 absorption reaction Methods 0.000 description 32
- 238000004140 cleaning Methods 0.000 description 17
- 230000002045 lasting effect Effects 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 16
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 16
- 230000004048 modification Effects 0.000 description 15
- 238000012986 modification Methods 0.000 description 15
- 238000001035 drying Methods 0.000 description 13
- -1 polyoxyethylene Polymers 0.000 description 13
- 239000010457 zeolite Substances 0.000 description 13
- 229910021536 Zeolite Inorganic materials 0.000 description 12
- 239000002253 acid Substances 0.000 description 11
- 239000004094 surface-active agent Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- 239000002734 clay mineral Substances 0.000 description 7
- 150000002632 lipids Chemical class 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 230000000704 physical effect Effects 0.000 description 6
- 238000010008 shearing Methods 0.000 description 6
- 229920003169 water-soluble polymer Polymers 0.000 description 6
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000003352 sequestering agent Substances 0.000 description 4
- 210000005239 tubule Anatomy 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000013522 chelant Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 239000007850 fluorescent dye Substances 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 102220207670 rs748889500 Human genes 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 235000019832 sodium triphosphate Nutrition 0.000 description 3
- JSYPRLVDJYQMAI-ODZAUARKSA-N (z)-but-2-enedioic acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)\C=C/C(O)=O JSYPRLVDJYQMAI-ODZAUARKSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 2
- 229920013701 VORANOL™ Polymers 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 241000345998 Calamus manan Species 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 241000282326 Felis catus Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical class OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 101710194948 Protein phosphatase PhpP Proteins 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- 231100000987 absorbed dose Toxicity 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical group 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000012867 bioactive agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013461 design Methods 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
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical class [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 244000144992 flock Species 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 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 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001983 poloxamer Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 235000012950 rattan cane Nutrition 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 210000002374 sebum Anatomy 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [H+].[H+].[Na+].[O-]S([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 235000020985 whole grains Nutrition 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
-
- 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
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)
Abstract
Disclosed is a method for producing detergent granules containing an anionic surfactant, wherein the method does not involve spray drying, and produces a higher yield of detergent granules having the necessary particle size. Detergent granules having a sharp particle size distribution can be produced with a high yield by employing said method. Moreover, having a sharp particle size distribution exerts the effects of not only improving the appearance, but also of being able to efficiently produce a detergent exhibiting good flow properties, and thus improving productivity.
Description
Technical field
The present invention relates to that the tensio-active agent that uses the rotary-type tablets press of container, contain anion surfactant is stuck with paste and the detergent particles group's of many fluid tips manufacturing process.In addition, the invention still further relates to and contain the detergent composition that this detergent particles group forms.
Background technology
In recent years, powder detergent composition and manufacturing process thereof are required to meet economy, environment friendly etc.
About being combined with the powder detergent as the compound of the anion surfactant representing with formula (1) of tensio-active agent, so far, to for active the carrying out of can, improve the objects such as environment friendly of abrasive various open.The common skin irritation of known described anion surfactant is less, and Biodegradable is good.
For example,, from the viewpoint of economy, environment friendly, as not using spray-dired manufacture method to disclose the manufacturing process of using the detergent composition of anion surfactant by non-spray-drying process.The method of tensio-active agent being stuck with paste and manufactured continuously through homogenizer/middling speed stirrer/drying machine for detergent materials of super-dry detergent composition is disclosed in patent documentation 1.In patent documentation 2, disclose and used tensio-active agent to stick with paste and through the detergent raw material of super-dry, by homogenizer/middling speed stirrer/setting device, while make micropartical recirculation manufacture continuously the method for detergent composition.
Yet, in the method for making of patent documentation 1, be difficult to adjust granularity, in addition, in the method for making of patent documentation 2, for carrying out the adjusting of granularity, adopt the method for making that makes micropartical recirculation, be the manufacturing process that productivity is low.Therefore the detergent particles group's who, require more simply, yield obtains having necessary granularity well method for making.
Prior art document
Patent documentation
Patent documentation 1: the flat 10-500716 communique of Japanese Unexamined Patent Application Publication
Patent documentation 2: the flat 10-506141 communique of Japanese Unexamined Patent Application Publication
Summary of the invention
Solve the means of problem
; main contents of the present invention relate to a kind of detergent particles group's manufacture method; wherein; described manufacture method comprises that tensio-active agent sticks with paste mixed processes: with many fluid tips, add and contain following a) composition and b in the powder of powder detergent raw material) the tensio-active agent paste of composition; by the rotary-type tablets press of container, mix
A) anion surfactant representing with following formula (1),
R-O-SO
3M （1）
In formula, R represents that carbonatoms is 10 ~ 18 alkyl or alkenyl, and M represents alkali metal atom or amine,
B) the above-mentioned a) composition with respect to 100 weight parts is the water of 25 ~ 70 weight parts.
The present invention relates to provide with containing spray-dired method, manufacture the method that contains anion surfactant and there is the detergent particles group that the yield of detergent particles of necessary granularity is good.In addition, the invention still further relates to provide and contain the detergent composition that this detergent particles group forms.
The manufacture method of the application of the invention, can obtain and can manufacture well the detergent particles group's of narrow diameter distribution effect by yield.Size distribution narrow not only can be obtained and improve the effect of outward appearance, and can obtain and make also good effect of mobility, thereby obtain the effect that can obtain efficiently the washing composition of productivity excellence.
Embodiment
Detergent particles group's of the present invention manufacture method is to have the manufacture method of the powder of powder detergent raw material and the tensio-active agent that contains the anion surfactant representing with formula (1) being stuck with paste to the detergent particles group of the operation of mixing; one of feature of this manufacture method is; when mixing; use the rotary-type tablets press of container; and, with many fluid tips such as two-fluid spray nozzles, add the tensio-active agent that contains the anion surfactant representing with formula (1) and stick with paste.
Conventionally; use the granulation of the rotary-type tablets press of container; can make the powder in tablets press flow equably; in addition; because it is to be attended by the mixing device that the particle that brings of rotation rises and deadweight causes slip falls; thereby can suppress to put on the shearing force on powder, be therefore non-densification prilling process.In addition, if the tackiness when paste that contains the anion surfactant representing with formula (1) contact with powder by force with regard to can not carrying out granulation, thereby, while contacting with powder, must show tackiness.If be used as single fluid nozzle or the pipe arrangement of common supply method, the paste that contains such anion surfactant representing with formula (1) is supplied in to the rotary-type tablets press of container; be difficult to make the liquid component of supplying with to disperse equably in mixing machine, because part produces large liquid piece, cause easily forming big particle.
So; the inventor is by using many fluid tips such as two-fluid spray nozzle; show when contacting with powder when the adhesive paste that contains the anion surfactant representing with formula (1) spray to be supplied in the rotary-type tablets press of container and find, granulation equably in the formation of inhibition big particle.Its reason is considered to; by using many fluid tips in advance by so small drop of pasting into of anion surfactant that contains; even thereby in the rotary-type tablets press of container, also can realize the high dispersive of such paste that contains anion surfactant, do not produce the large liquid piece that forms big particle.Therefore, with many fluid tips, showing that adhesive such paste that contains anion surfactant makes an addition in the rotary-type tablets press of container when contacting with powder is also one of feature of the present invention.
As mentioned above, in the present invention, by being used in combination the rotary-type tablets press of container and many fluid tips, can obtain not expectable the situation from using separately respectively, can manufacture well the detergent particles group's of narrow particle size distribution effect by yield.
As the hypothesis of mechanism that obtains the particle of narrow particle size distribution with high yield, be considered to; thereby put on by using the rotary-type tablets press of container to obtain the uniform particle that the shearing force on powder is inhibited; and; the cohesion that tackiness was caused that makes drop microminiaturization and make it high dispersive thereby can suppress to be stuck with paste by the tensio-active agent that contains the anion surfactant representing with formula (1) by many fluid tips, addition effect.
Yet, in the situation that stirring or mix with the rotary-type tablets press of container, exist liquid component (in this manual for tensio-active agent is stuck with paste) to be difficult to the problem of disperseing equably in tablets press.For this reason, for example, inquire into the supply method of liquid component, considered the means that liquid component is disperseed equably.For example, as the method that liquid component is disperseed equably, considered to realize with many fluid tips such as two-fluid spray nozzles the method for the microminiaturization of liquid component.Yet, even those skilled in the art also can not produce many fluid tips for making the design of the tensio-active agent paste microminiaturization that viscosity is high.
Mode as the mixing in manufacture method of the present invention; so long as use the rotary-type tablets press of container; and be not particularly limited by the mode that many fluid tips are sprayed the tensio-active agent paste that contains the anion surfactant representing with formula (1); below, the mode of an example as manufacture method of the present invention is illustrated in greater detail.
In the present invention, detergent particles refers to the particle that contains tensio-active agent and washing assistant etc., and detergent particles group refers to its aggregate.Detergent composition refers to, contain detergent particles group, and according to hope, the composition of the detergent ingredients that contains the other interpolation except detergent particles group (for example, lotion-aid particle, fluorescence dye, enzyme, spices, defoamer, SYNTHETIC OPTICAL WHITNER, bleach-activating agent etc.).
In this manual, water-solublely refer to that the solubleness of the water with respect to 25 ℃ is more than 0.5g/100g, water-insoluble refers to that the solubleness of the water with respect to 25 ℃ is lower than 0.5g/100g.
1. powder detergent raw material
As the essential composition in the present invention, can enumerate powder detergent raw material.Specifically, can enumerate following 1) alkaline agent, 2) water-soluble substances, 3) clay mineral.These are 1 years old) ~ 3) composition can use individually alkaline agent, water-soluble substances, clay mineral, in addition, also Multiple components mix can be used.From granular viewpoint, as the median size of this powder detergent raw material, be preferably 10 ~ 250 μ m, more preferably 50 ~ 200 μ m, 80 ~ 200 μ m more preferably.
In addition, the median size of alkaline agent, water-soluble substances, clay mineral is not particularly limited, in the situation that a large amount of, coordinate the tensio-active agent that contains the anion surfactant representing with formula (1) to stick with paste, from improving the viewpoint of yield, also can be crushed to 1 ~ 50 μ m and re-use.
As alkaline agent, can be set forth in the material using as alkaline agent in common detergent composition, illustrated sodium carbonate (for example, light ash or heavy ash), sodium bicarbonate, water glass, salt of wormwood, calcium carbonate etc.From operation easiness and be easy to viewpoint in one's hands, be preferably light ash.These materials may be used alone, can also be two or more kinds in combination.
In the situation that using light ash as powder detergent raw material, the temperature while burning till by adjusting sodium bicarbonate, can further improve the ability that supports tensio-active agent.From supporting the viewpoint of ability, firing temperature is preferably 120 ~ 250 ℃, more preferably 150 ~ 220 ℃, more preferably 150 ~ 200 ℃.
As water-soluble substances, can enumerate the powder using in the common detergent composition such as saltcake, tripoly phosphate sodium STPP or the porous powder that the dry making of their hydrate is obtained etc.
As clay mineral, can be set forth in the clay mineral using in common detergent composition.As powder detergent raw material, in the situation that also with clay mineral and above-mentioned raw materials in addition, their mixture is by granulating.Itself and tensio-active agent are being stuck with paste mixes in the situation that, the powder detergent raw material of a contained water dissolution part in paste, is used in the cohesiveness of generation thus or the cohesiveness of clay mineral in granulating.
When by the powder of powder detergent raw material and the mixing of tensio-active agent paste, also can add above-mentioned powder detergent raw material powder raw material in addition according to hope, as addition, with respect to the powder detergent raw material of 100 weight parts, be preferably 0 ~ 150 weight part, more preferably 0 ~ 100 weight part, 0 ~ 50 weight part more preferably.As this powder raw material, for example can enumerate aluminosilicate, PREFEED(TOKUYAMA SILTEX CO., LTD. manufactures) etc. crystallized silicon hydrochlorate etc.In the situation that using described powder raw material, the content of this powder raw material in detergent particles group, from improving mobility, suppress to ooze out or lump, improve the viewpoint of cleaning capacity, be preferably 0.1 % by weight above, more preferably 1 % by weight above, more preferably more than 3 % by weight; From washability, deliquescent viewpoint, be preferably 40 % by weight following, more preferably 30 % by weight following, more preferably 20 % by weight following, further more preferably below 10 % by weight.
Viewpoint from easiness in one's hands with the detergent particles group's who obtains performance, as the preferred example of powder detergent raw material, can enumerate the raw material that comprises light ash and/or saltcake.
2. tensio-active agent is stuck with paste
As the essential composition in the present invention, can enumerate tensio-active agent and stick with paste.In the present invention, by add tensio-active agent in powder detergent raw material, stick with paste, and use the rotary-type tablets press of container, thereby by powder detergent feed particles, manufacture detergent particles group.
[composition that tensio-active agent is stuck with paste]
Anion surfactant in sticking with paste as the tensio-active agent using in the present invention is with formula (1): R-O-SO
3(in formula, R is the alkyl or alkenyl that carbonatoms is 10 ~ 18, preferably carbonatoms is 12 ~ 16 to the anion surfactant that M represents, M is the amine such as the alkali metal atoms such as Na, K or monoethanolamine, diethanolamine.From improving the viewpoint of the cleaning capacity of detergent composition, as the preferred Na of M, K.）。
[physical property that tensio-active agent is stuck with paste]
Tensio-active agent is stuck with paste and to be, the water that contains the anion surfactant (being recited as " a) composition " in this specification sheets) that represents with formula (1) and specified amount forms.From the viewpoint of the operability manufactured, it is in the use temperature territory of this surfactant composition, to have that the viscosity that this tensio-active agent is stuck with paste is preferably below 10Pas, the paste of the temperature field below 5Pas more preferably that tensio-active agent is stuck with paste.As the preferred existence range in such use temperature territory, the viewpoint of the stability of sticking with paste from tensio-active agent, preferably to 70 ℃, more preferably to 60 ℃.Here, viscosity by coaxial double rotating cylinder type rotational viscosimeter (HAAKE manufactures, sensor: SV-DIN) with velocity of shear 50[1/s] measure and try to achieve.
Tensio-active agent is stuck with paste according to its water ratio difference and viscosity changes greatly.For example, can with in alkali cpd and a) acid precursor of composition, prepare the paste of this tensio-active agent, now, thereby preferably regulate the amount of moisture of alkali cpd used to prepare tool water ratio likely, that is, the tensio-active agent of tool viscosity likely is stuck with paste.Conventionally known, this tensio-active agent is stuck with paste when the water that contains 25 ~ 70 weight parts (water ratio of this surfactant composition is approximately 20 ~ 40%) with respect to a) composition of 100 weight parts, thereby reduced viscosity easily operates, in the present invention, preferably use the moisture of surfactant composition is adjusted to the paste within the scope of this.The scope of the amount of the water in sticking with paste as tensio-active agent, from the viewpoint of operability, with respect to a) composition of 100 weight parts, is 25 ~ 70 weight parts, be preferably 30 ~ 65 weight parts, 35 ~ 65 weight parts more preferably.
In addition, due to a) the very unstable easy decomposition of acid precursor of composition, therefore, preferably can suppress the mode of its decomposition, be prepared.Preparation method is not particularly limited, and can use known method.For example, use loop reactor, by heat exchanger etc., remove neutralization heat, notice that the temperature of this acid precursor and tensio-active agent paste is manufactured on one side.Temperature field during as manufacture is preferably 30 ~ 60 ℃, as the storage temperature territory after manufacturing, is preferably below 60 ℃.In addition, during use, heat up as required, use this surfactant composition.
In addition, this anion surfactant obtaining is stuck with paste, and the viewpoint from suppressing to decompose, preferably has excessive basicity.
In addition, in sticking with paste, tensio-active agent also can contain: the secondary resultant saltcake while manufacturing the acid precursor of a) composition when unreacted alcohol, unreacted Voranol EP 2001, neutralization reaction, the pH buffer reagent adding during in neutralization reaction, discoloring agent etc.
In addition, the content of a) composition in the detergent particles group who obtains in the present invention, from cleaning capacity and deliquescent viewpoint, be preferably the scope of 10 ~ 55 % by weight, more preferably 10 ~ 45 % by weight, more preferably 15 ~ 40 % by weight, further 15 ~ 40 % by weight more preferably.
In tensio-active agent is stuck with paste, as tensio-active agent, can use separately a) composition, also can be used together following tensio-active agent and use.And use in the situation that, can be in advance stick with paste and mix use with containing a) tensio-active agent of composition, also can add respectively separately.In addition, and with following tensio-active agent in the situation that, following tensio-active agent preferably contains 1 ~ 70 weight part, more preferably contains 2 ~ 50 weight parts, more preferably contains 3 ~ 30 weight parts, further more preferably contains 5 ~ 15 weight parts with respect to a) composition of 100 weight parts.In addition, and with following tensio-active agent in the situation that, the content of a) composition in tensio-active agent paste is preferably 40 ~ 80 % by weight, more preferably 45 ~ 75 % by weight, 50 ~ 70 % by weight more preferably.
For example, also nonionogenic tenside can be mixed or use respectively.In the situation that use has the nonionogenic tenside of the fusing point below 30 ℃, preferably and be that 45 ~ 100 ℃, molecular weight are water-soluble nonionic organic compound (following, to be called fusing point rising agent) or its aqueous solution of 1,000 ~ 30,000 with the fusing point with the fusing point effect of increasing that makes tensio-active agent.In addition, as the fusing point rising agent that can use in the present invention, such as enumerating polyoxyethylene glycol, polypropylene glycol, Voranol EP 2001, Pluronic type nonionogenic tenside etc.Or, can and use amphoterics, cats product according to object.
For example, can, by a) composition anion surfactant mixing or use respectively in addition, as described anion surfactant, can enumerate polyoxyethylene alkyl ether sulfate salt or alkylbenzene sulfonate, alpha-sulfo fatty acid ester salt or secondary paraffin sulfonate.In addition, from improving the dispersed viewpoint of the detergent particles group the water of low temperature, the anion surfactants such as polyoxyethylene alkyl ether sulfate salt and alkylbenzene sulfonate can preferably contain 0 ~ 10 % by weight, more preferably contain 0 ~ 5 % by weight, further preferably contain 0 ~ 3 % by weight in detergent particles group.In addition, from improving the viewpoint of cleaning capacity, be preferably 0.1 % by weight above, more preferably 1 % by weight above, more preferably more than 3 % by weight; From improving the viewpoint of washing composition yield, be preferably 10 % by weight following, more preferably 8 % by weight following, more preferably below 5 % by weight.
In addition, in order to obtain defoaming effect, can be used together soap.
As nonionogenic tenside, be not particularly limited, from the viewpoint of cleaning capacity, preference as addition on the alcohol that is 10 ~ 14 at carbonatoms the polyoxyalkylene alkyl of alkylene oxide of 6 ~ 22 moles.
The content of the nonionogenic tenside in detergent particles group, the viewpoint of kicking up while dispersing from improving cleaning capacity, improve resistance to anti-caking and suppressing powder is preferably 0 ~ 10 % by weight, more preferably 0 ~ 5 % by weight, 0 ~ 3 % by weight more preferably in detergent particles group.In addition, from improving the viewpoint of cleaning capacity, be preferably 0.1 % by weight above, more preferably 1 % by weight above, more preferably more than 3 % by weight; From improving the viewpoint of washing composition yield, be preferably 10 % by weight following, more preferably 8 % by weight following, more preferably below 5 % by weight.
3. polymkeric substance
In addition; from cleaning capacity, for the viewpoint of granular bond effect; in detergent particles group in the present invention, can be used together the inorganic polymers such as water-soluble cellulose derivative, carbohydrate and carboxylic-acid polymkeric substance, amorphous silicate etc., more preferably the salt of vinylformic acid-maleic acid, polyacrylate.As salt, particular certain cancers, sylvite, ammonium salt.In addition, as the weight-average molecular weight of carboxylic-acid polymkeric substance, be preferably 1000 ~ 100000, more preferably 2000 ~ 80000.
4. other composition
In addition, the detergent particles group in the present invention can suitably coordinate the material the composition of enumerating in above-mentioned 1 ~ 3 as required.The interpolation time of described other composition is not particularly limited.
Sequestrant (metal chelator)
Inhibition cleaning action in order to suppress to be caused by metal ion, can coordinate sequestrant.As water-soluble chelator, so long as keep the material of metal ion-chelant ability to be all not particularly specified, can use crystallized silicon hydrochlorate, tri-polyphosphate, orthophosphoric acid salt, pyrophosphate salt etc.For water-insoluble sequestrant, from the dispersed viewpoint water, the median size of preferred particulates is the sequestrant of 0.1 ~ 20 μ m, can enumerate crystallinity aluminosilicate, can use such as A type zeolite, P type zeolite, X-type zeolite etc.
Water-soluble inorganic salt
For improve washings ionic strength, improve the effect of clean sebum dirt etc., preferably add water-soluble inorganic salt.
Water-insoluble vehicle
So long as in water favorable dispersity and cleaning capacity is not produced to dysgenic material and be all not particularly specified.From the dispersed viewpoint water, preferably the median size of primary particle is the material of 0.1 ~ 20 μ m.
Other ancillary component
Can enumerate fluorescence dye, pigment, dyestuff etc.
In addition, the method that the mensuration of the median size of described composition is recorded in can the measuring method by physical property described later is measured.
< detergent particles group's method for making >
Detergent particles group's of the present invention manufacture method is to comprise following tensio-active agent paste mixed processes,, be included in the powder of powder detergent raw material add, the method for operation that mixed surfactant is stuck with paste, through described operation, carry out making detergent particle swarm.
1. tensio-active agent is stuck with paste mixed processes
In the powder of powder detergent raw material, add to contain with the anion surfactant of formula (1) expression and the tensio-active agent of water and stick with paste, the operation of being mixed to come making detergent particle swarm by the rotary-type tablets press of container.
The amount of sticking with paste as the tensio-active agent mixing in this operation, with respect to the powder detergent raw material of 100 weight parts, be preferably 25 ~ 200 weight parts, more preferably 25 ~ 180 weight parts, more preferably 25 ~ 160 weight parts, further more preferably 25 ~ 100 weight parts, be particularly preferably 30 ~ 90 weight parts, 35 ~ 85 weight parts especially more preferably.From the viewpoint of cleaning capacity, more than being preferably 25 weight parts; From washing composition yield, deliquescent viewpoint, be preferably 200 weight parts following, more preferably 180 weight parts following, more preferably 160 weight parts following, further more preferably below 100 weight parts.
The rotary-type tablets press of container using in this operation is not give the strong shearing of particle not carry out the device of very large densification.For example, even possess and can give the main wing of high shear force and pulverize in the perpendicular type or horizontal type tablets press of the wing at script, by the Froude number of revolution or following record is set as to low value, suppress densification, can be used in granule manufacture of the present invention.That is, even can give the tablets press of particle high shear force, as long as its be can be by operational condition the tablets press that makes its shearing force reduce to operate such as setting be also contained in the rotary-type tablets press of container in this specification sheets.
As the rotary-type tablets press of container, from the granular viewpoint that easily supports ability with raising, preferably by the rotation of body body portion, carry out granular dish-type granulators or rotating cylinder type tablets press (rotary drum mixer).These devices can be used in any method of batch-type, continous way.In addition, from powder Combination and the blended viewpoint of solid-liquid, the auxiliary baffle plate mixing is preferably set on dish or rotating cylinder.
In addition; in order to use as the rotary-type tablets press of container; from making powder flow equably; and; guarantee that it is that the viewpoint that is attended by the mixing device that the particle that brings of rotation rises and deadweight causes slip falls is set out; preferably the Froude number of the tablets press of the formula definition with following is set as below 1.0, more preferably below 0.8, more preferably below 0.6, further more preferably below 0.4.
Froude number: Fr=V
2/ (R * g)
V: peripheral speed [m/s]
R: the radius of the circumference from rotation center to whirl [m]
G: universal gravity constant [m/s
2]
The viewpoint of sticking with paste from add equably tensio-active agent mixed powder, is preferably set as the Froude number of tablets press more than 0.001, more preferably more than 0.005, more preferably more than 0.01, further more preferably more than 0.05.
In addition, possessing main wing and pulverizing in the perpendicular type or horizontal type tablets press of the wing, V and R are used the value of main shaft; By the rotation of body body portion, undertaken in granular dish-type granulators or rotating cylinder type tablets press, V and R are used the value of body body portion.In addition, in possessing the dish-type granulators of pulverizing the wing, V and R are used the value of pulverizing the wing.
The rotational time of tablets press is not particularly limited, and for example preferred surfactant is stuck with paste 0 ~ 10 minute that adds after starting.
In the present invention, preferably making tensio-active agent stick with paste disperses to add equably.As its method, have and use many fluid tips to carry out the method for microminiaturization.
Many fluid tips be by stream independently make liquid component and for micronize gas (air, nitrogen etc.) be circulated near the nozzle that carries out hybrid fine particles nozzle top, can use two-fluid spray nozzle or three fluid tips, four fluid tips etc.In addition, liquid component and micronize can be any of the internal mix type of mixing in nozzle top or the external mix type of mixing outside nozzle top with the mixing portion of gas.
In the present invention, preferably with many fluid tips, liquid component fine droplet is added, more preferably use two-fluid spray nozzle.As so many fluid tips, for example, can enumerate Spraying Systems Co., Japan manufactures, (strain) found altogether alloy and made manufacturing, IKEUCHI Co., LTD. the internal mix type two-fluid spray nozzle, the Spraying Systems Co. that manufacture etc., external mix type four fluid tips that Japan manufactures, (strain) rugged motor of external mix type two-fluid spray nozzle, rattan (strain) that vertical alloy makes that manufacturing, ATMAX Inc. are manufactured etc. is altogether manufactured etc.
In the situation that using two-fluid spray nozzle, for example, preferably under following condition, supply with above-mentioned paste.For example, as micronize, with air-atomizing, press and be preferably 0.05 ~ 0.7MPa.
The microminiaturization of the drop that the full-bodied tensio-active agent using in the present invention is stuck with paste, from preventing the viewpoint of the obstruction of nozzle tip, in the present invention, is preferably used external mix type two-fluid spray nozzle.
The inventor has carried out wholwe-hearted discussion for drop footpath difference to the impact of the detergent particles group's who obtains yield and coarse grain amount, its result is as follows, viewpoint from yield, the median size that preferably makes the drop footpath of above-mentioned paste is 1 ~ 300 μ m, more preferably 1 ~ 200 μ m, 1 ~ 150 μ m more preferably.
In addition, in the situation that want to improve the interpolation speed of above-mentioned paste, use a plurality of many fluid tips, it is also effective when maintaining the microminiaturization of drop, improving interpolation speed.
By using such method, even also can disperse equably, improve yield in full-bodied above-mentioned paste, obtain the detergent particles group of narrow particle size distribution.
In addition, the median size in the drop footpath that tensio-active agent is stuck with paste is calculated with volume reference, is to use laser diffraction formula particle size distribution device: the value of the manufacture of SPRAY-TEC(Malvern company) measuring.
< detergent particles group's physical property >
By manufacture method of the present invention, can obtain having the detergent particles group of predetermined characteristic.The detergent particles group who obtains by related manufacture method of the present invention is also contained in the present invention.The detergent particles group's who is made by the present invention preferred physical property as described below.
As volume density, be preferably that 400g/L is above, more preferably 450～1000g/L, more preferably 450 ~ 950g/L, 500 ~ 900g/L more preferably.As median size, be preferably 150 ~ 800 μ m, more preferably 180 ~ 700 μ m, 200 ~ 500 μ m more preferably.
In addition, the method that described volume density, median size are recorded in can the measuring method by physical property described later is measured.
In addition, as the index of detergent particles group's according to the present invention preferred size-grade distribution, can use Rosin-Rammler number (the R-R number in table).Following formula for the calculating of Rosin-Rammler number.
log(log(100/R(Dp)))=nlog(Dp)+log(β)
R (Dp): particle diameter is the cumulative percentage [%] of powder more than Dp μ m
Dp: particle diameter [μ m]
N:Rosin-Rammler number
β: particle property coefficient
It is narrower that Rosin-Rammler counts the higher expression size-grade distribution of n.As n, from the viewpoint of detergent particles group's taste, be preferably more than 1.5, more preferably more than 1.7, more preferably more than 1.9, further more preferably more than 2.0.
Yield as the detergent particles group's who is made by the present invention preferred size, as mesh size, be the ratio of the particle of 125 ~ 1000 μ m, be preferably more than 70%, more preferably more than 75%, more preferably more than 80%, further more preferably more than 85%, be particularly preferably more than 87%, especially more preferably more than 90%.
As the amount of moisture of the detergent particles group in the present invention, from a) viewpoint of composition of a large amount of cooperations, preferably water component is less.Specifically, in the situation that measure detergent particles group's amount of moisture with infrared rays moisture meter, its amount of moisture be preferably 20 % by weight following, more preferably 15 % by weight following, more preferably 10 % by weight following, more preferably below 5 % by weight.
The detergent particles group's who is made by the present invention oil absorption is to be that oil absorption after particles more than 2000 μ m is determined as removing mesh size.The preferred viewpoint from making the tolerable limit of the combined amount of liquid washing agent raw material expand liquid washing agent raw material oil suction operation, oil absorption be preferably 0.15mL/g above, more preferably 0.2mL/g above, more preferably 0.3mL/g above, further more preferably more than 0.4mL/g.The detergent particles group's who is made by the present invention higher oil absorption is considered to by adopting the rotary-type tablets press of said vesse to carry out that granulating reaches.
In addition, the combined amount of sticking with paste the tensio-active agent paste in mixed processes due to tensio-active agent is fewer, oil absorption is higher, thereby, can come adjustment sheet surface-active agent to stick with paste the combined amount that the tensio-active agent in mixed processes is stuck with paste by the combined amount of the liquid washing agent raw material in liquid washing agent raw material oil suction operation, thereby adjust arbitrarily the detergent particles group's who is made by the present invention oil absorption.
The preferred method for making that obtains detergent particles group also can further comprise following liquid washing agent raw material oil suction operation or surfaction operation or drying process as required.
2. manufacturing process arbitrarily
Liquid washing agent raw material oil suction operation: be the operation of mixing with the liquid washing agent raw material of above-mentioned nonionogenic tenside or above-mentioned polymkeric substance etc. stuck with paste detergent particles group that mixed processes obtains by tensio-active agent.
Surface modification operation: be to stick with paste with surperficial coating Surfactant the operation that the detergent particles group who obtains in mixed processes or liquid washing agent raw material oil suction operation carries out surface modification.But, in surface modification operation, also can pulverize simultaneously.
Drying process: be to make tensio-active agent stick with paste the dry operation of detergent particles group obtaining in mixed processes, liquid washing agent raw material oil suction operation or surface modification operation.
2-1. liquid washing agent raw material oil suction operation
In this operation, by tensio-active agent being stuck with paste to the detergent particles group who obtains in mixed processes, mix with liquid washing agent raw material, thereby can make liquid washing agent raw material support in this detergent particles group, be operation arbitrarily.
In liquid washing agent raw material oil suction operation, at least use by tensio-active agent and stick with paste the detergent particles group that mixed processes obtains.That is, in this operation, also can be used together other particle swarm with the ability that supports tensio-active agent, such as be dried the particle swarm that waits other method to obtain by spraying.
Ratio as this detergent particles group in liquid washing agent raw material oil suction operation, viewpoint from cleaning capacity, oil absorption, be preferably the particle swarm that is added with liquid washing agent raw material more than 50 % by weight in 100 % by weight, more preferably 70 % by weight above, more preferably more than 90 % by weight.
As described method, can be set forth in the method for mixing in the rotary-type tablets press of container of manufacturing this detergent particles group.In addition, for example, can enumerate the method for mixing this detergent particles group and liquid washing agent raw material with the mixing machine of batch-type or continous way.At this, in the situation that carrying out with batch-type, as to the reinforced method of mixing machine, can take (1) first to add after this detergent particles group in mixing machine, then add liquid detergent raw material; (2) in mixing machine, repeat each a small amount of this detergent particles group of interpolation and liquid washing agent raw material; (3), add this detergent particles group of a part in mixing machine after, repeat the methods such as each a small amount of remaining this detergent particles group of interpolation and liquid washing agent raw material.
In this detergent particles group, adding in liquid detergent raw material, the use level of liquid washing agent raw material is more, and interpolation speed is more important.Specifically, preferably make the interpolation speed of liquid washing agent raw material below this detergent particles group's speed of oil absorption.By the interpolation speed with such, implement to add, the oil suction that can make liquid washing agent raw material is more inner to this detergent particles group's, as its result, can suppress the cohesion of the detergent particles that the tackiness due to liquid washing agent raw material causes, can be so that the detergent particles group's who arrives size distribution narrow.As concrete interpolation speed, for example, in the situation that the tensio-active agent using in adding the present invention is stuck with paste, with respect to this detergent particles group of 100 weight parts, be preferably 35 weight parts/minute following, more preferably 20 weight parts/minute following, more preferably 10 weight parts/minute following, further more preferably 7.5 weight parts/minute below.
In addition, as liquid washing agent raw material, can enumerate the liquid component arbitrarily using in common detergent composition such as above-mentioned nonionogenic tenside, water-soluble polymers (polyoxyethylene glycol, sodium polyacrylate, vinylformic acid maleic acid etc.), lipid acid.Liquid component can only be used a kind of composition, also can be by the above also use of two kinds of compositions.As liquid component, can add this composition with liquid form, or also can add with the form of the aqueous solution or dispersion liquid.As the usage quantity of liquid washing agent raw material, with respect to this detergent particles group of 100 weight parts, from improving the viewpoint of cleaning capacity, be preferably 0.1 weight part above, more preferably 1 weight part above, more preferably more than 3 weight parts; Interparticle coagulation, the high speed solvability of the detergent particles containing from suppress detergent particles group and the viewpoint that suppresses exudative or anti-caking, be preferably 30 weight parts following, more preferably 20 weight parts following, more preferably below 10 weight parts.
As preferred mixing device, specifically, except the rotary-type tablets press of above-mentioned container, can also enumerate following device.In the situation that carrying out with batch-type, the mixing device of preferred following (1) ~ (3).There is (1) Henschel mixer (Henschel mixer) (Mitsui three pond chemical industry machines (strain) are manufactured), homogenizer (dark river industry (strain) is manufactured), vertical tablets press (Vertical granulator) (Powrex Corporation manufacture), LODIGE stirrer (Matuzaka skill is ground (strain) and manufactured), Plough Share stirrer (Pacific Ocean machine work (strain) manufacture), the mixing device that Japanese kokai publication hei 10-296064 communique is recorded, the mixing device that Japanese kokai publication hei 10-296065 communique is recorded etc., (2) ribbon blender (day and mechanical industry (strain) are manufactured), batch-type kneader (assistant bamboo chemical machinery industry (strain) is manufactured), Ribocone((strain) the former making manufacturing in great river), (3) Nautamixer (Nautamixer) (HOSOKAWA MICRON CORPORATION manufacture), SV stirrer (Shinko Pantec Co., Ltd. manufacture) etc.In above-mentioned mixing machine; except the rotary-type tablets press of above-mentioned container; the mixing device that preferably LODIGE stirrer, Plough Share stirrer, Japanese kokai publication hei 10-296064 communique are recorded, the mixing device that Japanese kokai publication hei 10-296065 communique is recorded etc.; because by using described device; can in same device, carry out surface modification operation described later; the viewpoint of the simplification of slave unit is set out, so preferably.Wherein, because the mixing device of Japanese kokai publication hei 10-296064 communique record, the mixing device that Japanese kokai publication hei 10-296065 communique is recorded can regulate the humidity and temperature of mixture by ventilation, thereby can suppress detergent particles group's disintegration, thus preferably it.In addition, never give strong shearing force and can mixed powder and the mixing device such as Nautamixer of liquid, SV stirrer, the ribbon blender viewpoint that also can suppress detergent particles group's disintegration set out, preferably it.
In addition, also can use the device of successive type that this detergent particles group and liquid washing agent raw material are mixed.In addition, as the device of successive type, can enumerate FLEXOMIX type (Powrex Corporation manufacture), Turbulizer(HOSOKAWA MICRON CORPORATION manufacture) etc.
Temperature in mixing machine in this operation, is preferably adjusted into the temperature of the decomposition that can suppress the anion surfactant in this detergent particles, and the temperature field when manufacturing is preferably 30 ~ 60 ℃, as the storage temperature territory after manufacturing, is preferably below 60 ℃.
In order to obtain preferred detergent particles group's batch-wise mixing time, and the average retention time in the mixing of continous way is preferably 1 ~ 30 minute, more preferably 2 ~ 25 minutes, more preferably 3 ~ 20 minutes.
In liquid washing agent raw material oil suction operation, also can under ventilation, carry out the mixing of this detergent particles group and liquid washing agent raw material.More particularly, can be set forth in liquid washing agent raw material oil suction operation, in the interpolation of each raw material and/or in mixing, carry out being blown into the operation of the gases such as air in the tempering tank of mixing device.By carrying out described operation, can make this detergent particles group further support liquid washing agent raw material, thereby the detergent particles flock mating obtaining has closed more substantial liquid washing agent raw material.
As the reason that produces such effect, supposition is because by carrying out described operation, has removed that the anion surfactant existing on this detergent particles group surface is stuck with paste and the moisture of other liquid washing agent raw material causes.Its result, detergent particles group's tackiness reduces, and detergent particles group's cohesion is suppressed, thus the detergent particles group's who obtains size-grade distribution also narrows down.
As the condition of air-supply, for example the temperature of the gas of air-supply is preferably 10 ~ 65 ℃, more preferably 30 ~ 60 ℃, more preferably 50 ~ 60 ℃.
As air output, preferably with respect to this detergent particles group of 100 weight parts be 1 ~ 15 weight part/minute, more preferably 2 ~ 10 weight parts/minute, more preferably 3 ~ 8 weight parts/minute.
Before adding liquid detergent raw material, with add simultaneously, in adding procedure or after adding, also can add powder washing assistant.By adding described composition, can control detergent particles group's particle diameter, and can realize the raising of cleaning capacity.In addition, here so-called powder washing assistant refers to, beyond tensio-active agent, the clean power reinforcer of powder, specifically, refer to that zeolite, Citrate trianion etc. show the base of metal ion-chelant ability, sodium carbonate, salt of wormwood etc. shows the base of alkalization ability, crystallized silicon hydrochlorate etc. has the base of metal ion-chelant ability alkalization ability simultaneously, and other sodium sulfate etc. can improve the base of ionic strength etc.
Here, as crystallized silicon hydrochlorate, preferably use the crystallized silicon hydrochlorate of recording in Japanese kokai publication hei 5-279013 communique the 3rd hurdle the 17th row (preferably burning till the silicate that makes it crystallization at 500 ~ 1000 ℃), Japanese kokai publication hei 7-89712 communique the 2nd hurdle the 45th row, hurdle, Japanese kokai publication sho 60-227895 communique page 2 bottom right the 18th row (the preferably silicate of the 2nd table) as powder washing assistant.Here, more preferably use the SiO of alkalimetal silicate
2/ M
2still, M represents basic metal to O(.) be 0.5 ~ 3.2, be preferably 1.5 ~ 2.6 silicate.
As the usage quantity of this powder washing assistant, with respect to this detergent particles group of 100 weight parts, be preferably 0 ~ 12 weight part, 0 ~ 6 weight part more preferably.When described composition is within the scope of this, favorable solubility.
In addition,, after liquid washing agent raw material oil suction operation, preferably increase the surface modification operation of detergent particles group being carried out to surface modification.
2-2. surface modification operation
In this operation, be that Surfactant is stuck with paste the operation arbitrarily that the detergent particles group's who obtains in mixed processes or liquid washing agent raw material oil suction operation particle surface carries out modification.Therefore, the form during as interpolation, the various surperficial coating of interpolation as following (1) powder body, (2) fraction carries out surface modification operation.The number of times of surface modification operation can be for more than 1 time.
If detergent particles group's particle surface is carried out to modification with surperficial coating, there are detergent particles group's mobility and the tendency that resistance to anti-caking improves.Therefore,, in manufacture method of the present invention, be preferably provided with surface modification operation.As the device using in surface modification operation, for example, can be set forth in the mixing machine that possesses agitating wing simultaneously and pulverize the wing in the mixing machine of liquid washing agent raw material oil suction operation illustrated as preferred device.Below distinguish instruction card face coating.
(1) powder body
As powder body, preferably the median size of its primary particle is that 10 μ m are following, the powder of 0.1 ~ 10 μ m more preferably.From improving the clad ratio of detergent particles group's particle surface, the mobility that improves detergent particles group and the viewpoint of resistance to anti-caking, preferably median size is within the scope of this.The median size of this powder body can be by the method for utilizing scattering of light, such as using grain analyser ((strain) hole field makes manufacturing) or fractographic mensuration etc. to measure.In addition,, from the viewpoint of cleaning capacity, preferably this powder body has macroion exchange capacity or high alkalization ability.Described powder body can consist of a kind of composition, also can consist of Multiple components.
As this powder body, preferred aluminosilicate, can be crystallinity, unbodied any one.Except aluminosilicate, also preferably as the powder body of sodium sulfate, Calucium Silicate powder, silicon-dioxide, wilkinite, talcum, clay, amorphous silica derivative, crystallized silicon hydrochlorate.In addition, similarly also can use the median size of primary particle is that 0.1 ~ 10 metallic soap of μ m for example,, the tensio-active agent of powder (, alkyl-sulphate etc.) or water-soluble organic salt.In the situation that using crystallized silicon hydrochlorate, from preventing due to moisture absorption or inhaling the deteriorated object that the cohesion etc. of the crystallized silicon hydrochlorate that carbonic acid gas causes brings, preferably mix use with the powder body beyond crystallized silicon hydrochlorate.
As the usage quantity of powder body, with respect to the detergent particles group of 100 weight parts, be preferably 0 ~ 40 weight part, more preferably 0.5 ~ 40 weight part, more preferably 1 ~ 30 weight part, further 2 ~ 20 weight parts more preferably.When the usage quantity of this powder body is within the scope of this, mobility improves, and gives human consumer good use sense.From improving mobility, suppress the viewpoint of exudative and anti-caking, the usage quantity of powder body be preferably 0.1 weight part above, more preferably 0.5 weight part above, more preferably 1 weight part above, further more preferably 2 weight parts above, be again preferably 3 weight parts more than; From improving the viewpoint of washability, mobility, be preferably 40 weight parts following, more preferably 30 weight parts following, more preferably 20 weight parts following, further more preferably below 10 weight parts.
(2) fraction
As fraction, can enumerate water-soluble polymers and lipid acid etc., can add with the aqueous solution or the state that dissolves.Described fraction can consist of a kind of composition, also can consist of Multiple components.
(2-1) water-soluble polymers
As water-soluble polymers, can enumerate polycarboxylates such as the multipolymer of carboxymethyl cellulose, polyoxyethylene glycol, sodium polyacrylate, vinylformic acid and toxilic acid or its salt etc.As the usage quantity of this water-soluble polymers, with respect to the detergent particles group of 100 weight parts, be preferably 0 ~ 10 weight part, more preferably 0 ~ 8 weight part, 0 ~ 6 weight part more preferably.When the usage quantity of this water-soluble polymers is within the scope of this, can obtain showing the detergent particles group of good solubility, good mobility, resistance to anti-caking.
(2-2) lipid acid
As lipid acid, such as enumerating carbonatoms, be lipid acid of 10 ~ 22 etc.As the usage quantity of this lipid acid, with respect to the detergent particles group of 100 weight parts, be preferably 0 ~ 5 weight part, 0 ~ 3 weight part more preferably.In the situation that lipid acid is solid at normal temperatures, be preferably heated to show the temperature spraying supply afterwards of mobility.
2-3. drying process
In this operation, the operation that the detergent particles group that can also make to obtain is dried.By carrying out described operation, can from detergent particles group, remove the moisture coming from tensio-active agent paste etc.
This operation is that tensio-active agent is stuck with paste to the operation arbitrarily that the detergent particles group that obtains in mixed processes, liquid washing agent raw material oil suction operation or surface modification operation is dried.By removing moisture, can improve the content of the bioactive agent composition in detergent particles group.
From suppressing the viewpoint of detergent particles group's disintegration, preferably do not give the drying mode of strong shearing force as far as possible.For example, in batch-type, can enumerate and put into container and carry out dry method, with batch-type fluidised bed, carry out dry method etc. with electric drying apparatus or hot air dryer; In continous way, can enumerate fluidised bed, rotary drier, vapour pipe drying machine etc.
For drying temperature, from a) inhibition of the decomposition of composition and the viewpoint of rate of drying, be preferably 40 ~ 110 ℃, more preferably 50 ~ 100 ℃, more preferably 60 ~ 90 ℃.
< detergent composition >
Detergent composition of the present invention is to contain the composition that above-mentioned detergent particles group forms, and then, it is the composition that the detergent ingredients (for example, lotion-aid particle, fluorescence dye, enzyme, spices, defoamer, SYNTHETIC OPTICAL WHITNER, bleach-activating agent etc.) that also contains other interpolation except this detergent particles group forms.
The content of detergent particles group in detergent composition, from the viewpoint of cleaning capacity, be preferably 50 % by weight above, more preferably 60 % by weight above, more preferably 70 % by weight above, be further preferably 80 ~ 100 % by weight.
The content of detergent ingredients beyond detergent particles group in detergent composition is preferably below 50 % by weight, more preferably below 40 % by weight, more preferably below 30 % by weight, be further preferably below 20 % by weight.
The method for making > of < detergent composition
The method for making of detergent composition is not particularly limited, for example, can enumerate the method that the detergent ingredients of above-mentioned detergent particles group and interpolation is in addition mixed.The detergent composition obtaining is like this owing to containing a large amount of a) detergent particles of composition that coordinated, thereby, with also showing sufficient cleaning effect on a small quantity.As the purposes of described detergent composition, so long as use the purposes of powder detergent to be just not particularly limited, such as enumerating powder detergent for dress material, automatic tableware with washing composition etc.
The measuring method > of < physical property
1. volume density
Volume density is measured by the method for JIS K 3362 defineds.In addition, the volume density of the detergent particles group in the application is the volume density after the particle of removing more than 2000 μ m.
2. median size
For median size, by following method, measure.
(1) for median size, be particles more than 125 μ m, after the standard sieve (aperture 2000 ~ 125 μ m) of use JIS Z 8801-1 makes it to vibrate 5 minutes, by calculating median particle diameter according to the weight percent of the size of sieve mesh.In more detail, using aperture is 125 μ m, 180 μ m, 250 μ m, 355 μ m, 500 μ m, 710 μ m, 1000 μ m, 1400 μ m, the sieve of 9 grades of 2000 μ m and connect dish, sieve is piled up in successively and is connect on dish from small to large by aperture, from the sieve of topmost 2000 μ m, add 100g particle, cover lid is positioned over Ro-Tap type vibratory screening apparatus, and (HEIKO makes manufacturing, knock speed (tapping): 156 beats/min, rotating speed (rolling): 290 beats/min), make it to vibrate after 5 minutes, measure the weight of respectively sieving and connect upper this residual particle of dish, calculate the part by weight (%) of this particle on each sieve.From connecing dish, add up in order the part by weight of this particle the little sieve in aperture, will add up to 50% particle diameter as median size.
(2) for median size, be that 80 μ m are above and be less than the particle of 125 μ m, use aperture to be the sieve of 12 grades of 45 μ m, 63 μ m, 90 μ m, 125 μ m, 180 μ m, 250 μ m, 355 μ m, 500 μ m, 710 μ m, 1000 μ m, 1400 μ m, 2000 μ m and to connect dish, carry out same mensuration, average the calculating of particle diameter.
(3) for median size, be less than the particle of 80 μ m, use laser diffraction/diffuse transmission type particle size distribution device LA-920((strain) the making manufacturing of hole field), make it to be scattered in the solvent that does not dissolve this particle, using the median particle size recording as median size.
In addition, detergent particles group's median size is as the median size of wholegrain.
3.Rosin-Rammler number
Rosin-Rammler number is the number as above-mentioned defined.In this manual, specifically try to achieve as described below.By the same method of the mensuration with above-mentioned median size, measure the weight respectively sieve and connect upper this residual particle of dish, calculate the part by weight (cumulative percentage R (Dp) [μ m]) of this particle on each sieve (aperture Dp[μ m]).The obliquity n of least square fitting straight line when then, the log to respect to each logDp (log (100/R (Dp))) is mapped is as Rosin-Rammler number.
4. moisture
Utilize infrared rays moisture meter method to carry out moisture determination.That is, in the known test portion ware of weight, take 3g test portion, use infrared rays moisture meter (KETT Science Institute (strain) manufactures FD-240) to be heated to 105 ℃, in 30 seconds, do not have the time of changes in weight to finish as dry.Then, from dried weight and dry weight calculate amount of moisture.
5. mobility
Flowing time is that the funnel (hopper) that the volume density stipulated from JIS K 3362 of the powder of 100mL is measured use flows out the needed time.As flowing time, be preferably 10 seconds following, more preferably 8 seconds following, more preferably below 7 seconds.
In addition, the mobility of the detergent particles group in the application is the mobility of removing after more than 2000 μ m particle.
< method for evaluating quality >
1. oil absorption
In absorbed dose tester (S410, Asahisouken Inc. manufactures), drop into 30 ~ 35g powder, with driving wing 200r/m rotation.With liquid supply speed 4mL/min, drip aqueous nonionogenic tenside (flower king (strain) manufactures EMULGEN 108) therein, determine the point that becomes peak torque.Liquid addition by powder input amount when becoming the point of 70% moment of torsion of point of this peak torque, using it as oil absorption.
In addition, the oil absorption of the detergent particles group in the application is the oil absorption of removing after more than 2000 μ m particle.
2. washing composition yield
The part by weight of detergent particles group between 125 ~ 1000 μ m in the detergent particles group that washing composition yield in the present invention represents to make.
Embodiment
Below, by embodiment, further record, disclose mode of the present invention.This embodiment is only illustration of the present invention, does not have the meaning of any restriction.In following embodiment etc., as long as no special record, use following raw material.
Light ash: median size is 100 μ m(Central Glass Co., Ltd. manufactures, and oil absorption is 0.45mL/g, amount of moisture is 2 % by weight)
Pulverize light ash: median size is the product after 8 μ m(pulverize above-mentioned light ash)
Saltcake: median size is that 200 μ m, four countries change into industry (strain) manufacture " neutral thenardite "
Pulverize saltcake: median size is the product after 10 μ m(pulverize above-mentioned saltcake)
Zeolite: median size is 3.5 μ m, ZEOBUILDER company manufactures
In following examples etc., as the rotary-type tablets press of container, use the 75L rotating cylinder type tablets press (φ 40cm * L60cm) with baffle plate.As two-fluid spray nozzle, use ATMAX Inc. manufacture, model BN90.In addition, as single fluid nozzle, use Spraying Systems Co., Japan manufactures, model UNIJET 8003, as tubule nozzle, uses the nozzle that mouth of pipe footpath is 8.1mm.
Embodiment based on following illustrates in greater detail the present invention.
Embodiment 1
The tensio-active agent that contains anion surfactant is stuck with paste to (R-OSO
3na, C12/C14/C16=64/24/12(weight ratio), amount of moisture is 33 % by weight, and the viscosity at 60 ℃ is about 2Pas, hereinafter referred to as " composition A ") be heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 5.6kg.After stirring 10 seconds, with respect to the above-mentioned light ash of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing), with drop footpath approximately 130 μ m, in 6.5 minutes, add the above-mentioned composition A of 25 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from rotating cylinder type tablets press, discharge detergent particles group 1.
The detergent particles group's 1 who obtains moisture is 6.9%, median size is that 221 μ m, Rosin-Rammler number are 2.05, washing composition yield is 94.6%, volume density is that 543g/L, mobility are that 6.4s, oil absorption are 0.40mL/g.
Embodiment 2
Composition A is heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 4.9kg.After stirring 10 seconds, with respect to the above-mentioned light ash of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing), with drop footpath approximately 130 μ m, in 9.8 minutes, add the above-mentioned composition A of 43 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from rotating cylinder type tablets press, discharge detergent particles group 2.
The detergent particles group's 2 who obtains moisture is 9.1%, median size is that 318 μ m, Rosin-Rammler number are 2.79, washing composition yield is 98.9%, volume density is that 550g/L, mobility are that 6.1s, oil absorption are 0.36mL/g.
Embodiment 3
Composition A is heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 4.2kg.After stirring 10 seconds, with respect to the above-mentioned light ash of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing), with drop footpath approximately 130 μ m, in 13 minutes, add the above-mentioned composition A of 67 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from rotating cylinder type tablets press, discharge detergent particles group 3.
The detergent particles group's 3 who obtains moisture is 11.1%, median size is that 416 μ m, Rosin-Rammler number are 2.44, washing composition yield is 98.9%, volume density is that 624g/L, mobility are that 5.8s, oil absorption are 0.26mL/g.
Embodiment 4
Composition A is heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 3.5kg.After stirring 10 seconds, with respect to the above-mentioned light ash of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing), with drop footpath approximately 130 μ m, in 16.3 minutes, add the above-mentioned composition A of 100 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from rotating cylinder type tablets press, discharge detergent particles group 4.
The detergent particles group's 4 who obtains moisture is 14.8%, median size is that 678 μ m, Rosin-Rammler number are 2.49, washing composition yield is 87.4%, volume density is that 636g/L, mobility are that 6.9s, oil absorption are 0.13mL/g.
Embodiment 5
By method similarly to Example 1, manufacture detergent particles group, to its detergent particles, use electric drying apparatus at 105 ℃, to be dried 2 hours, discharge detergent particles group 5.
The detergent particles group's 5 who obtains moisture is 1.1%, median size is that 208 μ m, Rosin-Rammler number are 1.73, washing composition yield is 87.7%, volume density is that 522g/L, mobility are that 7.1s, oil absorption are 0.43mL/g.
Embodiment 6
By method similarly to Example 2, manufacture detergent particles group, to its detergent particles, use electric drying apparatus at 105 ℃, to be dried 2 hours, discharge detergent particles group 6.
The detergent particles group's 6 who obtains moisture is 1.4%, median size is that 272 μ m, Rosin-Rammler number are 1.98, washing composition yield is 90.9%, volume density is that 519g/L, mobility are that 6.5s, oil absorption are 0.42mL/g.
Embodiment 7
By method similarly to Example 3, manufacture detergent particles group, to its detergent particles, use electric drying apparatus at 105 ℃, to be dried 2 hours, discharge detergent particles group 7.
The detergent particles group's 7 who obtains moisture is 2.1%, median size is that 442 μ m, Rosin-Rammler number are 2.29, washing composition yield is 98.1%, volume density is that 573g/L, mobility are that 6.1s, oil absorption are 0.33mL/g.
Embodiment 8
By method similarly to Example 4, manufacture detergent particles group, to its detergent particles, use electric drying apparatus at 105 ℃, to be dried 2 hours, discharge detergent particles group 8.
The detergent particles group's 8 who obtains moisture is 1.7%, median size is that 651 μ m, Rosin-Rammler number are 2.04, washing composition yield is 98.7%, volume density is that 579g/L, mobility are that 6.6s, oil absorption are 0.15mL/g.
Comparative example 1
Composition A is heated to 60 ℃.Then, at LODIGE stirrer FKM-130D(MATSUBO Corporation, manufacture) in to stir 26kg gently grey.In addition, in chuck, pass into the warm water of 60 ℃.Agitating wing revolution be under the condition that 115r/m, Froude number are 3.7, shears revolution is 3600r/m, stir 10 seconds after, with respect to the above-mentioned light ash of 100 weight parts, use tubule nozzle in 7 minutes, to add the above-mentioned composition A of 25 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from LODIGE stirrer, discharge detergent particles group 9.
The detergent particles group's 9 who obtains moisture is 6.6%, median size is that 128 μ m, Rosin-Rammler number are 0.85, washing composition yield is 50.3%, volume density is that 739g/L, mobility can not be measured.
Comparative example 2
Composition A is heated to 60 ℃.Then, at LODIGE stirrer FKM-130D(MATSUBO Corporation, manufacture) in to stir 22.8kg gently grey.In addition, in chuck, pass into the warm water of 60 ℃.Agitating wing revolution be under the condition that 115r/m, Froude number are 3.7, shears revolution is 3600r/m, stir 10 seconds after, with respect to the above-mentioned light ash of 100 weight parts, use tubule nozzle in 10.5 minutes, to add the above-mentioned composition A of 43 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from LODIGE stirrer, discharge detergent particles group 10.
The detergent particles group's 10 who obtains moisture is 10.0%, median size is that 219 μ m, Rosin-Rammler number are 1.16, washing composition yield is 85.5%, volume density is that 720g/L, mobility are that 6.1s, oil absorption are 0.18mL/g.
Comparative example 3
Composition A is heated to 60 ℃.Then, at LODIGE stirrer FKM-130D(MATSUBO Corporation, manufacture) in to stir 19.5kg gently grey.In addition, in chuck, pass into the warm water of 60 ℃.Agitating wing revolution be under the condition that 115r/m, Froude number are 3.7, shears revolution is 3600r/m, stir 10 seconds after, with respect to the above-mentioned light ash of 100 weight parts, use tubule nozzle in 14.1 minutes, to add the above-mentioned composition A of 67 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from LODIGE stirrer, discharge detergent particles group 11.
The detergent particles group's 11 who obtains moisture is 12.1%, median size coarse to can not measure, Rosin-Rammler number is 1.65, washing composition yield is 4.8%, volume density is that 798g/L, mobility are 8.2s.
Comparative example 4
Composition A is heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 5.6kg.After stirring 10 seconds, with respect to the above-mentioned light ash of 100 weight parts, use single fluid nozzle in 2.2 minutes, to add the above-mentioned composition A of 25 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from rotating cylinder type tablets press, discharge detergent particles group 12.
The detergent particles group's 12 who obtains moisture is 5.1%, median size is that 148 μ m, Rosin-Rammler number are 0.77, washing composition yield is 55.9%, volume density is that 656g/L, mobility are 9.5s.
Comparative example 5
Composition A is heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 4.9kg.After stirring 10 seconds, with respect to the above-mentioned light ash of 100 weight parts, use single fluid nozzle in 3.3 minutes, to add the above-mentioned composition A of 43 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from rotating cylinder type tablets press, discharge detergent particles group 13.
The detergent particles group's 13 who obtains moisture is 10.9%, median size is that 502 μ m, Rosin-Rammler number are 1.25, washing composition yield is 69.5%, volume density is that 642g/L, mobility are that 6.4s, oil absorption are 0.33mL/g.
Comparative example 6
Composition A is heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 4.2kg.After stirring 10 seconds, with respect to the above-mentioned light ash of 100 weight parts, use single fluid nozzle in 4.4 minutes, to add the above-mentioned composition A of 67 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from rotating cylinder type tablets press, discharge detergent particles group 14.
The detergent particles group's 14 who obtains moisture is 13.9%, median size is that 983 μ m, Rosin-Rammler number are 1.46, washing composition yield is 48.7%, volume density is that 784g/L, mobility are 7.2s.
Embodiment 9
The tensio-active agent that contains anion surfactant is stuck with paste to (R-OSO
3na, C12/C14/C16=64/24/12(weight ratio), amount of moisture is 30 % by weight, and the viscosity at 60 ℃ is about 2Pas, hereinafter referred to as " composition B ") be heated to 55 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir 1.73kg and pulverize light ash and 1.63kg saltcake.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing), with drop footpath approximately 130 μ m, in 13.3 minutes, add the above-mentioned composition B of 81 weight parts.After interpolation, further continue to mix within 1 minute, to carry out granulating., with respect to the detergent particles group that obtain of 100 weight parts, add the zeolite of 15 weight parts, further mix 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 15 thereafter.
The detergent particles group's 15 who obtains moisture is 11.0%, median size is that 406 μ m, Rosin-Rammler number are 2.05, washing composition yield is 93.9%, volume density is that 712g/L, mobility are that 6.9s, oil absorption are 0.16mL/g.
Embodiment 10
Composition B is heated to 55 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir the light ash of 1.73kg and 1.63kg and pulverize saltcake.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing), with drop footpath approximately 130 μ m, in 13.3 minutes, add the above-mentioned composition B of 81 weight parts.After interpolation, further continue to mix within 1 minute, to carry out granulating., with respect to the detergent particles group that obtain of 100 weight parts, add the zeolite of 15 weight parts, further mix 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 16 thereafter.
The detergent particles group's 16 who obtains moisture is 13.9%, median size is that 447 μ m, Rosin-Rammler number are 2.17, washing composition yield is 95.5%, volume density is that 629g/L, mobility are that 6.9s, oil absorption are 0.18mL/g.
Embodiment 11
Composition B is heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir 2.8kg and pulverize light ash.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing), with drop footpath approximately 130 μ m, in 20.6 minutes, add the above-mentioned composition B of 150 weight parts.After interpolation, after further lasting mixing is carried out granulating in 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 17.
The detergent particles group's 17 who obtains moisture is 16.1%, median size is that 395 μ m, Rosin-Rammler number are 1.76, washing composition yield is 92.8%, volume density is that 555g/L, mobility are that 6.1s, oil absorption are 0.47mL/g.
Embodiment 12
The polyoxyethylene lauryl ether of the composition B of 92.4 weight parts and 7.6 weight parts (EO21 mole of affixture) is mixed to (hereinafter referred to as " composition C ") and be heated to 55 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 4.2kg.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing) in 15.1 minutes, to add the above-mentioned composition C of 67 weight parts.After interpolation, after further lasting mixing is carried out granulating in 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 18.
The detergent particles group's 18 who obtains moisture is 11.3%, median size is that 480 μ m, Rosin-Rammler number are 1.52, washing composition yield is 79.7%, volume density is that 590g/L, mobility are that 6.3s, oil absorption are 0.29mL/g.
Embodiment 13
Composition C is heated to 55 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir 3.15kg and pulverize light ash.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing) in 18.9 minutes, to add the above-mentioned composition C of 122 weight parts.After interpolation, after further lasting mixing is carried out granulating in 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 19.
The detergent particles group's 19 who obtains moisture is 14.2%, median size is that 698 μ m, Rosin-Rammler number are 2.37, washing composition yield is 72.5%, volume density is that 684g/L, mobility are that 6.6s, oil absorption are 0.17mL/g.
Embodiment 14
The polyoxyethylene lauryl ether sodium sulfate of the composition B of 93 weight parts and 7 weight parts (flower king (strain) manufactures EMULGEN 270J) is mixed to (hereinafter referred to as " composition D ") and be heated to 55 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 4.2kg.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing) in 14.6 minutes, to add the above-mentioned composition D of 67 weight parts.After interpolation, after further lasting mixing is carried out granulating in 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 20.
The detergent particles group's 20 who obtains moisture is 16.5%, median size is that 431 μ m, Rosin-Rammler number are 2.22, washing composition yield is 93.9%, volume density is that 622g/L, mobility are that 6.4s, oil absorption are 0.56mL/g.
Embodiment 15
Composition D is heated to 55 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir 3.5kg and pulverize light ash.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing) in 18.2 minutes, to add the above-mentioned composition D of 100 weight parts.After interpolation, after further lasting mixing is carried out granulating in 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 21.
The detergent particles group's 21 who obtains moisture is 16.0%, median size is that 408 μ m, Rosin-Rammler number are 1.87, washing composition yield is 92.4%, volume density is that 642g/L, mobility are that 6.1s, oil absorption are 0.24mL/g.
Embodiment 16
Composition B is heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir 4.2kg saltcake.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing) in 14.5 minutes, to add the above-mentioned composition B of 67 weight parts.After interpolation, after further lasting mixing is carried out granulating in 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 22.
The detergent particles group's 22 who obtains moisture is 9.6%, median size is that 411 μ m, Rosin-Rammler number are 2.15, washing composition yield is 95.4%, volume density is that 796g/L, mobility are that 6.2s, oil absorption are 0.25mL/g.
Embodiment 17
The detergent particles group who obtains in 100g embodiment 11 17 is dropped in 500mL beaker.With respect to the above-mentioned detergent particles group of 100 weight parts, add the polyoxyethylene lauryl ether (EO21 mole of affixture, hereinafter referred to as " composition E ") of 5 weight parts, use little spoon hand mix to make it oil suction in above-mentioned detergent particles group.Thereafter, the detergent particles group who obtains is dropped in bag, with respect to the above-mentioned detergent particles group of 100 weight parts, the zeolite that adds 5 weight parts carries out 20 times to be mixed, and obtains detergent particles group 23.
The detergent particles group's 23 who obtains median size is that 440 μ m, Rosin-Rammler number are 1.88, washing composition yield is 86.2%, volume density is that 515g/L, mobility are 6.4s.
Embodiment 18
The detergent particles group who obtains in 100g embodiment 11 17 is dropped in 500mL beaker.With respect to the above-mentioned detergent particles group of 100 weight parts, add the composition E of 10 weight parts, use stirring rod hand mix to make it oil suction in above-mentioned detergent particles group., with respect to the detergent particles group that obtain of 100 weight parts, add the zeolite of 10 weight parts, further mix, obtain detergent particles group 24 thereafter.
The detergent particles group's 24 who obtains median size is that 590 μ m, Rosin-Rammler number are 2.96, washing composition yield is 90.2%, volume density is that 640g/L, mobility are 6.8s.
Comparative example 7
The tensio-active agent that contains anion surfactant is stuck with paste to (R-OSO
3na, C12/C14/C16=64/24/12(weight ratio), amount of moisture is 70 % by weight, hereinafter referred to as " composition F ") and be heated to 60 ℃.The state of this paste at 60 ℃ is the state that mobility is very high.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 3.85kg.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing) in 14.6 minutes, to add the above-mentioned composition F of 82 weight parts.After interpolation, after further lasting mixing is carried out granulating in 3 minutes, from rotating cylinder type tablets press, discharge detergent particles group 25.
Detergent particles group 25 coarsenings that obtain, can not evaluate.
Comparative example 8
Polyoxyethylene lauryl ether (flower king (strain) manufactures EMULGEN 106, hereinafter referred to as " composition G ") is heated to 60 ℃.The state of composition G at 60 ℃ is liquid.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 4.93kg.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing) in 9.4 minutes, to add the above-mentioned composition G of 35 weight parts.After interpolation, further continue to mix within 1 minute, to carry out granulating., with respect to the detergent particles group that obtain of 100 weight parts, add the zeolite of 5 weight parts, further carry out mixing for 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 26 thereafter.
Detergent particles group 26 tacks that obtain are high, can not evaluate.
Comparative example 9
Composition G is heated to 60 ℃.Then, in thering is the rotating cylinder type tablets press of baffle plate (revolution 30r/m, Froude number 0.2), stir gently ash of 4.93kg.After stirring 10 seconds, with respect to the above-mentioned powder detergent raw material of 100 weight parts, use two-fluid spray nozzle (it is 0.3MPa that micronize is pressed with air-atomizing) in 9.4 minutes, to add the above-mentioned composition G of 35 weight parts.After interpolation, further continue to mix within 1 minute, to carry out granulating., with respect to the detergent particles group that obtain of 100 weight parts, add the zeolite of 30 weight parts, further carry out mixing for 1 minute, from rotating cylinder type tablets press, discharge detergent particles group 27 thereafter.
The detergent particles group's 27 who obtains moisture is 2.8%, median size is that 138 μ m, Rosin-Rammler number are 1.0, washing composition yield is 59.4%, volume density is that 698g/L, mobility are 12.1s.
The condition of above-described embodiment, comparative example, result are shown in following table.
Table-1
Table-2
Table-3
Table-4
Table-5
In table, 1000 μ m with top grade be more than 1000 μ m in the whole detergent particles groups shared ratio (% by weight) of particle swarm, the 125 μ m product that are less than are the shared ratios (% by weight) of the particle swarm that is less than 125 μ m in whole detergent particles groups.In addition, in table 3 ~ table 5, the amount of zeolite is detergent particles group after tensio-active agent the is stuck with paste mixed processes amount during as 100 weight part.
From embodiment 1 ~ 8, passing through of being obtained by the present invention stuck with paste powder detergent raw material and the tensio-active agent that contains the anion surfactant representing with formula (1) to mix, and can yield obtains well the detergent particles of narrow particle size distribution.
In addition; more known by embodiment 1 ~ 4 and comparative example 1 ~ 3; by using the rotary-type tablets press of container tablets press in addition; and by single fluid nozzle, add, mix the tensio-active agent that contains the anion surfactant representing with formula (1) and stick with paste, thereby size-grade distribution broadens and washing composition yield step-down.
In addition; more known by embodiment 1 ~ 4 and comparative example 4 ~ 6; in the situation that using the rotary-type tablets press of container, by add, mix the tensio-active agent that contains the anion surfactant representing with formula (1) by single fluid nozzle, to stick with paste, size-grade distribution also broadens and washing composition yield step-down.
From embodiment 9,10, in the situation that using Multiple components as powder detergent raw material, also can manufacture well-behaved detergent particles group.Known as described in Example 16, the in the situation that powder detergent raw material being used saltcake not using light ash, also can manufacture well-behaved detergent particles group.From embodiment 11 and 13, in the situation that the weight that tensio-active agent is stuck with paste surpasses the weight of powder detergent raw material, also can manufacture well-behaved detergent particles group.And then, as used as shown in the embodiment 12 ~ 15 of surfactant composition C or D, in the tensio-active agent using is stuck with paste except the anion surfactant that contains formula (1) regulation, also contain in the situation of the anion surfactant beyond the anion surfactant that nonionogenic tenside or formula (1) record, also can manufacture well-behaved detergent particles group.
And then, known as shown in embodiment 17 and 18, by tensio-active agent being stuck with paste to the detergent particles group who obtains after mixed processes, mix with liquid washing agent raw material, can manufacture the detergent particles group of hope.
On the other hand, even known in the situation that having used rotating cylinder type tablets press or two-fluid spray nozzle, also there is the detergent particles group's that can not manufacture hope situation.As comparative example 7 in the situation that the amount of the water of tensio-active agent in sticking with paste is too much, tensio-active agent as comparative example 8 in tensio-active agent is stuck with paste is nonionogenic tenside, in the situation that the anion surfactant of not stipulating containing formula (1) in this pastes can only obtain the manufacture thing of poor quality that can not evaluate as detergent particles group.As shown in comparative example 9, even if add in a large number zeolites in comparative example 8, the detergent particles group's who obtains character also can not meet the scope of hope completely.
The possibility of utilizing in industry
According to the present invention, use the tensio-active agent contain anion surfactant to stick with paste, can yield manufacture well narrow particle size distribution and there is the detergent particles group of necessary granularity.Described detergent particles group can be as the constituent with washing composition etc. such as powder detergent for dress material, automatic tableware.
Claims (19)
1. detergent particles group's a manufacture method, wherein,
Described manufacture method comprises that tensio-active agent sticks with paste mixed processes: with many fluid tips, add and contain following a) composition and b in the powder of powder detergent raw material) the tensio-active agent paste of composition; by the rotary-type tablets press of container, mix; the rotary-type tablets press of described container is dish-type granulators or turns simple type tablets press
A) anion surfactant representing with following formula (1),
R-O-SO
3M (l)
In formula, R represents that carbonatoms is 10～18 alkyl or alkenyl, and M represents alkali metal atom or amine,
B) the above-mentioned a) composition with respect to 100 weight parts is the water of 25～70 weight parts.
2. manufacture method as claimed in claim 1, wherein,
Many fluid tips are two-fluid spray nozzle.
3. manufacture method as claimed in claim 1 or 2, wherein,
The median size of powder detergent raw material is 10 ~ 250 μ m.
4. manufacture method as claimed in claim 1 or 2, wherein,
Powder detergent raw material is the powder detergent raw material that comprises light ash and/or saltcake.
5. manufacture method as claimed in claim 1 or 2, wherein,
With respect to the powder detergent raw material of 100 weight parts, mix the tensio-active agent of 25 ~ 200 weight parts and stick with paste.
6. manufacture method as claimed in claim 1 or 2, wherein,
With respect to the powder detergent raw material of 100 weight parts, mix the tensio-active agent of 25～180 weight parts and stick with paste.
7. manufacture method as claimed in claim 1 or 2, wherein,
With respect to the powder detergent raw material of 100 weight parts, mix the tensio-active agent of 25～160 weight parts and stick with paste.
8. manufacture method as claimed in claim 1 or 2, wherein,
With respect to the powder detergent raw material of 100 weight parts, mix the tensio-active agent of 30～90 weight parts and stick with paste.
9. manufacture method as claimed in claim 1 or 2, wherein,
The content of a) composition in detergent particles group is 10～55 % by weight.
10. manufacture method as claimed in claim 1 or 2, wherein,
The content of a) composition in detergent particles group is 10～45 % by weight.
11. manufacture method as claimed in claim 1 or 2, wherein,
The content of a) composition in detergent particles group is 15～40 % by weight.
12. manufacture method as claimed in claim 1 or 2, wherein,
The content of the nonionogenic tenside in detergent particles group is 0～10 % by weight.
13. manufacture method as claimed in claim 1 or 2, wherein,
Use many fluid tips, the median size in the drop footpath that the tensio-active agent of take is stuck with paste is stuck with paste as 1～300 μ m adds tensio-active agent.
14. manufacture method as claimed in claim 1 or 2, wherein,
Use many fluid tips, the median size in the drop footpath that the tensio-active agent of take is stuck with paste is stuck with paste as 1～2OO μ m adds tensio-active agent.
15. manufacture method as claimed in claim 1 or 2, wherein,
The mean number footpath of powder detergent raw material is 50～200 μ m.
16. manufacture method as claimed in claim 1 or 2, wherein,
Detergent particles group's volume density is 450～1000g/L.
17. manufacture method as claimed in claim 1 or 2, wherein,
Detergent particles group's median size is 150-800 μ m.
18. manufacture method as claimed in claim 1 or 2, wherein,
Also comprise the operation of mixing with liquid washing agent raw material stuck with paste the resulting detergent particles group of mixed processes by tensio-active agent.
19. manufacture method as claimed in claim 1 or 2, wherein,
Also comprise the dry operation by this detergent particles group.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009-263327 | 2009-11-18 | ||
| JP2009263327 | 2009-11-18 | ||
| PCT/JP2010/070595 WO2011062236A1 (en) | 2009-11-18 | 2010-11-18 | Method for producing detergent granules |
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| Publication Number | Publication Date |
|---|---|
| CN102712884A CN102712884A (en) | 2012-10-03 |
| CN102712884B true CN102712884B (en) | 2014-03-12 |
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| CN201080061447.XA Active CN102712884B (en) | 2009-11-18 | 2010-11-18 | Method for producing detergent granules |
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| EP (1) | EP2502981A4 (en) |
| JP (1) | JP2011127106A (en) |
| CN (1) | CN102712884B (en) |
| AU (1) | AU2010320064B2 (en) |
| BR (1) | BR112012011975A2 (en) |
| WO (1) | WO2011062236A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AU2010267108B2 (en) * | 2009-06-30 | 2013-05-16 | Kao Corporation | Method for producing high bulk density detergent granules |
| JP6417116B2 (en) * | 2013-05-31 | 2018-10-31 | 旭化成株式会社 | Polymer electrolyte composition, and polymer electrolyte membrane, electrode catalyst layer, membrane electrode assembly, and solid polymer fuel cell using the same |
| JP6321951B2 (en) * | 2013-12-02 | 2018-05-09 | 花王株式会社 | Process for producing dentifrice granules |
| JP6321958B2 (en) * | 2013-12-18 | 2018-05-09 | 花王株式会社 | Process for producing dentifrice granules |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6072999A (en) * | 1983-09-30 | 1985-04-25 | 花王株式会社 | Manufacture of super concentrated powder detergent |
| DE3413571A1 (en) | 1984-04-11 | 1985-10-24 | Hoechst Ag, 6230 Frankfurt | USE OF CRYSTALLINE LAYERED SODIUM SILICATES FOR WATER SOFTENING AND METHOD FOR WATER SOFTENING |
| EP0506184B1 (en) * | 1991-03-28 | 1998-07-01 | Unilever N.V. | Detergent compositions and process for preparing them |
| JP2525318B2 (en) | 1991-12-29 | 1996-08-21 | 花王株式会社 | Synthetic inorganic builder |
| JP2525342B2 (en) | 1993-06-26 | 1996-08-21 | 花王株式会社 | Synthetic inorganic builder and detergent composition |
| US5565137A (en) | 1994-05-20 | 1996-10-15 | The Proctor & Gamble Co. | Process for making a high density detergent composition from starting detergent ingredients |
| US5516448A (en) | 1994-09-20 | 1996-05-14 | The Procter & Gamble Company | Process for making a high density detergent composition which includes selected recycle streams for improved agglomerate |
| MX9708236A (en) * | 1995-04-27 | 1997-12-31 | Procter & Gamble | Process for producing granular detergent components or compositions. |
| JP3209941B2 (en) | 1997-04-28 | 2001-09-17 | 花王株式会社 | Mixing method and mixing device |
| JP3136117B2 (en) | 1997-04-28 | 2001-02-19 | 花王株式会社 | Mixing device |
| JP2001520273A (en) * | 1997-10-10 | 2001-10-30 | ザ、プロクター、エンド、ギャンブル、カンパニー | Method for producing detergent using high-active surfactant paste containing medium-chain branched surfactant |
| JP2001181691A (en) * | 1999-12-22 | 2001-07-03 | Lion Corp | Vessel rotary type mixing machine and method for producing granular detergent composition |
| JP4339043B2 (en) * | 2003-08-04 | 2009-10-07 | 花王株式会社 | Surfactant-supporting granules |
| JP4088793B2 (en) * | 2004-02-24 | 2008-05-21 | ライオン株式会社 | Nonionic surfactant-containing particles, method for producing the same, and detergent composition |
| CN101001943B (en) * | 2004-08-06 | 2010-05-05 | 花王株式会社 | Process for production of uni-core detergent particles |
| JP4799951B2 (en) * | 2004-10-14 | 2011-10-26 | 花王株式会社 | Method for producing mononuclear detergent particles |
| JP5465872B2 (en) * | 2008-12-15 | 2014-04-09 | 花王株式会社 | Anionic surfactant composition |
| AU2010267108B2 (en) * | 2009-06-30 | 2013-05-16 | Kao Corporation | Method for producing high bulk density detergent granules |
-
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- 2010-11-18 WO PCT/JP2010/070595 patent/WO2011062236A1/en active Application Filing
- 2010-11-18 CN CN201080061447.XA patent/CN102712884B/en active Active
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| EP2502981A4 (en) | 2014-07-23 |
| BR112012011975A2 (en) | 2016-05-10 |
| JP2011127106A (en) | 2011-06-30 |
| CN102712884A (en) | 2012-10-03 |
| WO2011062236A1 (en) | 2011-05-26 |
| AU2010320064A1 (en) | 2012-05-31 |
| AU2010320064B2 (en) | 2014-04-24 |
| EP2502981A1 (en) | 2012-09-26 |
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