CN102459555A - Method for producing high bulk density detergent granules - Google Patents
Method for producing high bulk density detergent granules Download PDFInfo
- Publication number
- CN102459555A CN102459555A CN2010800262184A CN201080026218A CN102459555A CN 102459555 A CN102459555 A CN 102459555A CN 2010800262184 A CN2010800262184 A CN 2010800262184A CN 201080026218 A CN201080026218 A CN 201080026218A CN 102459555 A CN102459555 A CN 102459555A
- Authority
- CN
- China
- Prior art keywords
- manufacture
- crowd
- blapharoplast
- particulate detergent
- detergent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003599 detergent Substances 0.000 title claims abstract description 194
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 58
- 239000008187 granular material Substances 0.000 title abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 123
- 238000000034 method Methods 0.000 claims abstract description 102
- 239000000843 powder Substances 0.000 claims abstract description 72
- 239000004094 surface-active agent Substances 0.000 claims abstract description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000010521 absorption reaction Methods 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims description 71
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 17
- 239000000853 adhesive Substances 0.000 claims description 15
- 230000001070 adhesive effect Effects 0.000 claims description 15
- 239000012530 fluid Substances 0.000 claims description 15
- 239000011812 mixed powder Substances 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 125000002769 thiazolinyl group Chemical group 0.000 claims description 4
- 150000001340 alkali metals Chemical group 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 83
- 238000009826 distribution Methods 0.000 abstract description 12
- 206010040880 Skin irritation Diseases 0.000 abstract description 2
- 239000003945 anionic surfactant Substances 0.000 abstract description 2
- 239000011230 binding agent Substances 0.000 abstract description 2
- 230000036556 skin irritation Effects 0.000 abstract description 2
- 231100000475 skin irritation Toxicity 0.000 abstract description 2
- 239000007858 starting material Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 48
- 239000013543 active substance Substances 0.000 description 36
- 238000001035 drying Methods 0.000 description 35
- -1 polyoxyethylene Polymers 0.000 description 27
- 239000003921 oil Substances 0.000 description 26
- 239000002734 clay mineral Substances 0.000 description 24
- 238000003756 stirring Methods 0.000 description 19
- 239000000243 solution Substances 0.000 description 16
- 239000003795 chemical substances by application Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 14
- 238000004140 cleaning Methods 0.000 description 13
- 239000007788 liquid Substances 0.000 description 13
- 230000000630 rising effect Effects 0.000 description 13
- 239000002253 acid Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 238000012797 qualification Methods 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- 238000005507 spraying Methods 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 7
- 238000010008 shearing Methods 0.000 description 7
- 238000001694 spray drying Methods 0.000 description 7
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910021536 Zeolite Inorganic materials 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000010457 zeolite Substances 0.000 description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 229910000323 aluminium silicate Inorganic materials 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 150000002632 lipids Chemical class 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229920003169 water-soluble polymer Polymers 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 239000010445 mica Substances 0.000 description 4
- 229910052618 mica group Inorganic materials 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000003352 sequestering agent Substances 0.000 description 4
- 235000019832 sodium triphosphate Nutrition 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 241000282326 Felis catus Species 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229920013701 VORANOL™ Polymers 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910021647 smectite Inorganic materials 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 239000000454 talc Substances 0.000 description 3
- 229910052623 talc Inorganic materials 0.000 description 3
- 235000012222 talc Nutrition 0.000 description 3
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 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
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- 230000002546 agglutinic effect Effects 0.000 description 2
- 229910001413 alkali metal ion Inorganic materials 0.000 description 2
- 150000003973 alkyl amines Chemical class 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 230000002596 correlated effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000010981 drying operation Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001983 poloxamer Polymers 0.000 description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 102220207670 rs748889500 Human genes 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000005496 tempering Methods 0.000 description 2
- 229910052902 vermiculite Inorganic materials 0.000 description 2
- 239000010455 vermiculite Substances 0.000 description 2
- 235000019354 vermiculite Nutrition 0.000 description 2
- 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 1
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 1
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-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
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 208000006558 Dental Calculus Diseases 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 241001595840 Margarites Species 0.000 description 1
- MBBZMMPHUWSWHV-BDVNFPICSA-N N-methylglucamine Chemical compound CNC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO MBBZMMPHUWSWHV-BDVNFPICSA-N 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
- 229920002472 Starch Polymers 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 231100000987 absorbed dose Toxicity 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 description 1
- 229910001588 amesite Inorganic materials 0.000 description 1
- 229910052898 antigorite Inorganic materials 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 239000012867 bioactive agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- VNSBYDPZHCQWNB-UHFFFAOYSA-N calcium;aluminum;dioxido(oxo)silane;sodium;hydrate Chemical compound O.[Na].[Al].[Ca+2].[O-][Si]([O-])=O VNSBYDPZHCQWNB-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910001919 chlorite Inorganic materials 0.000 description 1
- 229910052619 chlorite group Inorganic materials 0.000 description 1
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 238000004033 diameter control Methods 0.000 description 1
- 229910001649 dickite Inorganic materials 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
- 238000004090 dissolution Methods 0.000 description 1
- 230000009977 dual effect Effects 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
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052621 halloysite Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910000271 hectorite Inorganic materials 0.000 description 1
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 description 1
- 238000011086 high cleaning Methods 0.000 description 1
- 229910052855 humite Inorganic materials 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052899 lizardite Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 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
- 238000013507 mapping Methods 0.000 description 1
- 229910052630 margarite Inorganic materials 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000273 nontronite Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 235000011837 pasties Nutrition 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
- 229910052628 phlogopite Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052903 pyrophyllite Inorganic materials 0.000 description 1
- 235000012950 rattan cane Nutrition 0.000 description 1
- 229910000275 saponite Inorganic materials 0.000 description 1
- 229910000276 sauconite Inorganic materials 0.000 description 1
- 210000002374 sebum Anatomy 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229940047670 sodium acrylate Drugs 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- IBPRKWGSNXMCOI-UHFFFAOYSA-N trimagnesium;disilicate;hydrate Chemical compound O.[Mg+2].[Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IBPRKWGSNXMCOI-UHFFFAOYSA-N 0.000 description 1
- 238000009966 trimming Methods 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
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
- C11D17/065—High-density particulate detergent compositions
-
- 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
- C11D1/146—Sulfuric acid esters
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/10—Carbonates ; Bicarbonates
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)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
- Glanulating (AREA)
Abstract
Disclosed is a method for producing detergent granules having a bulk density of not less than 650 g/L, which comprises the following steps 1-3. Step 1: a step wherein starting material powders having an oil absorption capacity of not less than 0.4 mL/g are mixed. Step 2: a step wherein water or an aqueous binder solution is added to the powder mixture obtained in step 1 and base granules are prepared using a low-shear granulator. Step 3: a step wherein the base granules obtained in step 2 are mixed with a surfactant composition that contains an anionic surfactant and water. By employing the method, high bulk density detergent granules which generally have extremely low skin irritation, good biodegradability and sharp particle size distribution can be produced with high yield. By having a sharp particle size distribution, a detergent is able to have not only improved appearance but also good fluidity and excellent manufacturability, and can be produced efficiently.
Description
Technical field
The present invention relates to use blapharoplast crowd and the surfactant compsn that contains AS to make the method for manufacture of detergent having high bulk density using population.And then, the present invention relates to contain the detergent composition that this particulate detergent forms.
Background technology
In recent years, people are seeking its economy, environment correspondence etc. to powder detergent composition and method of manufacture thereof.
Support method for making as obtaining one of method of manufacture of powder detergent, have comprising aqueous tensio-active agent supported in tensio-active agent with the operation of particle swarm.In this method for making, hope tensio-active agent support with particle swarm have to aqueous tensio-active agent high support ability.That is, to support with desired the supporting of particle swarm can be by can support a large amount of aqueous tensio-active agents (supporting capacity) and in case the aqueous tensio-active agent that has absorbed can not ooze out and can remain in these 2 factors of granule interior (supporting power) constitutes powerfully to tensio-active agent.And be respectively: support capacity because the reason of clean-up performance will cooperate the tensio-active agent aspect of necessary amount important; And the power that supports is suppressing aspect the oozing out of aqueous tensio-active agent, and the flowability that reduces powder detergent, prevents caking and prevent that aqueous tensio-active agent from moving aspect to container or its surface important.
On the other hand, as tensio-active agent, be combined with the powder detergent of the compound of the AS of being represented by formula (1), having with high cleaning action ability, raising environment correspondence etc. so far is that purpose is various open.
About using such tensio-active agent to support particulate detergent, all discussions have also been carried out so far with particle swarm and promoting agent.For example; In patent documentation 1; Disclose the method for manufacture of particulate detergent, wherein this particulate detergent has used the modulating liquid spraying drying that will contain the water-soluble inorganic salt and the tensio-active agent that obtains supports with particle swarm with by the compound of the AS of formula (1) expression.But, in the manufacturing of this particle swarm, must use spraying drying, from the viewpoint of economy, need not use spray-dired method of manufacture.
On the other hand, for example, disclose method of manufacture with the high density detergent composition of the use AS of non-spray drying process.In patent documentation 2, disclose with the tensio-active agent mashed prod with through the exsiccant detergent materials and come to make continuously the method for detergent composition with high-speed mixer/middling speed mixing machine/drying machine.In patent documentation 3, the method for with high-speed mixer/middling speed mixing machine/trimming device (conditioning apparatus) particulate recycling on one side being made continuously detergent composition with the tensio-active agent mashed prod with through the exsiccant detergent materials is on one side disclosed.But the method for making of patent documentation 2 is difficult to adjust granularity, and the method for making of patent documentation 3 is used the method for making with particulate recycling in order to address this problem, and but is the low method of manufacture of productivity.Therefore, demand more simply yield obtain being necessary the method for making of the high density detergent particle of granularity well.
The prior art document
Patent documentation
Patent documentation 1: the spy opens the 2006-137925 communique
Patent documentation 2: the flat 10-500716 communique of special table
Patent documentation 3: the flat 10-506141 communique of special table
Summary of the invention
Solve the method for problem
Main contents of the present invention relate to:
[1] a kind of volume density is the method for manufacture of the above particulate detergent of 650g/L, and it comprises following operation 1～3:
Operation 1: with oil absorption is the powder stock blended operation more than the 0.4mL/g;
Operation 2: in the mixed powder that obtains through operation 1, add water or adhesive solution, modulate blapharoplast crowd's operation with low shear granulator;
Operation 3: the blapharoplast crowd that will obtain through operation 2 with contain following a) composition and b) the surfactant compsn blended operation of composition,
A): by the represented AS of following formula (1),
R-O-SO
3M (1)
(in the formula, R is that carbonatoms is 10～18 alkyl or thiazolinyl, and M representes alkali metal atom or amine), and
B): with respect to said a) composition 100 weight parts is the water of 25～70 weight parts.
[2] a kind of particulate detergent, its method of manufacture of being put down in writing by above-mentioned [1] obtains; And
[3] a kind of detergent composition, it contains the particulate detergent that the method for manufacture put down in writing by above-mentioned [1] obtains and forms.
Embodiment
The present invention relates to use the surfactant compsn that supports the blapharoplast crowd of surfactant compsn and contain AS by being used to of not containing that spray-dired method obtains, make the method for the good particulate detergent of the yield of the high density detergent particle that is necessary granularity.And then, the present invention relates to provide and contain the detergent composition that this particulate detergent forms.
Through using the blapharoplast crowd that will obtain by the method that does not contain the spraying drying operation of the present invention and carry out the blended method of manufacture by the compound of the AS of formula (1) expression, can yield make well general few to skin irritation, Biodegradable is good and the high density detergent population of narrow diameter distribution.Make narrow particle size distribution, can realize obtaining efficiently not only outward appearance and promote, and the effect of good fluidity, washing composition that productivity is excellent.
In the present invention, blapharoplast is meant that containing oil absorption (Oil-Absorbing Ability) at least is the powder stock more than the 0.4mL/g and the particle of water or adhesive solution.Being preferably in containing the mixed powder that oil absorption is the powder stock more than the 0.4mL/g at least and adding water or adhesive solution, carry out prilling and the particle that obtains with low shear granulator, is the particle that is used to support aqueous surfactant compsn.This particulate aggregate is called the blapharoplast crowd.Detergent granules is to instigate blapharoplast to support the particle that contains tensio-active agent and auxiliary agent etc. that surfactant compsn forms, and particulate detergent is meant its aggregate.Detergent composition is meant and contains particulate detergent; And contain as required the compsn of the detergent ingredients (for example, builder granule, optical dye, enzyme, spices, skimmer, SYNTHETIC OPTICAL WHITNER, bleach-activating agent etc.) that beyond particulate detergent, adds in addition.
Water-solublely be meant that the solubleness for 25 ℃ water is more than the 0.5g/100g, water-insoluble is meant that solubleness for 25 ℃ water is less than 0.5g/100g.
Aqueous surfactant compsn is meant that supporting in the blapharoplast group time be the compsn that contains tensio-active agent of aqueous or pasty state, also comprises the compsn that contains by the AS of formula (1) expression.
<blapharoplast crowd's composition >
1. oil absorption is the above powder stock of 0.4mL/g
As the neccessary composition among the present invention, can enumerate oil absorption is the above powder stock of 0.4mL/g.In this manual, raw material, blapharoplast crowd's etc. oil absorption be meant according to after the method put down in writing of the method for evaluating quality stated and definite value.What the powder stock that has oil absorption and be an above oil absorption of 0.4mL/g was meant that powder inside has a fine pore below the 10 μ m is essentially the porous material, is the material that in this pore, can support tensio-active agent.The upper limit of oil absorption does not have specific qualification, but for example is preferably below the 1.0mL/g.Said powder stock can be to be made up of a kind of composition, also can be to be made up of multiple composition.Through the operation 1 of this powder stock of enforcement mixing, thus the modulation mixed powder.
From granular viewpoint, the median size of this powder stock is preferably 50～250 μ m, further is preferably 50～200 μ m, is more preferably 80～200 μ m.
In addition, from deliquescent viewpoint, preferred water miscible material.As the example of described powder stock, can enumerate the hydrate of the SODA ASH LIGHT 99.2 that burns till sodium hydrogencarbonate and process (for example, Soda Ash Light 99.2min. or Soda Ash Danse), saltcake, tripoly phosphate sodium STPP is dry and the voluminous powder processed etc.From the easy property of operation and the viewpoint that obtains easily, preferred Soda Ash Light 99.2min..
Use as powder stock under the situation of Soda Ash Light 99.2min., the temperature when burning till sodium hydrogencarbonate through adjusting can further improve the ability that supports of tensio-active agent.From supporting the viewpoint of ability, preferred firing temperature is 120～250 ℃, further is preferably 150～220 ℃, is more preferably 150～200 ℃.
As the content of this powder stock, from supporting the viewpoint of ability, be preferably 40～95 weight %, further be preferably 45～90 weight %, be more preferably 50～85 weight %, be more preferably 50～80 weight %.In addition, when regulating above-mentioned the composition, in the particle swarm before carrying out drying process, be preferably 25～80 weight %, be more preferably 30～77 weight %, be more preferably 32～77 weight %, be more preferably 32～73 weight % by drying process.
2. sticker
In the present invention, in mixed powder, add the aqueous solution of water or sticker, through using low shear granulator, with the mixed powder prilling, modulation blapharoplast crowd.Using under the situation of clay mineral as a composition of powder stock, making the compound particles granulation of the powder stock beyond clay mineral and the clay mineral.Under the situation of water, utilize powder stock is dissolved in the cohesiveness that produced in a part of water or the cohesiveness of clay mineral is come prilling.Using under the situation of adhesive solution, because the cohesiveness that can further utilize sticker and produced, so the prilling of being more prone to.
In addition, comprising under the situation of drying process,, can worry that particle intensity reduces, under the situation of using adhesive solution, even can also expect the effect of sticker generation after dry though be accompanied by drying making under the situation of water.Therefore, preferably use adhesive solution.
As sticker, constitute the ability that mutually combines between the particulate composition in the powder stock so long as have to make, and have rapid dissolving and/or dispersive character in water, just there is not special qualification.For example, can enumerate polyoxyethylene glycol, W 166, Voranol EP 2001 and their verivate; Z 150PH and verivate thereof; Water-soluble cellulose derivative (, can enumerate ether compound) as their verivate; Organic polymers such as carboxylic-acid polymkeric substance, starch, carbohydrate; Inorganic polymers such as amorphous silicate etc.
From the viewpoint of cohesiveness with cleaning power, preferred water-soluble cellulose derivative, carbohydrate and carboxylic-acid polymkeric substance are more preferably salt, the polyacrylate of vinylformic acid-maleic acid.As salt, particular certain cancers, sylvite, ammonium salt.In addition,, be preferably 1000～100000, be more preferably 2000～80000 as the weight-average molecular weight of carboxylic-acid polymkeric substance.
The content of sticker among the blapharoplast crowd from the viewpoint of sticker and oil absorption, is preferably 0～35 weight % among the blapharoplast crowd, is more preferably 5～30 weight %, is more preferably 8～20 weight %, is more preferably 10～20 weight %.In addition, regulating through drying process under the situation of said composition, in the particle swarm before carrying out drying, be preferably 0～30 weight %, be more preferably 3～25 weight %, be more preferably 5～17 weight %, further be preferably 7～17 weight %.
Concentration for adhesive solution does not have special qualification, but because particle diameter when prilling receives the considerable influence that volume caused of adhesive solution, so preferably decide concentration according to the amount and the desirable grain diameter of the sticker of necessity.
3. clay mineral
Clay mineral has laminate structure, and its interlayer can support aqueous tensio-active agent.Therefore, cooperate clay mineral, in the capacity that supports that increases aqueous tensio-active agent, improve the power that supports as a composition of powder stock.
In addition, because clay mineral is brought into play cohesiveness through containing water, therefore, also can control the particle diameter of blapharoplast through adjusting its use level.
As such clay mineral; For example, can lift talcum, pyrophyllite, smectite (saponite, hectorite, sauconite, humite, polynite (Montmorillonite), beidellite, nontronite etc.), vermiculite, mica (phlogopite, blotite, zinnwaldite, white mica, palagonite, celedonite, glaukonine etc.), chlorite (clinochlore, chamosite, nepouite, manganchlorite, mackensite, donbassite etc.), brittle mica (xanthophyllite, margarite etc.), thulite, serpentine minerals (antigorite, lizardite, chrystile, amesite, cronstedtite, berthierine, noumeite etc.), kaolin mineral (kaolinite, dickite, nakrite, halloysite etc.) etc.Wherein, from the viewpoint of flexibility, preferably talc, smectite, swelling property mica, vermiculite, chrystile, kaolin mineral etc. are more preferably smectite, further preferred polynite.These can use separately also and can appropriate combination use more than 2 kinds.
In addition, from tensio-active agent support can viewpoint, preferably will be by the clay mineral of following general formula (A) expression staple as clay mineral.：
[Si
8(Mg
aAl
b)O
20(OH)
4]
X-·Me
X+ (A)
At this, a, b and x are 0＜a≤6,0＜b≤4, x=12-2a-3b, and Me is from Na, K, Li, Ca1/2, Mg1/2 and NH
4Middle at least a kind of ion selecting.
As clay mineral by said general formula (A) expression; Can lift " ROUNDROSIL DGA212 ", " ROUNDROSIL PR414 ", " ROUNDROSIL DG214 ", " ROUNDROSIL DGA Powder ", " EXM0242 ", " the Fulasoft-1 powder " of
manufactured; " the DETERSOFT A " of LAVIOSA manufactured, " DETERSOFT GIS ", " DETERSOFT GIB ", " DETERSOFT GISW ", the pure wilkinite of CSM manufactured, standard wilkinite, high-quality wilkinite etc.In the material of lifting as the example of described clay mineral, though there is the granule type clay mineral that adds the granulation of sticker composition, the addition that needs only this sticker composition does not damage effect of the present invention yet.
Use in the present invention under the situation of the above-mentioned clay mineral of lifting, from granular viewpoint, preferably its form is Powdered, so long as the granulation thing preferably is being crushed to suitable granularity in advance.As the broken kibbler that can utilize, can lift hammer mill impact crushers such as (hammer crusher), atomizer (atomizer), needle mill impact grinders such as (pin mill), wash away shearing primary crusher such as mill (flush mill) etc.These can carry out single job, also can carry out multi-pass operations with kibbler of the same race or not of the same race.
Median size as clay mineral is preferably below the 100 μ m, is more preferably below the 50 μ m, is more preferably below the 30 μ m.
In addition; By supporting power and deliquescent viewpoint is set out; In the clay mineral by general formula (A) expression; The mol ratio [(Na+K+Li)/(Ca+Mg)] of the total of the total of alkalimetal ion (Na ion, K ion, Li ion) and alkaline-earth metal ion (Ca ion, Mg ion) is preferably more than 1.0, further is preferably more than 1.5, is more preferably more than 2.0.
For the high clay mineral of ratio that obtains alkalimetal ion,, when making clay granulation thing, can add an alkali metal salt and modulate if natural article can be selected the place of production.In addition, if synthetics can be come modulation arbitrarily through known method.
4. moisture
Blapharoplast crowd of the present invention can be contained the moisture of employed appropriate amount in manufacturing process.From improving the viewpoint that this particle swarm supports the capacity of surfactant compsn, the amount of moisture of measuring with the infrared rays moisture meter is preferably few more good more, is preferably below the 15 weight %, is more preferably below the 10 weight %, is more preferably below the 5 weight %.
5. other composition
In addition, in blapharoplast crowd of the present invention, even lifted in above-mentioned 1～4 beyond material, also can be as required and proper fit.But from supporting the viewpoint of ability, the use level of these materials is preferably below the 20 weight %, is more preferably below the 10 weight %, is more preferably below the 5 weight %.The examples of substances that can cooperate is as follows.
Sequestrant
In order to suppress the obstruction cleaning function that metals ion produces, can cooperate sequestrant.As water-soluble chelator, so long as keep the material of metals ion interdiction capacity, just there is not special regulation, can use crystallized silicon hydrochlorate, tri-polyphosphate, orthophosphoric acid salt, pyrophosphate salt etc.Wherein, preferred crystallized silicon hydrochlorate and tri-polyphosphate.For the water-insoluble sequestrant, from the viewpoint of the dispersiveness water, the median size of preferred particle is 0.1～20 μ m.As suitable water-insoluble sequestrant, can lift the crystallinity aluminosilicate, A type zeolite, P type zeolite, X type zeolite etc. are for example arranged, from the viewpoint of metals ion interdiction capacity and economy, preferred A type zeolite.
Water-soluble inorganic salt
In order to improve the ionic strength of washings, the effect of raising sebum dirt washing etc. is preferably added water-soluble inorganic salt.
So long as favorable solubility brings dysgenic material can for cleaning power, just there is not special regulation.For example, can enumerate an alkali metal salt with sulfate radical, inferior sulfate radical, ammonium salt etc.
Wherein, preferably use the high sodium sulfate of ion degree of ionization, S-WAT, vitriolate of tartar as vehicle.In addition, from improving the viewpoint of dissolution rate, preferably with sal epsom and usefulness.
The water-insoluble vehicle
So long as the good dispersibility in water does not have dysgenic material to cleaning power, just there is not special qualification.For example, can lift crystallinity or unbodied aluminosilicate and silicon-dioxide, silicate hydrate compound etc.From the viewpoint of the dispersiveness water, the median size of preferred primary particle is 0.1～20 μ m.
Other ancillary component
Can lift optical dye, pigment, dyestuff etc.
In addition, for the median size of said composition can through after the method put down in writing in the measuring method of the rerum natura stated measure.
The method of manufacture of particulate detergent of the present invention comprises following operation 1～3.Modulate the blapharoplast crowd through operation 1 and operation 2, modulate particulate detergent through operation 3.
<blapharoplast crowd's method for making >
Blapharoplast crowd of the present invention obtains through following method modulation; Said method does not comprise the spraying drying operation; But comprise stirring and perhaps mix the operation that oil absorption is at least the above powder stock of 0.4mL/g; And in the mixed powder that obtains, add water or adhesive solution, come granular operation with low shear granulator.
1. operation 1
Mixing oil absorption is in the operation of the powder stock more than the 0.4mL/g, so long as can just can adopt any method basically with these material uniform mixing.For example, can be employed in the low shear granulator of using in the operation 2 and mix, also can use in advance after other mixing machine mixing, be transferred to again in the low shear granulator.As this other mixing machine that in powder mixes, uses, for example can lift rotary drum mixer (rotary drum mixer), pan type mixer (pan mixer), ribbon mixer (ribbon mixer), nauta mixer (Nauta Mixer), Shugi mixing machine,
mixing machine, high-speed mixer etc.
At this, as clay mineral content,, be preferably 0～45 weight % from supporting the viewpoint of ability and particle diameter control, be more preferably 0～40 weight %, be more preferably 0～35 weight %, further be preferably 0～30 weight %.In addition, after prilling, can carry out drying according to hope; But be adjusted into through such drying process under the situation of said composition; In the particle swarm before carrying out drying process, be preferably 0～40 weight %, further be preferably 0～35 weight %; Be more preferably 0～30 weight %, be more preferably 0～25 weight %.
In addition, the weight ratio of clay mineral and powder stock (clay mineral/powder stock) is preferably 0/1～0/30, is more preferably 0/1～0/20, is more preferably 0/2～0/20.
2. operation 2
Operation 2 is modulated blapharoplast crowd's operation in the mixed powder that is obtained by operation 1, adding water or adhesive solution with low shear granulator.In this operation, generate the particle of the slow agglutinative structure of powder stock.In addition, operation 1 can also be carried out with operation 2 simultaneously.
As low shear granulator used in this operation, can be to give particle with strong shearing but do not produce big densification result's device.For example; Even in perpendicular type that possesses the main wing that can apply high shear and the broken wing originally or horizontal type tablets press; Hang down through Froude number (Froude number) with being provided with and to suppress densification, thereby can in granule manufacture of the present invention, utilize rotating speed or following record.That is, in the low shear granulator in this manual,, also comprise the tablets press that can pass through the operation of reduction shearing forces such as setting operation condition even can give the tablets press of particle with high shear.
As the low tablets press of shearing; Support the viewpoint of ability from easy prilling and raising; Preferably carry out the rotary-type tablets press of granular container, wherein be more preferably pan-type pelletizer (pan granulator) or rotary drum granulator (rotary drum granulator) through the rotation of body main body section.These devices can use any means in batch-type, the continous way.In addition, from powder property and the blended viewpoint of solid-liquid, the plate of preferably placing obstacles is assisted the mixing of disc type or rotary drum.
In addition, in order to use as low shear granulator, from support can viewpoint, preferably the Froude number with the tablets press of following formula definition is set at below 1.0, is more preferably below 0.8, further is preferably below 0.6, is more preferably below 0.4.
Froude number: Fr=V
2/ (R * g)
V: rotating speed [m/s]
R: the radius of the circumference from the rotation center to the whirl [m]
G: universal gravity constant [m/s
2]
From to mixed powder, evenly adding the viewpoint of water or adhesive solution, preferably the Froude number with tablets press is set at more than 0.001, further is preferably more than 0.005, is more preferably more than 0.01, more further is preferably more than 0.05.
In addition, in perpendicular type that possesses the main wing and the broken wing or horizontal type tablets press, V and R use the value of main shaft, are carrying out in granular pan-type pelletizer or the rotary drum granulator through the rotation of body main body section, and V and R use the value of body main body section.In addition, in possessing the pan-type pelletizer of the broken wing, V and R use the value of the broken wing.
In the present invention, preferably water or adhesive solution homodisperse are added.As the method that is used for this purpose, for example, the method with such liquid component miniaturization such as the multithread body nozzle that uses a fluid nozzle and second fluid nozzle is arranged.
Multithread body nozzle is that liquid component and micronize are passed near the spray nozzle front end portion through stream independently with gas (air, nitrogen etc.), and the nozzle of hybrid fine particlesization, can use second fluid nozzle, three fluid tips, four fluid tips etc.In addition, liquid component and micronize be with the mixing portion of gas, can be in spray nozzle front end portion the blended internal mix type, or outside spray nozzle front end portion any in the blended external mix type.
In the present invention, preferably use multithread body nozzle, be more preferably the use second fluid nozzle adding after the liquid component fine dropletsization.As such multithread body nozzle, for example can use second fluid nozzle ((strain) ATOMAX manufacturing), four fluid tips (the rugged motor of rattan (strain) manufacturing) of round second fluid nozzle of wide-angle (Spraying Systems (Japan) (strain) manufacturing) and solid cone (full cone) type etc.
In addition, improve in hope under the situation of interpolation speed of sticker, uses a plurality of such a fluid or multithread body nozzles, also have the effect of raising interpolation speed in the miniaturization of keeping drop.
Through using such method,, improve productive rate and obtain the blapharoplast crowd of narrow particle size distribution even also can homodisperse in full-bodied adhesive solution.
In this operation, can further make resulting blapharoplast crowd exsiccant operation.Through the operation of being correlated with, can increase the intragranular space that constitutes the blapharoplast crowd, and further improve blapharoplast crowd's the capacity that supports.
From the viewpoint that the capacity that supports that suppresses to cause owing to the particulate disintegration reduces, preferably do not apply the drying mode of strong shearing force as much as possible.For example, in batch-type, can lift in the container of packing into,, in continous way, can lift fluid bed dryer or rotary drier, vapour pipe drying machine etc. with method of batch-type fluidised bed drying etc. with electric drying apparatus or hot air dryer exsiccant method.
For drying temperature, from the viewpoint of rate of drying, be preferably more than 80 ℃, further be preferably more than 120 ℃, be more preferably more than 150 ℃, be more preferably more than 180 ℃.In addition, using under the situation of organic binder bond as sticker, the viewpoint from the decomposition that suppresses sticker is preferably below 300 ℃, further is preferably below 250 ℃, is more preferably below 220 ℃.
<blapharoplast crowd's rerum natura >
Blapharoplast crowd of the present invention is at least the particle swarm of the slow agglutinative structure of powder stock more than the 0.4mL/g for oil absorption.Therefore, 2 that have little space (the for example space below the 10 μ m) in big space between (1) powder stock, (2) powder stock support the site.Wherein (1), (2) both with supporting big influence can be arranged all for supporting capacity, and (1) has big influence for the speed of supporting, can through regulate these 2 support the site obtain having desirable support can the blapharoplast crowd.
In addition, under the situation that cooperates clay mineral, because also can support aqueous surfactant compsn, so be expected to improve the power that supports at its interlayer.
From the viewpoint of the capacity that supports of guaranteeing aqueous surfactant compsn and the viewpoint of guaranteeing to support the high volume density after the aqueous surfactant compsn; Blapharoplast crowd's of the present invention volume density is preferably 400～550g/L, further is preferably 400～500g/L.Blapharoplast crowd's of the present invention lower volume density is considered to that prilling realizes through carrying out with aforementioned low shear granulator.
In addition; One-tenth mealiness and deliquescent viewpoint when use contains the detergent particles crowd's who among the blapharoplast crowds, supports aqueous surfactant compsn and form detergent composition; Median size as the blapharoplast crowd; Be preferably 140～600 μ m, be more preferably 200～500 μ m, be more preferably 200～400 μ m.
From the viewpoint of the allowed band that increases aqueous surfactant compsn use level, the oil absorption of the aqueous surfactant compsn of preferred substrate particle swarm is more than the 0.4mL/g, is more preferably more than the 0.45mL/g, is more preferably more than the 0.5mL/g.The blapharoplast crowd's of the present invention higher oil absorption of ratio is considered to that prilling realizes through carrying out with said low shear granulator.
In addition, the oil absorption of said volume density, mean particle size, aqueous surfactant compsn, amount of moisture can through after the method put down in writing in the physical property measurement method stated measure.
[composition in the surfactant compsn]
By formula (1): R-O-SO
3In the formula of the AS that M representes, R is that carbonatoms is 10～18, to be preferably carbonatoms be 12～16 alkyl or thiazolinyl.As M, alkali metal atoms such as preferred Na, K; Amine such as monoethanolamine, diethylolamine, from the viewpoint of the cleaning power of detergent composition, preferred Na, K.
[rerum natura of surfactant compsn]
Contain surfactant compsn by the water of the AS of formula (1) expression and specified amount; Viewpoint from the operability made; In the use temperature scope of this surfactant compsn; The viscosity of this surfactant compsn is below the 10Pas, is preferably to hope that it has the TR that can reach below the 5Pas.As such TR, from the viewpoint of the stability of surfactant compsn, be preferably existence to 70 ℃, be more preferably existence to 60 ℃.At this, viscosity can be passed through coaxial dual round tube type rotational viscosimeter, and (HAAKE makes, transmitter: be to measure under 50 [l/s] to try to achieve in velocity of shear SV-DIN).
The surfactant compsn that in operation 3, uses has bigger variation according to its viscosity of water ratio.For example; In with alkali cpd and a) acid precursor of composition regulates through the amount of moisture of used alkali cpd in the modulometer surface-active agent, thereby obtains desirable water ratio; That is, preferred regulate have hope the surfactant compsn of viscosity.If usually known this surfactant compsn is being to contain under 100 weight parts under the situation of water of 25～70 weight parts (water ratio of this surfactant compsn is about 20～40%) with respect to a) composition; Viscosity can reduce; Simple to operate; Therefore, the moisture of preferably adjusting surfactant compsn in the present invention is in this scope.As the scope of the amount of water in tensio-active agent, from the viewpoint of operation, a) composition with respect to 100 weight parts is preferably 30～70 weight parts, is more preferably 35～65 weight parts.
In addition, a) acid precursor of composition is very unstable decomposes easily, and therefore, preferred modulation becomes can suppress its decomposition.Inflation method does not have special qualification, can use known method.For example, can use annular reactor, remove neutralization heat, note the temperature control of the acid precursor and the surfactant compsn of composition simultaneously with heat exchanger etc.TR during as manufacturing is 30～60 ℃, as the storage temperature range after making, can enumerate below 60 ℃.In addition, during use, can heat up, use this surfactant compsn according to necessity.
In addition, from the viewpoint that suppresses to decompose, resulting this anionic surfactant compositions preferably has superfluous basicity.
In addition; In the surfactant compsn that in operation 3, uses, add the pH buffer reagent that obtains, discoloring agent etc. when the by product saltcake that generates when unreacted alcohol or unreacted Voranol EP 2001, neutralization reaction in the time of also can containing the acid precursor of making a) composition, neutralization reaction.
In addition, a) content of composition in the resulting particulate detergent of the present invention from cleaning power and deliquescent viewpoint, is preferably the scope of 10～45 weight %, is more preferably 15～40 weight %.
In surfactant compsn, can use a) composition separately as tensio-active agent, also can mix the use nonionogenic tenside.Have under the situation of the nonionogenic tenside of fusing point below 30 ℃ in use especially; Preferred and to use effect, fusing point with the fusing point that improves tensio-active agent be that 45～100 ℃ and molecular weight are 1,000～30,000 water-soluble nonionic organic cpds (below, be called fusing point rising agent) or its aqueous solution.And, for example can lift polyoxyethylene glycol, W 166, Voranol EP 2001, Pluronic type nonionogenic tenside etc. as the fusing point rising agent of using in the present invention.In addition, also can be according to purpose and with amphoterics and cats product.In addition; The viewpoint of the dispersiveness of particulate detergent from improve cryogenic water; Can use the AS AS in addition by formula (1) expression of polyoxyethylene alkyl ether sulfate salt and sulfonated alkylbenzene etc.; Its amount in particulate detergent is in the scope of 0～10 weight %, is more preferably 0～5 weight %, is more preferably 0～3 weight %.Specifically, be more preferably at the AS AS in addition that contains nonionogenic tenside and/or represent in the surfactant compsn of operation 3 by formula (1).In the case, the amount of relevant composition is preferably 0.1～10 weight % in the particulate detergent, is more preferably 0.2～5 weight %, further is preferably 0.5～3 weight %.
Further, can and use soap in order to obtain defoaming effect.
As nonionogenic tenside, can lift polyoxyethylene polyoxypropylene glycol, polyoxyethylene alkyl amine, higher fatty acid alkylolamide, alkyl-glucoside, methyl glucamine, oxidation of alkyl amine of polyxyethylated or alkene ether, polyxyethylated or thiazolinyl phenyl ether, polyoxyethylene polyoxypropylene alkyl or alkene ether, trade mark Pluronic representative etc.Wherein, nonionogenic tenside that preferred hydrophilic is high and the formation that when mixing with water, generates liquid crystal can be hanged down the nonionogenic tenside that does not perhaps generate liquid crystal, are more preferably polyoxyalkylene alkyl or alkene ether.Be preferably ethylene oxide (the following EO of the being) affixture of alcohol, the EO affixture and propylene oxide (following PO) affixture of other alcohols.As the addition order, the affixture of addition EO after the preferred affixture that uses addition PO after addition EO, the addition PO, or the affixture of random addition EO and PO, but as the affixture with the addition order that is more preferably; For after block addition EO, block addition PO again, the further material of representing by following general formula of block addition EO; Wherein, The relation of relevant preferred average addition mole number is X＞0, Y＞0, X+Y+Z=6～14, X+Z=5～12, Y=1～4.
R-O-(EO)
X-(PO)
Y-(EO)
Z-H
[in the formula, R is an alkyl, is preferably alkyl or thiazolinyl, and EO representes that ethenoxy group, PO represent oxypropylene group, and X, Y and Z represent average addition mole number respectively.]
From improving cleaning power, the people's that chokes when improving anti-anti-caking and being suppressed to powder viewpoint; The use level of nonionogenic tenside preferably is the scope of 0～10 weight % in the detergent particle crowd in the particulate detergent; Be more preferably 0～5 weight %, be more preferably 0～3 weight %.
With surfactant compsn and blapharoplast crowd blended the time, can add the powder raw material beyond the said powder stock according to expection, as 100 weight parts of addition, preferably add 0～150 weight part with respect to this particle swarm.As this powder raw material, for example can lift the crystallized silicon hydrochlorate of aluminosilicate, PREFEED (TOKUYAMA SILTECH manufactured) etc. etc.
< rerum natura of particulate detergent >
Manufacturing method according to the invention, the particulate detergent that can obtain having the defined characteristic.The particulate detergent that obtains through described method of manufacture of the present invention also is contained among the present invention.The preferred rerum natura of the resulting particulate detergent of the present invention is described below.
Volume density is more than the 650g/L, to be preferably 650～1000g/L, is more preferably 650～950g/L, further is preferably 650～900g/L.Median size is preferably 150～600 μ m, is more preferably 180～550 μ m, is more preferably 250～500 μ m.
In addition, said volume density, median size can through after the method put down in writing of the measuring method of the rerum natura stated measure.
In addition, as the index of the preferred size-grade distribution of particulate detergent of the present invention, can use the Rosin-Rammler number.The calculating of Rosin-Rammler number can be used following formula.
log(log(100/R(Dp)))＝nlog(Dp/De)
R (Dp): the cumulative percentage [%] of the powder that particle diameter Dp μ m is above
Dp: particle diameter [μ m]
De: particle property number [μ m]
N:Rosin-Rammler number [-]
It is narrow more that Rosin-Rammler counts the high more expression size-grade distribution of n.Be preferably more than 1.0 as n, be more preferably more than 1.3, be more preferably more than 1.5, be more preferably more than 1.8, more further be preferably more than 2.0.
As the yield of particulate detergent preferred size of the present invention, be the ratio of the particle of 250～500 μ m as sieve aperture, be preferably more than 35%; Be more preferably more than 40%; Be more preferably more than 45%, be more preferably more than 50%, further be more preferably more than 60%.In addition, be the proportion of particles of 125～500 μ m as sieve aperture, be preferably more than 45%, be more preferably more than 50%, further be preferably more than 55%, be more preferably more than 60%, further be more preferably more than 70%.
As the amount of moisture of particulate detergent of the present invention, cooperate a) viewpoint of composition from height, preferably few more good more.Specifically, when measuring the amount of moisture of particulate detergent with the infrared rays moisture meter, preferably its amount of moisture is below the 20 weight %, is more preferably below the 15 weight %, is more preferably below the 10 weight %, more further is preferably below the 5 weight %.
< method for making of particulate detergent >
Obtain the suitable method for making of particulate detergent, comprise following operation 3, further also can comprise operation 4 or operation 5 as required.
3. operation 3
This operation be with operation 2 resulting blapharoplast crowds with below contain a) composition and b) the surfactant compsn blended operation of composition.
In method of manufacture of the present invention, a) composition is the AS by formula (1) expression, and b) composition is to be 25～70 weight parts, to be preferably the water of 25～65 weight parts with respect to said a) composition 100 weight parts.
And in this operation, can use the blapharoplast crowd who obtains in the operation 2 at least.That is, in this operation, can be with other particle swarm with the ability that supports tensio-active agent, the particle swarm and this blapharoplast crowd and the usefulness that for example obtain through other methods such as spray-drying processes.In addition, and the situation of usefulness under, can this blapharoplast crowd be handled as the blapharoplast crowd with the mixture of the particle swarm that obtains through other method.
As this blapharoplast crowd's among the blapharoplast crowd ratio, from the viewpoint of oil absorption, be preferably more than the 50 weight %, be more preferably more than the 70 weight %, be more preferably more than the 90 weight %.
3-1. operation 3
In this operation,, tensio-active agent is supported on the blapharoplast crowd through blapharoplast crowd and surfactant compsn are mixed.As method involving, for example can enumerate the mixing machine that uses batch-type or continous way, with blapharoplast crowd and surfactant compsn method of mixing.At this; Under the situation of carrying out,, can use after (1) first blapharoplast crowd that in mixing machine, packs into as the method for in mixing machine, feeding with batch-type; Add surfactant compsn again; (2) repeat at every turn in mixing machine, to add on a small quantity blapharoplast crowd and surfactant compsn, pack blapharoplast crowd's a part into after the mixing machine (3), repeats each a small amount of method of adding remaining blapharoplast crowd and surfactant compsn etc. again.
When tensio-active agent being added among the blapharoplast crowd, the use level of tensio-active agent is many more, and interpolation speed is important more.Specifically, preferably with the interpolation speed setting of surfactant compsn below blapharoplast crowd's speed of oil absorption.Through implementing to add according to such interpolation speed; Can make the blapharoplast crowd can both carry out the oil suction of surfactant compsn in inside more; Its result can suppress the aggegation of the detergent granules that the tackiness owing to tensio-active agent causes, and makes the size-grade distribution of resulting particulate detergent narrow.
Concrete interpolation speed as this surfactant compsn; With respect to this blapharoplast crowd 100 weight parts; Be preferably 35 weight parts/minute below; Be more preferably 20 weight parts/minute below, be more preferably 10 weight parts/minute below, further be more preferably 7.5 weight parts/minute below.
As the addition of the surfactant compsn that in the blapharoplast crowd, adds, for example,, be preferably more than 30～100 weight parts with respect to blapharoplast crowd 100 weight parts.Viewpoint from cleaning power with respect to blapharoplast crowd 100 weight parts, is preferably more than 30 weight parts, is more preferably more than 40 weight parts, is more preferably more than 50 weight parts.In addition,,, be preferably below 100 weight parts, be more preferably below 80 weight parts, be more preferably below 60 weight parts with respect to blapharoplast crowd 100 weight parts from deliquescent viewpoint.
As preferred mixing device, specifically can lift following device.Under the situation of carrying out, be preferably the device of following (1)～(3) with batch-type.Have (1) Henschel (Henschel) mixing machine (manufacturing of Mitsui three pond chemical industry machines (strain)), high-speed mixer (dark river industry (strain) is made), vertical tablets press (Vertical Granulator) ((strain) Powrex manufacturing),
mixing machine (the Matuzaka skill is ground (strain) and made), ploughshare mixing machine (Ploughshare Mixer) (Pacific Ocean machine worker (strain) manufacturing), spy to drive the mixing device of flat 10-296064 communique record, the spy drives the mixing device of flat 10-296065 communique record etc.; (2) ribbon mixer (day and mechanical industry (strain) are made), batch kneading machine (Batch Kneader) (assistant bamboo chemical machinery industry (strain) is made), Ribocone (the former making manufacturing in (strain) great river) etc.; (3) nauta mixer (HOSOKAWA MICRON (strain) manufacturing), SV mixing machine (Shinko Pantec (strain) manufacturing) etc.Because the operation of stating after can in same device, carrying out 4; So the viewpoint of the simplification of slave unit is set out, mixing device, the spy that preferred
stirrer, ploughshare mixing machine, spy open flat 10-296064 communique record in described mixing machine drives the mixing device of flat 10-296065 communique record etc.Wherein, Because special mixing device, the spy who opens flat 10-296064 communique record opens humidity and temperature that the mixing device put down in writing in the flat 10-296065 communique can be regulated mixture through ventilation, so be preferred from the viewpoint of the disintegration that suppresses the blapharoplast crowd.In addition,, also preferably strong shearing force can be do not applied, the mixing device of the blended nauta mixer, SV mixing machine, ribbon mixer etc. of powder and liquid can be carried out from the viewpoint of the disintegration that can suppress the blapharoplast crowd.
In addition, also can use the device of successive type that blapharoplast crowd and surfactant compsn are mixed.In addition, as the device of successive type, can lift FLEXOMIX ((strain) Powrex manufacturing), Turbulizer (HOSOKAWA MICRON (strain) manufacturing) etc.
In addition; In this operation; Under the situation of using nonionogenic tenside; Preferably with fusing point rise agent or its aqueous solution before the interpolation of surfactant compsn, surfactant compsn add in, in the interpolation way of surfactant compsn or surfactant compsn add after adding, perhaps add in the surfactant compsn in advance and add.Can suppress the anti-caking of particulate detergent, tensio-active agent exudative in the particulate detergent through adding fusing point rising agent.In addition, as these fusing point rising agent, can use the same material of material of example shown in the fusing point rising agent in the composition with said particulate detergent.With respect to blapharoplast crowd 100 weight parts, the usage quantity of fusing point rising agent is preferably 0.5～8 weight part, is more preferably 0.5～5 weight part, is more preferably 1～3 weight part.Aggegation, high speed solvability and the viewpoint that suppresses exudative and anti-caking, preferably this scope between the particle of the detergent granules that from suppress particulate detergent, contains.As the addition means of fusing point rising agent, add through mixing with arbitrary method with tensio-active agent in advance, perhaps after the interpolation of tensio-active agent, add fusing point rising agent again, this is favourable for the exudative and anti-caking that suppresses particulate detergent.
Temperature in the mixing machine in this operation is preferably adjusted it so that can suppress the decomposition of this AS, and the TR during as manufacturing is preferably 30～60 ℃, and the storage temperature range as after making is preferably below 60 ℃.
Be used to obtain the batch-wise mixing time of suitable particulate detergent, and the average retention time in the mixing of continous way, be preferably 1～30 minute, be more preferably 2～25 minutes, be more preferably 3～20 minutes.
In operation 3, also can under ventilation, carry out the mixing of blapharoplast crowd and surfactant compsn.More specifically, in operation 3, in the interpolation of each raw material and/or in mixing, can enumerate the operation of the gases such as bubbling air of in the tempering tank of mixing device, blowing.Through carrying out relating operation, the blapharoplast crowd can further deliver surfactant compsn, and resulting particulate detergent can higher matching surface surfactant composition.
As the reason that reaches such effect, be estimated as through carrying out relating operation, remove the moisture of existing surfactant compsn on blapharoplast crowd's the surface.Its result can reduce the tackiness of the particulate detergent of gained, suppresses the aggegation of particulate detergent, and it is narrow that the size-grade distribution of resulting particulate detergent also becomes.
As the condition of air-supply, for example the temperature of the gas of air-supply is preferably 10～65 ℃, is more preferably 30～60 ℃, is more preferably 50～60 ℃.
As air output, with respect to these particulate detergent 100 weight parts, be preferably 1～15 weight part/minute, be more preferably 2～10 weight parts/minute, be more preferably 3～8 weight parts/minute.
Before the interpolation of surfactant compsn, in its interpolation, it adds in the way or it can add powder surface promoting agent and/or powder auxiliary after adding.Through adding powder auxiliary, can control the particle diameter of particulate detergent, can also reach the purpose that improves cleaning power in addition.Under the situation of the acid precursor that adds AS, from promoting the viewpoint of neutralization reaction, the powder auxiliary that is alkalescence in the interpolation before of this acid precursor of interpolation is more effective.In addition, be meant the powder cleaning power reinforcer except that tensio-active agent, specifically, be meant that zeolite, Citrate trianion etc. show that metals ion blocks the base of ability in this said powder auxiliary; Yellow soda ash, salt of wormwood etc. show the base of alkali ability; Crystal type silicate etc. has the base that metals ion blocks ability alkali ability simultaneously; Other sodium sulfate etc. improve the base of ionic strength etc.
At this,, can the spy be opened flat 5-279013 communique the 3rd hurdle the 17th row (the crystallized silicon hydrochlorate that burns till under preferred 500～1000 ℃ as crystal type silicate.), the spy opens flat 7-89712 communique the 2nd hurdle the 45th row, the spy opens hurdle, clear 60-227895 communique page 2 bottom right the 18th row (silicate of preferred the 2nd table.) the preferred powder auxiliary use of the middle crystallized silicon hydrochlorate conduct of putting down in writing.Here, the SiO of alkalimetal silicate
2/ M
2(but M representes basic metal to O.) be 0.5～3.2, preferably be fit to more use 1.5～2.6.
As the usage quantity of this powder auxiliary, with respect to blapharoplast crowd 100 weight parts, be preferably 0～12 weight part, be more preferably 0～6 weight part.This detergent use powder auxiliary in this scope, favorable solubility.
Further, after operation 3, preferably increase the operation 4 of surface-treated particulate detergent.
Operation 4: the particulate detergent that will in operation 3, obtain carries out the operation of surface-treated with surface coating agent (surface-coating agent).But, in operation 3, also can carry out fragmentation simultaneously.
Operation 5: make the particulate detergent exsiccant operation that in operation 3 or operation 4, obtains.
3-2. operation 4
In this operation, can the particle surface of the particulate detergent that in operation 3, obtains be carried out modification.For this reason, add the operation 4 of the so various surface coating agents of when adding following (1) powder body, (2) fraction of form.The number of times of operation 4 also can be for more than 1 time.
If come the particle surface of modification particulate detergent, the flowability that improves particulate detergent and the tendency of anti-anti-caking are arranged then through surface coating agent.Therefore, in method of manufacture of the present invention, preferably be provided with the surface-treated operation.As the device that in operation 4, uses, for example can lift in operation 3 in the illustrative mixing machine of institute, the device that has the agitating wing and the broken wing concurrently is as preferred embodiment.Below describe respectively to surface coating agent.
(1) powder body
As powder body, its particulate median size is preferably below the 10 μ m, is more preferably 0.1～10 μ m.From the coating rate of the particle surface that improves particulate detergent, improve the viewpoint of the mobile and anti-anti-caking of particulate detergent, median size is adapted in this scope.The median size of this powder body can be through utilizing the method for scattering of light, and particle-size analyzer ((strain) hole field makes manufacturing) for example perhaps utilizes fractographic mensuration etc. to measure.Further, from the viewpoint of cleaning power, preferably this powder body has high IX ability and high alkali ability.Relevant powder body can be made up of a kind of composition, also can be made up of multiple components.
As this powder body, hope to be aluminosilicate, crystallinity, amorphously all can.Except aluminosilicate, also preferably sulfuric acid sodium, Calucium Silicate powder, silicon-dioxide, wilkinite, talcum, clay, soft silica verivate, the such powder body of crystallized silicon hydrochlorate.The median size that equally also can use primary particle in addition is the metallic soap of 0.1～10 μ m, the tensio-active agent of powder (for example alkyl-sulphate etc.) and water-soluble organic salt.Under the situation of using the crystallized silicon hydrochlorate, from preventing since the purpose of the deterioration of generation such as aggegation of the crystallized silicon hydrochlorate that moisture absorption or absorbing carbon dioxide gas cause preferably mix and use with crystallized silicon hydrochlorate powder body in addition.
As the usage quantity of powder body, with respect to particulate detergent 100 weight parts, be preferably 0.5～40 weight part, further be preferably 1～30 weight part, be more preferably 2～20 weight parts.The usage quantity of this powder body in this scope, can improve mobile, give with the human consumer with good usability.
(2) fraction
As fraction, can lift water-soluble polymers and lipid acid etc., can add with the aqueous solution or molten state.Fraction as relevant can be made up of a kind of composition, also can be made up of multiple composition.
(2-1) water-soluble polymers
As water-soluble polymers, can enumerate the polycarboxylates such as multipolymer or its salt of CMC 99.5, polyoxyethylene glycol, ZX-I, sodium acrylate and toxilic acid etc.As the usage quantity of this water-soluble polymers, with respect to particulate detergent 100 weight parts, be preferably 0～10 weight part, further be preferably 0～8 weight part, be more preferably 0～6 weight part.The usage quantity of this water-soluble polymers can obtain showing good solubility, good flowability, the particulate detergent of anti-anti-caking in this scope.
(2-2) lipid acid
As lipid acid, for example can enumerate carbonatoms is lipid acid of 10～22 etc.As the usage quantity of this lipid acid, with respect to these particulate detergent 100 weight parts, be preferably 0～5 weight part, be more preferably 0～3 weight part.Be under the solid situation at normal temperatures, preferably be heated to after the temperature that shows flowability, supply with through spraying.
3-3. operation 5
In this operation, can further make resulting particulate detergent exsiccant operation.Through the operation of being correlated with, can from particulate detergent, remove the moisture that brings by surfactant compsn etc.
This operation is any operation of the dry particulate detergent that in operation 3 or operation 4, obtains.Through removing moisture, can improve the bioactive agent composition in the particulate detergent.
From the viewpoint of the disintegration that suppresses particulate detergent, preferably do not apply the drying mode of strong shearing force as far as possible.For example, in batch-type, can enumerate and be encased in the container, in continous way, can enumerate fluid bed dryer or rotary drier, vapour pipe drying machine etc. with electric seasoning or hot air dryer exsiccant method, with method of batch-type fluidised bed drying etc.
For drying temperature, from the inhibition of the decomposition of this AS and the viewpoint of rate of drying, be preferably 40～110 ℃, further be preferably 50～100 ℃, be more preferably 60～90 ℃.
< detergent composition >
Detergent composition of the present invention is to contain above-mentioned particulate detergent and the compsn that constitutes; And then be to contain the detergent ingredients (for example, builder granule, optical dye, enzyme, spices, skimmer, SYNTHETIC OPTICAL WHITNER, bleach activator etc.) that adds in addition beyond this particulate detergent and the compsn that constitutes.
Viewpoint from cleaning power; The content of particulate detergent is preferably more than the 50 weight % in the detergent composition; Further be preferably more than the 60 weight %, be more preferably more than the 70 weight %, further be more preferably more than the 80 weight %, below the 100 weight %.
The content of detergent ingredients in detergent composition beyond the particulate detergent is preferably below the 50 weight %, is more preferably below the 40 weight %, is more preferably below the 30 weight %, further is more preferably below the 20 weight %.
< method for making of detergent composition >
The method for making of detergent composition does not have special qualification, for example, can lift said particulate detergent and the detergent ingredients method of mixing of adding in addition.Through the detergent composition that obtains like this, because contain the many detergent granules of the capacity that supports of tensio-active agent, so even also can bring into play sufficient cleaning effect on a small quantity.As the purposes of said detergent composition, so long as use the purposes of powder detergent, just not special the qualification, for example can enumerate clothing with powder detergent, automatic tableware with washing composition etc.
< measuring method of rerum natura >
1. volume density
Volume density uses the method for JIS K 3362 defineds to measure.
In addition, blapharoplast crowd's volume density is to remove the above particle of 2000 μ m volume density afterwards in the present invention, and the volume density of particulate detergent is to remove the above particle of 1180 μ m volume density afterwards.
2. volume density rising degree
In the method for manufacture of the particulate detergent that uses the blapharoplast crowd,, can use the volume density rising degree of following formula definition as the index of the oil absorbency of representing particulate detergent.The value of volume density rising degree is big more, and then the oil absorbency of particulate detergent is high more.In the present invention, the volume density rising degree as particulate detergent is preferably 1.2～1.7, is more preferably 1.3～1.6.
Volume density rising degree=(volume density of particulate detergent)/(blapharoplast crowd's volume density)
3. median size
For median size, can measure through following 2 methods.
(1) is the particle more than the 80 μ m for median size, uses after standard sieve (sieve aperture 2000～125 μ m) vibration 5 minutes of JIS K 8801, calculate median particle diameter from weight percent according to the size of sieve aperture.In more detail, using sieve aperture is 9 grades of sieves and a receiving plate of 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, on a receiving plate, begins to stack from the little sieve of sieve aperture; Add the particle of 100g from the sieve of 2000 μ m of topmost; Cover lid is installed in that (HEIKO makes manufacturing, bounces: 156 times/minute on the Ro-Tap type riddler machine; Rotation: 290 rev/mins); After making it to vibrate 5 minutes, measure and remain in this particulate weight on each sieve and a receiving plate, calculate this particulate part by weight (%) on each sieve.Begin to calculate successively this particulate part by weight on the little sieve of sieve aperture from a receiving plate, with adding up to 50% o'clock particle diameter as median size.
In addition; For median size is the particle below the 125 μ m; Using sieve aperture is that 12 grades of sieves and a receiving plate 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 carries out same mensuration, calculates median size.
In addition, in this application, blapharoplast crowd's median size is to remove the above particle of 2000 μ m median size afterwards, and the median size of particulate detergent is the median size of all particles.
(2) be particle for median size less than 80 μ m; Can use laser diffraction/diffuse transmission type particle size distribution device LA-920 ((strain) hole field makes manufacturing); This particle is scattered in the solvent that can not be dissolved in wherein, measures the median particle diameter that obtains, as median size.In addition, as for (2), also can measure the particle below the 150 μ m.
4.Rosin-Rammler number
The same method of mensuration of utilization and above-mentioned median size, mensuration residues on each sieve and the weight of this particle on a receiving plate, calculates the part by weight (cumulative percentage R (Dp) [μ m]) of this particle on each sieve (sieve aperture Dp [μ m]).Least square fitting collinear slope n in the time of will mapping with respect to the log (log (100/R (Dp))) of each logDp then is as the Rosin-Rammler number.
5. moisture
Moisture determination is carried out with infrared rays moisture meter method.Promptly; Measure the 3g sample with the sample disc of known weight, use infrared rays moisture meter (Kett Science Institute (strain) makes FD-240) that the blapharoplast crowd is heated down at 200 ℃, in addition; Particulate detergent 105 ℃ of down heating, is finished the indeclinable time point of weight in 30 seconds as drying.Then, calculate amount of moisture from dried weight and dry preceding weight.
6. mobile
Flowing time is from the hopper of the volume density mensuration usefulness of JIS K 3362 defineds, to flow out the 100mL needed time of powder.Flowing time was preferably below 10 seconds, further was preferably below 8 seconds, was more preferably below 7 seconds.
In addition, among the application, blapharoplast crowd's flowability is to remove the above particle of 2000 μ m flowability afterwards, and the flowability of particulate detergent is to remove the above particle of 1180 μ m flowability afterwards.
< method for evaluating quality >
1. oil absorption
30～35g powder is dropped in the absorbed dose tester ((strain) ASAHISOUKEN makes S410), make it to rotate with 200r.p.m. with driving the wing.At this, be that 4mL/min drips with aqueous nonionogenic tenside (flower king (strain) makes EMULGEN 108) with the liquid feed speed, can accurately lean out the point that reaches peak torque.The liquid addition of point of 70% moment of torsion of point that will reach this peak torque is divided by the powder input amount, as oil absorption.
2. blapharoplast crowd's yield
Particle yield of the present invention is illustrated in the part by weight of the blapharoplast in the specified particle diameter scope among the resulting blapharoplast crowd.
3. washing composition yield
Washing composition yield of the present invention is illustrated in the part by weight of the particulate detergent of particle diameter in 250～500 mu m ranges in the resulting particulate detergent, perhaps representes the part by weight of the particulate detergent in 125～500 mu m ranges.
Below, further put down in writing, disclose embodiment of the present invention through embodiment.This embodiment is an example of the present invention only, and does not mean that any qualification.
Embodiment
In the present embodiment, if not special the qualification, the raw material below then using.
Soda Ash Light 99.2min.: median size is that (CENTRAL GLASS (strain) makes 100 μ m; Oil absorption 0.45mL/g)
Clay mineral: DETERSOFT A (LAVIOSA manufactured)
ZX-I: weight-average molecular weight 10,000 (flower king (strain) makes)
Embodiment based on following further specifies the present invention.
<blapharoplast crowd 1 manufacturing >
Be manufactured on the blapharoplast crowd 1 who uses among the embodiment 1～7 according to following order.
4.2kg Soda Ash Light 99.2min. and 0.3kg clay mineral, are mixed by the 75L rotary drum granulator of division board (φ 40cm * L60cm/ rotating speed 30r.p.m./Froude number 0.2) in being housed.Mix after 10 seconds, use 1 internal mix type second fluid nozzle (Spraying Systems (Japan) (strain) makes: the sticker spraying presses the 0.15MPa/ micronize to press 0.3MPa with air-atomizing) with the ROHM sodium water solution that added 2.5kg35% in 7 minutes.After the interpolation, carry out from rotary drum granulator, discharging after 3 minutes prillings, use electric drying apparatus 200 ℃ dry 2 hours down.Dried moisture is 0.5 weight %.
The rerum natura of the particle swarm 1 that obtains is: median size is 336 μ m, and volume density is the particle swarm of 486g/L, and oil absorption is 0.48mL/g.In addition, the particle yield less than 2000 μ m is 96%.
<blapharoplast crowd 2 manufacturing >
Be manufactured on the blapharoplast crowd 2 who uses among the embodiment 8～13 according to following order.
The Soda Ash Light 99.2min. of 11.6kg, is mixed by the 122L drum type tablets press of division board (φ 50cm * L62cm/ rotating speed 18.5r.p.m./Froude number 0.1) in being housed.Mix after 10 seconds, ((strain) ATOMAX makes to use 2 external mix type second fluid nozzles; Micronize is pressed 0.3MPa with air-atomizing), with the ROHM sodium water solution that added 6.4kg35% in 7 minutes.After the interpolation, carry out from the drum type tablets press, discharging after 1 minute the prilling, with electric drying apparatus 200 ℃ dry 3 hours down.Dried moisture is 1.9 weight %.
The rerum natura of the particle swarm 2 of gained is: median size is 305 μ m, and volume density is the particle swarm of 487g/L, and oil absorption is 0.56mL/g.In addition, the particle yield less than 2000 μ m is 94%.
Make example 1
In addition, make the spray-dried granules crowd who uses in the comparative example 1～4 according to following order.
In tempering tank, add the water of 375 weight parts, water temperature reaches after 35 ℃, adds the sodium sulfate of 127 weight parts, the S-WAT of 5 weight parts, the optical dye of 1 weight part, stirs 10 minutes.Add 127 weight parts of sodium carbonate, add the ROHM sodium water solution of 40 weight % of 75 weight parts again, stirred 10 minutes, thereby process the 1st modulating liquid.In the 1st modulating liquid, add the sodium-chlor of 24 weight parts, stirred 10 minutes as the fine crystalline precipitation agent.Further add the zeolite of 266 weight parts, stirred 30 minutes, thereby obtain uniform the 2nd modulating liquid (slurry moisture 42 weight %).
In spray-drying tower (reverse-flow), supply with the 2nd modulating liquid with pump, press near the press atomization nozzle being installed on cat head with the spraying of 2.5MPa and spray.The high-temperature gas of supply spray-drying tower, is discharged with 90 ℃ temperature from cat head with 200 ℃ temperature supply from the tower bottom.Resulting spray-dried granules crowd is that moisture is 4 weight %, and median size is 304 μ m, and volume density is the particle swarm of 494g/L.
Embodiment 1
Surfactant compsn (the R-OSO that will contain AS
3Na; C12/C14/C16=64/24/12 (weight ratio); Amount of moisture 33 weight %; Below be called " compsn A ") be heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 1 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn A of 60 weight parts was dropped into wherein with 8 minutes, stirred then 3 minutes, discharge particulate detergent, with electric drying apparatus 100 ℃ dry 2 hours down, discharge particulate detergent 1.
Resulting particulate detergent 1 is: moisture is 0.6%, and median size is 353 μ m, and the Rosin-Rammler number is 1.65; The washing composition yield of 250-500 μ m is 52%; The yield of 125-500 μ m washing composition is 73%, and volume density is 755g/L, and flowability is 6.0s.
Embodiment 2
Compsn A is heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 1 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn A of 60 weight parts was dropped into wherein with 8 minutes.Further after beginning to drop into 1 minute of said compsn A, begin in mixing machine, to blow.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 7.3 weight parts/minute under carry out.Add said compsn A and finish to stir 3 minutes afterwards, discharge particulate detergent 2.
Resulting particulate detergent 2 is: moisture is 9.2%, and median size is 376 μ m, and the Rosin-Rammler number is 2.04; The washing composition yield of 250-500 μ m is 61%; The washing composition yield of 125-500 μ m is 76%, and volume density is 696g/L, and flowability is 5.5s.
Embodiment 3
Compsn A is heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 1 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn A of 60 weight parts was dropped into wherein with 8 minutes.Further after beginning to drop into 1 minute of said compsn A, begin in mixing machine, to blow.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 7.3 weight parts/minute under carry out.Add said compsn A and stirred 3 minutes after finishing, discharge particulate detergent, use electric drying apparatus 100 ℃ dry 2 hours down, discharge particulate detergent 3.
Resulting particulate detergent 3 is: moisture is 0.5%, and median size is 374 μ m, and the Rosin-Rammler number is 2.10; The washing composition yield of 250-500 μ m is 61%; 125-500 μ m washing composition yield is 76%, and volume density is 688g/L, and flowability is 5.9s.
Embodiment 4
Compsn A is heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 1 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn A of 96.7 weight parts was dropped into wherein with 13 minutes.Further after beginning to drop into 1 minute of said compsn A, begin air blast in mixing machine.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 5.9 weight parts/minute under carry out.Add said compsn A and stirred 3 minutes after finishing, discharge particulate detergent, use electric drying apparatus 100 ℃ dry 2 hours down, discharge particulate detergent 4.
The moisture of resulting particulate detergent 4 is 0.3%, and median size is 447 μ m, and the Rosin-Rammler number is 1.81; The washing composition yield of 250-500 μ m is 47%; 125-500 μ m washing composition yield is 57%, and volume density is 716g/L, and flowability is 6.2s.
Comparative example 1
Use and make resulting spray-dried granules crowd in the example 1, use with embodiment 1 same method and obtain particulate detergent 5.
Resulting particulate detergent 5 is: moisture is 0.5%, and median size is 411 μ m, and the Rosin-Rammler number is 2.40; The washing composition yield of 250-500 μ m is 58%; 125-500 μ m washing composition yield is 69%, and volume density is 562g/L, and flowability is 6.0s.
Comparative example 2
Use and make resulting spray-dried granules crowd in the example 1, use with embodiment 2 same methods and obtain particulate detergent 6.
Resulting particulate detergent 6 is: moisture is 10.6%, and median size is 423 μ m, and the Rosin-Rammler number is 2.51; The washing composition yield of 250-500 μ m is 58%; 125-500 μ m washing composition yield is 67%, and volume density is 559g/L, and flowability is 5.5s.
Comparative example 3
Use and make resulting spray-dried granules crowd in the example 1, use with embodiment 3 same methods and obtain particulate detergent 7.
Resulting particulate detergent 7 is: moisture is 0.4%, and median size is 410 μ m, and the Rosin-Rammler number is 2.38; The washing composition yield of 250-500 μ m is 59%; 125-500 μ m washing composition yield is 70%, and volume density is 544g/L, and flowability is 5.9s.
Comparative example 4
Use and make resulting spray-dried granules crowd in the example 1, use with embodiment 4 same methods and obtain particulate detergent 8.
Resulting particulate detergent 8 is: moisture is 0.4%, and median size is 454 μ m, and the Rosin-Rammler number is 2.57; The washing composition yield of 250-500 μ m is 53%; 125-500 μ m washing composition yield is 60%, and volume density is 565g/L, and flowability is 6.2s.
Comparative example 5
Use Soda Ash Light 99.2min. to replace blapharoplast crowd 1, use with embodiment 1 same method and obtain particulate detergent 9.
The moisture of resulting particulate detergent 9 is 0.5%, and median size is 321 μ m, and the Rosin-Rammler number is 1.40; The washing composition yield of 250-500 μ m is 42%; 125-500 μ m washing composition yield is 71%, and volume density is 627g/L, and flowability is 6.1s.
Comparative example 6
Use Soda Ash Light 99.2min. to replace blapharoplast crowd 1, use with embodiment 2 same methods and obtain particulate detergent 10.
Resulting particulate detergent 10 is: moisture is 9.7%, and median size is 291 μ m, and the Rosin-Rammler number is 0.92; The washing composition yield of 250-500 μ m is 17%; 125-500 μ m washing composition yield is 49%, and volume density is 761g/L, and flowability is 5.6s.
Comparative example 7
Use Soda Ash Light 99.2min. to replace blapharoplast crowd 1, use with embodiment 3 same methods and obtain particulate detergent 11.
Resulting particulate detergent 11 is: moisture is 0.7%, and median size is 278 μ m, and the Rosin-Rammler number is 0.90; The washing composition yield of 250-500 μ m is 17%; 125-500 μ m washing composition yield is 49%, and volume density is 712g/L, and flowability is 6.4s.
Comparative example 8
Use Soda Ash Light 99.2min. to replace blapharoplast crowd 1, use with embodiment 4 same methods and obtain particulate detergent 12.
Resulting particulate detergent 12 is: moisture is 0.3%, and median size is 728 μ m, and the Rosin-Rammler number is 1.29; The washing composition yield of 250-500 μ m is 20%; 125-500 μ m washing composition yield is 32%, and volume density is 655g/L, and flowability is 6.7s.
Embodiment 5
Compsn A is heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 1 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn A of 60 weight parts was dropped into wherein with 2 minutes, stirred then 3 minutes, discharge particulate detergent, use electric drying apparatus 105 ℃ dry 2 hours down, discharge particulate detergent 13.
Resulting particulate detergent 13 is: moisture is 0.5%, and median size is 508 μ m, and the Rosin-Rammler number is 1.89; The washing composition yield of 250-500 μ m is 38%; 125-500 μ m washing composition yield is 48%, and volume density is 663g/L, and flowability is 6.3s.
Embodiment 6
Compsn A is heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 1 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn A of 60 weight parts was dropped into wherein with 4 minutes, stirred then 3 minutes, discharge particulate detergent, use electric drying apparatus 105 ℃ dry 2 hours down, discharge particulate detergent 14.
Resulting particulate detergent 14 is: moisture is 0.7%, and median size is 475 μ m, and the Rosin-Rammler number is 1.63; The washing composition yield of 250-500 μ m is 38%; 125-500 μ m washing composition yield is 51%, and volume density is 679g/L, and flowability is 5.9s.
Embodiment 7
Compsn A is heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 1 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn A of 60 weight parts was dropped into wherein with 4 minutes.Further after beginning to drop into 1 minute of said compsn A, begin air blast in mixing machine.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 7.2 weight parts/minute under carry out.Add said compsn A and stirred 3 minutes after finishing, discharge particulate detergent, use electric drying apparatus 105 ℃ dry 2 hours down, discharge particulate detergent 15.
Resulting particulate detergent 15 is: moisture is 0.4%, and median size is 353 μ m, and the Rosin-Rammler number is 1.88; The washing composition yield of 250-500 μ m is 57%; 125-500 μ m washing composition yield is 75%, and volume density is 687g/L, and flowability is 5.9s.
Embodiment 8
Surfactant compsn (the R-OSO that will contain AS
3Na; C12/C14/C16=64/24/12 (weight ratio); Amount of moisture 35 weight %; Below be called " compsn B ") be heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 2 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn B of 60 weight parts was dropped into wherein with 8 minutes.Further after beginning to drop into 1 minute of said compsn B, begin in mixing machine, to blow.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 7.5 weight parts/minute under carry out.Add said compsn B and finish to stir 3 minutes afterwards, discharge particulate detergent 16.
Resulting particulate detergent 16 is: moisture is 9.7%, and median size is 358 μ m, and the Rosin-Rammler number is 1.74; The washing composition yield of 250-500 μ m is 48%; 125-500 μ m washing composition yield is 71%, and volume density is 665g/L, and flowability is 5.6s.
Embodiment 9
The compsn B of 60 weight parts and the polyoxyethylene lauryl ether sodium sulfate of 5 weight parts (flower king (strain) makes EMULGEN 270J) are mixed (below, be called " compsn C ") be heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 2 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn C of 65 weight parts was dropped into wherein with 8.7 minutes.Further after beginning to drop into 1 minute of said compsn C, begin in mixing machine, to blow.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 7.3 weight parts/minute under carry out.Add said compsn C and finish to stir 3 minutes afterwards, discharge particulate detergent 17.
Resulting particulate detergent 17 is: moisture is 9.7%, and median size is 429 μ m, and the Rosin-Rammler number is 1.93; The washing composition yield of 250-500 μ m is 44%; 125-500 μ m washing composition yield is 59%, and volume density is 706g/L, and flowability is 6.3s.
Embodiment 10
Compsn C is heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 2 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn C of 65 weight parts was dropped into wherein with 8.7 minutes.Further after beginning to drop into 1 minute of said compsn C, begin in mixing machine, to blow.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 7.3 weight parts/minute under carry out.Add said compsn C and stirred 3 minutes after finishing, discharge particulate detergent, use electric drying apparatus 105 ℃ dry 2 hours down, discharge particulate detergent 18.
Resulting particulate detergent 18 is: moisture is 0.5%, and median size is 380 μ m, and the Rosin-Rammler number is 1.54; The washing composition yield of 250-500 μ m is 42%; 125-500 μ m washing composition yield is 64%, and volume density is 706g/L, and flowability is 5.9s.
Embodiment 11
The compsn B of 60 weight parts and the polyoxyethylene lauryl ether sodium sulfate of 10 weight parts (flower king (strain) makes EMULGEN 270J) are mixed (below, be called " compsn D ") be heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 2 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn D of 70 weight parts was dropped into wherein with 9.3 minutes.Further after beginning to drop into 1 minute of said compsn D, begin in mixing machine, to blow.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 7.1 weight parts/minute under carry out.Add said compsn D and stirred 3 minutes after finishing, discharge particulate detergent, use electric drying apparatus 105 ℃ dry 2 hours down, discharge particulate detergent 19.
Resulting particulate detergent 19 is: moisture is 0.6%, and median size is 421 μ m, and the Rosin-Rammler number is 1.56; The washing composition yield of 250-500 μ m is 40%; 125-500 μ m washing composition yield is 58%, and volume density is 728g/L, and flowability is 5.7s.
Embodiment 12
The compsn B of 60 weight parts and the polyoxyethylene lauryl ether sodium sulfate of 5 weight parts (flower king (strain) makes EMULGEN 106) are mixed (below, be called " compsn E ") be heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 2 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn E of 65 weight parts was dropped into wherein with 8.7 minutes.Further after beginning to drop into 1 minute of said compsn E, begin in mixing machine, to blow.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 7.3 weight parts/minute under carry out.Add said compsn E and finish to stir 3 minutes afterwards, discharge particulate detergent 20.
Resulting particulate detergent 20 is: moisture is 9.0%, and median size is 435 μ m, and the Rosin-Rammler number is 1.86; The washing composition yield of 250-500 μ m is 40%; 125-500 μ m washing composition yield is 58%, and volume density is 700g/L, and flowability is 7.1s.
Embodiment 13
Compsn E is heated to 60 ℃.Next; In
mixing machine (the Matuzaka skill is ground (strain) and made, capacity 20L, jacketed); Drop into the resulting blapharoplast crowd 2 of 100 weight parts; Beginning main shaft (agitating wing, rotating speed: 60rpm, SFM: stirring 0.9m/s).And, feed 60 ℃ warm water in the chuck with 10L/ minute speed.The said compsn E of 65 weight parts was dropped into wherein with 8.7 minutes.Further after beginning to drop into 1 minute of said compsn E, begin in mixing machine, to blow.In addition, the air-supply condition be 60 ℃ of temperature, air output for respect to these particulate detergent 100 weight parts be 7.3 weight parts/minute under carry out.Add said compsn E and stirred 3 minutes after finishing, discharge particulate detergent, use electric drying apparatus 105 ℃ dry 2 hours down, discharge particulate detergent 21.
Resulting particulate detergent 21 is: moisture is 0.6%, and median size is 412 μ m, and the Rosin-Rammler number is 1.65; The washing composition yield of 250-500 μ m is 41%; 125-500 μ m washing composition yield is 60%, and volume density is 697g/L, and flowability is 6.8s.
Condition, the result of the above embodiment etc. are as shown in the table.
[table 1]
[table 2]
[table 3]
Can know that from embodiment 1～7 blapharoplast crowd 1 and the compsn mixing that contains by the AS of formula (1) expression without spray-drying process through with gained of the present invention can obtain the above high density detergent particle of 650g/L by yield well.In addition; Can know from embodiment 8～13; Through mixing the compsn that further contains polyoxyethylene lauryl ether sodium sulfate or polyoxyethylene lauryl ether without the blapharoplast crowd of spray-drying process 2 and the compsn that contains by the AS of formula (1) expression, can obtain the above high density detergent particle of 650g/L well by yield what obtain from the present invention.
In addition; Can know from the comparison of embodiment 1～4 and comparative example 1～4; Through mixing with spray-drying process particle swarm that obtains and the compsn that contains the AS of representing by formula (1); Though can access the detergent granules of narrow particle size distribution, can not stably obtain the above high density detergent particle of 650g/L.
In addition; Can know from the comparison of embodiment 1～4 and comparative example 5～8; Using Soda Ash Light 99.2min. to replace mixing through the compound that uses the AS of representing by formula (1) under blapharoplast crowd 1 the situation, though can obtain the above high density detergent particle of 650g/L; But size-grade distribution is wide, and yield is low.
Utilize possibility on the industry
According to the present invention, do not comprise blapharoplast crowd that spray-dired method obtains and, can make high density detergent particle well by yield with necessary granularity by the compound of the AS of formula (1) expression through using.
Claims (13)
1. a volume density is the method for manufacture of the particulate detergent more than the 650g/L, wherein,
Said method of manufacture comprises following operation 1～3:
Operation 1: with oil absorption is the powder stock blended operation more than the 0.4mL/g;
Operation 2: in the mixed powder that obtains through operation 1, add water or adhesive solution, modulate blapharoplast crowd's operation with low shear granulator; With
Operation 3: the blapharoplast crowd that will obtain through operation 2 with contain following a) composition and b) the surfactant compsn blended operation of composition,
A) AS of representing by following formula (1),
R-O-SO
3M (1)
In the formula, R representes that carbonatoms is 10～18 alkyl or thiazolinyl, and M representes alkali metal atom or amine, and
B) be the water of 25～70 weight parts with respect to above-mentioned a) composition 100 weight parts.
2. method of manufacture as claimed in claim 1, wherein,
Low shear granulator in operation 2 is pan-type pelletizer or rotary drum granulator.
3. according to claim 1 or claim 2 method of manufacture, wherein,
The AS AS in addition that surfactant compsn in operation 3 further contains nonionogenic tenside and/or represented by formula (1).
4. like each described method of manufacture in the claim 1～3, wherein,
With respect to blapharoplast crowd 100 weight parts, mix the surfactant compsn of 30～100 weight parts.
5. like each described method of manufacture in the claim 1～4, wherein,
Said method of manufacture further comprises following operation 4:
Operation 4: the particulate detergent that will in operation 3, obtain carries out the operation of surface-treated with surface coating agent.
6. like each described method of manufacture in the claim 1～5, wherein,
Said method of manufacture further comprises following operation 5:
Operation 5: make the particulate detergent exsiccant operation that in operation 3 or operation 4, obtains.
7. like each described method of manufacture in the claim 1～6, wherein,
In operation 2, further make the blapharoplast crowd exsiccant operation that in this operation, obtains.
8. like each described method of manufacture in the claim 1～7, wherein,
In operation 3, under ventilation, carry out the mixing of blapharoplast crowd and surfactant compsn.
9. like each described method of manufacture in the claim 1～8, wherein,
In operation 2, use multithread body nozzle to add water or adhesive solution.
10. the method for manufacture described in claim 9, wherein,
Multithread body nozzle is a second fluid nozzle.
11. like each described method of manufacture in the claim 1～10, wherein,
Powder stock in operation 1 is the powder stock that contains Soda Ash Light 99.2min..
12. a particulate detergent, it is obtained by each said method of manufacture in the claim 1～11.
13. a detergent composition, it contains the particulate detergent that is obtained by each said method of manufacture in the claim 1～11 and forms.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009-155157 | 2009-06-30 | ||
| JP2009155157 | 2009-06-30 | ||
| PCT/JP2010/061038 WO2011001966A1 (en) | 2009-06-30 | 2010-06-29 | Method for producing high bulk density detergent granules |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102459555A true CN102459555A (en) | 2012-05-16 |
| CN102459555B CN102459555B (en) | 2014-05-07 |
Family
ID=43411038
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201080026218.4A Expired - Fee Related CN102459555B (en) | 2009-06-30 | 2010-06-29 | Method for producing high bulk density detergent granules |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP2450428A4 (en) |
| JP (1) | JP5624811B2 (en) |
| CN (1) | CN102459555B (en) |
| AU (1) | AU2010267108B2 (en) |
| BR (1) | BRPI1015946A2 (en) |
| WO (1) | WO2011001966A1 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011127106A (en) * | 2009-11-18 | 2011-06-30 | Kao Corp | Method for producing detergent granule cluster |
| JP5713644B2 (en) * | 2009-11-18 | 2015-05-07 | 花王株式会社 | Method for producing surfactant-supporting granules |
| CN103547665B (en) * | 2011-05-18 | 2016-04-13 | 花王株式会社 | The manufacture method of detergent particles group |
| JP6139994B2 (en) * | 2012-06-20 | 2017-05-31 | 花王株式会社 | Process for producing dentifrice granules |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0873888A (en) * | 1994-09-09 | 1996-03-19 | Lion Corp | Production of high bulk density granular detergent composition |
| JP2004176055A (en) * | 2002-11-15 | 2004-06-24 | Lion Corp | Producing method of particulate detergent |
| CN101001943A (en) * | 2004-08-06 | 2007-07-18 | 花王株式会社 | Process for production of uni-core detergent particles |
| WO2009142135A1 (en) * | 2008-05-19 | 2009-11-26 | 花王株式会社 | Surfactant-supporting granule cluster |
Family Cites Families (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| TW326472B (en) * | 1994-08-12 | 1998-02-11 | Kao Corp | Method for producing nonionic detergent granules |
| 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 |
| CN1117849C (en) * | 1995-04-27 | 2003-08-13 | 普罗格特-甘布尔公司 | Process for producing granular detergent components or compositions |
| JP4497488B2 (en) * | 1996-08-26 | 2010-07-07 | 花王株式会社 | Method for producing high bulk density detergent composition |
| TW397862B (en) * | 1996-09-06 | 2000-07-11 | Kao Corp | Detergent granules and method for producing the same, and high-bulk density detergent composition |
| JP3136117B2 (en) | 1997-04-28 | 2001-02-19 | 花王株式会社 | Mixing device |
| JP3209941B2 (en) | 1997-04-28 | 2001-09-17 | 花王株式会社 | Mixing method and mixing device |
| JP4108199B2 (en) * | 1998-05-13 | 2008-06-25 | ライオン株式会社 | Method for producing granular detergent composition |
| JP3444817B2 (en) * | 1999-06-16 | 2003-09-08 | 花王株式会社 | Manufacturing method of detergent particles |
| JP2002266000A (en) * | 2001-03-12 | 2002-09-18 | Lion Corp | High bulk density detergent composition and its manufacturing method |
| JP4417195B2 (en) * | 2003-08-06 | 2010-02-17 | 花王株式会社 | Production method of granular anionic surfactant |
| JP4772415B2 (en) * | 2004-08-06 | 2011-09-14 | 花王株式会社 | Method for producing mononuclear detergent particles |
| JP4799951B2 (en) * | 2004-10-14 | 2011-10-26 | 花王株式会社 | Method for producing mononuclear detergent particles |
| JP2011127106A (en) * | 2009-11-18 | 2011-06-30 | Kao Corp | Method for producing detergent granule cluster |
-
2010
- 2010-06-29 WO PCT/JP2010/061038 patent/WO2011001966A1/en active Application Filing
- 2010-06-29 BR BRPI1015946A patent/BRPI1015946A2/en not_active IP Right Cessation
- 2010-06-29 JP JP2010147330A patent/JP5624811B2/en active Active
- 2010-06-29 CN CN201080026218.4A patent/CN102459555B/en not_active Expired - Fee Related
- 2010-06-29 EP EP10794135.3A patent/EP2450428A4/en not_active Withdrawn
- 2010-06-29 AU AU2010267108A patent/AU2010267108B2/en not_active Ceased
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0873888A (en) * | 1994-09-09 | 1996-03-19 | Lion Corp | Production of high bulk density granular detergent composition |
| JP2004176055A (en) * | 2002-11-15 | 2004-06-24 | Lion Corp | Producing method of particulate detergent |
| CN101001943A (en) * | 2004-08-06 | 2007-07-18 | 花王株式会社 | Process for production of uni-core detergent particles |
| WO2009142135A1 (en) * | 2008-05-19 | 2009-11-26 | 花王株式会社 | Surfactant-supporting granule cluster |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2450428A1 (en) | 2012-05-09 |
| EP2450428A4 (en) | 2014-12-03 |
| WO2011001966A1 (en) | 2011-01-06 |
| JP5624811B2 (en) | 2014-11-12 |
| JP2011026583A (en) | 2011-02-10 |
| AU2010267108A1 (en) | 2012-01-19 |
| BRPI1015946A2 (en) | 2016-04-19 |
| AU2010267108B2 (en) | 2013-05-16 |
| CN102459555B (en) | 2014-05-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102015992B (en) | Surfactant-supporting granule cluster | |
| KR100904970B1 (en) | Detergent particles | |
| CN102459555B (en) | Method for producing high bulk density detergent granules | |
| CN102712884B (en) | Method for producing detergent granules | |
| CN103221527B (en) | Method for producing detergent particle aggregates | |
| CN102686716A (en) | Process for producing detergent particles | |
| CN103228776B (en) | Method for producing detergent particle group | |
| EP2123744A1 (en) | Manufacture of dertergent granules by dry neutralisation | |
| EP1788071B1 (en) | Process for production of uni-core detergent particles | |
| CN102666827B (en) | Method for producing surfactant-supporting granule cluster | |
| JP6097003B2 (en) | Granular detergent composition | |
| JPH0959699A (en) | Production of nonionic detergent granule | |
| CN102712885A (en) | Method for producing detergent granules | |
| JP5971753B2 (en) | Method for producing detergent particles | |
| JP2004115791A (en) | Detergent particle group | |
| JP2005060149A (en) | Method for processing crystalline alkali metal silicate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140507 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |