JP4466091B2 - Metal soap manufacturing method - Google Patents
Metal soap manufacturing method Download PDFInfo
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- JP4466091B2 JP4466091B2 JP2004023277A JP2004023277A JP4466091B2 JP 4466091 B2 JP4466091 B2 JP 4466091B2 JP 2004023277 A JP2004023277 A JP 2004023277A JP 2004023277 A JP2004023277 A JP 2004023277A JP 4466091 B2 JP4466091 B2 JP 4466091B2
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- component
- metal soap
- aqueous solution
- salt
- metal
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Links
- 229910052751 metal Inorganic materials 0.000 title claims description 99
- 239000002184 metal Substances 0.000 title claims description 99
- 239000000344 soap Substances 0.000 title claims description 89
- 238000004519 manufacturing process Methods 0.000 title claims description 32
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 36
- 239000000194 fatty acid Substances 0.000 claims description 36
- 229930195729 fatty acid Natural products 0.000 claims description 36
- 239000007864 aqueous solution Substances 0.000 claims description 34
- -1 alkali metal salt Chemical class 0.000 claims description 29
- 150000004665 fatty acids Chemical class 0.000 claims description 23
- 150000003839 salts Chemical class 0.000 claims description 20
- 150000003863 ammonium salts Chemical class 0.000 claims description 14
- 229910052783 alkali metal Inorganic materials 0.000 claims description 13
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 description 35
- 239000002245 particle Substances 0.000 description 24
- 238000000034 method Methods 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 239000002994 raw material Substances 0.000 description 14
- 239000002002 slurry Substances 0.000 description 14
- 229910001111 Fine metal Inorganic materials 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000005649 metathesis reaction Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229940114930 potassium stearate Drugs 0.000 description 4
- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 4
- 229960001763 zinc sulfate Drugs 0.000 description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000001154 acute effect Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- YWWVWXASSLXJHU-AATRIKPKSA-N (9E)-tetradecenoic acid Chemical compound CCCC\C=C\CCCCCCCC(O)=O YWWVWXASSLXJHU-AATRIKPKSA-N 0.000 description 2
- XDOFQFKRPWOURC-UHFFFAOYSA-N 16-methylheptadecanoic acid Chemical compound CC(C)CCCCCCCCCCCCCCC(O)=O XDOFQFKRPWOURC-UHFFFAOYSA-N 0.000 description 2
- 235000021357 Behenic acid Nutrition 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 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 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- BJOYVZZDDFVLPI-UHFFFAOYSA-N azanium;tetradecanoate Chemical compound [NH4+].CCCCCCCCCCCCCC([O-])=O BJOYVZZDDFVLPI-UHFFFAOYSA-N 0.000 description 2
- 229940116226 behenic acid Drugs 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- UTOPWMOLSKOLTQ-UHFFFAOYSA-N octacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O UTOPWMOLSKOLTQ-UHFFFAOYSA-N 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- SECPZKHBENQXJG-FPLPWBNLSA-N palmitoleic acid Chemical compound CCCCCC\C=C/CCCCCCCC(O)=O SECPZKHBENQXJG-FPLPWBNLSA-N 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- ZONJATNKKGGVSU-UHFFFAOYSA-N 14-methylpentadecanoic acid Chemical compound CC(C)CCCCCCCCCCCCC(O)=O ZONJATNKKGGVSU-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- YWWVWXASSLXJHU-UHFFFAOYSA-N 9E-tetradecenoic acid Natural products CCCCC=CCCCCCCCC(O)=O YWWVWXASSLXJHU-UHFFFAOYSA-N 0.000 description 1
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 1
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- URXZXNYJPAJJOQ-UHFFFAOYSA-N Erucic acid Natural products CCCCCCC=CCCCCCCCCCCCC(O)=O URXZXNYJPAJJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 235000021353 Lignoceric acid Nutrition 0.000 description 1
- CQXMAMUUWHYSIY-UHFFFAOYSA-N Lignoceric acid Natural products CCCCCCCCCCCCCCCCCCCCCCCC(=O)OCCC1=CC=C(O)C=C1 CQXMAMUUWHYSIY-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 235000019482 Palm oil Nutrition 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 235000021319 Palmitoleic acid Nutrition 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- LSFBQOPXRBJSSI-UHFFFAOYSA-L calcium;tetradecanoate Chemical compound [Ca+2].CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O LSFBQOPXRBJSSI-UHFFFAOYSA-L 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- SECPZKHBENQXJG-UHFFFAOYSA-N cis-palmitoleic acid Natural products CCCCCCC=CCCCCCCCC(O)=O SECPZKHBENQXJG-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- DPUOLQHDNGRHBS-KTKRTIGZSA-N erucic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-KTKRTIGZSA-N 0.000 description 1
- FARYTWBWLZAXNK-WAYWQWQTSA-N ethyl (z)-3-(methylamino)but-2-enoate Chemical compound CCOC(=O)\C=C(\C)NC FARYTWBWLZAXNK-WAYWQWQTSA-N 0.000 description 1
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 229960002446 octanoic acid Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- WBHHMMIMDMUBKC-XLNAKTSKSA-N ricinelaidic acid Chemical compound CCCCCC[C@@H](O)C\C=C\CCCCCCCC(O)=O WBHHMMIMDMUBKC-XLNAKTSKSA-N 0.000 description 1
- 229960003656 ricinoleic acid Drugs 0.000 description 1
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000009777 vacuum freeze-drying Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
本発明は、金属石鹸の製造方法に関する。 The present invention relates to a method for producing a metal soap.
金属石鹸は、電子印刷分野、粉末冶金分野、化粧品分野、塗料分野、樹脂加工分野など、多くの分野において幅広く用いられている。現在行われている代表的な金属石鹸の製造方法としては、脂肪酸と無機金属酸化物あるいは無機金属水酸化物とを反応する方法（直接法）、あるいは脂肪酸のアルカリ金属塩やアンモニウム塩の溶液と無機金属塩類とを反応する方法（複分解法）が挙げられる。 Metal soaps are widely used in many fields such as electronic printing, powder metallurgy, cosmetics, paint, and resin processing. As a typical method for producing a metal soap, a method of reacting a fatty acid with an inorganic metal oxide or an inorganic metal hydroxide (direct method), or a solution of an alkali metal salt or an ammonium salt of a fatty acid Examples include a method of reacting with inorganic metal salts (metathesis method).
複分解法は、直接法と比較して、未反応の原料脂肪酸や無機金属化合物の含有量が少なく、高純度で微細粒子の金属石鹸を得やすく、また色相が良好な金属石鹸を得ることができる。複分解法を利用した金属石鹸の製造方法としては、脂肪酸アルカリ塩や脂肪酸アンモニウム塩の水溶液と、無機金属塩類の水溶性とを連続的に反応装置内に供給して反応させ、金属石鹸含有スラリーを得る連続複分解法が知られている。 Compared to the direct method, the metathesis method has a low content of unreacted raw fatty acids and inorganic metal compounds, makes it easy to obtain metal soaps with high purity and fine particles, and can obtain metal soaps with good hues. . As a method for producing metal soap using the metathesis method, an aqueous solution of a fatty acid alkali salt or a fatty acid ammonium salt and a water solubility of an inorganic metal salt are continuously fed into a reaction device to cause a reaction. Obtained continuous metathesis methods are known.
例えば、オーバーフロー排出口でつながる４つの反応槽を用いて、第１槽に脂肪酸ナトリウム塩水溶液と硫酸アルミニウム水溶液とを供給し混合しながらオーバーフローさせ、第２槽以降で反応を完結しつつ粒子を熟成させることで脂肪酸アルミニウムのスラリーを得る方法（特許文献１参照）が知られている。しかし、この方法では、２つの原料を第１槽で反応させる際、各槽の内部やオーバーフロー排出口付近に金属石鹸が付着し、別槽にスラリーを安定に移動させることが難しい。そのため、原料脂肪酸や無機塩を金属石鹸の中に内包しやすく、金属石鹸の純度を上げることが難しい場合がある。 For example, using four reaction tanks connected to the overflow discharge port, supply the fatty acid sodium salt aqueous solution and the aluminum sulfate aqueous solution to the first tank and allow them to overflow while mixing, and mature the particles while completing the reaction in the second tank and beyond. There is known a method of obtaining a fatty acid aluminum slurry (see Patent Document 1). However, in this method, when the two raw materials are reacted in the first tank, metal soap adheres to the inside of each tank or the vicinity of the overflow outlet, and it is difficult to stably move the slurry to another tank. Therefore, it may be difficult to increase the purity of the metal soap because the raw fatty acids and inorganic salts are easily included in the metal soap.
これらの問題を解決するため、脂肪酸ナトリウム塩またはアンモニウム塩の水溶液と、無機金属塩の水溶液とを、フロージェットミキサー、片吸い込み式渦巻きポンプ、ラインホモミクサーなどの混合機に直接供給して両者を混合後、反応生成物を直ちに混合機から排出して金属石鹸のスラリーを得る方法（特許文献２、特許文献３参照）が知られている。しかし、この方法では、原料水溶液の反応の際に強力な機械的混合力がかけられるため、反応系内に大きな攪拌乱流が生じ、反応装置内の壁に金属石鹸の粒子が接触しやすい。そのため、製造装置内の壁で成長した金属石鹸粒子によって反応装置の内部が閉塞し、反応装置内に原料の水溶液が安定に供給できなくなり、生産効率が低下する場合がある。上述の方法では、いずれも金属石鹸を長時間にわたり連続的に製造することが困難であった。
In order to solve these problems, an aqueous solution of a fatty acid sodium salt or ammonium salt and an aqueous solution of an inorganic metal salt are directly supplied to a mixer such as a flow jet mixer, a single suction centrifugal pump, a line homomixer, etc. After mixing, a method is known in which a reaction product is immediately discharged from a mixer to obtain a metal soap slurry (see
反応装置内で合成される金属石鹸が反応容器内面へ付着するのを軽減し、反応装置内に原料水溶液の供給を安定に行うことで、長時間の連続製造が可能な金属石鹸の製造方法を提供することを目的とする。 A method for producing metal soap that can be manufactured continuously for a long period of time by reducing the amount of metal soap synthesized in the reactor from adhering to the inner surface of the reaction vessel and stably supplying the raw material aqueous solution into the reactor. The purpose is to provide.
発明者らは、上記課題を達成するために鋭意研究を重ねた結果、特定の構造を有する反応装置に２つの原料水溶液を供給することで、装置内面に金属石鹸が滞留し付着することなく金属石鹸を製造可能であることを見出した。そして、この反応方法を用いることで、反応装置内に閉塞を生じることなく、金属石鹸を長時間にわたり連続製造できることを見出し本発明に至った。 As a result of intensive studies to achieve the above-mentioned problems, the inventors have supplied two raw material aqueous solutions to a reactor having a specific structure, so that metal soap does not stay and adhere to the inner surface of the apparatus. We have found that soap can be manufactured. And by using this reaction method, it discovered that a metal soap could be continuously manufactured over a long time, without producing a blockade in a reaction apparatus, and came to this invention.
すなわち本発明は、
（１）脂肪酸のアルカリ金属塩またはアンモニウム塩の水溶液と、無機金属塩の水溶液とを反応させて金属石鹸を製造する製造方法であって、外筒の中に内筒を配置した内外筒間に環状空間を有する共軸筒型反応装置を用いて、ａ）炭素数４〜３０の脂肪酸のアルカリ金属塩またはアンモニウム塩を０．００１〜２０重量％含有する水溶液と、ｂ）無機金属塩を０．００１〜２０重量％含有する水溶液とを、ｂ成分中の無機金属塩に対する、ａ成分中の脂肪酸塩の当量比（ａ／ｂ）が０．５〜１．１となるよう、異なる供給口からそれぞれ供給する金属石鹸の製造方法である。
That is, the present invention
(1) A method for producing a metal soap by reacting an aqueous solution of an alkali metal salt or ammonium salt of a fatty acid with an aqueous solution of an inorganic metal salt, wherein the inner tube is disposed between the inner and outer cylinders. Using a coaxial cylindrical reactor having an annular space, a) an aqueous solution containing 0.001 to 20% by weight of an alkali metal salt or ammonium salt of a fatty acid having 4 to 30 carbon atoms, and b) 0 inorganic metal salt 0.001 to 20% by weight of aqueous solution containing different supply ports so that the equivalent ratio (a / b) of fatty acid salt in component a to inorganic metal salt in component b is 0.5 to 1.1 It is a manufacturing method of the metal soap each supplied from.
本発明の金属石鹸の製造方法を用いることにより、図１のような特定の構造を有する反応装置を用いる事により、反応装置内で合成される金属石鹸の反応容器内面への付着を大幅に軽減することができる。そして、反応装置内に供給される原料水溶液の反応比の変動を抑え、金属石鹸を長時間にわたり連続製造することができる。 By using the metal soap manufacturing method of the present invention, by using a reactor having a specific structure as shown in FIG. 1, the adhesion of the metal soap synthesized in the reactor to the inner surface of the reaction vessel is greatly reduced. can do. And the fluctuation | variation of the reaction ratio of the raw material aqueous solution supplied in the reaction apparatus can be suppressed, and a metal soap can be manufactured continuously over a long time.
本発明の金属石鹸の製造方法において用いる原料成分としては、ａ）脂肪酸塩水溶液とｂ）無機金属塩の水溶液が用いられる。
ａ成分の脂肪酸塩水溶液の調整に用いる脂肪酸塩としては、炭素数４〜３０の脂肪酸のアルカリ金属塩またはアンモニウム塩が挙げられる。該脂肪酸は飽和、不飽和のいずれであってもよく、また、直鎖状、分岐状のいずれであってもよい。このような脂肪酸塩の例としては、カプリル酸、カプリン酸、ラウリン酸、ミリスチン酸、ミリストレイン酸、パルミチン酸、イソパルミチン酸、パルミトレイン酸、ステアリン酸、ベヘン酸、リグノセリン酸、セロチン酸、モンタン酸、イソステアリン酸、オレイン酸、アラキン酸、リシノレイン酸、リノレイン酸、ベヘニン酸やエルカ酸などに代表される単体脂肪酸のナトリウム、カリウムなどのアルカリ金属塩またはアンモニウム塩、あるいは、牛脂脂肪酸、大豆油脂肪酸、ヤシ油脂肪酸、パーム油脂肪酸などに代表される動植物油脂由来の脂肪酸のナトリウム、カリウムなどのアルカリ金属塩またはアンモニウム塩が挙げられる。
これらの中で、特に炭素数１２〜２２を有する脂肪酸のアルカリ金属塩またはアンモニウム塩が好ましい。これらの脂肪酸塩は単独で用いてもよく、二種類以上を組み合わせて用いてもよい。炭素数３以下の脂肪酸のアルカリ金属塩やアンモニウム塩を用いた場合、得られる金属石鹸の水に対する溶解度が高いので、収率が低下する。一方、炭素数３１以上の脂肪酸のアルカリ金属塩やアンモニウム塩を用いた場合、水に対する溶解度が低すぎて、水溶液濃度が低くなり、生産効率が低下する。
As raw material components used in the method for producing a metal soap of the present invention, a) an aqueous solution of a fatty acid salt and b) an aqueous solution of an inorganic metal salt are used.
Examples of the fatty acid salt used for preparing the fatty acid salt aqueous solution of component a include alkali metal salts or ammonium salts of fatty acids having 4 to 30 carbon atoms. The fatty acid may be saturated or unsaturated, and may be linear or branched. Examples of such fatty acid salts include caprylic acid, capric acid, lauric acid, myristic acid, myristoleic acid, palmitic acid, isopalmitic acid, palmitoleic acid, stearic acid, behenic acid, lignoceric acid, serotic acid, montanic acid Isostearic acid, oleic acid, arachinic acid, ricinoleic acid, linolenic acid, simple fatty acids represented by sodium, potassium, and other alkali metal salts such as behenic acid and erucic acid, or beef tallow fatty acid, soybean oil fatty acid, Examples thereof include alkali metal salts such as sodium and potassium, or ammonium salts of fatty acids derived from animal and vegetable oils and fats typified by coconut oil fatty acid and palm oil fatty acid.
Among these, an alkali metal salt or an ammonium salt of a fatty acid having 12 to 22 carbon atoms is particularly preferable. These fatty acid salts may be used alone or in combination of two or more. When an alkali metal salt or an ammonium salt of a fatty acid having 3 or less carbon atoms is used, the yield of the metal soap is reduced because the resulting metal soap has high solubility in water. On the other hand, when an alkali metal salt or ammonium salt of a fatty acid having 31 or more carbon atoms is used, the solubility in water is too low, the aqueous solution concentration is lowered, and the production efficiency is lowered.
本発明の製造方法に用いるａ成分の脂肪酸塩水溶液において、脂肪酸のアルカリ金属塩またはアンモニウム塩の含有量は、０．００１〜２０重量％の範囲である。含有量が０．００１重量％未満では、得られる金属石鹸量が反応液量に対して著しく低く生産効率が悪い。また、２０重量％を超えると、反応後の金属石鹸分散液の濃度が高すぎ、反応装置内の金属石鹸の付着が生じやすくなる。反応装置内の金属石鹸の付着が少なく、より効率的に連続して金属石鹸を製造する場合、水溶液中の上記脂肪酸のアルカリ金属塩またはアンモニウム塩の好ましい含有量は、０．０１〜１０重量％の範囲である。 In the fatty acid salt aqueous solution of component a used in the production method of the present invention, the content of the alkali metal salt or ammonium salt of the fatty acid is in the range of 0.001 to 20% by weight. When the content is less than 0.001% by weight, the amount of metal soap obtained is remarkably low with respect to the amount of the reaction solution, and the production efficiency is poor. On the other hand, if it exceeds 20% by weight, the concentration of the metal soap dispersion after the reaction is too high, and the metal soap in the reaction apparatus tends to adhere. In the case of producing metal soap more efficiently and continuously with less metal soap adhesion in the reaction apparatus, the preferable content of the alkali metal salt or ammonium salt of the fatty acid in the aqueous solution is 0.01 to 10% by weight. Range.
本発明の製造方法に用いるｂ成分の無機金属塩の水溶液の調整に用いる無機金属塩の例としては、カルシウム、バリウム、マグネシウムなどのアルカリ土類金属の塩化物、硫酸塩、炭酸塩、硝酸塩、燐酸塩など、あるいは、チタン、亜鉛、銅、マンガン、カドミウム、水銀、ジルコニウム、鉛、鉄、アルミニウム、コバルト、ニッケル、銀などの金属の塩化物、硫酸塩、炭酸塩、硝酸塩、燐酸塩などが挙げられる。これらの物質は単独で用いてもよく、二種類以上を組み合わせて用いてもよい。 Examples of the inorganic metal salt used for preparing the aqueous solution of the inorganic metal salt of component b used in the production method of the present invention include chlorides, sulfates, carbonates, nitrates of alkaline earth metals such as calcium, barium, and magnesium. Phosphate, etc., or titanium, zinc, copper, manganese, cadmium, mercury, zirconium, lead, iron, aluminum, cobalt, nickel, silver, and other metal chlorides, sulfates, carbonates, nitrates, phosphates, etc. Can be mentioned. These substances may be used alone or in combination of two or more.
本発明の製造方法に用いるｂ成分の無機金属塩の水溶液において、無機金属塩の含有量は０．００１〜２０重量％の範囲である。含有量が０．００１重量％未満では、得られる金属石鹸量が反応液量に対して著しく低く、生産効率が悪い。また、２０重量％を超えると、得られる金属石鹸粒子の凝集が進みやすく、反応装置内面への金属石鹸の付着が促進され、連続的な製造が困難な場合がある。反応装置内の金属石鹸の付着が少なく、より効率的に連続して金属石鹸を製造する場合、水溶液中の無機金属塩の好ましい含有量は、０．０１〜１０重量％の範囲である。 In the aqueous solution of the inorganic metal salt of component b used in the production method of the present invention, the content of the inorganic metal salt is in the range of 0.001 to 20% by weight. When the content is less than 0.001% by weight, the amount of metal soap obtained is remarkably low with respect to the amount of the reaction solution, and the production efficiency is poor. On the other hand, if it exceeds 20% by weight, aggregation of the obtained metal soap particles tends to proceed, the adhesion of the metal soap to the inner surface of the reactor is promoted, and continuous production may be difficult. When metal soap is less likely to adhere to the reaction apparatus and is produced more efficiently and continuously, the preferred content of the inorganic metal salt in the aqueous solution is in the range of 0.01 to 10% by weight.
ａ成分およびｂ成分の調整に用いられる水としては特に制限はなく、一般的に使用されるものを用いても良いが、イオン交換水、精製水、または蒸留水などのように、金属イオンなどの不純物の少ないものが好ましい。また、水溶性金属イオン等の不純物を含有する水を用いる場合は、エチレンジアミン四酢酸ナトリウム（ＥＤＴＡ）などの水溶性キレート剤を添加して水中の金属イオンを水溶性錯塩としてから反応させることが好ましい。このように処理された水を用いた場合、脂肪酸アルカリ塩やアンモニウム塩に対して水中の不純金属イオンが反応しにくくなり、反応時における金属石鹸の凝集が発生し難くなり、その結果、応装置内での金属石鹸の付着が生じにくい。また、水洗により金属石鹸から水溶性の不純金属錯体を除去することができるため、不純分の少ない金属石鹸が得られる。 The water used for the adjustment of the a component and the b component is not particularly limited, and commonly used water may be used. However, metal ions such as ion-exchanged water, purified water, or distilled water may be used. Those having less impurities are preferred. In addition, when water containing impurities such as water-soluble metal ions is used, it is preferable to add a water-soluble chelating agent such as sodium ethylenediaminetetraacetate (EDTA) and react the metal ions in water as water-soluble complex salts. . When water treated in this way is used, it becomes difficult for impure metal ions in water to react with fatty acid alkali salts and ammonium salts, and it is difficult for metal soap to agglomerate during the reaction. It is difficult for metal soap to adhere inside. In addition, since the water-soluble impure metal complex can be removed from the metal soap by washing with water, a metal soap with less impure content can be obtained.
本発明には、外筒の中に内筒が配置された、内外筒間に環状空間を有する図１に示す共軸筒型反応装置を用いる。図１において、１は内筒、２は外筒をそれぞれ表し、３および４は各原料水溶液の供給口であり、５はａ成分とｂ成分を反応して得られる金属石鹸スラリーの吐出口であり、Ｒ１は外筒の内径であり、Ｒ２は内筒の内径を示し、ｎは外筒において内筒が挿入されていない、ａ成分とｂ成分が接触する外筒部分である。 In the present invention, the coaxial cylindrical reactor shown in FIG. 1 having an annular space between the inner and outer cylinders, in which the inner cylinder is disposed in the outer cylinder, is used. In FIG. 1, 1 represents an inner cylinder, 2 represents an outer cylinder, 3 and 4 are supply ports for each raw material aqueous solution, and 5 is a discharge port for a metal soap slurry obtained by reacting the component a and component b. Yes, R1 is the inner diameter of the outer cylinder, R2 is the inner diameter of the inner cylinder, and n is the outer cylinder part where the inner cylinder is not inserted in the outer cylinder and where the a component and b component are in contact.
本発明では、この反応装置を用いて、内外筒間の環状空間３および内筒内の空間４から、ａ成分とｂ成分をそれぞれ流し、外筒のｎの領域にてａ成分とｂ成分を接触させ、その結果、５から金属石鹸スラリーを得る。ａ成分とｂ成分は、反応装置内にポンプを用いて３と４からそれぞれ反応装置内に圧入しても良く、または５から反応装置を減圧し、ａ成分とｂ成分を３と４からそれぞれ反応装置内に吸引しても良い。また本発明に用いられる反応装置は、均一にａ成分とｂ成分を接触させ反応させる上で円筒管であることが好ましいが、各原料の反応状態や所望の粒子径の金属石鹸を調整するために、管断面を楕円や多角形など、形状を円筒形以外のものに変更することができる。
In the present invention, by using this reaction apparatus, the a component and the b component are respectively flowed from the
本発明の製造方法においては、ａ成分とｂ成分は、３および４のいずれから供給してもよく、例えば、ａ成分を３から供給する場合にはｂ成分を４から供給し、ａ成分を４から供給する場合にはｂ成分を３から供給するといった方法が用いられる。その中でも、特にａ成分を３から供給し、ｂ成分を４から供給することが好ましい。このような送液方法を用いた場合、反応装置内面に金属石鹸がより付着しにくくなり、各原料をより均一に反応させることができる。その結果、反応装置内に閉塞がより生じ難く、また均一な粒子形状の金属石鹸を連続して製造できる。 In the production method of the present invention, the a component and the b component may be supplied from either 3 or 4. For example, when the a component is supplied from 3, the b component is supplied from 4, and the a component is supplied. When supplying from 4, the method of supplying b component from 3 is used. Among these, it is particularly preferable to supply the a component from 3 and the b component from 4. When such a liquid feeding method is used, metal soap is less likely to adhere to the inner surface of the reaction apparatus, and each raw material can be reacted more uniformly. As a result, clogging is less likely to occur in the reaction apparatus, and a metal soap having a uniform particle shape can be continuously produced.
本発明の製造方法に用いる反応装置は何れの材質で構成されても良く、例えば高圧にてａ成分とｂ成分とを反応する場合には耐久性のある金属や硬質樹脂などの材質を用いることが好ましい。
外筒の内径（図１におけるＲ１）、内筒の内径（図１におけるＲ２）および外筒において内筒が挿入されていない部分（図１におけるｎ）は、原料の送液能力、各原料の反応状態や所望の粒子径の金属石鹸を調整するために適宜選定すればよい。また、本装置の内筒において、吐出口に段差を有さないよう鋭角に加工されていることが好ましい。このような形状を有する内筒を用いた場合、内筒の吐出口付近における原料の乱流が生じ難くなり、より均一にａ成分とｂ成分とが会合分散し、反応装置内面に金属石鹸が滞留し付着することなく反応することができる。その結果、反応装置内の閉塞がより生じ難く、均一な粒子形状の金属石鹸を連続して製造できる。
また、反応装置の具体例としては、例えば、Ｒ１およびＲ２がそれぞれ１〜５ｍｍと０．１ｍｍ〜２ｍｍであり、かつ、Ｒ１／Ｒ２の値が２〜２０であり、ｎの部分の長さが１５ｍｍ以上のものを用いることができる。そして、この条件を満たす装置に、０．１〜５重量％の濃度を有するａ成分とｂ成分を１〜５００ｍｌ／ｍｉｎの速度で供給することで、反応装置内壁への金属石鹸粒子の付着を抑えたまま、連続的に金属石鹸を反応させることができる。加えて、内筒の先端を鋭角に削ることで、内筒におけるａ成分とｂ成分との接触状態をスムーズにし、さらに反応装置の内壁に金属石鹸が付着しにくくすることができる。
The reaction apparatus used in the production method of the present invention may be composed of any material. For example, when the a component and the b component are reacted at a high pressure, a material such as a durable metal or hard resin is used. Is preferred.
The inner diameter of the outer cylinder (R1 in FIG. 1), the inner diameter of the inner cylinder (R2 in FIG. 1), and the portion of the outer cylinder in which the inner cylinder is not inserted (n in FIG. 1) What is necessary is just to select suitably in order to adjust the reaction state and the metal soap of a desired particle diameter. Moreover, it is preferable that the inner cylinder of the apparatus is processed at an acute angle so that the discharge port does not have a step. When the inner cylinder having such a shape is used, the turbulent flow of the raw material near the discharge port of the inner cylinder is less likely to occur, and the a component and the b component are more uniformly associated and dispersed. It can react without staying and adhering. As a result, clogging in the reaction apparatus is less likely to occur, and a metal soap having a uniform particle shape can be continuously produced.
As specific examples of the reactor, for example, R1 and R2 are 1 to 5 mm and 0.1 mm to 2 mm, respectively, the value of R1 / R2 is 2 to 20, and the length of the n portion is The thing of 15 mm or more can be used. Then, by supplying a component having a concentration of 0.1 to 5% by weight and a component b at a rate of 1 to 500 ml / min to an apparatus satisfying this condition, the metal soap particles adhere to the inner wall of the reactor. The metal soap can be continuously reacted while being suppressed. In addition, by sharpening the tip of the inner cylinder at an acute angle, the contact state between the a component and the b component in the inner cylinder can be made smooth, and metal soap can be made difficult to adhere to the inner wall of the reactor.
本発明の製造方法では、共軸筒型反応装置にする供給するａ成分とｂ成分との混合割合において、ｂ成分中の無機金属塩に対する、ａ成分中の脂肪酸塩の当量比（ａ／ｂ）は０．５〜１．１の範囲である。この条件を満たすために、ａ成分とｂ成分の濃度や送液量、内筒と外筒の内径の比率を調整することが必要である。当量比（ａ／ｂ）が１．１よりも大きい場合、反応後の金属石鹸スラリー中に未反応の脂肪酸可溶塩が多量に存在するようになり、金属石鹸の水に対する親和性が上がる。そのため、金属石鹸スラリーを濾過して金属石鹸を単離する際に、著しく濾過効率が低下する。一方、当量比（ａ／ｂ）が０.５よりも小さい場合、反応中に反応装置の外筒内部に金属石鹸が付着しやすくなる。そのため、各原料を安定に反応させることができなくなることがある。残存不純物を少なくし、生成する金属石鹸スラリーの濾過工程と洗浄工程をより効率的に行うためには、該当量比は０．９５〜１．０５の範囲が特に好ましい。 In the production method of the present invention, the equivalent ratio of the fatty acid salt in the a component to the inorganic metal salt in the b component (a / b) in the mixing ratio of the a component and the b component to be supplied to the coaxial cylindrical reactor. ) Is in the range of 0.5 to 1.1. In order to satisfy this condition, it is necessary to adjust the concentration of the a component and the b component, the liquid feeding amount, and the ratio of the inner diameter of the inner cylinder to the outer cylinder. When the equivalent ratio (a / b) is larger than 1.1, a large amount of unreacted fatty acid-soluble salt is present in the metal soap slurry after the reaction, and the affinity of the metal soap for water increases. Therefore, when the metal soap slurry is filtered to isolate the metal soap, the filtration efficiency is significantly reduced. On the other hand, when the equivalent ratio (a / b) is smaller than 0.5, metal soap tends to adhere to the inside of the outer cylinder of the reactor during the reaction. Therefore, it may be impossible to react each raw material stably. In order to reduce the residual impurities and more efficiently perform the filtration step and the washing step of the resulting metal soap slurry, the amount ratio is particularly preferably in the range of 0.95 to 1.05.
本発明の製造方法においては、ａ成分が反応装置中のｎの部分を移動する線速度（ｍ/ｓ）と、ｂ成分が反応装置中のｎの部分を移動する線速度（ｍ/ｓ）との比率は、前述した当量比を満たすことができれば特に制約はない。
本発明の製造方法において、共軸二重筒型反応装置を用いてａ成分とｂ成分を反応することにより得られた金属石鹸スラリーは、一般的な濾過装置を使用して金属石鹸ケーキと濾液に分離することができる。この金属石鹸ケーキは、水溶性無機塩などの不純物量を低下させるために、温水などで充分に洗浄した後、乾燥処理することにより、金属石鹸微粒子が得られる。なお、濾過水洗により水溶性無機塩などの不純物を除去することが困難な場合は、浸透膜などを用いて金属石鹸スラリーや金属石鹸ケーキから不純物を除去するなどの方法を用いてもよい。
この操作により得られた金属石鹸スラリーや金属石鹸ケーキを乾燥処理して、金属石鹸の粉体を得ることができる。また、乾燥後の金属石鹸の凝集が高い場合は、通常の粉砕機を用いて所望の粒子径にまで解砕することができる。乾燥は常圧で行ってもよいが、より効率的に乾燥するために、減圧乾燥、真空乾燥、凍結乾燥を行ってもよい。また、低沸点溶剤などで金属石鹸ケーキを洗浄処理した後、得られた金属石鹸ケーキを乾燥してもよい。この際用いられる低沸点溶剤としては、金属石鹸から水を効率よく除去しうるものが好ましく、例えばメタノール、エタノール、アセトン、塩化メチレンなどが挙げられる。
In the production method of the present invention, the linear velocity (m / s) at which the a component moves through the n portion in the reactor, and the linear velocity (m / s) at which the b component moves through the n portion in the reactor. The ratio is not particularly limited as long as the above-described equivalent ratio can be satisfied.
In the production method of the present invention, a metal soap slurry obtained by reacting the component a and the component b using a coaxial double cylinder reactor is obtained by using a general filter device and a metal soap cake and a filtrate. Can be separated. In order to reduce the amount of impurities such as water-soluble inorganic salts, the metal soap cake is sufficiently washed with warm water and then dried to obtain metal soap fine particles. In addition, when it is difficult to remove impurities such as water-soluble inorganic salt by filtration water washing, a method of removing impurities from a metal soap slurry or metal soap cake using a permeable membrane or the like may be used.
The metal soap slurry or metal soap cake obtained by this operation can be dried to obtain metal soap powder. Moreover, when the aggregation of the metal soap after drying is high, it can be crushed to a desired particle size using a normal pulverizer. Drying may be performed at normal pressure, but in order to dry more efficiently, drying under reduced pressure, vacuum drying, or freeze drying may be performed. Further, after the metal soap cake is washed with a low boiling point solvent or the like, the obtained metal soap cake may be dried. As the low boiling point solvent used in this case, those which can efficiently remove water from a metal soap are preferable, and examples thereof include methanol, ethanol, acetone, methylene chloride and the like.
本発明の製造方法は、平均粒子径が３〜１００μｍである金属石鹸を安定に連続製造できるほか、特に平均粒子径が０．０１μｍ〜３μｍの微細な金属石鹸をも効率的に連続製造できる。０．０１μｍ〜３μｍの微細な金属石鹸は表面積が大きいため反応装置内への付着性が高く、かつ凝集性が特に高い。そのため反応装置内へ付着した金属石鹸粒子の周辺に、粒子が更に付着蓄積しやすい。そのため、既知の製造方法を用いて０．０１μｍ〜３μｍの微細な金属石鹸を製造した場合、長時間にわたる安定製造が困難な場合がある。このような微細な金属石鹸を製造するにあたり本発明の製造方法は有効であり、平均粒子径が０．０１μｍ〜３μｍの微細な金属石鹸を連続製造する際に、反応装置内に金属石鹸が凝集し付着しにくい。 The production method of the present invention can stably and continuously produce a metal soap having an average particle diameter of 3 to 100 μm, and can also efficiently and continuously produce a fine metal soap having an average particle diameter of 0.01 to 3 μm. Since the fine metal soap of 0.01 μm to 3 μm has a large surface area, the adhesion to the reaction apparatus is high and the cohesion is particularly high. Therefore, the particles are more likely to adhere and accumulate around the metal soap particles adhering to the reactor. Therefore, when a fine metal soap of 0.01 μm to 3 μm is manufactured using a known manufacturing method, stable manufacturing over a long time may be difficult. In producing such a fine metal soap, the production method of the present invention is effective. When continuously producing a fine metal soap having an average particle size of 0.01 μm to 3 μm, the metal soap aggregates in the reactor. It is hard to adhere.
０．０１μｍ〜３μｍの微細な金属石鹸を製造する場合、ａ成分とｂ成分は、生成する金属石鹸の結晶転移開始温度以下で反応することが必要である。実際の反応時の温度は、得られる金属石鹸の脂肪酸鎖および金属の種類により異なるが、例えばカルシウムステアレートの微細粒子を製造する場合、９４℃以下の温度で製造することが好ましい。９４℃を超える温度で反応を行うと、金属石鹸の微細粒子同士の凝集が起こり、平均粒子径が大きくなることがある。また、平均粒子径が０．０１μｍ〜１μｍである微細な金属石鹸粒子を得るためには、７０℃以下のできる限り低い温度条件にて反応から乾燥までを行うことが好ましい。 When manufacturing a fine metal soap of 0.01 μm to 3 μm, it is necessary that the a component and the b component react at a temperature lower than the crystal transition start temperature of the metal soap to be produced. The actual reaction temperature varies depending on the fatty acid chain and metal type of the resulting metal soap. For example, when producing calcium stearate fine particles, it is preferably produced at a temperature of 94 ° C. or lower. When the reaction is carried out at a temperature exceeding 94 ° C., the fine particles of the metal soap may aggregate and the average particle size may increase. Moreover, in order to obtain fine metal soap particles having an average particle diameter of 0.01 μm to 1 μm, it is preferable to carry out from reaction to drying under the lowest possible temperature condition of 70 ° C. or less.
以下、実施例および比較例により本発明を更に詳しく説明するが、本発明はこれらの実施例などにより何ら限定されるものではない。
実施例１
ａ成分として７０℃に調整したステアリン酸カリウムの０．５重量％水溶液、ｂ成分として７０℃に調整した硫酸亜鉛の０.１２重量％水溶液をそれぞれ用意した。また、外円筒の内径（Ｒ１）が２ｍｍ、内円筒の内径（Ｒ２）が０.３ｍｍ、および内円筒の外径が１.６ｍｍであり（Ｒ１／Ｒ２が６．７であり）、外円筒のｎの部分の長さが８０ｍｍである図１の反応装置を用意した。次に、定容ポンプを用いて、供給口３からｂ成分、供給口４からからａ成分をそれぞれ供給した。反応装置に供給する際のａ成分とｂ成分の供給速度は１０ｍｌ／ｍｉｎとした。このような条件で各液を供給すると、ｂ成分中の硫酸亜鉛に対する、ａ成分中のステアリン酸カリウムの当量比が１.０、またｎの部分において、４から供給されたａ成分と３から供給されたｂ成分の線速度比は１６：１であった。
この条件で３０分間製造を続けたところ、反応装置の内壁に金属石鹸は付着せず、ａ成分とｂ成分は詰まることなく安定に反応装置に供給できた。また、平均粒子径が０.２７μｍのステアリン酸亜鉛粒子が得られた。
EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further in detail, this invention is not limited at all by these Examples.
Example 1
A 0.5 wt% aqueous solution of potassium stearate adjusted to 70 ° C. was prepared as component a, and a 0.12 wt% aqueous solution of zinc sulfate adjusted to 70 ° C. was prepared as component b. The inner diameter (R1) of the outer cylinder is 2 mm, the inner diameter (R2) of the inner cylinder is 0.3 mm, and the outer diameter of the inner cylinder is 1.6 mm (R1 / R2 is 6.7). The reactor of FIG. 1 in which the length of the n portion of 80 mm was 80 mm was prepared. Next, the component b was supplied from the
When the production was continued for 30 minutes under these conditions, the metal soap did not adhere to the inner wall of the reactor, and the components a and b could be stably supplied to the reactor without clogging. In addition, zinc stearate particles having an average particle size of 0.27 μm were obtained.
実施例２
実施例１と同じ装置を用い、ａ成分として７５℃に調整したミリスチン酸アンモニウムの１重量％水溶液、ｂ成分として７５℃に調整した塩化カルシウムの０.０２４重量％の水溶液をそれぞれ用意し、定容ポンプを用いて、供給口３からｂ成分、供給口４からからａ成分をそれぞれ供給した。反応装置に供給する際のａ成分の４への供給速度は１ｍｌ／ｍｉｎとし、ｂ成分の３への供給速度は１０ｍｌ／ｍｉｎとした。このような条件にて各液を供給すると、ｂ成分中の塩化カルシウムに対する、ａ成分中のミリスチン酸アンモニウムの当量比が０.９９〜１.００、またｎの部分において、４から供給されたａ成分と３から供給されたｂ成分の線速度比は５：３であった。
この条件で３０分間製造を続けたところ、反応装置の内壁に金属石鹸が付着せず、ａ成分とｂ成分は詰まることなく安定に反応装置に供給できた。また、平均流子径が０．５μｍのミリスチン酸カルシウム粒子が得られた。
Example 2
Using the same apparatus as in Example 1, a 1% by weight aqueous solution of ammonium myristate adjusted to 75 ° C. was prepared as component a, and a 0.024% by weight aqueous solution of calcium chloride adjusted to 75 ° C. was prepared as component b. The component b was supplied from the
When the production was continued for 30 minutes under these conditions, metal soap did not adhere to the inner wall of the reactor, and the components a and b could be stably supplied to the reactor without clogging. Moreover, calcium myristate particles having an average flow diameter of 0.5 μm were obtained.
実施例３
実施例１と同じ濃度と成分を含有する、６０℃に液温を調整したａ成分とｂ成分を用意した。一方、実施例１と同じ外円筒と内円筒の内径、内円筒の外径、およびｎの部分長を有し、かつ内円筒におけるｂ成分の吐出口を鋭角に加工し、内円筒の先端における外径を０．７ｍｍとした装置を用意した。そして定容ポンプにて供給口３からａ成分、供給口４からからｂ成分をそれぞれ供給した。反応装置に供給する際のａ成分とｂ成分の供給速度は１０ｍｌ／ｍｉｎとした。このような条件にて各液を供給すると、ｂ成分中の硫酸亜鉛に対する、ａ成分中のステアリン酸カリウムの当量比が１.０、またｎの部分において、３から供給されたａ成分と４から供給されたｂ成分の線速度比は１：３１であった。
この条件で３０分間製造を続けたところ、反応装置の内壁に金属石鹸が付着せず、ａ成分とｂ成分を詰まることなく安定に反応装置に供給することができた。また、平均粒子径が０.０９μｍのステアリン酸亜鉛粒子が得られた。
Example 3
The a component and b component which adjusted the liquid temperature to 60 degreeC containing the same density | concentration and component as Example 1 were prepared. On the other hand, it has the same inner cylinder, inner cylinder outer diameter, inner cylinder outer diameter, and n partial length as in Example 1, and the b component discharge port in the inner cylinder is processed into an acute angle, and at the tip of the inner cylinder. A device having an outer diameter of 0.7 mm was prepared. And a component and the b component were supplied from the
When the production was continued for 30 minutes under these conditions, metal soap did not adhere to the inner wall of the reactor, and the components a and b could be stably supplied to the reactor without clogging. Further, zinc stearate particles having an average particle diameter of 0.09 μm were obtained.
比較例１
実施例１と同じ条件で調整したａ成分、ｂ成分を用意した。そして、ａ成分とｂ成分の２つの液を同時に吸入し吐出できるラインホモミクサーを用い、ａ成分とｂ成分を同時にミキサーから吸入した。反応装置に吸入する際のａ成分の供給速度は１０ｍｌ／ｍｉｎ、ｂ成分の供給速度は２５ｍｌ／ｍｉｎ、このときのｂ成分中の硫酸亜鉛に対する、ａ成分中のステアリン酸カリウムの当量比は０.４であった。そしてａ成分とｂ成分とを反応して得られた金属石鹸スラリーをラインホモミクサーから連続的に吐出した。このような製造方法を３０分間続けたところ、ラインホモミクサーの内部とスラリーの吐出口付近にステアリン酸亜鉛が多量に付着し、ａ成分とｂ成分を安定して反応装置に供給できなかった。その結果、ステアリン酸亜鉛粒子を連続して製造することができなかった。
Comparative Example 1
The a component and b component adjusted under the same conditions as in Example 1 were prepared. Then, using a line homomixer capable of simultaneously sucking and discharging the two liquids of component a and component b, the components a and b were simultaneously sucked from the mixer. The supply rate of component a during inhalation into the reactor is 10 ml / min, the supply rate of component b is 25 ml / min, and the equivalent ratio of potassium stearate in component a to zinc sulfate in component b at this time is 0. .4. And the metal soap slurry obtained by reacting a component and b component was discharged continuously from the line homomixer. When such a production method was continued for 30 minutes, a large amount of zinc stearate adhered to the inside of the line homomixer and the vicinity of the discharge port of the slurry, and the components a and b could not be stably supplied to the reactor. As a result, the zinc stearate particles could not be produced continuously.
１：内筒、２：外筒、３：原料水溶液ａ成分またはｂ成分の供給口、４：原料水溶液ａ成分またはｂ成分の供給口、５：ａ成分およびｂ成分が反応した金属石鹸スラリーの吐出口、Ｒ１：外筒の内径、Ｒ２：内筒の内径、ｎ：外筒において内筒が挿入されていない部分 1: Inner cylinder, 2: Outer cylinder, 3: Supply port of raw material aqueous solution a or b component, 4: Supply port of raw material aqueous solution a or b component, 5: Metal soap slurry in which a component and b component reacted Discharge port, R1: inner diameter of the outer cylinder, R2: inner diameter of the inner cylinder, n: portion of the outer cylinder where the inner cylinder is not inserted
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| KR101040470B1 (en) * | 2011-03-29 | 2011-06-09 | 정재홍 | Soap-scrub process |
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