JP2014084256A - Method for producing zinc oxide particle - Google Patents
Method for producing zinc oxide particle Download PDFInfo
- Publication number
- JP2014084256A JP2014084256A JP2012235107A JP2012235107A JP2014084256A JP 2014084256 A JP2014084256 A JP 2014084256A JP 2012235107 A JP2012235107 A JP 2012235107A JP 2012235107 A JP2012235107 A JP 2012235107A JP 2014084256 A JP2014084256 A JP 2014084256A
- Authority
- JP
- Japan
- Prior art keywords
- zinc oxide
- zinc
- oxide particles
- particles
- poe
- 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
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 256
- 239000002245 particle Substances 0.000 title claims abstract description 176
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 128
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 75
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000002904 solvent Substances 0.000 claims abstract description 27
- 229920005862 polyol Polymers 0.000 claims abstract description 25
- 150000003077 polyols Chemical class 0.000 claims abstract description 24
- 150000003751 zinc Chemical class 0.000 claims abstract description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 14
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000011187 glycerol Nutrition 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 claims abstract description 4
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920000166 polytrimethylene carbonate Polymers 0.000 claims abstract description 4
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 abstract description 26
- 238000000034 method Methods 0.000 abstract description 18
- 238000009826 distribution Methods 0.000 abstract description 14
- 238000010304 firing Methods 0.000 abstract description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 49
- 239000000284 extract Substances 0.000 description 40
- -1 SF-15 Chemical compound 0.000 description 36
- 239000002002 slurry Substances 0.000 description 35
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 33
- 238000003756 stirring Methods 0.000 description 28
- 238000006243 chemical reaction Methods 0.000 description 23
- 239000003921 oil Substances 0.000 description 23
- 235000019198 oils Nutrition 0.000 description 23
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 21
- 239000007787 solid Substances 0.000 description 21
- 239000000126 substance Substances 0.000 description 21
- 239000000945 filler Substances 0.000 description 20
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 description 19
- 239000011164 primary particle Substances 0.000 description 18
- 239000002537 cosmetic Substances 0.000 description 17
- 235000014113 dietary fatty acids Nutrition 0.000 description 16
- 239000000194 fatty acid Substances 0.000 description 16
- 229930195729 fatty acid Natural products 0.000 description 16
- 238000005406 washing Methods 0.000 description 16
- 238000003828 vacuum filtration Methods 0.000 description 15
- 238000010438 heat treatment Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 14
- 229920005989 resin Polymers 0.000 description 14
- 239000011347 resin Substances 0.000 description 14
- 239000004166 Lanolin Substances 0.000 description 12
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 12
- 235000019388 lanolin Nutrition 0.000 description 12
- 229940039717 lanolin Drugs 0.000 description 12
- 239000004246 zinc acetate Substances 0.000 description 12
- 239000004359 castor oil Substances 0.000 description 11
- 235000019438 castor oil Nutrition 0.000 description 11
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 238000003917 TEM image Methods 0.000 description 10
- 238000000635 electron micrograph Methods 0.000 description 10
- 229920000642 polymer Polymers 0.000 description 10
- 239000011342 resin composition Substances 0.000 description 10
- 230000017525 heat dissipation Effects 0.000 description 9
- 230000000704 physical effect Effects 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000012266 salt solution Substances 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 150000004665 fatty acids Chemical class 0.000 description 7
- 230000005484 gravity Effects 0.000 description 7
- 238000001291 vacuum drying Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 150000003752 zinc compounds Chemical class 0.000 description 6
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 5
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 description 5
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- DSSYKIVIOFKYAU-OIBJUYFYSA-N (S)-camphor Chemical compound C1C[C@]2(C)C(=O)C[C@H]1C2(C)C DSSYKIVIOFKYAU-OIBJUYFYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229920001214 Polysorbate 60 Polymers 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- GPLRAVKSCUXZTP-UHFFFAOYSA-N diglycerol Chemical compound OCC(O)COCC(O)CO GPLRAVKSCUXZTP-UHFFFAOYSA-N 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- ZQBAKBUEJOMQEX-UHFFFAOYSA-N phenyl salicylate Chemical compound OC1=CC=CC=C1C(=O)OC1=CC=CC=C1 ZQBAKBUEJOMQEX-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000344 soap Substances 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 229920003169 water-soluble polymer Polymers 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 238000004438 BET method Methods 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 150000005215 alkyl ethers Chemical class 0.000 description 3
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 3
- 235000013871 bee wax Nutrition 0.000 description 3
- 235000015278 beef Nutrition 0.000 description 3
- 239000012166 beeswax Substances 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 235000019864 coconut oil Nutrition 0.000 description 3
- 239000003240 coconut oil Substances 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000010445 mica Substances 0.000 description 3
- 229910052618 mica group Inorganic materials 0.000 description 3
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 3
- 239000008107 starch Substances 0.000 description 3
- 235000019698 starch Nutrition 0.000 description 3
- 239000003760 tallow Substances 0.000 description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 239000001993 wax Substances 0.000 description 3
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 3
- 229940007718 zinc hydroxide Drugs 0.000 description 3
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 3
- YBJHBAHKTGYVGT-ZKWXMUAHSA-N (+)-Biotin Chemical compound N1C(=O)N[C@@H]2[C@H](CCCCC(=O)O)SC[C@@H]21 YBJHBAHKTGYVGT-ZKWXMUAHSA-N 0.000 description 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 2
- DSEKYWAQQVUQTP-XEWMWGOFSA-N (2r,4r,4as,6as,6as,6br,8ar,12ar,14as,14bs)-2-hydroxy-4,4a,6a,6b,8a,11,11,14a-octamethyl-2,4,5,6,6a,7,8,9,10,12,12a,13,14,14b-tetradecahydro-1h-picen-3-one Chemical compound C([C@H]1[C@]2(C)CC[C@@]34C)C(C)(C)CC[C@]1(C)CC[C@]2(C)[C@H]4CC[C@@]1(C)[C@H]3C[C@@H](O)C(=O)[C@@H]1C DSEKYWAQQVUQTP-XEWMWGOFSA-N 0.000 description 2
- GHOKWGTUZJEAQD-ZETCQYMHSA-N (D)-(+)-Pantothenic acid Chemical compound OCC(C)(C)[C@@H](O)C(=O)NCCC(O)=O GHOKWGTUZJEAQD-ZETCQYMHSA-N 0.000 description 2
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 2
- RZRNAYUHWVFMIP-KTKRTIGZSA-N 1-oleoylglycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-KTKRTIGZSA-N 0.000 description 2
- WNWHHMBRJJOGFJ-UHFFFAOYSA-N 16-methylheptadecan-1-ol Chemical compound CC(C)CCCCCCCCCCCCCCCO WNWHHMBRJJOGFJ-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 244000144730 Amygdalus persica Species 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 2
- ZCTQGTTXIYCGGC-UHFFFAOYSA-N Benzyl salicylate Chemical compound OC1=CC=CC=C1C(=O)OCC1=CC=CC=C1 ZCTQGTTXIYCGGC-UHFFFAOYSA-N 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 108010035532 Collagen Proteins 0.000 description 2
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- 229920000742 Cotton Polymers 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- 239000011627 DL-alpha-tocopherol Substances 0.000 description 2
- 235000001815 DL-alpha-tocopherol Nutrition 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 2
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- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
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- 150000003973 alkyl amines Chemical class 0.000 description 2
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- 239000002280 amphoteric surfactant Substances 0.000 description 2
- RWZYAGGXGHYGMB-UHFFFAOYSA-N anthranilic acid Chemical compound NC1=CC=CC=C1C(O)=O RWZYAGGXGHYGMB-UHFFFAOYSA-N 0.000 description 2
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- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 2
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- 238000004898 kneading Methods 0.000 description 2
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- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- 239000012860 organic pigment Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229960000969 phenyl salicylate Drugs 0.000 description 2
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- 238000011085 pressure filtration Methods 0.000 description 2
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- 239000004711 α-olefin Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
本発明は、酸化亜鉛粒子の製造方法に関する。 The present invention relates to a method for producing zinc oxide particles.
酸化亜鉛粒子は、化粧品分野、電気・電子分野等の多くの分野において使用されている。このような用途において使用される酸化亜鉛粒子は、一般的には焼成を経る製造方法によって得たものが知られている。しかしながら、焼成による製造は焼成の際に粒子同士が融着して形成された粗大粒子の影響により粒子サイズが不均一なものとなってしまうという点で好ましくない。 Zinc oxide particles are used in many fields such as the cosmetics field and the electric / electronic field. The zinc oxide particles used in such applications are generally obtained by a production method that undergoes firing. However, the production by calcination is not preferable in that the particle size becomes non-uniform due to the influence of coarse particles formed by fusing the particles together during calcination.
また、焼成を経ずに酸化亜鉛粒子を得る方法はいくつか知られているが、不純物が混在しやすく、純度が高い酸化亜鉛粒子を焼成工程を経ずに得ることは困難である。 Several methods for obtaining zinc oxide particles without firing are known. However, it is difficult to obtain zinc oxide particles having high purity without going through the firing step.
特許文献1には、水酸化亜鉛を2価以上の多価アルコールまたはそれらのアルキルエーテル又はそれらの混合溶液中で分散・加熱処理して、酸化亜鉛微粒子を得ることが記載されている。しかし、このような製造方法は、亜鉛化合物を塩基で分解することで得られる水酸化亜鉛を更に分解して酸化亜鉛を得る方法であり、本製法とは異なる。また、使用する塩基に含まれる不純物や金属イオンによって、得られる酸化亜鉛粒子の形態に影響を及ぼす可能性があるだけでなく、残存する塩基成分によって酸化亜鉛の純度を低下させてしまう可能性があるという問題がある。 Patent Document 1 describes that zinc hydroxide fine particles are obtained by dispersing and heating zinc hydroxide in a dihydric or higher polyhydric alcohol or an alkyl ether thereof or a mixed solution thereof. However, such a production method is a method in which zinc hydroxide obtained by further decomposing a zinc compound with a base is further decomposed to obtain zinc oxide, which is different from the present production method. In addition, impurities and metal ions contained in the base used may not only affect the form of the resulting zinc oxide particles, but may also reduce the purity of zinc oxide due to the remaining base component. There is a problem that there is.
特許文献2には、亜鉛化合物と酢酸とグリコールを混合して混合液を調製し、加熱条件で保持することによって得る酸化亜鉛微粒子の製造方法が記載されている。しかし、このような製造方法は、原料となる亜鉛化合物を完全に溶解した溶液を加熱することで沈殿物を得る方法であり、本製法とは異なるものである。また、特許文献2によって得られる粒子は、反応液から酸化亜鉛粒子を単離するために遠心分離を行う必要がある。これは、得られる酸化亜鉛の収率が低く、反応液の酸化亜鉛濃度が低いため、真空ろ過や、プレスフィルターを用いた加圧ろ過では、酸化亜鉛粒子を捕捉・単離することが困難なためであり、工業生産の観点から好ましいものではない。発明者らによって試験したところ、真空ろ過や加圧ろ過による粒子の単離は困難であった。また、反応条件によっては反応後に粒子が得られない場合があり、粒子が得られた場合においても粒度分布がブロードで、凝集が強い酸化亜鉛粒子となった。 Patent Document 2 describes a method for producing zinc oxide fine particles obtained by mixing a zinc compound, acetic acid, and glycol to prepare a mixed solution and holding the mixture under heating conditions. However, such a production method is a method of obtaining a precipitate by heating a solution in which a zinc compound as a raw material is completely dissolved, and is different from the present production method. Moreover, it is necessary to centrifuge the particle | grains obtained by patent document 2 in order to isolate a zinc oxide particle from a reaction liquid. This is because the yield of zinc oxide obtained is low and the concentration of zinc oxide in the reaction solution is low, so it is difficult to capture and isolate zinc oxide particles by vacuum filtration or pressure filtration using a press filter. Therefore, it is not preferable from the viewpoint of industrial production. When tested by the inventors, it was difficult to isolate particles by vacuum filtration or pressure filtration. Depending on the reaction conditions, particles may not be obtained after the reaction, and even when particles were obtained, zinc oxide particles having a broad particle size distribution and strong aggregation were obtained.
更に、酸化亜鉛粒子の化粧品への使用に際してはその形状によって使用感や紫外線遮蔽性能が変化するため、目的に応じた効果を得るために、高度に形状や粒子径を制御することが好ましい。電子部品材料、例えば、放熱性材料として使用する場合においても、組成物中の充填率を高めるためには、粒子形状や粒子径において均一性が高い粒子を得ることが望まれている。 Furthermore, when the zinc oxide particles are used in cosmetics, the feeling of use and the ultraviolet shielding performance vary depending on the shape, and therefore it is preferable to highly control the shape and particle diameter in order to obtain an effect according to the purpose. Even when used as an electronic component material, for example, a heat dissipation material, in order to increase the filling rate in the composition, it is desired to obtain particles having high uniformity in particle shape and particle diameter.
本発明は、このような問題に鑑み、焼成工程を経ることなく、粒子径や粒径分布がコントロールされ、アルカリフリーであり不純物が少なく、純度が高い酸化亜鉛粒子を得ることができる酸化亜鉛粒子の製造方法を提供することを目的とするものである。 In view of such a problem, the present invention provides a zinc oxide particle in which the particle diameter and the particle size distribution are controlled without passing through a firing step, and an alkali-free, low-impurity, high-purity zinc oxide particle can be obtained. An object of the present invention is to provide a manufacturing method.
本発明は、シードとなる酸化亜鉛を、亜鉛塩を溶解したポリオール系溶媒又は亜鉛塩を溶解した水とポリオール系溶媒の混合溶液中で反応する工程を有し、前記ポリオール系溶媒は、エチレングリコール、ジエチレングリコール、プロピレングリコール、1,3−プロパンジオール、1,3−ブタンジオール、トリエチレングリコール及びグリセリンからなる群より選択される少なくとも1種の化合物であることを特徴とする酸化亜鉛粒子の製造方法である。 The present invention includes a step of reacting zinc oxide as a seed in a polyol solvent in which a zinc salt is dissolved or in a mixed solution of water in which a zinc salt is dissolved and a polyol solvent, and the polyol solvent includes ethylene glycol. And at least one compound selected from the group consisting of diethylene glycol, propylene glycol, 1,3-propanediol, 1,3-butanediol, triethylene glycol, and glycerin. It is.
本発明の酸化亜鉛粒子の製造方法は、上述したものであることによって、焼成工程を経ずに純度が高い酸化亜鉛粒子を得ることができるという点で好ましいものである。更に、使用する溶媒、濃度、反応温度、反応時間等を変化させることによって、種々の形状・粒径分布のものを得るためのコントロールを容易に行うことができる。このため、目的とする酸化亜鉛粒子を安定して製造することができるという利点も有する。 The method for producing zinc oxide particles of the present invention is preferable in that the zinc oxide particles having high purity can be obtained without going through the firing step by the above-described method. Furthermore, by changing the solvent used, the concentration, the reaction temperature, the reaction time, etc., it is possible to easily perform control for obtaining various shapes and particle size distributions. For this reason, it has the advantage that the target zinc oxide particle can be manufactured stably.
本発明の酸化亜鉛粒子の製造方法は、シードとなる酸化亜鉛を、亜鉛塩を溶解したポリオール系溶媒又は亜鉛塩を溶解した水とポリオール系溶媒の混合溶液中で反応する工程を有することに特徴を有するものである。このような製造方法によって、粒子径や粒径分布がコントロールされた酸化亜鉛粒子を焼成工程を経ることなく安定して得ることができるという利点を有する。 The method for producing zinc oxide particles of the present invention includes a step of reacting zinc oxide as a seed in a polyol solvent in which a zinc salt is dissolved or in a mixed solution of water in which a zinc salt is dissolved and a polyol solvent. It is what has. By such a production method, there is an advantage that zinc oxide particles whose particle size and particle size distribution are controlled can be stably obtained without going through a firing step.
上述したような酸化亜鉛粒子の製造においては、シードとなる微粒子酸化亜鉛を使用する。上記シードとなる酸化亜鉛としては特に限定されるものではないが、粒子径が0.005〜1.0μmであることが好ましい。上記シードとなる酸化亜鉛の粒子径は、0.01〜1.0μmであることがより好ましく、0.01〜0.8μmであることが更に好ましい。酸化亜鉛の粒子径は、BET法によって求められる比表面積と同一の表面積を有する球の直径に相当する。すなわち、粒子径は、全自動BET比表面積測定装置Macsorb(Mountech社製)により測定して求めた比表面積:Sgと、酸化亜鉛の真比重:ρから、下記計算式により求めた値である。
粒子径(μm)=[6/(Sg×ρ)]
(Sg(m2/g):比表面積、ρ(g/cm3):粒子の真比重)
なお、粒子の真比重:ρは、酸化亜鉛の真比重の値である5.6を上記計算に用いた。
In the manufacture of zinc oxide particles as described above, fine zinc oxide serving as a seed is used. Although it does not specifically limit as zinc oxide used as the said seed, It is preferable that a particle diameter is 0.005-1.0 micrometer. The particle diameter of zinc oxide serving as the seed is more preferably 0.01 to 1.0 μm, and still more preferably 0.01 to 0.8 μm. The particle diameter of zinc oxide corresponds to the diameter of a sphere having the same surface area as that obtained by the BET method. That is, the particle diameter is a value obtained by the following formula from specific surface area: Sg determined by a fully automatic BET specific surface area measuring device Macsorb (manufactured by Mountaintech) and true specific gravity of ρ: ρ.
Particle diameter (μm) = [6 / (Sg × ρ)]
(Sg (m 2 / g): specific surface area, ρ (g / cm 3 ): true specific gravity of particles)
Note that the true specific gravity of the particles: ρ was 5.6, which is the value of the true specific gravity of zinc oxide.
原料として使用することができるシードとなる酸化亜鉛としては特に限定されず、公知の方法によって製造された酸化亜鉛を使用することができる。市販のものとしては、堺化学工業社製FINEX−75、FINEX−50、FINEX−30、微細酸化亜鉛、SF−15、酸化亜鉛1種等を挙げることができる。 It does not specifically limit as a seed zinc oxide which can be used as a raw material, The zinc oxide manufactured by the well-known method can be used. Examples of commercially available products include FINEX-75, FINEX-50, FINEX-30, fine zinc oxide, SF-15, and zinc oxide 1 type manufactured by Sakai Chemical Industry.
本発明の酸化亜鉛粒子の製造方法において使用する亜鉛塩は特に限定されず、酢酸亜鉛、硝酸亜鉛、硫酸亜鉛、塩化亜鉛、ぎ酸亜鉛等を挙げることができる。亜鉛塩のなかでも、特に酢酸亜鉛を使用した場合に好適に酸化亜鉛粒子が得られる。これらの亜鉛塩化合物のうち、2種以上を併用して使用するものであってもよい。亜鉛塩溶液中の亜鉛塩濃度は0.005〜4.00mol/lであることが好ましく、特に、酢酸亜鉛溶液中の亜鉛塩濃度は、0.005〜2.00mol/lであることが好ましい。 The zinc salt used in the method for producing zinc oxide particles of the present invention is not particularly limited, and examples thereof include zinc acetate, zinc nitrate, zinc sulfate, zinc chloride, and zinc formate. Among the zinc salts, zinc oxide particles are suitably obtained particularly when zinc acetate is used. Of these zinc salt compounds, two or more may be used in combination. The zinc salt concentration in the zinc salt solution is preferably 0.005 to 4.00 mol / l, and in particular, the zinc salt concentration in the zinc acetate solution is preferably 0.005 to 2.00 mol / l. .
また、これらの亜鉛塩溶液は、酸化亜鉛を酸で溶解することで調製したものであっても良い。この場合に使用する酸化亜鉛の粒子形状、粒子サイズは特に限定されないが、不純物をなるべく少なくするという観点から、酸化亜鉛のZn純度は95%以上であることが好ましい。また、酸としては、酢酸、硝酸、硫酸、塩酸、ぎ酸、クエン酸、蓚酸、プロピオン酸、マロン酸、ステアリン酸等が挙げられるが、特に酢酸を使用することが好ましい。 These zinc salt solutions may be prepared by dissolving zinc oxide with an acid. The particle shape and particle size of zinc oxide used in this case are not particularly limited, but from the viewpoint of reducing impurities as much as possible, the zinc purity of zinc oxide is preferably 95% or more. Examples of the acid include acetic acid, nitric acid, sulfuric acid, hydrochloric acid, formic acid, citric acid, succinic acid, propionic acid, malonic acid, stearic acid and the like, and it is particularly preferable to use acetic acid.
本発明の酸化亜鉛粒子の製造方法においては、ポリオール系溶媒又はポリオール系溶媒と水の混合溶媒中で反応を行うものである。これによって、水単独での反応に対し、水に対する溶解性とは別のポリオールに対する溶解性を利用して粒子の溶解析出速度を任意に制御することで様々なサイズ、形状の粒子を得ることができる。また、ポリオールの沸点を利用して常圧下の反応においても反応温度を100℃以上に上げることができ、これにより酸化亜鉛粒子のサイズ、形状についての広範な制御が可能になる、という点で好ましい酸化亜鉛粒子を得ることができる。 In the method for producing zinc oxide particles of the present invention, the reaction is carried out in a polyol solvent or a mixed solvent of a polyol solvent and water. This makes it possible to obtain particles of various sizes and shapes by arbitrarily controlling the dissolution and precipitation rate of particles by utilizing the solubility in polyols different from the solubility in water for the reaction with water alone. it can. In addition, the reaction temperature can be raised to 100 ° C. or higher even in a reaction under normal pressure using the boiling point of the polyol, which is preferable in that it enables a wide range of control over the size and shape of the zinc oxide particles. Zinc oxide particles can be obtained.
本発明において使用することができるポリオール系溶媒は、エチレングリコール、ジエチレングリコール、プロピレングリコール、1,3−プロパンジオール、1,3−ブタンジオール、トリエチレングリコール及びグリセリンからなる群から選択される少なくとも1種の化合物である。これらの化合物の2種以上を併用してもよいし、これらの化合物の2種以上と水とを併用してもよい。 The polyol solvent that can be used in the present invention is at least one selected from the group consisting of ethylene glycol, diethylene glycol, propylene glycol, 1,3-propanediol, 1,3-butanediol, triethylene glycol, and glycerin. It is a compound of this. Two or more of these compounds may be used in combination, or two or more of these compounds and water may be used in combination.
水とポリオール系溶媒の混合溶媒を使用する場合は、ポリオール系溶媒の混合割合が5%以上の範囲で混合することが好ましい。水とポリオール系溶媒との配合比は、得られる粒子の形状、アスペクト比、一次粒子径に影響を与えるものであることから、目的に応じてこれらを任意の割合で調整することが好ましい。 When using a mixed solvent of water and a polyol solvent, it is preferable to mix in a range where the mixing ratio of the polyol solvent is 5% or more. Since the compounding ratio of water and the polyol solvent affects the shape, aspect ratio, and primary particle size of the particles obtained, it is preferable to adjust them at an arbitrary ratio according to the purpose.
スラリーの調製方法は特に限定されず、例えば、上記シードとなる酸化亜鉛を亜鉛塩溶液に添加し、18〜30℃で10〜30分間、分散させることによって、シードとなる酸化亜鉛の濃度が10〜500g/lの均一なスラリーとする方法を挙げることができる。 The method for preparing the slurry is not particularly limited. For example, the zinc oxide serving as the seed is added to the zinc salt solution and dispersed at 18 to 30 ° C. for 10 to 30 minutes, whereby the concentration of the zinc oxide serving as the seed is 10 A method for preparing a uniform slurry of ˜500 g / l can be mentioned.
上記スラリーを調製する順序としては特に限定されないが、好ましい態様として、まず、ポリオール系溶媒、もしくはポリオール系溶媒と水とを混合した混合溶媒中に、亜鉛塩を添加し完全に溶解する方法を挙げることができる。なお、ポリオール系溶媒と水とを混合した混合溶媒を調製する場合、ポリオール系溶媒に水を添加して調製しても良く、水にポリオール系溶媒を添加して調製しても良い。 The order of preparing the slurry is not particularly limited, but a preferable embodiment is a method in which a zinc salt is first added and completely dissolved in a polyol solvent or a mixed solvent obtained by mixing a polyol solvent and water. be able to. In addition, when preparing the mixed solvent which mixed the polyol solvent and water, you may prepare by adding water to a polyol solvent, and you may prepare by adding a polyol solvent to water.
続いて、亜鉛塩を完全に溶解した亜鉛塩溶液中に、シードとなる酸化亜鉛を添加してスラリーを調製する。亜鉛塩溶液中にシードとなる酸化亜鉛を添加してスラリーとする場合、スラリー全量に対してシードとなる酸化亜鉛の濃度が10〜500g/lであることが好ましい。 Subsequently, zinc oxide as a seed is added to a zinc salt solution in which the zinc salt is completely dissolved to prepare a slurry. When adding zinc oxide as a seed to a zinc salt solution to form a slurry, the concentration of zinc oxide as a seed is preferably 10 to 500 g / l with respect to the total amount of the slurry.
このとき、シードとなる酸化亜鉛は溶液中で完全に溶解することなく、シードとして機能するための充分な量が残らなくてはならない。このようにして得られたスラリーを加熱、反応することにより、所望の酸化亜鉛粒子を得ることができる。 At this time, the zinc oxide used as a seed does not completely dissolve in the solution, but a sufficient amount for functioning as a seed must remain. Desired zinc oxide particles can be obtained by heating and reacting the slurry thus obtained.
なお、亜鉛塩溶液は上述したように酸化亜鉛などの亜鉛化合物を酸で溶解して調製したものであっても良い。このとき、シードとなる酸化亜鉛を亜鉛塩溶液中に充分に残した状態で反応させるためには、亜鉛もしくは酸が過剰な状態になっていない亜鉛塩溶液を使用することが好ましい。たとえば、酢酸亜鉛溶液を調製する場合、酸化亜鉛1モルに対し2モルの酢酸を用いて溶解し、亜鉛と酢酸が過不足無く反応した状態の酢酸亜鉛溶液を調製して使用することが好ましい。 The zinc salt solution may be prepared by dissolving a zinc compound such as zinc oxide with an acid as described above. At this time, it is preferable to use a zinc salt solution that is not in an excessive state of zinc or acid in order to cause the reaction in a state in which zinc oxide as a seed is sufficiently left in the zinc salt solution. For example, when preparing a zinc acetate solution, it is preferable to use a zinc acetate solution prepared by dissolving 2 mol of acetic acid with respect to 1 mol of zinc oxide and reacting zinc and acetic acid without excess or deficiency.
上記反応に際しては、本発明の効果を損なわない範囲で、シードとなる酸化亜鉛、亜鉛塩、水以外の成分を少量添加してもよい。例えば、分散剤等を添加することもできる。 In the above reaction, a small amount of components other than zinc oxide, zinc salt, and water serving as seeds may be added as long as the effects of the present invention are not impaired. For example, a dispersant or the like can be added.
反応は、45〜110℃において行うことが好ましい。時間は0.5〜24時間を挙げることができる。反応温度、反応時間、シードとなる酸化亜鉛濃度、亜鉛塩濃度等の条件によって粒子径の調整を図ることができるため、これらの条件については目的とする酸化亜鉛粒子の形状や粒子径に応じて適宜設定して行うことが好ましい。 The reaction is preferably performed at 45 to 110 ° C. Time can mention 0.5 to 24 hours. The particle size can be adjusted according to the reaction temperature, reaction time, seed zinc oxide concentration, zinc salt concentration, etc., so these conditions depend on the shape and particle size of the target zinc oxide particles. It is preferable to set appropriately.
このようにして得られた酸化亜鉛粒子は、必要に応じて、濾過、水洗、乾燥等の後処理を行ってもよい。
上記方法によって製造された酸化亜鉛粒子は、必要に応じて篩による分級を行うものであっても良い。篩による分級方法としては、湿式分級、乾式分級を挙げることができる。また、湿式粉砕、乾式粉砕等の処理を行ってもよい。
The zinc oxide particles obtained in this way may be subjected to post-treatment such as filtration, washing with water, and drying as necessary.
The zinc oxide particles produced by the above method may be classified by a sieve as necessary. Examples of the classification method using a sieve include wet classification and dry classification. Further, a treatment such as wet pulverization or dry pulverization may be performed.
上述したように、本発明の酸化亜鉛粒子の製造方法は、焼成処理を行わずに酸化亜鉛粒子を得ることができるものであるが、上述した方法によって得られた酸化亜鉛粒子に焼成処理を施しても差し支えない。焼成に際しては、公知の任意の装置を利用した方法を挙げることができ、処理条件等も特に限定されない。 As described above, the method for producing zinc oxide particles of the present invention can obtain zinc oxide particles without performing the baking treatment. However, the zinc oxide particles obtained by the above-described method are subjected to the baking treatment. There is no problem. In firing, a method using any known apparatus can be exemplified, and the processing conditions and the like are not particularly limited.
このような製造方法によって得られた酸化亜鉛粒子は、その製造方法において温度・濃度、処理時間等を調整することによって、種々の形状とすることができる。また、その形状や粒子径の分布が狭く、均一性の高い粒子を得ることができる点で好ましいものである。 The zinc oxide particles obtained by such a production method can be made into various shapes by adjusting temperature, concentration, treatment time, etc. in the production method. In addition, the shape and particle size distribution are narrow, which is preferable in that particles with high uniformity can be obtained.
粒子形状としては特に限定されず、柱状、丸み状、板状等の形状とすることができる。このような粒子形状は、上述した溶媒の種類、濃度、反応温度等を調製することにより作り分けることができる。 The particle shape is not particularly limited, and may be a columnar shape, a round shape, a plate shape, or the like. Such a particle shape can be made by adjusting the type, concentration, reaction temperature, and the like of the solvent described above.
本発明の酸化亜鉛粒子の製造方法によって製造される酸化亜鉛粒子の粒子径等は特に限定されるものではなく、上述した溶媒の種類、濃度、反応温度等を調整することにより作り分けることができる。また、本発明の酸化亜鉛粒子の製造方法によって製造された酸化亜鉛粒子は、粒径分布がシャープなものになる、という特徴を有するものである。より具体的には、D90/D10が2.0〜6.0となるような酸化亜鉛粒子を好適に製造することができるものである。また、D50/一次粒子径が1.0〜4.0であるような酸化亜鉛粒子を好適に製造できるものである。なお、D90、D10、D50の測定方法は実施例に記載した。このようなパラメータを満たす粒径分布がシャープな酸化亜鉛粒子は、化粧料原料や放熱性フィラーとして使用した場合に好適に使用することができる点で好ましい。 The particle diameter and the like of the zinc oxide particles produced by the method for producing zinc oxide particles of the present invention are not particularly limited, and can be made by adjusting the type, concentration, reaction temperature, etc. of the solvent described above. . Moreover, the zinc oxide particle manufactured by the manufacturing method of the zinc oxide particle of this invention has the characteristics that a particle size distribution will become a sharp thing. More specifically, zinc oxide particles having D90 / D10 of 2.0 to 6.0 can be preferably produced. Moreover, the zinc oxide particle whose D50 / primary particle diameter is 1.0-4.0 can be manufactured suitably. In addition, the measuring method of D90, D10, D50 was described in the Example. Zinc oxide particles having a sharp particle size distribution satisfying such parameters are preferable in that they can be suitably used when used as a cosmetic raw material or a heat dissipating filler.
本発明の酸化亜鉛粒子の製造方法によって得られた酸化亜鉛粒子はその用途を特に限定するものではないが、例えば、化粧料の原料、放熱性フィラーの用途において好適に使用することができる。このような化粧料及び放熱性フィラーも本発明の一部である。 Although the use of the zinc oxide particles obtained by the method for producing zinc oxide particles of the present invention is not particularly limited, for example, it can be suitably used in the use of a raw material for cosmetics and a heat dissipating filler. Such cosmetics and heat dissipating fillers are also part of the present invention.
上記酸化亜鉛粒子を配合した化粧料としては、ファンデーション、化粧下地、アイシャドウ、頬紅、マスカラ、口紅、サンスクリーン剤等を挙げることができる。本発明の化粧料は、油性化粧料、水性化粧料、O/W型化粧料、W/O型化粧料の任意の形態とすることができる。 Examples of cosmetics containing the zinc oxide particles include foundations, makeup bases, eye shadows, blushers, mascaras, lipsticks, sunscreen agents, and the like. The cosmetics of the present invention can be in any form of oily cosmetics, aqueous cosmetics, O / W type cosmetics, and W / O type cosmetics.
上記化粧料は、上記混合物を構成する成分以外に、化粧品分野において使用することができる任意の水性成分、油性成分を併用するものであってもよい。上記水性成分及び油性成分としては特に限定されず、例えば、油分、界面活性剤、保湿剤、高級アルコール、金属イオン封鎖剤、天然及び合成高分子、水溶性及び油溶性高分子、紫外線遮蔽剤、各種抽出液、無機及び有機顔料、無機及び有機粘土鉱物、金属石鹸処理又はシリコーンで処理された無機及び有機顔料、有機染料等の色剤、防腐剤、酸化防止剤、色素、増粘剤、pH調整剤、香料、冷感剤、制汗剤、殺菌剤、皮膚賦活剤等の成分を含有するものであってもよい。具体的には、以下に列挙した配合成分の1種又は2種以上を任意に配合して常法により目的の化粧料を製造することが可能である。これらの配合成分の配合量は、本発明の効果を損なわない範囲であれば特に限定されない。 The said cosmetics may use together the arbitrary aqueous component and oil-based component which can be used in the cosmetics field | area other than the component which comprises the said mixture. The aqueous component and the oil component are not particularly limited, and examples thereof include oils, surfactants, moisturizers, higher alcohols, sequestering agents, natural and synthetic polymers, water-soluble and oil-soluble polymers, UV shielding agents, Various extracts, inorganic and organic pigments, inorganic and organic clay minerals, inorganic and organic pigments treated with metal soaps or silicones, organic dyes and other colorants, preservatives, antioxidants, pigments, thickeners, pH You may contain components, such as a regulator, a fragrance | flavor, a cooling agent, an antiperspirant, a disinfectant, and a skin activator. Specifically, it is possible to produce any desired cosmetic by a conventional method by arbitrarily blending one or more of the blending ingredients listed below. The compounding amounts of these compounding components are not particularly limited as long as the effects of the present invention are not impaired.
上記油分としては特に限定されず、例えば、アボガド油、ツバキ油、タートル油、マカデミアナッツ油、トウモロコシ油、ミンク油、オリーブ油、ナタネ油、卵黄油、ゴマ油、パーシック油、小麦胚芽油、サザンカ油、ヒマシ油、アマニ油、サフラワー油、綿実油、エノ油、大豆油、落花生油、茶実油、カヤ油、コメヌカ油、シナギリ油、日本キリ油、ホホバ油、胚芽油、トリグリセリン、トリオクタン酸グリセリン、トリイソパルミチン酸グリセリン、カカオ脂、ヤシ油、馬脂、硬化ヤシ油、パーム油、牛脂、羊脂、硬化牛脂、パーム核油、豚脂、牛骨脂、モクロウ核油、硬化油、牛脚脂、モクロウ、硬化ヒマシ油、ミツロウ、カンデリラロウ、綿ロウ、カルナウバロウ、ベイベリーロウ、イボタロウ、鯨ロウ、モンタンロウ、ヌカロウ、ラノリン、カポックロウ、酢酸ラノリン、液状ラノリン、サトウキビロウ、ラノリン脂肪酸イソプロピル、ラウリン酸ヘキシル、還元ラノリン、ジョジョバロウ、硬質ラノリン、セラックロウ、POEラノリンアルコールエーテル、POEラノリンアルコールアセテート、POEコレステロールエーテル、ラノリン脂肪酸ポリエチレングリコール、POE水素添加ラノリンアルコールエーテル、流動パラフィン、オゾケライト、プリスタン、パラフィン、セレシン、スクワレン、ワセリン、マイクロクリスタリンワックス等を挙げることができる。 The oil content is not particularly limited. For example, avocado oil, camellia oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil, sasanqua oil, castor Oil, flaxseed oil, safflower oil, cottonseed oil, eno oil, soybean oil, peanut oil, tea seed oil, kaya oil, rice bran oil, cinnagari oil, Japanese kiri oil, jojoba oil, germ oil, triglycerin, glycerin trioctanoate, Glycerin triisopalmitate, cocoa butter, coconut oil, horse fat, hydrogenated coconut oil, palm oil, beef tallow, sheep fat, hydrogenated beef tallow, palm kernel oil, pork tallow, beef bone oil, owl kernel oil, hydrogenated oil, cow leg Fat, Owl, Hardened castor oil, Beeswax, Candelilla wax, Cotton wax, Carnauba wax, Bayberry wax, Ibotaro, Whale wax, Montan wax, Nukarou, Norin, Kapok, lanolin acetate, liquid lanolin, sugarcane wax, lanolin fatty acid isopropyl, hexyl laurate, reduced lanolin, jojoballow, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin fatty acid polyethylene glycol POE hydrogenated lanolin alcohol ether, liquid paraffin, ozokerite, pristane, paraffin, ceresin, squalene, petrolatum, microcrystalline wax and the like.
上記親油性非イオン界面活性剤としては特に限定されず、例えば、ソルビタンモノオレエート、ソルビタンモノイソステアレート、ソルビタンモノラウレート、ソルビタンモノパルミテート、ソルビタンモノステアレート、ソルビタンセスキオレエート、ソルビタントリオレエート、ペンタ−2−エチルヘキシル酸ジグリセロールソルビタン、テトラ−2−エチルヘキシル酸ジグリセロールソルビタン等のソルビタン脂肪酸エステル類、モノ綿実油脂肪酸グリセリン、モノエルカ酸グリセリン、セスキオレイン酸グリセリン、モノステアリン酸グリセリン、α,α’−オレイン酸ピログルタミン酸グリセリン、モノステアリン酸グリセリンリンゴ酸等のグリセリンポリグリセリン脂肪酸類、モノステアリン酸プロピレングリコール等のプロピレングリコール脂肪酸エステル類、硬化ヒマシ油誘導体、グリセリンアルキルエーテル等を挙げることができる。 The lipophilic nonionic surfactant is not particularly limited. For example, sorbitan monooleate, sorbitan monoisostearate, sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan sesquioleate, sorbitan trioleate. Sorbitan fatty acid esters such as diglycerol sorbitan penta-2-ethylhexylate, diglycerol sorbitan tetra-2-ethylhexylate, mono-cotton oil fatty acid glycerin, glyceryl monoerucate, glyceryl sesquioleate, glyceryl monostearate, α, α '-Glycerol polyglycerin fatty acids such as glyceryl oleate pyroglutamate, glyceryl monostearate malate, propylene glycol monostearate Glycol fatty acid esters, hardened castor oil derivatives, glycerin alkyl ethers and the like.
上記親水性非イオン界面活性剤としては特に限定されず、例えば、POEソルビタンモノステアレート、POEソルビタンモノオレエート、POEソルビタンテトラオレエート等のPOEソルビタン脂肪酸エステル類、POEソルビットモノラウレート、POEソルビットモノオレエート、POEソルビットペンタオレエート、POEソルビットモノステアレート等のPOEソルビット脂肪酸エステル類、POEグリセリンモノステアレート、POEグリセリンモノイソステアレート、POEグリセリントリイソステアレート等のPOEグリセリン脂肪酸エステル類、POEモノオレエート、POEジステアレート、POEモノジオレエート、システアリン酸エチレングリコール等のPOE脂肪酸エステル類、POEラウリルエーテル、POEオレイルエーテル、POEステアリルエーテル、POEベヘニルエーテル、POE2−オクチルドデシルエーテル、POEコレスタノールエーテル等のPOEアルキルエーテル類、POEオクチルフェニルエーテル、POEノニルフェニルエーテル、POEジノニルフェニルエーテル等のPOEアルキルフェニルエーテル類、ブルロニック等のプルアロニック型類、POE・POPセチルエーテル、POE・POP2−デシルテトラデシルエーテル、POE・POPモノブチルエーテル、POE・POP水添ラノリン、POE・POPグリセリンエーテル等のPOE・POPアルキルエーテル類、テトロニック等のテトラPOE・テトラPOPエチレンジアミン縮合物類、POEヒマシ油、POE硬化ヒマシ油、POE硬化ヒマシ油モノイソステアレート、POE硬化ヒマシ油トリイソステアレート、POE硬化ヒマシ油モノピログルタミン酸モノイソステアリン酸ジエステル、POE硬化ヒマシ油マレイン酸等のPOEヒマシ油硬化ヒマシ油誘導体、POEソルビットミツロウ等のPOEミツロウ・ラノリン誘導体、ヤシ油脂肪酸ジエタノールアミド、ラウリン酸モノエタノールアミド、脂肪酸イソプロパノールアミド等のアルカノールアミド、POEプロピレングリコール脂肪酸エステル、POEアルキルアミン、POE脂肪酸アミド、ショ糖脂肪酸エステル、POEノニルフェニルホルムアルデヒド縮合物、アルキルエトキシジメチルアミンオキシド、トリオレイルリン酸等を挙げることができる。 The hydrophilic nonionic surfactant is not particularly limited, and examples thereof include POE sorbitan fatty acid esters such as POE sorbitan monostearate, POE sorbitan monooleate, POE sorbitan tetraoleate, POE sorbite monolaurate, and POE sorbit. POE glycerin fatty acid esters such as monooleate, POE sorbite pentaoleate, POE sorbite fatty acid esters such as POE sorbite monostearate, POE glycerin monostearate, POE glycerin monoisostearate, POE glycerin triisostearate, POE fatty acid esters such as POE monooleate, POE distearate, POE monodiolate, ethylene glycol stearate, POE lauryl ether, PO POE alkyl ethers such as oleyl ether, POE stearyl ether, POE behenyl ether, POE2-octyldodecyl ether, POE cholestanol ether, POE alkyl phenyl ethers such as POE octyl phenyl ether, POE nonyl phenyl ether, POE dinonyl phenyl ether Pluronic type such as brulonic, POE / POP cetyl ether, POE / POP2-decyltetradecyl ether, POE / POP monobutyl ether, POE / POP hydrogenated lanolin, POE / POP alkyl ethers such as POE / POP glycerin ether, Tetronic PEO / TetraPOP ethylenediamine condensates, POE castor oil, POE hydrogenated castor oil, POE hydrogenated castor oil monoy POE castor oil hardened castor oil derivatives such as stearate, POE hardened castor oil triisostearate, POE hardened castor oil monopyroglutamic acid monoisostearic acid diester, POE hardened castor oil maleic acid, POE beeswax and lanolin derivatives such as POE sorbite beeswax Alkanolamides such as coconut oil fatty acid diethanolamide, lauric acid monoethanolamide, fatty acid isopropanolamide, POE propylene glycol fatty acid ester, POE alkylamine, POE fatty acid amide, sucrose fatty acid ester, POE nonylphenyl formaldehyde condensate, alkylethoxydimethyl Examples include amine oxide and trioleyl phosphoric acid.
その他の界面活性剤としては、例えば、脂肪酸セッケン、高級アルキル硫酸エステル塩、POEラウリル硫酸トリエタノールアミン、アルキルエーテル硫酸エステル塩等のアニオン界面活性剤、アルキルトリメチルアンモニウム塩、アルキルピリジニウム塩、アルキル四級アンモニウム塩、アルキルジメチルベンジルアンモニウム塩、POEアルキルアミン、アルキルアミン塩、ポリアミン脂肪酸誘導体等のカチオン界面活性剤、及び、イミダゾリン系両性界面活性剤、ベタイン系界面活性剤等の両性界面活性剤を安定性及び皮膚刺激性に問題のない範囲で配合してもよい。 Examples of other surfactants include anionic surfactants such as fatty acid soaps, higher alkyl sulfates, POE lauryl sulfate triethanolamine, alkyl ether sulfates, alkyltrimethylammonium salts, alkylpyridinium salts, alkyl quaternary salts. Stabilizes cationic surfactants such as ammonium salts, alkyldimethylbenzylammonium salts, POE alkylamines, alkylamine salts, polyamine fatty acid derivatives, and amphoteric surfactants such as imidazoline-based amphoteric surfactants and betaine-based surfactants. And you may mix | blend in the range which does not have a problem in skin irritation.
上記保湿剤としては特に限定されず、例えば、キシリトール、ソルビトール、マルチトール、コンドロイチン硫酸、ヒアルロン酸、ムコイチン硫酸、カロニン酸、アテロコラーゲン、コレステリル−12−ヒドロキシステアレート、乳酸ナトリウム、胆汁酸塩、dl−ピロリドンカルボン酸塩、短鎖可溶性コラーゲン、ジグリセリン(EO)PO付加物、イザヨイバラ抽出物、セイヨウノコギリソウ抽出物、メリロート抽出物等を挙げることができる。 The moisturizing agent is not particularly limited, and examples thereof include xylitol, sorbitol, maltitol, chondroitin sulfate, hyaluronic acid, mucoitin sulfate, caronic acid, atelocollagen, cholesteryl-12-hydroxystearate, sodium lactate, bile salt, dl- Examples thereof include pyrrolidone carboxylate, short-chain soluble collagen, diglycerin (EO) PO adduct, Izayoi rose extract, yarrow extract, and merirot extract.
上記高級アルコールとしては特に限定されず、例えば、ラウリルアルコール、セチルアルコール、ステアリルアルコール、ベヘニルアルコール、ミリスチルアルコール、オレイルアルコール、セトステアリルアルコール等の直鎖アルコール、モノステアリルグリセリンエーテル(バチルアルコール)、2−デシルテトラデシノール、ラノリンアルコール、コレステロール、フィトステロール、ヘキシルドデカノール、イソステアリルアルコール、オクチルドデカノール等の分枝鎖アルコール等を挙げることができる。 The higher alcohol is not particularly limited, and examples thereof include linear alcohols such as lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol, monostearyl glycerin ether (batyl alcohol), 2-decyl. Examples thereof include branched chain alcohols such as tetradecinol, lanolin alcohol, cholesterol, phytosterol, hexyldodecanol, isostearyl alcohol, octyldodecanol, and the like.
金属イオン封鎖剤としては特に限定されず、例えば、1−ヒドロキシエタン−1,1−
ジフォスホン酸、1−ヒドロキシエタン−1,1−ジフォスホン酸四ナトリウム塩、クエン酸ナトリウム、ポリリン酸ナトリウム、メタリン酸ナトリウム、グルコン酸、リン酸、クエン酸、アスコルビン酸、コハク酸、エデト酸等を挙げることができる。
The sequestering agent is not particularly limited. For example, 1-hydroxyethane-1,1-
Diphosphonic acid, 1-hydroxyethane-1,1-diphosphonic acid tetrasodium salt, sodium citrate, sodium polyphosphate, sodium metaphosphate, gluconic acid, phosphoric acid, citric acid, ascorbic acid, succinic acid, edetic acid, etc. be able to.
上記天然の水溶性高分子としては特に限定されず、例えば、アラビアガム、トラガカントガム、ガラクタン、グアガム、キャロブガム、カラヤガム、カラギーナン、ペクチン、カンテン、クインスシード(マルメロ)、アルゲコロイド(カッソウエキス)、デンプン(コメ、トウモロコシ、バレイショ、コムギ)、グリチルリチン酸等の植物系高分子、キサンタンガム、デキストラン、サクシノグルカン、プルラン等の微生物系高分子、コラーゲン、カゼイン、アルブミン、ゼラチン等の動物系高分子を挙げることができる。 The natural water-soluble polymer is not particularly limited, and examples thereof include gum arabic, gum tragacanth, galactan, guar gum, carob gum, caraya gum, carrageenan, pectin, agar, quince seed (malmello), alge colloid (gypsum extract), starch (rice) Corn, potato, wheat), plant polymers such as glycyrrhizic acid, microbial polymers such as xanthan gum, dextran, succinoglucan and pullulan, and animal polymers such as collagen, casein, albumin and gelatin. it can.
半合成の水溶性高分子としては特に限定されず、例えば、カルボキシメチルデンプン、メチルヒドロキシプロピルデンプン等のデンプン系高分子、メチルセルロース、ニトロセルロース、エチルセルロース、メチルヒドロキシプロピルセルロース、ヒドロキシエチルセルロース、セルロース硫酸ナトリウム、ヒドロキシプロピルセルロース、カルボキシメチルセルロースナトリウム(CMC)、結晶セルロース、セルロース末等のセルロース系高分子、アルギン酸ナトリウム、アルギン酸プロピレングリコールエステル等のアルギン酸系高分子等を挙げることができる。 The semi-synthetic water-soluble polymer is not particularly limited. For example, starch-based polymers such as carboxymethyl starch and methylhydroxypropyl starch, methylcellulose, nitrocellulose, ethylcellulose, methylhydroxypropylcellulose, hydroxyethylcellulose, sodium cellulose sulfate, Examples thereof include cellulose polymers such as hydroxypropylcellulose, sodium carboxymethylcellulose (CMC), crystalline cellulose, and cellulose powder, and alginic acid polymers such as sodium alginate and propylene glycol alginate.
合成の水溶性高分子としては特に限定されず、例えば、ポリビニルアルコール、ポリビニルメチルエーテル、ポリビニルピロリドン等のビニル系高分子、ポリエチレングリコール20,000、40,000、60,000等のポリオキシエチレン系高分子、ポリオキシエチレンポリオキシプロピレン共重合体共重合系高分子、ポリアクリル酸ナトリウム、ポリエチルアクリレート、ポリアクリルアミド等のアクリル系高分子、ポリエチレンイミン、カチオンポリマー等を挙げることができる。 The synthetic water-soluble polymer is not particularly limited, and examples thereof include vinyl polymers such as polyvinyl alcohol, polyvinyl methyl ether, and polyvinyl pyrrolidone, and polyoxyethylene polymers such as polyethylene glycol 20,000, 40,000, and 60,000. Examples thereof include polymers, polyoxyethylene polyoxypropylene copolymer copolymer polymers, acrylic polymers such as sodium polyacrylate, polyethyl acrylate and polyacrylamide, polyethyleneimine, and cationic polymers.
無機の水溶性高分子としては特に限定されず、例えば、ベントナイト、ケイ酸AlMg(ビーガム)、ラポナイト、ヘクトライト、無水ケイ酸等を挙げることができる。 The inorganic water-soluble polymer is not particularly limited, and examples thereof include bentonite, silicate AlMg (beegum), laponite, hectorite, and silicic anhydride.
紫外線遮蔽剤としては特に限定されず、例えば、パラアミノ安息香酸(以下PABAと略す)、PABAモノグリセリンエステル、N,N−ジプロポキシPABAエチルエステル、N,N−ジエトキシPABAエチルエステル、N,N−ジメチルPABAエチルエステル、N,N−ジメチルPABAブチルエステル等の安息香酸系紫外線遮蔽剤;ホモメンチル−N−アセチルアントラニレート等のアントラニル酸系紫外線遮蔽剤;アミルサリシレート、メンチルサリシレート、ホモメンチルサリシレート、オクチルサリシレート、フェニルサリシレート、ベンジルサリシレート、p−イソプロパノールフェニルサリシレート等のサリチル酸系紫外線遮蔽剤;オクチルシンナメート、エチル−4−イソプロピルシンナメート、メチル−2,5−ジイソプロピルシンナメート、エチル−2,4−ジイソプロピルシンナメート、メチル−2,4−ジイソプロピルシンナメート、プロピル−p−メトキシシンナメート、イソプロピル−p−メトキシシンナメート、イソアミル−p−メトキシシンナメート、2−エトキシエチル−p−メトキシシンナメート、シクロヘキシル−p−メトキシシンナメート、エチル−α−シアノ−β−フェニルシンナメート、2−エチルヘキシル−α−シアノ−β−フェニルシンナメート、グリセリルモノ−2−エチルヘキサノイル−ジパラメトキシシンナメート等のケイ皮酸系紫外線遮蔽剤;2,4−ジヒドロキシベンゾフェノン、2,2’−ジヒドロキシ−4−メトキシベンゾフェノン、2,2’−ジヒドロキシ−4,4’−ジメトキシベンゾフェノン、2,2’,4,4’−テトラヒドロキシベンゾフェノン、2−ヒドロキシ−4−メトキシベンゾフェノン、2−ヒドロキシ−4−メトキシ−4’−メチルベンゾフェノン、2−ヒドロキシ−4−メトキシベンゾフェノン−5−スルホン酸塩、4−フェニルベンゾフェノン、2−エチルヘキシル−4’−フェニル−ベンゾフェノン−2−カルボキシレート、2−ヒドロキシ−4−n−オクトキシベンゾフェノン、4−ヒドロキシ−3−カルボキシベンゾフェノン等のベンゾフェノン系紫外線遮蔽剤;3−(4’−メチルベンジリデン)−d,l−カンファー、3−ベンジリデン−d,l−カンファー、ウロカニン酸、ウロカニン酸エチルエステル、2−フェニル−5− メチルベンゾキサゾール、2,2’−ヒドロキシ−5−メチルフェニルベンゾトリアゾール、2−(2’−ヒドロキシ−5’−t−オクチルフェニル)ベンゾトリアゾール、2−(2’−ヒドロキシ−5’−メチルフェニルベンゾトリアゾール、ジベンザラジン、ジアニソイルメタン、4−メトキシ−4’−t−ブチルジベンゾイルメタン、5−(3,3−ジメチル−2−ノルボルニリデン)−3−ペンタン−2−オン等を挙げることができる。 The ultraviolet screening agent is not particularly limited. For example, paraaminobenzoic acid (hereinafter abbreviated as PABA), PABA monoglycerin ester, N, N-dipropoxy PABA ethyl ester, N, N-diethoxy PABA ethyl ester, N, N-dimethyl Benzoic acid UV screening agents such as PABA ethyl ester and N, N-dimethyl PABA butyl ester; Anthranilic acid UV screening agents such as homomenthyl-N-acetylanthranylate; Amyl salicylate, menthyl salicylate, homomenthyl salicylate, octyl salicylate , Salicylic acid UV screening agents such as phenyl salicylate, benzyl salicylate, p-isopropanol phenyl salicylate; octylcinnamate, ethyl-4-isopropylcinnamate, methyl-2,5- Isopropyl cinnamate, ethyl-2,4-diisopropyl cinnamate, methyl-2,4-diisopropyl cinnamate, propyl-p-methoxycinnamate, isopropyl-p-methoxycinnamate, isoamyl-p-methoxycinnamate, 2- Ethoxyethyl-p-methoxycinnamate, cyclohexyl-p-methoxycinnamate, ethyl-α-cyano-β-phenylcinnamate, 2-ethylhexyl-α-cyano-β-phenylcinnamate, glyceryl mono-2-ethylhexa Cinnamic acid-based ultraviolet screening agents such as noyl-diparamethoxycinnamate; 2,4-dihydroxybenzophenone, 2,2′-dihydroxy-4-methoxybenzophenone, 2,2′-dihydroxy-4,4′-dimethoxybenzophenone , 2, 2 ', 4,4'-tetrahydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-4'-methylbenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfonate, 4 -Benzophenone-based UV shielding agents such as phenylbenzophenone, 2-ethylhexyl-4'-phenyl-benzophenone-2-carboxylate, 2-hydroxy-4-n-octoxybenzophenone, 4-hydroxy-3-carboxybenzophenone; (4'-methylbenzylidene) -d, l-camphor, 3-benzylidene-d, l-camphor, urocanic acid, urocanic acid ethyl ester, 2-phenyl-5-methylbenzoxazole, 2,2'-hydroxy- 5-methylphenylbenzotri Azole, 2- (2′-hydroxy-5′-t-octylphenyl) benzotriazole, 2- (2′-hydroxy-5′-methylphenylbenzotriazole), dibenzalazine, dianisoylmethane, 4-methoxy-4′- Examples thereof include t-butyldibenzoylmethane and 5- (3,3-dimethyl-2-norbornylidene) -3-pentan-2-one.
その他薬剤成分としては特に限定されず、例えば、ビタミンA油、レチノール、パルミチン酸レチノール、イノシット、塩酸ピリドキシン、ニコチン酸ベンジル、ニコチン酸アミド、ニコチン酸DL−α−トコフェロール、アルコルビン酸リン酸マグネシウム、2−O−α−D−グルコピラノシル−L−アスコルビン酸、ビタミンD2(エルゴカシフェロール)、dl−α−トコフェロール、酢酸dl−α−トコフェロール、パントテン酸、ビオチン等のビタミン類;エストラジオール、エチニルエストラジオール等のホルモン;アルギニン、アスパラギン酸、シスチン、システイン、メチオニン、セリン、ロイシン、トリプトファン等のアミノ酸;アラントイン、アズレン等の抗炎症剤、アルブチン等の美白剤、;タンニン酸等の収斂剤;L−メントール、カンフル等の清涼剤やイオウ、塩化リゾチーム、塩化ピリドキシン等を挙げることができる。 Other drug components are not particularly limited and include, for example, vitamin A oil, retinol, retinol palmitate, inosit, pyridoxine hydrochloride, benzyl nicotinate, nicotinamide, nicotinic acid DL-α-tocopherol, magnesium ascorbate phosphate, 2 Vitamins such as -O-α-D-glucopyranosyl-L-ascorbic acid, vitamin D2 (ergocaciferol), dl-α-tocopherol, dl-α-tocopherol acetate, pantothenic acid, biotin; estradiol, ethinylestradiol, etc. Hormones; amino acids such as arginine, aspartic acid, cystine, cysteine, methionine, serine, leucine and tryptophan; anti-inflammatory agents such as allantoin and azulene; whitening agents such as arbutin; astringents such as tannic acid; L Menthol, cooling agents and sulfur camphor such as, lysozyme chloride, can be mentioned pyridoxine chloride, and the like.
各種の抽出液としては特に限定されず、例えば、ドクダミエキス、オウバクエキス、メリロートエキス、オドリコソウエキス、カンゾウエキス、シャクヤクエキス、サボンソウエキス、ヘチマエキス、キナエキス、ユキノシタエキス、クララエキス、コウホネエキス、ウイキョウエキス、サクラソウエキス、バラエキス、ジオウエキス、レモンエキス、シコンエキス、アロエエキス、ショウブ根エキス、ユーカリエキス、スギナエキス、セージエキス、タイムエキス、茶エキス、海藻エキス、キューカンバーエキス、チョウジエキス、キイチゴエキス、メリッサエキス、ニンジンエキス、マロニエエキス、モモエキス、桃葉エキス、クワエキス、ヤグルマギクエキス、ハマメリスエキス、プラセンタエキス、胸腺抽出物、シルク抽出液、甘草エキス等を挙げることができる。 There are no particular limitations on the various extracts, for example, Dokudami extract, Oat extract, Merirot extract, Odorikosou extract, Licorice extract, Peonies extract, Soap extract, Loofah extract, Kina extract, Yukinoshita extract, Clara extract, Kouhone extract, Fennel Extract, Primrose Extract, Rose Extract, Giant Extract, Lemon Extract, Shikon Extract, Aloe Extract, Shobu Root Extract, Eucalyptus Extract, Horsetail Extract, Sage Extract, Thyme Extract, Tea Extract, Seaweed Extract, Cucumber Extract, Clove Extract, Raspberry Extract, Melissa Extract , Carrot extract, marronnier extract, peach extract, peach leaf extract, mulberry extract, cornflower extract, hamamelis extract, placenta extract, thymus extract, silk extract, licorice Mention may be made of the kiss and the like.
上記各種粉体としては、ベンガラ、黄酸化鉄、黒酸化鉄、雲母チタン、酸化鉄被覆雲母チタン、酸化チタン被覆ガラスフレーク等の光輝性着色顔料、マイカ、タルク、カオリン、セリサイト、二酸化チタン、シリカ等の無機粉末やポリエチレン末、ナイロン末、架橋ポリスチレン、セルロースパウダー、シリコーン末等の有機粉末等を挙げることができる。好ましくは、官能特性向上、化粧持続性向上のため、粉末成分の一部又は全部をシリコーン類、フッ素化合物、金属石鹸、油剤、アシルグルタミン酸塩等の物質にて、公知の方法で疎水化処理して使用される。また、本発明の方法以外の方法で得られた他の酸化亜鉛粒子を混合して使用するものであってもよい。 Examples of the various powders include bengara, yellow iron oxide, black iron oxide, titanium mica, iron oxide-coated mica titanium, titanium oxide-coated glass flakes and other bright colored pigments, mica, talc, kaolin, sericite, titanium dioxide, Examples thereof include inorganic powders such as silica and organic powders such as polyethylene powder, nylon powder, crosslinked polystyrene, cellulose powder, and silicone powder. Preferably, a part or all of the powder component is hydrophobized by a known method with a substance such as silicones, fluorine compounds, metal soaps, oils, acyl glutamates in order to improve sensory characteristics and cosmetic durability. Used. Moreover, you may mix and use the other zinc oxide particle obtained by methods other than the method of this invention.
本発明の酸化亜鉛粒子の製造方法によって得られた酸化亜鉛粒子は、放熱性フィラーとして使用することもできる。
上記酸化亜鉛粒子を放熱性フィラーとして使用する場合、単独での使用、他の放熱性フィラーとの併用のいずれの方法とすることもできる。単独での使用、他の放熱性フィラーとの併用使用に関わらず、上記酸化亜鉛粒子を樹脂組成物、グリース組成物等の放熱性組成物の全量に対して、10〜90体積%の割合で使用することが好ましい。
The zinc oxide particles obtained by the method for producing zinc oxide particles of the present invention can also be used as a heat dissipating filler.
When using the said zinc oxide particle as a heat dissipation filler, it can also be set as the method of any use of independent use and combined use with another heat dissipation filler. Regardless of whether used alone or in combination with other heat-dissipating fillers, the zinc oxide particles are used in a proportion of 10 to 90% by volume based on the total amount of the heat-dissipating composition such as the resin composition and the grease composition. It is preferable to use it.
上記酸化亜鉛粒子を放熱性フィラーとして使用する場合、樹脂と混合した放熱性樹脂組成物として使用することができる。この場合、使用する樹脂は、熱可塑性樹脂であっても熱硬化性樹脂であっても良く、エポキシ樹脂、フェノール樹脂、ポリフェニレンサルファイド(PPS)樹脂、ポリエステル系樹脂、ポリアミド、ポリイミド、ポリスチレン、ポリエチレン、ポリプロピレン、ポリ塩化ビニル、ポリ塩化ビニリデン、フッ素樹脂、ポリメタクリル酸メチル、エチレン・アクリル酸エチル共重合体(EEA)樹脂、ポリカーボネート、ポリウレタン、ポリアセタール、ポリフェニレンエーテル、ポリエーテルイミド、アクリロニトリル−ブタジエン−スチレン共重合体(ABS)樹脂、液晶樹脂(LCP)、シリコーン樹脂、アクリル樹脂等の樹脂を挙げることができる。 When using the said zinc oxide particle as a heat dissipation filler, it can be used as a heat dissipation resin composition mixed with resin. In this case, the resin used may be a thermoplastic resin or a thermosetting resin, and an epoxy resin, a phenol resin, a polyphenylene sulfide (PPS) resin, a polyester resin, polyamide, polyimide, polystyrene, polyethylene, Polypropylene, polyvinyl chloride, polyvinylidene chloride, fluororesin, polymethyl methacrylate, ethylene / ethyl acrylate copolymer (EEA) resin, polycarbonate, polyurethane, polyacetal, polyphenylene ether, polyetherimide, acrylonitrile-butadiene-styrene Examples of the resin include polymer (ABS) resin, liquid crystal resin (LCP), silicone resin, and acrylic resin.
本発明の放熱性樹脂組成物は、熱可塑性樹脂と上記酸化亜鉛粒子とを溶融状態で混練することによって得られた熱成型用の樹脂組成物、又は、熱硬化性樹脂と上記酸化亜鉛粒子とを混練後、加熱硬化させることによって得られた樹脂組成物、又は、樹脂溶液又は分散液中に上記酸化亜鉛粒子を分散させた塗料用の樹脂組成物であっても良い。 The heat dissipating resin composition of the present invention is a thermoforming resin composition obtained by kneading a thermoplastic resin and the zinc oxide particles in a molten state, or a thermosetting resin and the zinc oxide particles. After kneading, a resin composition obtained by heat-curing, or a resin composition for paint in which the zinc oxide particles are dispersed in a resin solution or a dispersion may be used.
本発明の酸化亜鉛粒子は、その他の放熱性フィラーと組み合わせた放熱性フィラー組成物として使用することもできる。特に、本発明においては、その他の放熱性フィラーと組み合わせて使用する場合、より粒子径が大きい放熱性フィラーと組み合わせて使用することも、より粒子径が小さい放熱性フィラーと組み合わせて使用することも、その両方と組み合わせて使用することも考えられる。 The zinc oxide particles of the present invention can also be used as a heat dissipating filler composition in combination with other heat dissipating fillers. In particular, in the present invention, when used in combination with other heat dissipating filler, it can be used in combination with a heat dissipating filler having a larger particle diameter, or in combination with a heat dissipating filler having a smaller particle diameter. It is also conceivable to use in combination with both.
上記その他の放熱性フィラーとしては特に限定されず、酸化亜鉛、酸化マグネシウム、酸化チタン、酸化アルミニウム等の金属酸化物、窒化アルミニウム、窒化ホウ素、炭化ケイ素、窒化ケイ素、窒化チタン、金属シリコン、ダイヤモンド等を挙げることができる。このように他の放熱性フィラーと併用して使用する場合、放熱性フィラー全量に対して本発明の製造方法によって得られた酸化亜鉛粒子を10〜90体積%の割合で含有することが好ましい。 The other heat dissipating fillers are not particularly limited, and include metal oxides such as zinc oxide, magnesium oxide, titanium oxide, and aluminum oxide, aluminum nitride, boron nitride, silicon carbide, silicon nitride, titanium nitride, metal silicon, diamond, and the like. Can be mentioned. Thus, when using together with another heat dissipation filler, it is preferable to contain the zinc oxide particle obtained by the manufacturing method of this invention in the ratio of 10-90 volume% with respect to the heat dissipation filler whole quantity.
上記放熱性樹脂組成物が熱成型用の樹脂組成物である場合、用途によって樹脂成分を自由に選択することができる。例えば、熱源と放熱板に接着し密着させる場合には、シリコーン樹脂やアクリル樹脂のような接着性が高く硬度の低い樹脂を選択すれば良い。 When the heat-dissipating resin composition is a resin composition for thermoforming, the resin component can be freely selected depending on the application. For example, when adhering and adhering to a heat source and a heat sink, a resin having high adhesiveness and low hardness such as silicone resin or acrylic resin may be selected.
上記放熱性樹脂組成物が塗料用の樹脂組成物である場合、樹脂は硬化性を有するものであっても、硬化性を有さないものであっても良い。塗料は、有機溶媒を含有する溶剤系のものであっても、水中に樹脂が溶解又は分散した水系のものであっても良い。 When the heat radiating resin composition is a resin composition for paint, the resin may be curable or non-curable. The paint may be a solvent-based one containing an organic solvent or a water-based one in which a resin is dissolved or dispersed in water.
上記酸化亜鉛粒子を放熱性フィラーとして使用する場合、鉱油又は合成油を含有する基油と混合した放熱性グリースとして使用することもできる。このような放熱性グリースとして使用する場合は、合成油としてα−オレフィン、ジエステル、ポリオールエステル、トリメリット酸エステル、ポリフェニルエーテル、アルキルフェニルエーテル等が使用できる。また、シリコーンオイルと混合した放熱性グリースとして使用することもできる。 When using the said zinc oxide particle as a heat dissipation filler, it can also be used as a heat dissipation grease mixed with the base oil containing mineral oil or synthetic oil. When used as such heat dissipating grease, α-olefin, diester, polyol ester, trimellitic acid ester, polyphenyl ether, alkylphenyl ether and the like can be used as synthetic oil. It can also be used as a heat dissipating grease mixed with silicone oil.
上記酸化亜鉛粒子は、放熱性フィラーとして使用する場合、その他の成分を併用して使用することもできる。併用して使用することができるその他の成分としては、酸化マグネシウム、酸化チタン、酸化アルミニウム等の金属酸化物、窒化アルミニウム、窒化ホウ素、炭化ケイ素、窒化ケイ素、窒化チタン、金属シリコン、ダイヤモンド等の酸化亜鉛以外の放熱性フィラー、樹脂、界面活性剤等を挙げることができる。 The zinc oxide particles can be used in combination with other components when used as a heat-dissipating filler. Other components that can be used in combination include metal oxides such as magnesium oxide, titanium oxide, and aluminum oxide, and oxidation of aluminum nitride, boron nitride, silicon carbide, silicon nitride, titanium nitride, metal silicon, diamond, etc. Examples include heat dissipating fillers other than zinc, resins, and surfactants.
上記酸化亜鉛粒子は、上述した化粧料や放熱性フィラーの他に、ゴムの加硫促進剤、塗料・インキ用顔料、フェライトやバリスタ等の電子部品、医薬品等の分野においても使用することができる。 The zinc oxide particles can be used in the fields of rubber vulcanization accelerators, paint / ink pigments, electronic parts such as ferrite and varistors, pharmaceuticals, etc., in addition to the cosmetics and heat dissipating fillers described above. .
以下、本発明を実施例によってより詳細に説明する。なお、本発明は以下の実施例に限定されるものではない。 Hereinafter, the present invention will be described in more detail with reference to examples. In addition, this invention is not limited to a following example.
(実施例1)
酢酸亜鉛二水和物(細井化学工業社製 酢酸亜鉛)266.07gをエチレングリコール(和光純薬工業社製 試薬一級)1048.18mlに溶解して酢酸亜鉛二水和物としての濃度が1mol/lとなるよう調製した酢酸亜鉛二水和物/エチレングリコール溶液1200mlに、FINEX−50(堺化学工業社製 粒子径0.020μm)80gをリパルプしスラリーとした。このとき、シードとなるFINEX−50は完全に溶解することなく充分に溶液中に残っている状態であった。続いて、そのスラリーを攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で3時間反応した。反応後、真空ろ過、水洗した。続いて、得られた固形物を水3リットルにリパルプしてスラリーとし、攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で30分間加熱洗浄した。加熱洗浄後、真空ろ過、水洗し、イソプロピルアルコール1リットルにリパルプしてスラリーとし、真空ろ過により固形物を単離し、その固形物を110℃で12時間乾燥することにより、一次粒子径が0.107μmの六角柱状酸化亜鉛粒子75.3gを得た。得られた粒子のサイズ・形態を透過型電子顕微鏡(TEM、JEM−1200EX II、日本電子社製)で観察した。得られた電子顕微鏡写真を図1に示した。更に高倍率での電子顕微鏡写真を図2に示した。また、得られた粒子のX線回折のスペクトルを図3に示した。また、得られた粒子の物性を表1に示した。
Example 1
266.07 g of zinc acetate dihydrate (Zinc acetate manufactured by Hosoi Chemical Co., Ltd.) was dissolved in 1048.18 ml of ethylene glycol (reagent first grade manufactured by Wako Pure Chemical Industries, Ltd.), and the concentration as zinc acetate dihydrate was 1 mol / Into 1200 ml of zinc acetate dihydrate / ethylene glycol solution prepared to be l, 80 g of FINEX-50 (manufactured by Sakai Chemical Industry Co., Ltd., particle size 0.020 μm) was repulped to form a slurry. At this time, FINEX-50 used as a seed was not dissolved completely but remained in the solution. Subsequently, the slurry was heated to 100 ° C. over 60 minutes with stirring, and reacted at 100 ° C. for 3 hours with stirring. After the reaction, it was vacuum filtered and washed with water. Subsequently, the obtained solid was repulped into 3 liters of water to form a slurry, heated to 100 ° C. over 60 minutes with stirring, and heated and washed at 100 ° C. for 30 minutes with stirring. After heating and washing, vacuum filtration, washing with water, repulping to 1 liter of isopropyl alcohol to make a slurry, isolating the solid matter by vacuum filtration, and drying the solid matter at 110 ° C. for 12 hours, the primary particle size becomes 0. 75.3 g of 107 μm hexagonal columnar zinc oxide particles were obtained. The size and form of the obtained particles were observed with a transmission electron microscope (TEM, JEM-1200EX II, manufactured by JEOL Ltd.). The obtained electron micrograph is shown in FIG. Further, an electron micrograph at a high magnification is shown in FIG. The X-ray diffraction spectrum of the obtained particles is shown in FIG. The physical properties of the obtained particles are shown in Table 1.
(実施例2)
酢酸亜鉛二水和物(細井化学工業社製 酢酸亜鉛)266.07gをエチレングリコール(和光純薬工業社製 試薬一級)1048.18mlに溶解して酢酸亜鉛二水和物としての濃度が1mol/lとなるよう調製した酢酸亜鉛二水和物/エチレングリコール溶液1200mlに、FINEX−50(堺化学工業社製 粒子径0.020μm)80gをリパルプしスラリーとした。このとき、シードとなるFINEX−50は完全に溶解することなく充分に溶液中に残っている状態であった。続いて、そのスラリーを攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で1時間反応した。反応後、真空ろ過、水洗した。続いて、得られた固形物を水3リットルにリパルプしてスラリーとし、攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で30分間加熱洗浄した。加熱洗浄後、真空ろ過、水洗し、イソプロピルアルコール1リットルにリパルプしてスラリーとし、真空ろ過により固形物を単離し、その固形物を110℃で12時間乾燥することにより、一次粒子径が0.104μmの六角柱状酸化亜鉛粒子76.2gを得た。得られた粒子のサイズ・形態を透過型電子顕微鏡(TEM、JEM−1200EX II、日本電子社製)で観察した。得られた電子顕微鏡写真を図4に示した。更に高倍率での電子顕微鏡写真を図5に示した。また、得られた粒子の物性を表1に示した。
(Example 2)
266.07 g of zinc acetate dihydrate (Zinc acetate manufactured by Hosoi Chemical Co., Ltd.) was dissolved in 1048.18 ml of ethylene glycol (reagent first grade manufactured by Wako Pure Chemical Industries, Ltd.), and the concentration as zinc acetate dihydrate was 1 mol / Into 1200 ml of zinc acetate dihydrate / ethylene glycol solution prepared to be l, 80 g of FINEX-50 (manufactured by Sakai Chemical Industry Co., Ltd., particle size 0.020 μm) was repulped to form a slurry. At this time, FINEX-50 used as a seed was not dissolved completely but remained in the solution. Subsequently, the slurry was heated to 100 ° C. over 60 minutes with stirring, and reacted at 100 ° C. for 1 hour with stirring. After the reaction, it was vacuum filtered and washed with water. Subsequently, the obtained solid was repulped into 3 liters of water to form a slurry, heated to 100 ° C. over 60 minutes with stirring, and heated and washed at 100 ° C. for 30 minutes with stirring. After heating and washing, vacuum filtration, washing with water, repulping to 1 liter of isopropyl alcohol to make a slurry, isolating the solid matter by vacuum filtration, and drying the solid matter at 110 ° C. for 12 hours, the primary particle size becomes 0. 76.2 g of 104 μm hexagonal columnar zinc oxide particles were obtained. The size and form of the obtained particles were observed with a transmission electron microscope (TEM, JEM-1200EX II, manufactured by JEOL Ltd.). The obtained electron micrograph is shown in FIG. Further, an electron micrograph at a high magnification is shown in FIG. The physical properties of the obtained particles are shown in Table 1.
(実施例3)
酢酸亜鉛二水和物(細井化学工業社製 酢酸亜鉛)266.07gをエチレングリコール(和光純薬工業社製 試薬一級)1048.18mlに溶解して酢酸亜鉛二水和物としての濃度が1mol/lとなるよう調製した酢酸亜鉛二水和物/エチレングリコール溶液1200mlに、FINEX−50(堺化学工業社製 粒子径0.020μm)80gをリパルプしスラリーとした。このとき、シードとなるFINEX−50は完全に溶解することなく充分に溶液中に残っている状態であった。続いて、そのスラリーを攪拌しながら54分間で90℃に昇温し、攪拌しながら90℃で3時間反応した。反応後、真空ろ過、水洗した。続いて、得られた固形物を水3リットルにリパルプしてスラリーとし、攪拌しながら54分間で90℃に昇温し、攪拌しながら90℃で30分間加熱洗浄した。加熱洗浄後、真空ろ過、水洗し、イソプロピルアルコール1リットルにリパルプしてスラリーとし、真空ろ過により固形物を単離し、その固形物を110℃で12時間乾燥することにより、一次粒子径が0.138μmの六角柱状酸化亜鉛粒子74.6gを得た。得られた粒子の物性を表1に示した。
(Example 3)
266.07 g of zinc acetate dihydrate (Zinc acetate manufactured by Hosoi Chemical Co., Ltd.) was dissolved in 1048.18 ml of ethylene glycol (reagent first grade manufactured by Wako Pure Chemical Industries, Ltd.), and the concentration as zinc acetate dihydrate was 1 mol / Into 1200 ml of zinc acetate dihydrate / ethylene glycol solution prepared to be l, 80 g of FINEX-50 (manufactured by Sakai Chemical Industry Co., Ltd., particle size 0.020 μm) was repulped to form a slurry. At this time, FINEX-50 used as a seed was not dissolved completely but remained in the solution. Subsequently, the slurry was heated to 90 ° C. over 54 minutes with stirring, and reacted at 90 ° C. for 3 hours with stirring. After the reaction, it was vacuum filtered and washed with water. Subsequently, the obtained solid was repulped into 3 liters of water to form a slurry, heated to 90 ° C. over 54 minutes with stirring, and heated and washed at 90 ° C. for 30 minutes with stirring. After heating and washing, vacuum filtration, washing with water, repulping to 1 liter of isopropyl alcohol to make a slurry, isolating the solid matter by vacuum filtration, and drying the solid matter at 110 ° C. for 12 hours, the primary particle size becomes 0. 74.6 g of hexagonal columnar zinc oxide particles of 138 μm were obtained. Table 1 shows the physical properties of the obtained particles.
(実施例4)
酢酸亜鉛二水和物(細井化学工業社製 酢酸亜鉛)266.07gをエチレングリコール(和光純薬工業社製 試薬一級)1048.18mlに溶解して酢酸亜鉛二水和物としての濃度が1mol/lとなるよう調製した酢酸亜鉛二水和物/エチレングリコール溶液1200mlに、FINEX−50(堺化学工業社製 粒子径0.020μm)80gをリパルプしスラリーとした。このとき、シードとなるFINEX−50は完全に溶解することなく充分に溶液中に残っている状態であった。続いて、そのスラリーを攪拌しながら92分間で153℃に昇温し、攪拌しながら153℃で3時間反応した。反応後、真空ろ過、水洗した。続いて、得られた固形物を水3リットルにリパルプしてスラリーとし、攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で30分間加熱洗浄した。加熱洗浄後、真空ろ過、水洗し、イソプロピルアルコール1リットルにリパルプしてスラリーとし、真空ろ過により固形物を単離し、その固形物を110℃で12時間乾燥することにより、一次粒子径が0.050μmの酸化亜鉛粒子73.1gを得た。得られた粒子のサイズ・形態を透過型電子顕微鏡(TEM、JEM−1200EX II、日本電子社製)で観察した。得られた電子顕微鏡写真を図6に示した。また、得られた粒子のX線回折のスペクトルを図7に示した。また、得られた粒子の物性を表1に示した。
(Example 4)
266.07 g of zinc acetate dihydrate (Zinc acetate manufactured by Hosoi Chemical Co., Ltd.) was dissolved in 1048.18 ml of ethylene glycol (reagent first grade manufactured by Wako Pure Chemical Industries, Ltd.), and the concentration as zinc acetate dihydrate was 1 mol / Into 1200 ml of zinc acetate dihydrate / ethylene glycol solution prepared to be l, 80 g of FINEX-50 (manufactured by Sakai Chemical Industry Co., Ltd., particle size 0.020 μm) was repulped to form a slurry. At this time, FINEX-50 used as a seed was not dissolved completely but remained in the solution. Subsequently, the slurry was heated to 153 ° C. over 92 minutes with stirring, and reacted at 153 ° C. for 3 hours with stirring. After the reaction, it was vacuum filtered and washed with water. Subsequently, the obtained solid was repulped into 3 liters of water to form a slurry, heated to 100 ° C. over 60 minutes with stirring, and heated and washed at 100 ° C. for 30 minutes with stirring. After heating and washing, vacuum filtration, washing with water, repulping to 1 liter of isopropyl alcohol to make a slurry, isolating the solid matter by vacuum filtration, and drying the solid matter at 110 ° C. for 12 hours, the primary particle size becomes 0. 73.1 g of 050 μm zinc oxide particles was obtained. The size and form of the obtained particles were observed with a transmission electron microscope (TEM, JEM-1200EX II, manufactured by JEOL Ltd.). The obtained electron micrograph is shown in FIG. The X-ray diffraction spectrum of the obtained particles is shown in FIG. The physical properties of the obtained particles are shown in Table 1.
(実施例5)
酢酸亜鉛二水和物(細井化学工業社製 酢酸亜鉛)266.07gをエチレングリコール(和光純薬工業社製 試薬一級)1048.18mlに溶解して酢酸亜鉛二水和物としての濃度が1mol/lとなるよう調製した酢酸亜鉛二水和物/エチレングリコール溶液1200mlに、FINEX−50(堺化学工業社製 粒子径0.020μm)80gをリパルプしスラリーとした。このとき、シードとなるFINEX−50は完全に溶解することなく充分に溶液中に残っている状態であった。続いて、そのスラリーを攪拌しながら92分間で153℃に昇温し、攪拌しながら153℃で1時間反応した。反応後、真空ろ過、水洗した。続いて、得られた固形物を水3リットルにリパルプしてスラリーとし、攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で30分間加熱洗浄した。加熱洗浄後、真空ろ過、水洗し、イソプロピルアルコール1リットルにリパルプしてスラリーとし、真空ろ過により固形物を単離し、その固形物を110℃で12時間乾燥することにより、一次粒子径が0.047μmの酸化亜鉛粒子73.9gを得た。得られた粒子のサイズ・形態を透過型電子顕微鏡(TEM、JEM−1200EX
II、日本電子社製)で観察した。得られた電子顕微鏡写真を図8に示した。また、得られた粒子の物性を表1に示した。
(Example 5)
266.07 g of zinc acetate dihydrate (Zinc acetate manufactured by Hosoi Chemical Co., Ltd.) was dissolved in 1048.18 ml of ethylene glycol (reagent first grade manufactured by Wako Pure Chemical Industries, Ltd.), and the concentration as zinc acetate dihydrate was 1 mol / Into 1200 ml of zinc acetate dihydrate / ethylene glycol solution prepared to be l, 80 g of FINEX-50 (manufactured by Sakai Chemical Industry Co., Ltd., particle size 0.020 μm) was repulped to form a slurry. At this time, FINEX-50 used as a seed was not dissolved completely but remained in the solution. Subsequently, the slurry was heated to 153 ° C. over 92 minutes with stirring, and reacted at 153 ° C. for 1 hour with stirring. After the reaction, it was vacuum filtered and washed with water. Subsequently, the obtained solid was repulped into 3 liters of water to form a slurry, heated to 100 ° C. over 60 minutes with stirring, and heated and washed at 100 ° C. for 30 minutes with stirring. After heating and washing, vacuum filtration, washing with water, repulping to 1 liter of isopropyl alcohol to make a slurry, isolating the solid matter by vacuum filtration, and drying the solid matter at 110 ° C. for 12 hours, the primary particle size becomes 0. As a result, 73.9 g of 047 μm zinc oxide particles were obtained. The size and form of the obtained particles were measured with a transmission electron microscope (TEM, JEM-1200EX).
II, manufactured by JEOL Ltd.). The obtained electron micrograph is shown in FIG. The physical properties of the obtained particles are shown in Table 1.
(実施例6)
酢酸亜鉛二水和物(細井化学工業社製 酢酸亜鉛)266.07gをエチレングリコール(和光純薬工業社製 試薬一級)698.79mlと水349.39mlの混合溶液に溶解して酢酸亜鉛二水和物としての濃度が1mol/lとなるよう調製した酢酸亜鉛二水和物/エチレングリコール/水の混合溶液1200mlに、FINEX−50(堺化学工業社製 粒子径0.020μm)80gをリパルプしスラリーとした。このとき、シードとなるFINEX−50は完全に溶解することなく充分に溶液中に残っている状態であった。続いて、そのスラリーを攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で3時間反応した。反応後、真空ろ過、水洗した。続いて、得られた固形物を水3リットルにリパルプしてスラリーとし、攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で30分間加熱洗浄した。加熱洗浄後、ろ過、真空水洗し、イソプロピルアルコール1リットルにリパルプしてスラリーとし、真空ろ過により固形物を単離し、その固形物を110℃で12時間乾燥することにより、一次粒子径が0.256μmの柱状酸化亜鉛粒子76.7gを得た。得られた粒子のサイズ・形態を透過型電子顕微鏡(TEM、JEM−1200EX II、日本電子社製)で観察した。得られた電子顕微鏡写真を図9に示した。また、得られた粒子の物性を表1に示した。
(Example 6)
26.07 g of zinc acetate dihydrate (Zinc acetate manufactured by Hosoi Chemical Co., Ltd.) was dissolved in a mixed solution of 698.79 ml of ethylene glycol (Reagent grade 1 manufactured by Wako Pure Chemical Industries, Ltd.) and 349.39 ml of water. 80 mg of FINEX-50 (manufactured by Sakai Chemical Industry Co., Ltd., particle size: 0.020 μm) was repulped into 1200 ml of a mixed solution of zinc acetate dihydrate / ethylene glycol / water prepared so that the concentration as a Japanese product was 1 mol / l. A slurry was obtained. At this time, FINEX-50 used as a seed was not dissolved completely but remained in the solution. Subsequently, the slurry was heated to 100 ° C. over 60 minutes with stirring, and reacted at 100 ° C. for 3 hours with stirring. After the reaction, it was vacuum filtered and washed with water. Subsequently, the obtained solid was repulped into 3 liters of water to form a slurry, heated to 100 ° C. over 60 minutes with stirring, and heated and washed at 100 ° C. for 30 minutes with stirring. After heating and washing, filtration, washing with vacuum water, repulping into 1 liter of isopropyl alcohol to make a slurry, isolating the solid by vacuum filtration, and drying the solid at 110 ° C. for 12 hours, the primary particle size becomes 0.00. 76.7 g of columnar zinc oxide particles of 256 μm were obtained. The size and form of the obtained particles were observed with a transmission electron microscope (TEM, JEM-1200EX II, manufactured by JEOL Ltd.). The obtained electron micrograph is shown in FIG. The physical properties of the obtained particles are shown in Table 1.
(実施例7)
酢酸亜鉛二水和物(細井化学工業社製 酢酸亜鉛)266.07gをエチレングリコール(和光純薬工業社製 試薬一級)349.39mlと水698.79mlの混合溶液に溶解して酢酸亜鉛二水和物としての濃度が1mol/lとなるよう調製した酢酸亜鉛二水和物/エチレングリコール/水の混合溶液1200mlに、FINEX−50(堺化学工業社製 粒子径0.020μm)80gをリパルプしスラリーとした。このとき、シードとなるFINEX−50は完全に溶解することなく充分に溶液中に残っている状態であった。続いて、そのスラリーを攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で3時間反応した。反応後、真空ろ過、水洗した。続いて、得られた固形物を水3リットルにリパルプしてスラリーとし、攪拌しながら60分間で100℃に昇温し、攪拌しながら100℃で30分間加熱洗浄した。加熱洗浄後、真空ろ過、水洗し、イソプロピルアルコール1リットルにリパルプしてスラリーとし、真空ろ過により固形物を単離し、その固形物を110℃で12時間乾燥することにより、一次粒子径が0.357μmの六角板状酸化亜鉛粒子77.5gを得た。得られた粒子のサイズ・形態を透過型電子顕微鏡(TEM、JEM−1200EX II、日本電子社製)で観察した。得られた電子顕微鏡写真を図10に示した。また、得られた粒子の物性を表1に示した。
(Example 7)
266.07 g of zinc acetate dihydrate (Zinc acetate manufactured by Hosoi Chemical Co., Ltd.) was dissolved in a mixed solution of 349.39 ml of ethylene glycol (Reagent Grade 1 manufactured by Wako Pure Chemical Industries, Ltd.) and 698.79 ml of water. 80 mg of FINEX-50 (manufactured by Sakai Chemical Industry Co., Ltd., particle size: 0.020 μm) was repulped into 1200 ml of a mixed solution of zinc acetate dihydrate / ethylene glycol / water prepared so that the concentration as a Japanese product was 1 mol / l. A slurry was obtained. At this time, FINEX-50 used as a seed was not dissolved completely but remained in the solution. Subsequently, the slurry was heated to 100 ° C. over 60 minutes with stirring, and reacted at 100 ° C. for 3 hours with stirring. After the reaction, it was vacuum filtered and washed with water. Subsequently, the obtained solid was repulped into 3 liters of water to form a slurry, heated to 100 ° C. over 60 minutes with stirring, and heated and washed at 100 ° C. for 30 minutes with stirring. After heating and washing, vacuum filtration, washing with water, repulping to 1 liter of isopropyl alcohol to make a slurry, isolating the solid matter by vacuum filtration, and drying the solid matter at 110 ° C. for 12 hours, the primary particle size becomes 0. 77.5 g of 357 μm hexagonal plate-like zinc oxide particles were obtained. The size and form of the obtained particles were observed with a transmission electron microscope (TEM, JEM-1200EX II, manufactured by JEOL Ltd.). The obtained electron micrograph is shown in FIG. The physical properties of the obtained particles are shown in Table 1.
(比較例1)
焼成によって得られる酸化亜鉛粒子FINEX−30(堺化学工業社製 粒子径0.043μm)のサイズ・形態を透過型電子顕微鏡(TEM、JEM−1200EX II、日本電子社製)で観察した。得られた電子顕微鏡写真を図11に示した。また、得られた粒子の物性を表1に示した。
(Comparative Example 1)
The size and form of zinc oxide particles FINEX-30 (manufactured by Sakai Chemical Industry Co., Ltd., particle size 0.043 μm) obtained by firing were observed with a transmission electron microscope (TEM, JEM-1200EX II, manufactured by JEOL Ltd.). The obtained electron micrograph is shown in FIG. The physical properties of the obtained particles are shown in Table 1.
(比較例2)
まず、亜鉛化合物として酸化亜鉛1種(堺化学工業社製 粒子径0.6μm)を、溶媒としてエチレングリコールをそれぞれ用意した。また、酢酸(和光純薬工業社製、純度99.9%)と水を用意した。次いで、フラスコにエチレングリコール900g、酸化亜鉛1種15gを順に投入し、更に酢酸180gと水24gを添加し、混合して混合液を調製した。このとき、酸化亜鉛1種は完全に溶解し、溶液は無色透明であった。なお、このときの混合物全体を100重量%としたとき、エチレングリコールの割合は78.3重量%、酸化亜鉛1種の割合は3.9重量%、酢酸の割合は15.7重量%、水の割合は2.1重量%である。続いて、調製した混合液をオイルバス中で、マグネチックスターラで攪拌し、還流しながら、150℃まで加熱しようとしたが、139℃以上に加熱することはできなかった。この139℃の加熱を2時間保持したが、粒子は析出しなかった。
(Comparative Example 2)
First, one type of zinc oxide (manufactured by Sakai Chemical Industry Co., Ltd., particle size 0.6 μm) was prepared as the zinc compound, and ethylene glycol was prepared as the solvent. In addition, acetic acid (manufactured by Wako Pure Chemical Industries, Ltd., purity 99.9%) and water were prepared. Next, 900 g of ethylene glycol and 15 g of zinc oxide 1 type were sequentially added to the flask, and 180 g of acetic acid and 24 g of water were further added and mixed to prepare a mixed solution. At this time, one kind of zinc oxide was completely dissolved, and the solution was colorless and transparent. When the total mixture at this time is 100% by weight, the proportion of ethylene glycol is 78.3% by weight, the proportion of one kind of zinc oxide is 3.9% by weight, the proportion of acetic acid is 15.7% by weight, water The ratio is 2.1% by weight. Subsequently, the prepared liquid mixture was stirred with a magnetic stirrer in an oil bath and heated to 150 ° C. while refluxing, but could not be heated to 139 ° C. or higher. This heating at 139 ° C. was maintained for 2 hours, but no particles were deposited.
(比較例3)
まず、亜鉛化合物として酸化亜鉛1種(堺化学工業社製 粒子径0.6μm)を、溶媒としてエチレングリコールをそれぞれ用意した。また、酢酸(和光純薬工業社製、純度99.9%)と水を用意した。次いで、フラスコにエチレングリコール900g、酸化亜鉛1種45gを順に投入し、更に酢酸94gと水4gを添加し、混合して混合液を調製した。このとき、酸化亜鉛1種は完全に溶解し、溶液は無色透明であった。なお、このときの混合物全体を100重量%としたとき、エチレングリコールの割合は86.3重量%、酸化亜鉛1種の割合は4.3重量%、酢酸の割合は9.0重量%、水の割合は0.4重量%である。続いて、調製した混合液をオイルバス中で、マグネチックスターラで攪拌し、還流しながら、150℃まで加熱した。この加熱の際、145℃に達した時点で溶液が濁りフラスコ中に粒子が析出した。この150℃の加熱を2時間保持した後、自然放冷した。次に、得られた反応液を1000Gにて5時間遠心分離することで、反応液から沈殿物を分離した。更に、分離した沈殿物をエタノールに再分散させ、この分散液を遠心分離して、分散液から沈殿物を分離する工程を3回繰り返すことにより、沈殿物を洗浄した。最後に、洗浄した沈殿物を50℃で真空乾燥して粉末22.1gを得た。得られた粉末は薄茶色に着色しており、洗浄によって白色にすることはできなかった。得られた粒子のサイズ・形態を透過型電子顕微鏡(TEM、JEM−2100(HR)、日本電子社製)で観察した。得られた電子顕微鏡写真を図12に示した。また、得られた粒子の物性を表1に示した。
(Comparative Example 3)
First, one type of zinc oxide (manufactured by Sakai Chemical Industry Co., Ltd., particle size 0.6 μm) was prepared as the zinc compound, and ethylene glycol was prepared as the solvent. In addition, acetic acid (manufactured by Wako Pure Chemical Industries, Ltd., purity 99.9%) and water were prepared. Next, 900 g of ethylene glycol and 45 g of zinc oxide type 1 were sequentially added to the flask, and 94 g of acetic acid and 4 g of water were further added and mixed to prepare a mixed solution. At this time, one kind of zinc oxide was completely dissolved, and the solution was colorless and transparent. When the total mixture at this time is 100% by weight, the proportion of ethylene glycol is 86.3% by weight, the proportion of one kind of zinc oxide is 4.3% by weight, the proportion of acetic acid is 9.0% by weight, water The proportion of is 0.4% by weight. Subsequently, the prepared mixed liquid was stirred with a magnetic stirrer in an oil bath and heated to 150 ° C. while refluxing. During this heating, when the temperature reached 145 ° C., the solution became turbid and particles were deposited in the flask. This heating at 150 ° C. was held for 2 hours and then allowed to cool naturally. Next, the obtained reaction solution was centrifuged at 1000 G for 5 hours to separate precipitates from the reaction solution. Furthermore, the precipitate was washed by redispersing the separated precipitate in ethanol, centrifuging the dispersion and separating the precipitate from the dispersion three times. Finally, the washed precipitate was vacuum-dried at 50 ° C. to obtain 22.1 g of powder. The obtained powder was colored light brown and could not be made white by washing. The size and form of the obtained particles were observed with a transmission electron microscope (TEM, JEM-2100 (HR), manufactured by JEOL Ltd.). The obtained electron micrograph is shown in FIG. The physical properties of the obtained particles are shown in Table 1.
(X線回折のスペクトル、得られた粒子の組成)
図3、図7に示すX線回折のスペクトル、及び表1における得られた粒子の組成は、銅管球をもつX線回折装置UltimaIII(リガク社製)により分析した結果を示したものである。
(X-ray diffraction spectrum, composition of the obtained particles)
The spectrum of the X-ray diffraction shown in FIGS. 3 and 7 and the composition of the particles obtained in Table 1 show the results of analysis by an X-ray diffractometer Ultima III (manufactured by Rigaku Corporation) having a copper tube. .
(一次粒子径)
一次粒子径は、BET法によって求められる比表面積と同一の表面積を有する球の直径に相当する。すなわち、一次粒子径は、
一次粒子径(μm)=[6/(Sg×ρ)]
(Sg(m2/g):比表面積、ρ(g/cm3):粒子の真比重)
の関係式に基づき求めた値である。
上記BET法による比表面積:Sgは、全自動BET比表面積測定装置Macsorb(Mountech社製)により測定し、その測定値を上記計算に用いた。また、粒子の真比重:ρは、酸化亜鉛の真比重の値である5.6を上記計算に用いた。
(Primary particle size)
The primary particle diameter corresponds to the diameter of a sphere having the same surface area as that obtained by the BET method. That is, the primary particle size is
Primary particle diameter (μm) = [6 / (Sg × ρ)]
(Sg (m 2 / g): specific surface area, ρ (g / cm 3 ): true specific gravity of particles)
This is a value obtained based on the relational expression
The specific surface area by the BET method: Sg was measured by a fully automatic BET specific surface area measuring device Macsorb (manufactured by Mountaintech), and the measured value was used for the calculation. In addition, the true specific gravity of the particles: ρ was 5.6, which is the value of the true specific gravity of zinc oxide.
(メジアン径(D50)、D90、D10、D90/D10、D50/一次粒子径)
本明細書において、メジアン径(D50)、D90及びD10は、レーザー回折/散乱式粒度分布測定装置LA−750(堀場製作所社製)によって測定した値である。実施例、比較例の酸化亜鉛粒子0.5g、ヘキサメタりん酸ナトリウムとしての濃度が0.025重量%のヘキサメタりん酸ナトリウム水溶液50mlに分散し、3分間超音波分散処理することにより分散液を調製し、その分散液をレーザー回折/散乱式粒度分布測定装置LA−750(堀場製作所社製)の0.025重量%ヘキサメタりん酸ナトリウム水溶液で満たした試料バスに適量投入し、循環速度:15、超音波強度:7、超音波時間:3分の設定条件下で測定を行った。室温下における酸化亜鉛の屈折率が1.9〜2.0、水の屈折率が1.3であることから、相対屈折率は1.5に設定してメジアン径(D50)、D10、D90を求めた。メジアン径(D50)とは、体積基準での50%積算粒径、D90とは、体積基準での90%積算粒径、D10とは、体積基準での10%積算粒径を意味する。粒度分布のシャープさの指標として、D90とD10の比:D90/D10を算出する。この値が大きい程粒度分布がブロードであり粒子径が不揃いであることを意味し、この値が小さい程粒度分布がシャープで粒子径が均一であることを意味する。また、分散性の指標としてメジアン径(D50)と上記一次粒子径の比:D50/一次粒子径を算出する。この値が大きい程一次粒子径と分散状態にある粒子の径との乖離が大きい、すなわち分散性が悪く凝集が強い粒子であることを意味し、この値が小さい程、一次粒子径と分散状態にある粒子の径との乖離が小さい、すなわち分散性に優れた粒子であることを意味する。
(Median diameter (D50), D90, D10, D90 / D10, D50 / primary particle diameter)
In this specification, the median diameter (D50), D90, and D10 are values measured by a laser diffraction / scattering particle size distribution analyzer LA-750 (manufactured by Horiba, Ltd.). Disperse in 50 ml of an aqueous solution of sodium hexametaphosphate having 0.5 g of zinc oxide particles of Examples and Comparative Examples and a sodium hexametaphosphate concentration of 0.025 wt%, and preparing a dispersion by ultrasonic dispersion for 3 minutes. Then, an appropriate amount of the dispersion was put into a sample bath filled with 0.025 wt% sodium hexametaphosphate aqueous solution of a laser diffraction / scattering particle size distribution measuring apparatus LA-750 (manufactured by Horiba Seisakusho Co., Ltd.). Measurement was performed under the setting conditions of ultrasonic intensity: 7, ultrasonic time: 3 minutes. Since the refractive index of zinc oxide at room temperature is 1.9 to 2.0 and the refractive index of water is 1.3, the relative refractive index is set to 1.5 to set the median diameter (D50), D10, D90. Asked. The median diameter (D50) means a 50% cumulative particle size on a volume basis, D90 means a 90% cumulative particle size on a volume basis, and D10 means a 10% cumulative particle size on a volume basis. A ratio of D90 and D10: D90 / D10 is calculated as an index of the sharpness of the particle size distribution. A larger value means that the particle size distribution is broader and the particle size is uneven, and a smaller value means that the particle size distribution is sharper and the particle size is uniform. Further, as a dispersibility index, the ratio of the median diameter (D50) to the primary particle diameter: D50 / primary particle diameter is calculated. The larger this value is, the larger the difference between the primary particle size and the dispersed particle size is, that is, the particles are poorly dispersible and strongly agglomerated, and the smaller this value, the primary particle size and the dispersed state. It means that the deviation from the particle diameter is small, that is, the particles are excellent in dispersibility.
上記実施例及び比較例の結果から、本発明の酸化亜鉛粒子の製造方法によって、粒子形状、粒度分布がコントロールされた酸化亜鉛粒子を得ることができることが明らかである。 From the results of the above examples and comparative examples, it is clear that zinc oxide particles with controlled particle shape and particle size distribution can be obtained by the method for producing zinc oxide particles of the present invention.
本発明の酸化亜鉛粒子の製造方法によって得られた酸化亜鉛粒子は、化粧品用や電気・電子分野等の多くの分野において使用することができる。 The zinc oxide particles obtained by the method for producing zinc oxide particles of the present invention can be used in many fields such as cosmetics and electric / electronic fields.
Claims (1)
前記ポリオール系溶媒は、エチレングリコール、ジエチレングリコール、プロピレングリコール、1,3−プロパンジオール、1,3−ブタンジオール、トリエチレングリコール及びグリセリンからなる群より選択される少なくとも1種の化合物
であることを特徴とする酸化亜鉛粒子の製造方法。
A step of reacting zinc oxide as a seed in a polyol solvent in which a zinc salt is dissolved or a mixed solution of water in which a zinc salt is dissolved and a polyol solvent,
The polyol solvent is at least one compound selected from the group consisting of ethylene glycol, diethylene glycol, propylene glycol, 1,3-propanediol, 1,3-butanediol, triethylene glycol, and glycerin. A method for producing zinc oxide particles.
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