CN101535417A - 疏水性氧化锌粉末 - Google Patents
疏水性氧化锌粉末 Download PDFInfo
- Publication number
- CN101535417A CN101535417A CNA2007800405985A CN200780040598A CN101535417A CN 101535417 A CN101535417 A CN 101535417A CN A2007800405985 A CNA2007800405985 A CN A2007800405985A CN 200780040598 A CN200780040598 A CN 200780040598A CN 101535417 A CN101535417 A CN 101535417A
- Authority
- CN
- China
- Prior art keywords
- zinc oxide
- oxide powder
- alkyl
- aggregate
- hydrophobic zinc
- 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.)
- Pending
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 34
- 239000011787 zinc oxide Substances 0.000 claims abstract description 58
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011164 primary particle Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 57
- 238000009472 formulation Methods 0.000 claims description 52
- -1 halo organosilane Chemical class 0.000 claims description 47
- 125000000217 alkyl group Chemical group 0.000 claims description 22
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 10
- 150000001721 carbon Chemical group 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 125000005103 alkyl silyl group Chemical group 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 5
- 238000012935 Averaging Methods 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011247 coating layer Substances 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- 150000001282 organosilanes Chemical class 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 abstract 1
- 239000000839 emulsion Substances 0.000 description 38
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 24
- 239000012071 phase Substances 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 18
- 239000003921 oil Substances 0.000 description 17
- 235000019198 oils Nutrition 0.000 description 17
- 239000002245 particle Substances 0.000 description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 15
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 10
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 8
- OSCJHTSDLYVCQC-UHFFFAOYSA-N 2-ethylhexyl 4-[[4-[4-(tert-butylcarbamoyl)anilino]-6-[4-(2-ethylhexoxycarbonyl)anilino]-1,3,5-triazin-2-yl]amino]benzoate Chemical compound C1=CC(C(=O)OCC(CC)CCCC)=CC=C1NC1=NC(NC=2C=CC(=CC=2)C(=O)NC(C)(C)C)=NC(NC=2C=CC(=CC=2)C(=O)OCC(CC)CCCC)=N1 OSCJHTSDLYVCQC-UHFFFAOYSA-N 0.000 description 8
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 8
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 8
- 229940075529 glyceryl stearate Drugs 0.000 description 8
- FMJSMJQBSVNSBF-UHFFFAOYSA-N octocrylene Chemical compound C=1C=CC=CC=1C(=C(C#N)C(=O)OCC(CC)CCCC)C1=CC=CC=C1 FMJSMJQBSVNSBF-UHFFFAOYSA-N 0.000 description 8
- 229960000601 octocrylene Drugs 0.000 description 8
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 7
- 235000021355 Stearic acid Nutrition 0.000 description 7
- 125000005907 alkyl ester group Chemical group 0.000 description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 7
- 239000000600 sorbitol Substances 0.000 description 7
- 239000008117 stearic acid Substances 0.000 description 7
- MEIRRNXMZYDVDW-MQQKCMAXSA-N (2E,4E)-2,4-hexadien-1-ol Chemical compound C\C=C\C=C\CO MEIRRNXMZYDVDW-MQQKCMAXSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 241000404883 Pisa Species 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- XVAMCHGMPYWHNL-UHFFFAOYSA-N bemotrizinol Chemical compound OC1=CC(OCC(CC)CCCC)=CC=C1C1=NC(C=2C=CC(OC)=CC=2)=NC(C=2C(=CC(OCC(CC)CCCC)=CC=2)O)=N1 XVAMCHGMPYWHNL-UHFFFAOYSA-N 0.000 description 6
- 239000002537 cosmetic Substances 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 6
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 6
- 239000002480 mineral oil Substances 0.000 description 6
- 235000010446 mineral oil Nutrition 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- YBGZDTIWKVFICR-JLHYYAGUSA-N Octyl 4-methoxycinnamic acid Chemical class CCCCC(CC)COC(=O)\C=C\C1=CC=C(OC)C=C1 YBGZDTIWKVFICR-JLHYYAGUSA-N 0.000 description 5
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 5
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 229920001615 Tragacanth Polymers 0.000 description 4
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000000305 astragalus gummifer gum Substances 0.000 description 4
- 239000004359 castor oil Substances 0.000 description 4
- 235000019438 castor oil Nutrition 0.000 description 4
- 229940073638 ceteareth-15 Drugs 0.000 description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 235000011187 glycerol Nutrition 0.000 description 4
- 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 4
- 239000004200 microcrystalline wax Substances 0.000 description 4
- 235000019808 microcrystalline wax Nutrition 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229960001679 octinoxate Drugs 0.000 description 4
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- CMCBDXRRFKYBDG-UHFFFAOYSA-N 1-dodecoxydodecane Chemical compound CCCCCCCCCCCCOCCCCCCCCCCCC CMCBDXRRFKYBDG-UHFFFAOYSA-N 0.000 description 3
- HBXWUCXDUUJDRB-UHFFFAOYSA-N 1-octadecoxyoctadecane Chemical compound CCCCCCCCCCCCCCCCCCOCCCCCCCCCCCCCCCCCC HBXWUCXDUUJDRB-UHFFFAOYSA-N 0.000 description 3
- CNXZMGRWEYQCOQ-UHFFFAOYSA-N 2-methoxy-3-phenylprop-2-enoic acid Chemical compound COC(C(O)=O)=CC1=CC=CC=C1 CNXZMGRWEYQCOQ-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- DTPCFIHYWYONMD-UHFFFAOYSA-N decaethylene glycol Polymers OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO DTPCFIHYWYONMD-UHFFFAOYSA-N 0.000 description 3
- UVCJGUGAGLDPAA-UHFFFAOYSA-N ensulizole Chemical compound N1C2=CC(S(=O)(=O)O)=CC=C2N=C1C1=CC=CC=C1 UVCJGUGAGLDPAA-UHFFFAOYSA-N 0.000 description 3
- 229960000655 ensulizole Drugs 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- NQBWNECTZUOWID-UHFFFAOYSA-N (E)-cinnamyl (E)-cinnamate Natural products C=1C=CC=CC=1C=CC(=O)OCC=CC1=CC=CC=C1 NQBWNECTZUOWID-UHFFFAOYSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- FDCJDKXCCYFOCV-UHFFFAOYSA-N 1-hexadecoxyhexadecane Chemical compound CCCCCCCCCCCCCCCCOCCCCCCCCCCCCCCCC FDCJDKXCCYFOCV-UHFFFAOYSA-N 0.000 description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- RFVNOJDQRGSOEL-UHFFFAOYSA-N 2-hydroxyethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCO RFVNOJDQRGSOEL-UHFFFAOYSA-N 0.000 description 2
- XZIIFPSPUDAGJM-UHFFFAOYSA-N 6-chloro-2-n,2-n-diethylpyrimidine-2,4-diamine Chemical compound CCN(CC)C1=NC(N)=CC(Cl)=N1 XZIIFPSPUDAGJM-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000004166 Lanolin Substances 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 description 2
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- WERKSKAQRVDLDW-ANOHMWSOSA-N [(2s,3r,4r,5r)-2,3,4,5,6-pentahydroxyhexyl] (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO WERKSKAQRVDLDW-ANOHMWSOSA-N 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- NOPFSRXAKWQILS-UHFFFAOYSA-N docosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCO NOPFSRXAKWQILS-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 2
- 238000010191 image analysis Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229940039717 lanolin Drugs 0.000 description 2
- 235000019388 lanolin Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000003380 propellant Substances 0.000 description 2
- ARIWANIATODDMH-UHFFFAOYSA-N rac-1-monolauroylglycerol Chemical group CCCCCCCCCCCC(=O)OCC(O)CO ARIWANIATODDMH-UHFFFAOYSA-N 0.000 description 2
- 229940035044 sorbitan monolaurate Drugs 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 2
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- HEOCBCNFKCOKBX-RELGSGGGSA-N (1s,2e,4r)-4,7,7-trimethyl-2-[(4-methylphenyl)methylidene]bicyclo[2.2.1]heptan-3-one Chemical compound C1=CC(C)=CC=C1\C=C/1C(=O)[C@]2(C)CC[C@H]\1C2(C)C HEOCBCNFKCOKBX-RELGSGGGSA-N 0.000 description 1
- OIQXFRANQVWXJF-QBFSEMIESA-N (2z)-2-benzylidene-4,7,7-trimethylbicyclo[2.2.1]heptan-3-one Chemical compound CC1(C)C2CCC1(C)C(=O)\C2=C/C1=CC=CC=C1 OIQXFRANQVWXJF-QBFSEMIESA-N 0.000 description 1
- QMMJWQMCMRUYTG-UHFFFAOYSA-N 1,2,4,5-tetrachloro-3-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=C(Cl)C(Cl)=CC(Cl)=C1Cl QMMJWQMCMRUYTG-UHFFFAOYSA-N 0.000 description 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- LGEZTMRIZWCDLW-UHFFFAOYSA-N 14-methylpentadecyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCCCCCCCCCCCCC(C)C LGEZTMRIZWCDLW-UHFFFAOYSA-N 0.000 description 1
- ZEMPKEQAKRGZGQ-AAKVHIHISA-N 2,3-bis[[(z)-12-hydroxyoctadec-9-enoyl]oxy]propyl (z)-12-hydroxyoctadec-9-enoate Chemical compound CCCCCCC(O)C\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CC(O)CCCCCC)COC(=O)CCCCCCC\C=C/CC(O)CCCCCC ZEMPKEQAKRGZGQ-AAKVHIHISA-N 0.000 description 1
- 239000000263 2,3-dihydroxypropyl (Z)-octadec-9-enoate Substances 0.000 description 1
- PRBXPAHXMGDVNQ-UHFFFAOYSA-N 2-[2-(2-hydroxyethoxy)ethoxy]acetic acid Chemical compound OCCOCCOCC(O)=O PRBXPAHXMGDVNQ-UHFFFAOYSA-N 0.000 description 1
- LSHGMOIQPURPAK-UHFFFAOYSA-N 2-benzylidene-1,4,7,7-tetramethylbicyclo[2.2.1]heptan-3-one Chemical compound CC1(C)C(C2=O)(C)CCC1(C)C2=CC1=CC=CC=C1 LSHGMOIQPURPAK-UHFFFAOYSA-N 0.000 description 1
- JGUMTYWKIBJSTN-UHFFFAOYSA-N 2-ethylhexyl 4-[[4,6-bis[4-(2-ethylhexoxycarbonyl)anilino]-1,3,5-triazin-2-yl]amino]benzoate Chemical compound C1=CC(C(=O)OCC(CC)CCCC)=CC=C1NC1=NC(NC=2C=CC(=CC=2)C(=O)OCC(CC)CCCC)=NC(NC=2C=CC(=CC=2)C(=O)OCC(CC)CCCC)=N1 JGUMTYWKIBJSTN-UHFFFAOYSA-N 0.000 description 1
- LODHFNUFVRVKTH-ZHACJKMWSA-N 2-hydroxy-n'-[(e)-3-phenylprop-2-enoyl]benzohydrazide Chemical compound OC1=CC=CC=C1C(=O)NNC(=O)\C=C\C1=CC=CC=C1 LODHFNUFVRVKTH-ZHACJKMWSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/04—Compounds of zinc
- C09C1/043—Zinc oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P2006/11—Powder tap density
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/12—Surface area
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Crystallography & Structural Chemistry (AREA)
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Abstract
本发明提供一种疏水性氧化锌粉末,其是以氧化锌初级粒子的部分或完全包覆的聚集体的形式,以该疏水性氧化锌粉末为基准,其具有0.4-1.5重量%的碳含量,和25-100m2/g的BET表面积,其中:该包覆的聚集体中0至<10%呈圆球形式,15至<30%呈椭球形式,15至<30%呈线型形式,40至<70%呈分支状形式,且各种不同形式的总和为100%,并且该包覆层包含化学键合的具有1至20个碳原子的线性和/或枝化的单烷基甲硅烷基Si-烷基和/或二烷基甲硅烷基Si-(烷基) 2。
Description
技术领域
本发明涉及疏水性氧化锌粉末,其制备方法及其用途。
背景技术
疏水性氧化锌粉末在现有技术中是已知的。US 5,486,631公开了疏水性氧化锌粒子,其通过氧化锌与通式R-Si-[-(-O-SiMe2-)a-OR’]3的疏水化剂反应而制备,其中R为具有1-10个碳原子的烷基,R’为甲基或乙基,和a为4-12。在该方法中,氧化锌的选择不是关键性的。但是,为了满足化妆品配制物的要求,例如透明性和UV吸收,该疏水化剂的结构必须满足前述要求。这些要求限制了其在化妆品配制物中的可用性。
EP-A-1 508599公开了一种疏水性氧化锌粉末,其确实可用许多种疏水化剂而获得,但其BET表面积限制为18±5m2/g,并且其碳含量限制为0.5-1.0重量%。该粉末在化妆品配制物中的分散性和透明性需要改善。
发明内容
本发明的一个目的是提供一种疏水性氧化锌粉末,其在化妆品配制物中的使用性不受限制,即,其不会与配制物的其它组份有负面交互作用,可容易地加入至配制物中,并且具有高UV吸收和高透明性。
本发明的另一目的是提供一种疏水性氧化锌粉末的制备方法。
本发明提供一种疏水性氧化锌粉末,其是以氧化锌初级粒子的部分或完全包覆的聚集体的形式,以所述疏水性氧化锌粉末为基准具有0.4-1.5重量%的碳含量,和25-100m2/g的BET表面积,其中:
-所述包覆的聚集体中0至<10%呈圆球形式,15至<30%呈椭球形式,15至<30%呈线型形式,40至<70%呈分支状形式,各种不同形式的总和为100%,和
-所述包覆层包含化学键合的具有1至20个碳原子的线性和/或枝化的烷基甲硅烷基。
出人意料地,已经发现所述粉末在化妆品配制物中具有优异的分散性。由于本领域技术人员不能预料到根据本发明的氧化锌粉末的聚集体形式,以及在25-100m2/g的BET表面积的面积上的低碳含量会显示所述效果,因此其是出人意料的。所述效果目前尚不能精确地解释,但是显示出分支状聚集体的高比例是共同决定性因素。
优选地,圆球形式的比例为0至5%,椭球形式为20至25%,线型形式为20至25%和分支状形式为45至60%。
所述聚集体是通过透射电子显微镜的图像分析而被分成上述形式的。为此,使用照相机对约1000至2000个聚集体进行评价。各参数的定义是根据ASTM 3849-89。
本发明的氧化锌粉末的聚集体以圆球、椭球形、线型和分支状形式存在。
另外,已经发现本发明的疏水性氧化锌粉末可以优选地具有如下聚集体:其具有8000-30 000nm2的平均投影聚集体面积,70-300nm的等圆直径(ECD)和500-2000nm的平均周长。这些数值同样是根据ASTM 3849-89测定。
根据本发明的疏水性氧化锌粉末的碳含量为0.4-1.5重量%。在该范围内,在化妆品配制物中的分散性达到最佳。优选地,碳含量为0.6-1.0重量%。
本发明的疏水性氧化锌粉末的碳含量源自在聚集体表面上的烷基甲硅烷基。该烷基甲硅烷基优选地具有1-10个碳原子,特别优选4-8个碳原子。烷基的类型可通过例如NMR光谱测定。
结构A-J是可能的根据本发明的烷基甲硅烷基。在此,在每一情况中,-O-Si键的氧原子代表氧化锌表面的氧原子。
本发明的疏水性氧化锌粉末的BET表面积优选为25-35m2/g。
而且,所述疏水性氧化锌粉末优选地具有最多20ppm的铅、最多3ppm的砷、最多15ppm的镉、最多200ppm的铁、最多1ppm的锑,和最多1ppm的汞。
本发明进一步提供本发明的疏水性氧化锌粉末的制备方法,其中用一种或多种含有1-20个碳原子的硅烷化剂喷洒以聚集的初级粒子形式的氧化锌粉末,所述氧化锌粉末具有25-100m2/g的BET表面积,其中所述聚集体中0-10%呈圆球形式,30-50%呈椭球形式,30-50%呈线型形式,和20-30%呈分支状形式,所述硅烷化剂任选地溶解在有机溶剂中,然后在120-200℃,优选140-180℃的温度下热处理所述混合物0.5-2小时,优选1-1.5小时。
根据本发明的方法可以优选地在保护性气体环境,例如氮气中进行。
而且,根据本发明的方法可在带有喷洒装置的可加热型混合器和干燥器中连续地或不连续地进行,例如,犁头型混合器、盘式干燥器、流化床干燥器或移动床干燥器。
所用的氧化锌粉末例如可以根据DE-A-10343728中所述的方法制备。
这是以聚集体形式存在的热解法氧化锌粉末,其中所述聚集体是由各种不同形态学性质的粒子所构成,并且其中该聚集体中有0-10%呈圆球形式,30-50%呈椭球形式、30-50%呈线型形式和20-30%呈分支状形式。
形态学被理解为意指各向同性与各向异性的粒子。其可以例如是球形或大致球形粒子、球茎状粒子,棒状粒子或针状粒子。必要的是聚集体由不同的粒子构成并且这些粒子通过烧结的面积接合在一起。
可以优选使用如下氧化锌粉末,其具有大约相同比例的30-40%的椭球形式和线型形式,和较低比例的20-25%的分支状形式和2-6%的圆球形式。
所用的氧化锌粉末可以优选地具有根据DIN ISO 787/11测定的至少为150g/l的夯实密度(tamped density)。特别优选地,夯实密度可在250与350g/l之间。
而且,有利的是所用的氧化锌粉末由如下聚集体构成:具有小于10000nm2的平均投影聚集体面积,小于100nm的等圆直径(ECD)和小于600nm的平均周长。这些尺寸可以通过对约1000至2000个聚集体进行透射电子显微图像分析而获得。
特别优选地,可以使用如下的氧化锌粉末:其平均投影聚集体面积为2000至8000nm2,其等圆直径(ECD)为25-80nm并且其平均周长为200-550nm。
如果使用所述氧化锌粉末,出人意料地发现所用的氧化锌粉末的聚集体形式的比例与所得的疏水性氧化锌粉末的聚集体形式的比例不同。因此,根据本发明的方法特别地导致在方法产物中的线型形式和椭球形式的比例小于在所用材料中的比例。在方法产物中的较高比例的分支状聚集体相应可以用作良好分散性的标准。
可以使用的硅烷化剂优选为:
-X3Si(CnH2n+1)、X2(R’)Si(CnH2n+1)、X(R’)2Si(CnH2n+1)、X3Si(CH2)m-R’、(R)X2Si(CH2)m-R’、(R)2XSi(CH2)m-R’类型的卤代有机硅烷,其中:X=Cl、Br;R=烷基;R’=烷基;n=1-20;m=1-20;
-(RO)3Si(CnH2n+1)、R’x(RO)ySi(CnH2n+1)、(RO)3Si(CH2)m-R’、(R”)u(RO)vSi(CH2)m-R’类型的有机硅烷,其中:R=烷基;R’=烷基;n=1-20;m=1-20;x+y=3;x=1、2;y=1、2;u+v=2;u=1、2;v=1、2;
-R’R2Si-NH-SiR2R’类型的硅氮烷,其中R=烷基;R’=烷基、乙烯基;
-如下类型的聚硅氧烷:
其中,R=烷基、H;R’=烷基、H;R”=烷基、H;R”’=烷基、H;Y=CH3、H、CpH2p+1,其中p=1-20;Y=Si(CH3)3、Si(CH3)2H、Si(CH3)2OH、Si(CH3)2(OCH3)、Si(CH3)2(CpH2p+1),其中,p=1-20;m=0、1、2、3、...∞;n=0、1、2、3、...∞;u=0、1、2、3、...∞;或
-D3、D4和/或D5类型的环状聚硅氧烷。
另一主题是一种分散体,其包含根据本发明的疏水性氧化锌粒子。
所述分散体的液相可以是水,一或多种有机溶剂、或水/有机组合物,其中各相是可混溶的。
有机液相可以特别地是甲醇、乙醇、正丙醇和异丙醇、丁醇、辛醇、环己醇、丙酮、丁酮、环己酮、乙酸乙酯、乙二醇酯、乙醚、丁醚、茴香醚、二氧杂环己烷、四氢呋喃、单乙二醇醚、二乙二醇醚、三乙二醇醚和多乙二醇醚、乙二醇、二乙二醇、丙二醇、二甲基乙酰胺、二甲基甲酰胺、吡啶、N-甲基吡咯烷、乙腈、环丁砜、二甲亚砜、硝基苯、二氯甲烷、氯仿、四氯甲烷、氯化乙烯、戊烷、己烷、庚烷和辛烷、环己烷、汽油、石油醚、甲基环己烷、十氢萘、苯、甲苯和二甲苯、特别优选使用乙醇、正-和异丙醇、乙二醇、己烷、庚烷、甲苯和邻-、间-和对-二甲苯作为有机液相。
本发明的分散体可以进一步地包含pH调节剂、表面活性添加剂和/或防腐剂。
本发明的疏水性氧化锌粒子的含量优选地可为0.5-60重量%。优选包含10-50重量%,特别地35-45重量%的本发明的疏水性氧化锌粒子的分散体。
分散体中的平均粒度可以使用合适的分散单元在广范围内改变。这些例如可以是转子-定子机,高能研磨机,其中粒子通过彼此的碰撞而互相研磨;行星型捏合机;搅拌球磨机;作为摇动单元操作的球磨机;摇盘;超声波单元或上述单元的组合。
特别小的粒度可通过使用转子-定子机和高能研磨机获得。在此,平均粒度d50可得到小于180nm,特别地小于140nm的值,这可以通过动态光散射测定。
本发明进一步提供防晒配制物,其包含本发明的疏水性氧化锌粒子或本发明的分散体。
这些在所述防晒配制物中的含量通常为0.5-20重量%,优选1-10重量%,特别优选3-8重量%。
本发明的防晒配制物也包含本领域技术人员所知的所有水溶性或油溶性的UVA和UVB过滤剂。
例如:
-对胺基苯甲酸(PABA)和其衍生物,如二甲基-、乙基二羟基丙基-、乙基己基二甲基-、乙基-、甘油基-和4-双(聚乙氧基)-PABA;
-肉桂酸酯类,如肉桂酸甲酯和甲氧基肉桂酸酯类,包括甲氧基肉桂酸辛酯、甲氧基肉桂酸乙酯、对-甲氧基肉桂酸2-乙基己酯、对-甲氧基肉桂酸异戊酯、肉桂酸二异丙酯、4-甲氧基肉桂酸2-乙氧基乙酯、甲氧基肉桂酸的DEA盐(对-甲氧基羟基肉桂酸酯的二乙醇胺盐)、肉桂酸二异丙基甲基酯;
-二苯甲酮类,如2,4-二羟基-、2-羟基-4-甲氧基-、2,2’-二羟基-4,4’-二甲氧基-、2,2’-二羟基-4-甲氧基-、2,2’,4,4’-四羟基-、2-羟基-4-甲氧基-4’-甲基二苯甲酮、2,2’-二羟基-4,4’-二甲氧基-5-磺基二苯甲酮钠;
-二苯甲酰基甲烷,如丁基甲氧基二苯甲酰基甲烷,特别是4-叔丁基-4’-甲氧基二苯甲酰基甲烷;
-2-苯基苯并咪唑-5-磺酸和苯基二苯并咪唑磺酸酯及其盐;
-二苯基丙烯酸酯类,如α-氰基-β,β-二苯基丙烯酸烷基酯,如奥克立林(氰双苯丙烯酸辛酯)(octocrylene);
-三嗪类,如2,4,6-三苯胺(对-羰-2-乙基己基-1-氧基)-1,3,5-三嗪,乙基己基三嗪酮和二乙基己基丁酰胺基三嗪酮;
-樟脑衍生物,如4-甲基亚苄基-和3-亚苄基-樟脑和对苯二亚甲基二樟脑磺酸、亚苄基樟脑磺酸、樟脑苄烷铵甲硫酸盐及聚丙烯酰胺基甲基亚苄基樟脑;
-水杨酸酯类,如二丙二醇、乙二醇、乙基己基、异丙基苯甲基、甲基、苯基、3,3,5-三甲基和TEA等的水杨酸酯(2-羟基苯甲酸和2,2’,2”-次氨基三乙醇的化合物);
-2-氨基苯甲酸的酯类。
该防晒配制物可进一步包含本领域技术人员已知的化合物,如有机溶剂;增稠剂;乳化剂;软化剂;消泡剂;抗氧化剂;植物萃取物;湿化剂;香料;防腐剂和/或染料;络合剂;阴离子、阳离子、非离子或两性聚合物或它们的混合物;推进剂气体和细分散的粉末,包括粒度从100nm至20μm的金属氧化物颜料。
合适的软化剂特别地是鳄梨油、棉仔油、山萮醇、肉荳蔻酸丁酯、硬脂酸丁酯、鲸蜡醇、棕榈酸鲸蜡基酯、油酸癸酯、癸二酸二正丁酯、蓟子油、廿烷醇、甘油基单蓖麻酸酯、月桂酸己酯、棕榈酸异丁酯、异鲸蜡醇、硬脂酸异鲸蜡酯、异硬脂酸异丙酯、月桂酸异丙酯、亚麻油酸异丙酯、肉荳蔻酸异丙酯、棕榈酸异丙酯、硬脂酸异丙酯、异硬脂酸、可可豆脂、椰子油、羊毛脂、乳酸月桂基酯、玉米油、乳酸肉豆蔻基酯、肉豆蔻酸肉豆蔻基酯、夜樱草油、十八烷-2-醇、橄榄油、棕榈酸、棕榈仁油、聚乙二醇、菜仔油、蓖麻油、芝麻油、大豆油、癸花油、硬脂酸、硬脂醇、三乙二醇。
合适的乳化剂特别地是甘油单月桂酸酯、甘油单油酸酯、甘油单硬脂酸酯、PEG 1000二月桂酸酯、PEG 1500二油酸酯、PEG 200二月桂酸酯、PEG 200单硬脂酸酯、PEG 300单油酸酯、PEG 400二油酸酯、PEG400单油酸酯、PEG400单硬脂酸酯、PEG4000单硬脂酸酯、PEG600单油酸酯、聚氧化乙烯(4)山梨糖醇单硬脂酸酯、聚氧化乙烯(10)鲸蜡基醚、聚氧化乙烯(10)单油酸酯、
聚氧化乙烯(10)硬脂基醚、
聚氧化乙烯(12)月桂基醚、
聚氧化乙烯(14)月桂酸酯、
聚氧化乙烯(2)硬脂基醚、
聚氧化乙烯(20)鲸蜡基醚、
聚氧化乙烯(20)山梨醇单月桂酸酯、
聚氧化乙烯(20)山梨醇单油酸酯、
聚氧化乙烯(20)山梨醇单棕榈酸酯、
聚氧化乙烯(20)山梨醇单硬脂酸酯、
聚氧化乙烯(20)山梨醇三油酸酯、
聚氧化乙烯(20)山梨醇三硬脂酸酯、
聚氧化乙烯(20)山梨醇三硬脂酸酯、
聚氧化乙烯(20)硬脂基醚、
聚氧化乙烯(23)月桂基醚、
聚氧化乙烯(25)氧化丙烯单硬脂酸酯、
聚氧化乙烯(3.5)壬酚、
聚氧化乙烯(4)月桂基醚、
聚氧化乙烯(4)山梨醇单月桂酸酯、
聚氧化乙烯(5)单硬脂酸酯、
聚氧化乙烯(5)山梨醇单硬脂酸酯、
聚氧化乙烯(50)单硬脂酸酯、
聚氧化乙烯(8)单硬脂酸酯、
聚氧化乙烯(9.3)辛基酚、
聚氧化乙烯山梨醇羊毛脂衍生物、
山梨醇单月桂酸酯、山梨醇单油酸酯、
山梨醇单棕榈酸酯、山梨醇单硬脂酸酯、
山梨醇倍半油酸酯、山梨醇三硬脂酸酯、
山梨醇三油酸酯。
合适的推进剂气体可以是丙烷、丁烷、异丁烷、甲醚和/或二氧化碳。
合适的细分散粉末可以是白垩、滑石、高岭土、胶体二氧化硅、聚丙烯酸钠、四烷基-和/或三烷基芳基铵蒙皂石、硅酸镁铝、蒙脱土、硅酸铝、热解法二氧化硅、和热解法二氧化钛。
典型地,本发明的防晒组合物可以是乳液(O/W、W/O或多相)的形式、含水或水-醇凝胶或油凝胶形式,并且可以以洗液、乳膏、喷乳剂(milk sprays)、慕斯(mousse)、硬膏(stick)或其它常见形式施加。
实施例
分析方法
BET表面积根据DIN 66131测定。
透射电子显微照片是使用Hitachi TEM仪器,型号H-75000-2获得。使用TEM仪器的CCD照相机和后续的图像分析,评定约1000至2000个聚集体。各参数的定义根据ASTM 3849-89。关于圆球、椭球形、线型和分支型形状的聚集体的形状分析根据Herd et al.,Rubber,Chem.Technol.66(1993)491进行。
进料:
氧化锌粉末:所用的氧化锌粉末1A-3A通过在DE-A-10343728中公开的方法制备。这些粉末的分析值示于表1中。
本发明的疏水性氧化锌粉末的制备:
首先将氧化锌粉末1A引入至混合器中。在强力混合下,首先任选地用水喷洒,然后用硅烷化剂喷洒。当喷洒操作完全时,将混合物后搅拌约15分钟,然后热处理。
以类似方式转化氧化锌2A和3A。进料和反应条件示于表2中。
防晒配制物:
以下列出本发明的防晒配制物,其与得自实施例1B的本发明的疏水性ZnO一起,与OC=奥克立林(octocrylene)、OMC=甲氧基肉桂酸乙基己酯、PISA=苯基苯并咪唑磺酸或BEMT=双乙基己氧基甲氧基苯基三嗪任一显示协同效果。出于统计理由,如果使用术语“协同”,则认为SPF应该大于或等于各个配制物的SPF的总和更高的2个单位。
SPF(防晒因子)测量使用optometrics SPF 290-S仪器在体外进行。
实施例4A-C
在这些实施例中,使用W/O乳液的标准配制物。将得自实施例1B的氧化锌引入至体系的油相中。从油相(硬脂酸乙基己酯和矿物油)除去氧化锌的额外部分。
A 标准配制物W/O乳液含ZnO
B 标准配制物W/O乳液含OC
C 标准配制物W/O乳液含ZnO和OC
实施例5A-D
在这些实施例中,使用O/W乳液的标准配制物。将得自实施例1B的氧化锌引入至体系的油相中。从水相(水)除去氧化锌的额外部分。作为实验,使用异硬脂酸作为表面改性剂和pH稳定剂。
A 标准配制物O/W乳液含ZnO
B 标准配制物O/W乳液含OC
C 标准配制物O/W乳液含ZnO
D 标准配制物O/W乳液含ZnO+异硬脂酸
实施例6A-C
在这些实施例中,使用W/O乳液的标准配制物。将得自实施例1B的氧化锌引入至体系的油相中。从油相(硬脂酸乙基己酯和矿物油)除去氧化锌的额外部分。
A 标准配制物W/O乳液含ZnO
B 标准配制物W/O乳液含OMC
C 标准配制物W/O乳液含ZnO和OMC
实施例7A-D
在这些实施例中,使用O/W乳液的标准配制物。将得自实施例1B的氧化锌引入到体系的油相中。从水相(水)除去氧化锌的额外部分。作为实验,使用异硬脂酸作为表面改性剂和pH稳定剂。
A 标准配制物O/W乳液含ZnO
B 标准配制物O/W乳液含OMC
C 标准配制物O/W乳液含ZnO和OMC
D 标准配制物O/W乳液含ZnO、OMC和异硬脂酸
实施例8A-C
在这些实施例中,使用W/O乳液的标准配制物。将得自实施例1B的氧化锌引入至体系的油相中。从油相(硬脂酸乙基己酯和矿物油)除去氧化锌的额外部分。
A 标准配制物W/O乳液含ZnO
B 标准配制物W/O乳液含PISA
C 标准配制物W/O乳液含ZnO和PISA
实施例9A-D
在这些实施例中,使用O/W乳液的标准配制物。将得自实施例1B的氧化锌引入至体系的油相中。从水相(水)除去氧化锌的额外部分。作为实验,使用异硬脂酸。
A 标准配制物O/W乳液含ZnO
B 标准配制物O/W乳液含PISA
C 标准配制物O/W乳液含ZnO和PISA
D 标准配制物O/W乳液含ZnO、PISA和异硬脂酸
实施例10A-C
在这些实施例中,使用W/O乳液的标准配制物。将得自实施例1B的氧化锌引入至体系的油相中。从油相(苯甲酸C12-C15烷基酯)除去氧化锌的额外部分。
A 标准配制物W/O乳液含ZnO
B 标准配制物W/O乳液含BEMT
C 标准配制物W/O乳液含ZnO和BEMT
实施例11A-D
在这些实施例中,使用O/W乳液的标准配制物。将得自实施例1B的氧化锌引入至体系的油相中。从水相(水)除去氧化锌的额外部分。作为实验,使用异硬脂酸作为表面改性剂和pH稳定剂。
A 标准配制物O/W乳液含ZnO
B 标准配制物O/W乳液含BEMT
C 标准配制物O/W乳液含ZnO和BEMT
D 标准配制物O/W乳液含ZnO、BEMT和异硬脂酸
表1:所用的氧化锌粉末
实施例 | 1A | 2A | 3A | |
BET表面积 | m2/g | 27 | 32 | 75 |
聚集体圆球椭球形线型分支型 | % | 4373623 | 1302940 | 9442621 |
平均聚集体面积 | nm2 | 4941 | 5502 | 2470 |
聚集体的等圆直径 | nm | 66 | 110 | 33 |
平均聚集体周长 | nm | 445 | 520 | 222 |
表2:进料和调整
实施例 | 1B | 2B | 3B | |
氧化锌 | 1A | 2A | 3A | |
硅烷化剂分量a) | 重量% | 辛基三甲氧基硅烷1.5 | 辛基三甲氧基硅烷3 | 聚二甲基硅氧烷2 |
H2Oa)分量 | 重量% | 0 | 0.2 | 0 |
温度 | ℃ | 140 | 140 | 160 |
时间 | 小时 | 1.2 | 1.2 | 1.4 |
a)以100份ZnO为基准
表3:本发明的疏水性氧化锌粉末
实施例 | 1B | 2B | 3B | |
BET表面积 | m2/g | 27 | 31 | 73 |
C含量 | 重量% | 0.8 | 1.1 | 0.7 |
Si-烷基Si-(烷基)2 | Si-辛基Si-(辛基)2 | Si-辛基Si-(辛基)2 | Si-甲基Si-(甲基)2 | |
聚集体圆球椭球形线型分支型 | % | 1182655 | 2212453 | 1172953 |
平均聚集体面积 | nm2 | 32635 | 31251 | 20345 |
聚集体的等圆直径 | nm | 167 | 152 | 140 |
平均聚集体周长 | nm | 1420 | 1240 | 980 |
表4:W/O配制物-实施例4(单位%)
相 | INCI | 4A | 4B | 4C |
A | 鲸蜡基PEG/PPG-10/1二甲基聚硅氧烷 | 2.5 | 2.5 | 2.5 |
硬脂酸乙基己酯 | 12.5 | 12.5 | 10.0 | |
矿物油 | 12.5 | 12.5 | 10.0 | |
异硬脂酸 | 1.0 | 1.0 | 1.0 | |
氢化蓖麻油 | 0.5 | 0.5 | 0.5 | |
微晶蜡 | 1.0 | 1.0 | 1.0 | |
奥克立林(octocrylene) | 5.0 | 5.0 | ||
氧化锌 | 5.0 | 5.0 | ||
B | 氯化钠 | 0.5 | 0.5 | 0.5 |
水 | 64.45 | 64.45 | 64.45 | |
2-溴-2-硝基丙烷-1,3-二醇 | 0.05 | 0.05 | 0.05 | |
SPF | 2 | 3 | 6 |
表5:O/W配制物-实施例5(单位%)
相 | INCI | 5A | 5B | 5C | 5D |
A | 鲸蜡硬脂醇聚醚-15,甘油基硬脂酸酯 | 2.5 | 2.5 | 2.5 | 2.5 |
甘油基硬脂酸酯 | 1.0 | 1.0 | 1.0 | 1.0 | |
硬脂醇 | 2.0 | 2.0 | 2.0 | 2.0 | |
苯甲酸C12-C15烷基酯 | 14.5 | 9.5 | 9.5 | 8.5 | |
奥克立林(octocrylene) | 5.0 | 5.0 | 5.0 | ||
氧化锌(w、c、) | 10.0 | 10.0 | 10.0 | ||
异硬脂酸 | 1.0 | ||||
B | 甘油 | 3.0 | 3.0 | 3.0 | 3.0 |
水 | 66.5 | 76.5 | 66.5 | 66.5 | |
氯乙酰胺 | 0.1 | 0.1 | 0.1 | 0.1 | |
C | 黄蓍胶 | 0.4 | 0.4 | 0.4 | 0.4 |
SPF | 2 | 3 | 8 | 9 |
表6:W/O配制物-实施例6(单位%)
相 | INCI | 6A | 6B | 6C |
A | 鲸蜡基PEG/PPG-10/1二甲基聚硅氧烷 | 2.5 | 2.5 | 2.5 |
硬脂酸乙基己酯 | 12.5 | 12.5 | 10.0 | |
矿物油 | 12.5 | 15.5 | 10.0 | |
异硬脂酸 | 1.0 | 1.0 | 1.0 | |
氢化蓖麻油 | 0.5 | 0.5 | 0.5 | |
微晶蜡 | 1.0 | 1.0 | 1.0 | |
甲氧基肉桂酸乙基己酯 | 5.0 | 5.0 | ||
氧化锌(w、c、) | 5.0 | 5.0 | ||
B | 氯化钠 | 0.5 | 0.5 | 0.5 |
水 | 64.45 | 64.45 | 64.45 |
2-溴-2-硝基丙烷-1,3-二醇 | 0.05 | 0.05 | 0.05 | |
SPF | 2 | 7 | 13 |
表7:O/W配制物-实施例7(单位%)
相 | INCI | 7A | 7B | 7C | 7D |
A | 鲸蜡硬脂醇聚醚-15,甘油基硬脂酸酯 | 2.5 | 2.5 | 2.5 | 2.5 |
甘油基硬脂酸酯 | 1.0 | 1.0 | 1.0 | 1.0 | |
硬脂醇 | 2.0 | 2.0 | 2.0 | 2.0 | |
苯甲酸C12-C15烷基酯 | 14.5 | 9.5 | 9.5 | 8.5 | |
甲氧基肉桂酸乙基己酯 | 5.0 | 5.0 | 5.0 | ||
氧化锌(w、c、) | 10.0 | 10.0 | 10.0 | ||
异硬脂酸 | 1.0 | ||||
B | 甘油 | 3.0 | 3.0 | 3.0 | 3.0 |
水 | 66.5 | 76.5 | 66.5 | 66.5 | |
氯乙酰胺 | 0.1 | 0.1 | 0.1 | 0.1 | |
C | 黄蓍胶 | 0.4 | 0.4 | 0.4 | 0.4 |
SPF | 2 | 6 | 11 | 16 |
表8:W/O配制物-实施例8(单位%)
相 | INCI | 8A | 8B | 8C |
A | 鲸蜡基PEG/PPG-10/1二甲基聚硅氧烷 | 2.5 | 2.5 | 2.5 |
硬脂酸乙基己酯 | 12.5 | 15.0 | 12.5 | |
矿物油 | 12.5 | 15.0 | 12.5 | |
异硬脂酸 | 1.0 | 1.0 | 1.0 | |
氢化蓖麻油 | 0.5 | 0.5 | 0.5 | |
微晶蜡 | 1.0 | 1.0 | 1.0 | |
氧化锌(w、c、) | 5.0 | 5.0 | ||
B | 氯化钠 | 0.5 | 0.5 | 0.5 |
水 | 64.45 | 49.45 | 49.45 | |
2-溴-2-硝基丙烷-1,3-二醇 | 0.05 | 0.05 | 0.05 | |
苯基苯并咪唑磺酸(20%水溶液) | 15.0 | 15.0 | ||
SPF | 2 | 5 | 9 |
表9:O/W配制物-实施例9(单位%)
相 | INCI | 9A | 9B | 9C | 9D |
A | 鲸蜡硬脂醇聚醚-15,甘油基硬脂酸酯 | 2.5 | 2.5 | 2.5 | 2.5 |
甘油基硬脂酸酯 | 1.0 | 1.0 | 1.0 | 1.0 | |
硬脂醇 | 2.0 | 2.0 | 2.0 | 2.0 | |
苯甲酸C12-C15烷基酯 | 14.5 | 14.5 | 14.5 | 13.5 | |
氧化锌(w、c、) | 10.0 | 10.0 | 10.0 | ||
异硬脂酸 | 1.0 | ||||
B | 甘油 | 3.0 | 3.0 | 3.0 | 3.0 |
水 | 66.5 | 61.5 | 51.5 | 51.5 | |
氯乙酰胺 | 0.1 | 0.1 | 0.1 | 0.1 | |
苯基苯并咪唑磺酸(20%水溶液) | 15.0 | 15.0 | 15.0 | ||
C | 黄蓍胶 | 0.4 | 0.4 | 0.4 | 0.4 |
SPF | 2 | 5 | 11 | 15 |
表10:W/O配制物-实施例10(单位%)
相 | INCI | 10A | 10B | 10C |
A | 鲸蜡基PEG/PPG-10/1二甲基聚硅氧烷 | 2.5 | 2.5 | 2.5 |
苯甲酸C12-C15烷基酯 | 27.0 | 25.0 | 22.0 | |
异硬脂酸 | 1.0 | 1.0 | 1.0 | |
氢化蓖麻油 | 0.5 | 0.5 | 0.5 | |
微晶蜡 | 1.0 | 1.0 | 1.0 | |
双-乙基己氧基酚甲氧基苯基三嗪 | 3.0 | 3.0 | ||
氧化锌(w、c、) | 5.0 | 5.0 | ||
B | 氯化钠 | 0.5 | 0.5 | 0.5 |
水 | 64.45 | 64.45 | 64.45 | |
2-溴-2-硝基丙烷-1,3-二醇 | 0.05 | 0.05 | 0.05 | |
SPF | 2 | 8 | 13 |
表11:O/W配制物-实施例11(单位%)
相 | INCI | 11A | 11B | 11C | 11D |
A | 鲸蜡硬脂醇聚醚-15,甘油基硬脂酸酯 | 2.5 | 2.5 | 2.5 | 2.5 |
甘油基硬脂酸酯 | 1.0 | 1.0 | 1.0 | 1.0 | |
硬脂醇 | 2.0 | 2.0 | 2.0 | 2.0 | |
苯甲酸C12-C15烷基酯 | 14.5 | 12.5 | 12.5 | 11.5 | |
双-乙基己氧基酚甲氧基苯基三嗪 | 2.0 | 2.0 | 2.0 | ||
氧化锌(w、c、) | 10.0 | 10.0 | 10.0 | ||
异硬脂酸 | 1.0 | ||||
B | 甘油 | 3.0 | 3.0 | 3.0 | 3.0 |
水 | 66.5 | 76.5 | 66.5 | 66.5 | |
氯乙酰胺 | 0.1 | 0.1 | 0.1 | 0.1 | |
C | 黄蓍胶 | 0.4 | 0.4 | 0.4 | 0.4 |
SPF | 2 | 3 | 6 | 8 |
Claims (8)
1、一种疏水性氧化锌粉末,其是以氧化锌初级粒子的部分或完全包覆的聚集体的形式,以所述疏水性氧化锌粉末为基准具有0.4-1.5重量%的碳含量,和25-100m2/g的BET表面积,其中:
-所述包覆的聚集体中0至<10%呈圆球形式,15至<30%呈椭球形式,15至<30%呈线型形式,40至<70%呈分支状形式,各种不同形式的总和为100%,和
-所述包覆层包含化学键合的具有1至20个碳原子的线性和/或枝化的烷基甲硅烷基。
2、如权利要求1所述的疏水性氧化锌粉末,其特征在于所述聚集体具有8000-30000nm2的平均投影聚集体面积,70-300nm的等圆直径(ECD)和500-2000nm的平均周长。
3、如权利要求1或2所述的疏水性氧化锌粉末,其特征在于铅的比例最多为20ppm,砷的比例最多为3ppm,镉的比例最多为15ppm,铁的比例最多为200ppm,锑的比例最多为1ppm和汞的比例最多为1ppm。
4、如权利要求1所述的疏水性氧化锌粉末,其中:
-化学键合至聚集体表面的烷基甲硅烷基含有1至8个碳原子,
-聚集体中0至5%呈圆球形式,20至25%呈椭球形式,20至25%呈线型形式,45至60%呈分支状形式,各种不同形式的总和为100%,
-以所述疏水性氧化锌粉末为基准,碳含量为0.6至1.2重量%,和
-BET表面积为25至40m2/g。
5、如权利要求1-4任一项所述的疏水性氧化锌粉末的制备方法,其特征在于用一种或多种含有1-20个碳原子的硅烷化剂喷洒聚集的初级粒子形式的氧化锌粉末,所述氧化锌粉末具有25-100m2/g之间的BET表面积,其中所述聚集体中0-10%呈圆球形式,30-50%呈椭球形式,30-50%呈线型形式和20-30%呈分支状形式,所述硅烷化剂任选地溶解在有机溶剂中,然后在120-200℃的温度下热处理混合物0.5-2小时。
6、如权利要求5所述的方法,其特征在于所述硅烷化剂选自如下:
-X3Si(CnH2n+1)、X2(R’)Si(CnH2n+1)、X(R’)2Si(CnH2n+1)、X3Si(CH2)m-R’、(R)X2Si(CH2)m-R’、(R)2XSi(CH2)m-R’类型的卤代有机硅烷,其中:X=Cl、Br;R=烷基;R’=烷基;n=1-20;m=1-20;
-(RO)3Si(CnH2n+1)、R’x(RO)ySi(CnH2n+1)、(RO)3Si(CH2)m-R’、(R”)u(RO)vSi(CH2)m-R’类型的有机硅烷,其中:R=烷基;R’=烷基;n=1-20;m=1-20;x+y=3;x=1、2;y=1、2;u+v=2;u=1、2;v=1、2;
-R’R2Si-NH-SiR2R’类型的硅氮烷,其中:R=烷基;R’=烷基、乙烯基;
-如下类型的聚硅氧烷:
其中,R=烷基、H;R’=烷基、H;R”=烷基、H;R”’=烷基、H;Y=CH3、H、CpH2p+1,其中,p=1-20;Y=Si(CH3)3、Si(CH3)2H、Si(CH3)2OH、Si(CH3)2(OCH3)、Si(CH3)2(CpH2p+1),其中,p=1-20;m=0、1、2、3、...∞;n=0、1、2、3、...∞;u=0、1、2、3、...∞;或
-D3、D4和/或D5类型的环状聚硅氧烷。
7、一种分散体,其包含如权利要求1-4所述的疏水性氧化锌粉末。
8、一种防晒配制物,其包含如权利要求1-4所述的疏水性氧化锌粉末或如权利要求7所述的分散体。
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DE102008035524A1 (de) | 2008-07-30 | 2010-02-04 | Ibu-Tec Advanced Materials Ag | Zinkoxid-Partikel, Zinkoxid-Pulver und Verwendung dieser |
EP2634083B1 (en) | 2012-03-02 | 2015-07-08 | Sea-Bird Electronics, Inc | Fluid-based buoyancy compensation |
WO2014186687A1 (en) * | 2013-05-16 | 2014-11-20 | Bnz Materials, Inc. | Refractory castables with hydrophobic aggregates |
JP5850189B1 (ja) * | 2015-01-30 | 2016-02-03 | 住友大阪セメント株式会社 | 酸化亜鉛粉体、分散液、塗料、化粧料 |
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