CN1454245A - 阳极电泳涂漆的方法和电泳漆 - Google Patents
阳极电泳涂漆的方法和电泳漆 Download PDFInfo
- Publication number
- CN1454245A CN1454245A CN00817286A CN00817286A CN1454245A CN 1454245 A CN1454245 A CN 1454245A CN 00817286 A CN00817286 A CN 00817286A CN 00817286 A CN00817286 A CN 00817286A CN 1454245 A CN1454245 A CN 1454245A
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- Prior art keywords
- acid
- phosphoric acid
- ester
- epoxy
- epoxy ester
- 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.)
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000003973 paint Substances 0.000 title claims description 47
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 75
- 150000002148 esters Chemical class 0.000 claims abstract description 63
- 239000004593 Epoxy Substances 0.000 claims abstract description 55
- 238000007598 dipping method Methods 0.000 claims abstract description 38
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 36
- 239000007787 solid Substances 0.000 claims abstract description 26
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims description 49
- 239000003795 chemical substances by application Substances 0.000 claims description 39
- 235000011007 phosphoric acid Nutrition 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- -1 allyl group phosphonic acids Chemical class 0.000 claims description 23
- 239000000049 pigment Substances 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 230000005611 electricity Effects 0.000 claims description 18
- 150000003009 phosphonic acids Chemical class 0.000 claims description 13
- 239000000945 filler Substances 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 10
- 239000004922 lacquer Substances 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 8
- 230000001070 adhesive effect Effects 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 6
- 150000002927 oxygen compounds Chemical class 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 125000003700 epoxy group Chemical group 0.000 claims description 5
- SEHJHHHUIGULEI-UHFFFAOYSA-N 2-hydroxyethylphosphonic acid Chemical class OCCP(O)(O)=O SEHJHHHUIGULEI-UHFFFAOYSA-N 0.000 claims description 2
- JYFHYPJRHGVZDY-UHFFFAOYSA-N Dibutyl phosphate Chemical compound CCCCOP(O)(=O)OCCCC JYFHYPJRHGVZDY-UHFFFAOYSA-N 0.000 claims description 2
- LXCYSACZTOKNNS-UHFFFAOYSA-N diethoxy(oxo)phosphanium Chemical compound CCO[P+](=O)OCC LXCYSACZTOKNNS-UHFFFAOYSA-N 0.000 claims description 2
- UCQFCFPECQILOL-UHFFFAOYSA-N diethyl hydrogen phosphate Chemical compound CCOP(O)(=O)OCC UCQFCFPECQILOL-UHFFFAOYSA-N 0.000 claims description 2
- ZTWTYVWXUKTLCP-UHFFFAOYSA-L ethenyl-dioxido-oxo-$l^{5}-phosphane Chemical compound [O-]P([O-])(=O)C=C ZTWTYVWXUKTLCP-UHFFFAOYSA-L 0.000 claims description 2
- GTTBQSNGUYHPNK-UHFFFAOYSA-N hydroxymethylphosphonic acid Chemical compound OCP(O)(O)=O GTTBQSNGUYHPNK-UHFFFAOYSA-N 0.000 claims description 2
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 2
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 abstract description 5
- 229920005989 resin Polymers 0.000 description 41
- 239000011347 resin Substances 0.000 description 41
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 33
- 229920000728 polyester Polymers 0.000 description 23
- 150000001875 compounds Chemical class 0.000 description 20
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 20
- 239000005056 polyisocyanate Substances 0.000 description 19
- 229920001228 polyisocyanate Polymers 0.000 description 19
- 238000000576 coating method Methods 0.000 description 18
- 239000011248 coating agent Substances 0.000 description 17
- 238000002360 preparation method Methods 0.000 description 17
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 15
- 239000006185 dispersion Substances 0.000 description 15
- 229920005862 polyol Polymers 0.000 description 14
- 150000003077 polyols Chemical class 0.000 description 14
- 125000001931 aliphatic group Chemical group 0.000 description 12
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 11
- 230000003472 neutralizing effect Effects 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 10
- 125000002723 alicyclic group Chemical group 0.000 description 10
- 238000010422 painting Methods 0.000 description 10
- 238000006068 polycondensation reaction Methods 0.000 description 10
- 150000008065 acid anhydrides Chemical class 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 description 9
- 229940043276 diisopropanolamine Drugs 0.000 description 9
- 239000000178 monomer Substances 0.000 description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 8
- 238000013019 agitation Methods 0.000 description 8
- 150000001412 amines Chemical class 0.000 description 8
- 239000002585 base Substances 0.000 description 8
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 8
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 229920003270 Cymel® Polymers 0.000 description 7
- 229920000877 Melamine resin Polymers 0.000 description 7
- 239000004640 Melamine resin Substances 0.000 description 7
- 125000003118 aryl group Chemical group 0.000 description 7
- 125000004432 carbon atom Chemical group C* 0.000 description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 7
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 7
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 6
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 238000007334 copolymerization reaction Methods 0.000 description 6
- LVHBHZANLOWSRM-UHFFFAOYSA-N itaconic acid Chemical compound OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 6
- 229920001225 polyester resin Polymers 0.000 description 6
- 239000004645 polyester resin Substances 0.000 description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- 229960002887 deanol Drugs 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 238000007654 immersion Methods 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 5
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 4
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 4
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 4
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 239000011541 reaction mixture Substances 0.000 description 4
- 239000003351 stiffener Substances 0.000 description 4
- 150000003512 tertiary amines Chemical class 0.000 description 4
- MNAHQWDCXOHBHK-UHFFFAOYSA-N 1-phenylpropane-1,1-diol Chemical compound CCC(O)(O)C1=CC=CC=C1 MNAHQWDCXOHBHK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000004721 Polyphenylene oxide Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical group CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002118 epoxides Chemical group 0.000 description 3
- 230000032050 esterification Effects 0.000 description 3
- 238000005886 esterification reaction Methods 0.000 description 3
- 239000001530 fumaric acid Substances 0.000 description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229940059574 pentaerithrityl Drugs 0.000 description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 3
- 229920000570 polyether Polymers 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- WRIFCFZXLZGSGD-UHFFFAOYSA-N 1-(dimethylamino)-2-methylpropan-1-ol Chemical compound CC(C)C(O)N(C)C WRIFCFZXLZGSGD-UHFFFAOYSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
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- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 description 2
- 229920003264 Maprenal® Polymers 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 2
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000002947 alkylene group Chemical group 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
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- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 150000008064 anhydrides Chemical class 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 description 2
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
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- PFURGBBHAOXLIO-UHFFFAOYSA-N cyclohexane-1,2-diol Chemical compound OC1CCCCC1O PFURGBBHAOXLIO-UHFFFAOYSA-N 0.000 description 2
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- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 2
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- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
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- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 2
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- 150000004706 metal oxides Chemical class 0.000 description 2
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 2
- 239000010445 mica Substances 0.000 description 2
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- 230000003641 microbiacidal effect Effects 0.000 description 2
- 229940124561 microbicide Drugs 0.000 description 2
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- 239000011707 mineral Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明涉及一种通过将导电表面浸在水性阳极电浸涂漆液中并连接做阳极来对它进行阳极电浸涂漆的方法,其中所用水性阳极电浸涂漆液基于电浸涂漆液的粘合剂固体含有1~15重量%的一种或多种磷酸环氧酯和/或膦酸环氧酯。所述磷酸环氧酯和/或膦酸环氧酯是在醇存在下制得的。
Description
本发明涉及一种尤其适合于生产具有期望的无光度和改进的边缘保护的涂膜的电浸涂漆方法和与此相配的电泳涂漆。电浸涂漆是一种完全自动化的、环保的和经济的涂漆方法,因此实际应用于导电表面尤其是金属表面的批量涂漆。电浸涂漆是一种完全自动化的高涂镀效率的涂镀方法。此工艺优选以闭合循环进行,并且允许重复利用多余的漆料以及所用辅助物质和加工助剂。
为提高涂膜的耐蚀性,经常往电泳涂漆中加入腐蚀抑制颜料如铅或铬的化合物,例如铬酸铅、碱式硅酸铅或铬酸锶。然而由于健康和环境的原因这些化合物并不是人们想要的。
那些被认为毒性小一些的颜料如磷酸锌、磷酸铝、氧化锌等不能提供满意的防腐结果。而且电浸涂漆液中的锌化合物可能导致不稳定性。
因此,在DE-A-43 06 024中提出了加镧的有机酸盐如醋酸镧。但却得不到关于边缘保护的满意结果。
在DE-A-42 25 999中描述了基于环氧树脂的交联聚合物微粒,其在作车身涂底漆的常规电泳涂漆中用作有机填料、消光剂和/或增强剂,这些电泳涂漆也不能提供关于边缘保护的满意结果。
EP-A-0 240 876、EP-A-0 216 337、WO 93/07206和EP-A-0 174628描述了浸液中加了磷酸环氧酯的电泳涂漆。该磷酸环氧酯是由环氧化合物和磷酸在水存在的情况下制得的。已经发现这些浸液的浸液稳定性不足而且在涂漆设备的漂洗区发生的沉积漆的再溶解相对较高。
因此本发明的一个目的就是提供一种阳极电浸涂漆方法,它没有这些缺点而且能生产具有跟现有技术相比性质改良了的漆膜,尤其是边缘保护增强,此外还允许任意调整无光度,而且高度通用,其中浸液也稳定,再溶解减少。
令人惊奇的发现,通过用含有少量的在醇类存在的情况下生产的磷酸环氧酯和/或膦酸环氧酯的水性阳极电浸涂漆液来沉积,这个目的就可以达到。因而本发明涉及导电表面尤其是金属表面的阳极电浸涂漆方法,该方法是通过将导电表面尤其是金属表面浸入水性阳极电浸涂漆液中并连接做阳极,其特征在于所用的水性阳极电浸涂漆液基于电浸涂漆液的结合剂固体含有1-15重量%,优选5-10重量%的一种或多种酸值10到50的磷酸环氧酯和/或膦酸环氧酯,也就是指电浸涂漆液中的粘合固体,它们是由一种或多种单体的、低聚或聚合环氧化合物与磷酸或膦酸或其酯或其混合物在一种或多种醇存在的情况下反应得到的。在文中粘合剂固体这个词是指成膜树脂(粘合剂)中的固体成分以及任选存在的交联剂和浆树脂(为分散颜料和/或填料)。
本发明还提供了一种含有一种或多种成膜树脂以及任选的交联剂、颜料、填料、有机溶剂和/或常用的漆添加剂的水性电浸涂漆液,其特征在于基于粘合剂固体它含有1-15重量%的一种或多种酸值10到50的磷酸环氧酯和/或膦酸环氧酯,它是通过一种或多种单体的、低聚或聚合环氧化合物与磷酸或膦酸或其酯或其混合物在一种或多种醇存在下反应而得到的。
此外,本发明还提供了上述磷酸环氧酯和/或膦酸环氧酯作电浸涂漆液的添加剂的用途。
在阳极电浸涂漆(ATL)中,将具有导电表面的金属或导电塑料材料或由带有导电涂层的基体的工件放入水性ATL液中并作为阳极连接到直流电源上。当施加一个直流电流时,通过至少部分成盐使之水溶或可水分散的ATL液中的水性分散体的聚合物颗粒迁移到阳极并在那里与同时发生的水的电解产生的离子反应重新形成水不溶性的聚合物,其从水相中凝结出来并和分散在那里的添加剂一起沉积在阳极上成为漆膜。电浸涂漆的原理是已知的且在文献中也有描述,例如在Metalloberflche 31(1997)10、第455到459页。
水性阳极电浸涂漆液通常是向水介质中加入阳极电泳涂漆的方法制得的。在此根据不同的用途,电泳涂漆可以呈单组分形式(着色粘合剂组分和任选的交联组分)或双组分形式(颜料浆和粘合剂组分以及任选的交联组分)作为浓缩物(补充物)或以具有不同中和度的水预稀释的形式(初始加入材料)。
根据需要可将磷酸环氧酯和/或膦酸环氧酯加入到电泳涂漆成品中或者在其生产中加入或者加入到备用的电浸涂漆液中或在其制备过程中加入。
例如阳极电泳涂漆可以用本领域技术人员已知的常用的方式,通过一种或多种合适的粘合剂或粘合剂分散剂与磷酸环氧酯和/或膦酸环氧酯和任选的一种或多种交联剂以及任选的常用添加剂和/或诸如催化剂、抗光剂、荧光增白剂、杀菌剂、中性树脂、成层剂、乳化剂和任选的颜料和/或填料进行混合制备。磷酸环氧酯或膦酸环氧酯也可以加入到电泳涂漆成品中和/或加入到电浸涂漆液成品中和/或加入到正在使用的电浸涂漆液中。
适合的磷酸环氧酯和/或膦酸环氧酯是通过一种或多种单体的、低聚或聚合环氧化合物与磷酸或膦酸或其酯或与这些酸或它们的酯的混合物在一种或多种醇存在的情况下反应而得到的。例子包括磷酸、磷酸二乙酯、磷酸三乙酯、磷酸二丁酯、磷酸三丁酯、羟甲基膦酸、羟乙基膦酸、乙烯基膦酸、烯丙基膦酸或苯甲基膦酸二乙酯;优选正磷酸。由于反应中醇类的存在,至少部分地形成10到50的低酸值的混合酯。
环氧化合物平均每个分子有至少一个,优选至少两个环氧基团且环氧当量在90到4000克/当量,优选150到3500克/当量,特别优选400到3000克/当量。
对此,环氧化合物可以是饱和的或不饱和的并且可以是脂族的、脂环族的、芳香族的和/或杂环的,还可以包含羟基。此外,它们可以包含那些在反应条件下不会引起干扰的副反应的取代基和/或官能团,例如烷基取代基或芳基取代基和醚基。
合适的环氧化合物的例子是表氯醇和双酚A的缩合产物,例如Shell公司的Epikote类、Ciba Geigy公司的Araldite或DowChemical公司的D.E.R.、D.E.M.、D.E.H.类、含环氧基的酚醛清漆、多元醇的缩水甘油醚、多元羧酸的缩水甘油酯、天然存在的脂肪和油的环氧化产物、环氧化聚丁二烯或有侧位环氧乙烷基的低分子量丙烯酸酯树脂。在维也纳慕尼黑Carl Hanser出版社于1996年出版的Stoye/Freitag的“Lackharze”,第247到251页中有适合本发明的环氧化合物的详细列举将这些环氧化物引入本文。
环氧化合物的环氧基团和要与之反应的磷酸或膦酸的酸基的比率优选是1∶1到3∶1。
环氧化合物与磷酸或膦酸的反应是在一种或多种醇存在的情况下,任选加入溶剂,例如在80℃到100℃的温度下进行。用于形成部分地作为混合酯存在的反应产物的醇的用量选择要使在此化学反应前由环氧化合物、磷酸或膦酸或它们的衍生物和醇形成的有机相中的固体含量优选在65~85重量%之间,特别优选为70~80重量%。反应可以在例如缓慢回流下进行。混合酯的形成优选在无水的情况下进行。反应进行到酸值在10到50,优选15到40。可将反应产物转化成水分散体。为此,可以加入中和剂来中和游离的酸性基团并用完全去离子水稀释到期望的固体含量,其中,例如至少50%的游离酸性基团被转化成盐的形式。
合适的醇是例如脂族醇,例如含1到6个碳原子的低级脂族醇如正丁醇、叔丁醇、仲丁醇、异丙醇、正丙醇、甲醇、乙醇和/或己醇。
可以用于此反应的合适的溶剂有酯、醚、酮和芳族化合物。
适合做中和剂的是也可用于制备阳极电泳涂漆的常用碱,例如NaOH、KOH、LiOH、氨、伯胺,仲胺和叔胺如二乙胺、三乙胺、吗啉;链烷醇胺如二异丙醇胺、二甲胺基乙醇、三异丙醇胺、二甲氨基-2-甲基丙醇、季铵氢氧化物或这些中和剂的混合物。
用于阳极电泳涂漆的合适的粘合剂可以是所有常用的粘合剂体系,例如酸值在20到150,优选20到120和羟基数在0到150,优选20到120的那些,例如它们常用于水性涂料系统,尤其是用于阳极电泳涂漆。
属于此类的粘合剂包括如聚酯树脂、聚丙烯酸酯树脂和聚氨酯树脂,例如醇酸树脂、聚氨酯聚酯树脂或丙烯酸化的聚酯树脂或聚氨酯树脂、马来酸化的油、环氧酯、马来酸化的聚丁二烯油、以及这些树脂的混合物。优选聚酯树脂。
合适的聚酯树脂是例如酸值20到150和羟基数20到150的含羧基和含羟基的聚酯。它们是按本领域技术人员所知的方法,通过多元醇和多元羧酸或羧酸酐以及任选的脂族和/或芳族一元羧酸进行缩聚来制备的。羧基和羟基的量的调整是按熟知的方法通过适当的选择起始成分的种类和用量比。羧基例如可以通过由预先备好的含羟基的聚酯树脂与酸酐形成半酯来引入。羧基的引入例如也可以通过在缩聚反应中共用羟基羧酸来进行。
适合用于缩聚反应的多元羧酸,特别是二元羧酸,和多元醇例如可以是脂族的、脂环族的或芳族的。
用于制备聚酯的多羟基化合物是例如二醇如亚烷基二醇,例如乙二醇、丁二醇、己二醇、氢化双酚A、2,2-丁基乙基丙二醇、新戊二醇和/或其它二醇例如二羟甲基环己烷。还可以用较高级官能的或单官能的与较高级官能的OH组分,例如三羟甲基丙醇、季戊四醇、丙三醇、己三醇的混合物;乙二醇和烯化氧缩合而得的聚醚多元醇;这些二元醇的单醚如二甘醇一乙醚、三丙二醇一甲醚。
聚酯中的酸组分优选由含有2到18个碳原子的低分子量的二元羧酸或它们的酐组成。合适的酸包括例如邻苯二甲酸、间苯二酸、对苯二酸、六氢邻苯二甲酸、己二酸、壬二酸、癸二酸、富马酸、马来酸、戊二酸、丁二酸、衣康酸和/或1,4-环己二酸。除了这些酸,它们的甲酯和酐存在时也可以用。为了得到支链聚酯,也可以加入一定量的高级官能的羧酸,例如三官能羧酸如偏苯三酸、羟基丁二酸、丙烯三甲酸、双羟乙基牛磺酸以及二羟甲基丙酸、二羟甲基丁酸或双酐。优选不形成环状酸酐的多元羧酸。
还可以通过掺入不饱和化合物、含异氰酸酯基化合物、或通过与不饱和烯化合物接种聚合或接枝聚合来改性聚酯树脂。优选的聚酯是例如含羧基聚酯,其酸值在20到150和羟基数为20到150,优选60到120。它们是例如二元和/或多元脂族或脂环族的饱和醇,脂族的、脂环族和/或单环芳族的二元或多元羧酸,和任选的直链或支链的、饱和或不饱和的脂族和/或脂环族的C3到C20的一元醇或一元羧酸的反应产物。起始成分的用量比是从导致树脂中期望的酸值和羟基数的摩尔比来计算的。本领域技术人员根据指定的用途可以轻易的选出各个起始成分。
可用的聚酯的数均分子量Mn,用聚苯乙烯做标准物质测得,在例如1000到6000,优选在2000到4000的范围内。
例如DE-A-32 47 756中所述按照一个优选实施方案,应用含羟基的无油聚酯。这些聚酯优选每克树脂含有缩合引入的0.3到3.0毫当量,特别优选0.5到2.5毫当量的脂族、脂环族和/或芳族二元羧酸。优选三元或多元环羧酸以每克树脂0.8到2.0,优选0.9到1.8,最好在1.1到1.5毫当量只通过一个羧基基团连接到聚酯上。多元羧酸可以用三元和/或多元羧酸,优选用三元和/或四元酸。这些聚酯的生产可以熟知的手段通过起始物质的缩聚来进行的,为避免混浊和形成凝胶,缩聚反应优选逐步进行。
在此优选实施方案中,那些不能形成分子内酸酐的优选芳族和脂环族的二元羧酸的酯化反应优选与二元醇进行,此二元醇或者含有仲OH基或含有通过β-取代空间位阻的伯OH基,由此,通过醇过量形成含OH基的聚酯。该醇类优选含有2到21个C原子,特别优选4到8个C原子。该二元羧酸优选含有5到10个C原子,特别优选6个C原子。
对此合适的二元羧酸的例子有间苯二酸、对苯二酸、1,3-环己二酸和1,4-环己二酸或烷基取代的二元羧酸如丁基间苯二酸。特别优选间苯二酸。
另一方面还可通过酯交换反应把二甲酯如对苯二酸二甲酯或1,4-环己二酸二甲酯引入聚酯中,任选在酯交换反应催化剂存在下进行。为得到支链,代替部分二元羧酸,可以通过缩合反应把相应量的三元羧酸如1,2,4-苯三酸酐引入树脂分子中。
用于该优选实施方案中的二元醇用的是例如新戊二醇、羟基特戊酸新戊二醇酯、己二醇-2,5、1,4-双(羟甲基)环己烷、1,1-异嘧啶-双-(对苯氧基)-2-丙醇、2,2,4-三羟甲基戊二醇-1,3以及它们的混合物。二元醇还可以用例如α-支链脂肪酸如一种有支链的烷烃酸的缩水甘油酯,由于脂肪酸是水解稳定地被引入分子结构中。也可使用环氧基已经和一元醇反应了的环氧树脂。
在该优选实施方案中,可部分地使用含有超过两个OH基团的多羟基化合物如三羟甲基丙烷或季戊四醇来调节适当的羟基数和粘度。同样也可用长链二元醇如己二醇-1,6或脂族二元羧酸如己二酸来轻微地调节其弹性。
在该优选实施方案中以及通常情况下,酯化反应(第一级)可以按已知方式共沸或高温(如高于190℃)的融化状态下进行,产生酸值在例如0到50,优选5到25,和例如在25℃下75%的丁二醇溶液中测得的粘度在200到3000mPas的透明产物。
在优选实施方案中以及通常情况下,为提高在碱性水介质中的溶解性,可另外向含OH基聚酯中引入羧基。对此,例如进行与如芳族或脂环族二元羧酸的反应,其优选由含三或四个羧基的多元羧酸如1,3,5-苯三酸、2,3-二甲基苯甲酸、连苯四酸和苯偏四甲酸通过与长链脂肪族疏水一元醇的去官能化作用进行。该反应可以简单的用酸酐化合物如1,2,4-苯三酸酐、1,2,4,5-苯四酸酐或相应的氢化环系、以及环戊烷四甲酸酐或吡嗪四酸酐来进行。该反应可在例如低于190℃的温度下进行。
作为一元醇可以用直链和/或支链的、饱和和/或不饱和的伯醇、仲醇和/或叔醇,优选伯醇和/或仲醇。也可以用这些醇的混合物,尤其是这些醇的异构体混合物。优选脂族C6到C18的一元醇以及苯甲醇和它的烷基取代物。特别优选C8到C13的支链异一元醇。特别水解稳定的半酯通过应用α支化的一元醇或仲一元醇如环己醇或仲甲基辛醇得到。通过树脂合成保证任选通过水解产生的分解产物(一元醇和苯偏三酸一酯)不影响电泳地与膜分离。
多元羧酸可以例如和足够的一元醇在两罐方法中按化学计量比反应,于是剩下二元羧酸,再把它加入到含OH基的聚酯中,例如在大约150℃到190℃温度下加入。
实践中已经证明单罐方法中通过按指定的顺序向含OH基聚酯中加入大约计量的一元醇和含酐基化合物如苯三偏酸酐可以可靠地的生产含羧基聚酯。
羧基的引入也可以在缩聚反应中通过同时应用羟基羧酸如二羟甲基丙酸进行,通常它的游离羧基由于位阻并不参与缩聚反应,结果使得此酸的引入完全通过羟基。
可以如此选择用于制备聚酯的总体组成的摩尔比,使得可以得到适合各自应用目的的粘度。粘度在25℃下50%的丁二醇溶液中测得,优选大约200到3000,特别优选250到2000,最好300到1500mPas。象分子量一样,粘度也可以通过混合低粘度和高粘度树脂,或低分子量和高分子量的树脂来调整。酸值的上限优选低于100,最好低于60;酸值的下限优选高于35,最好高于40。为了与低分子量碱形成盐以达到水稀释性,含羧基聚酯的每个分子含有至少一个、优选至少两个羧基。如果酸值过低,溶解性可能不足,而如果酸值过高,高度的中和可能会导致ATL浸液中的电解增大,反过来引起表面缺陷。选择醇过量导致树脂成品中羟基数为例如大约20到150,优选60到120。优选羟基数相对较高而酸值较低的树脂。
缩聚可以在例如共沸或在熔融下进行,例如反应温度介于160℃到240℃,优选介于160℃和210℃之间。在达到关于粘度和酸值的期望的最终值后,将反应混合物冷却到一定的温度,此温度下产物的粘度正好允许水被引入。实际中这意味着熔融粘度通常不高于40000mPas。只要不在加压下进行,该温度最高到例如大约100℃。为使产物变成水溶性或水分散体,缩聚产物的羧基通过加入中和剂至少被部分地中和。中和剂可以在水加入前或在水加入时加入,也可存在于缩聚产物分散于其中的水中。在此,可以应用例如高速叶轮搅拌器装置、转子/定子混合器或高压均质机。有机溶剂任选可以在转化成水溶液或分散体期间或之后通过蒸馏来去除。
合适的中和剂是常规的碱例如NaOH、KOH、LiOH、氨、伯、仲和叔胺如二乙胺、三乙胺、吗啉;链烷醇胺如二异丙醇胺、二甲氨基乙醇、三异丙醇胺、二甲氨基-2-甲基丙醇、季铵氢氧化物或任选的少量的亚烷基多胺如乙二胺。也可使用这些中和剂的混合物。
中和剂的用量选择例如要使得到的每100克固体树脂中MEQ的值为15到90,优选20到60毫当量胺。
适合做电泳漆粘合剂的聚丙烯酸酯树脂包括例如含羧基和/或含磺酸基的酸值20到150的共聚物。数均分子量Mn是例如1000到10000。
粘合剂的生产是根据常规方法通过烯属不饱和单体的共聚进行,其中含有酸性基团的单体和另外的单体共聚。用含有酸性基团的单体的目的是向共聚物中引入羧酸和/或磺酸基,以确保在部分地中和这些基团之后共聚物的水溶性和水分散性。
合适的含酸基的单体原则上是所有含有至少一个羧酸和/或磺酸基团的烯属不饱和可聚合化合物。例如烯属不饱和一元羧酸或二元羧酸如(甲基)丙烯酸、丁烯酸、反丁烯二酸、顺丁烯二酸、衣康酸或反丁烯二酸、顺丁烯二酸、衣康酸的半酯、或含有磺酸基的烯烃的不饱和化合物例如2-丙烯酰氨基-2-甲基丙磺酸或这些烯属不饱和酸的任意混合物。首选丙烯酸和甲基丙烯酸。
为在成品漆中得到想要的应用技术性能,除了含酸性基团的单体外,共聚物还可以包含含有其它官能团的单体,通过它们例如就可以进行交联反应。对此可以发生共聚物的自交联和与漆中另外引入的其它组分的外交联,而且在共聚物的生产中所有非官能的、烯属不饱和单体原则上都可以联合使用。
这类官能团的例子有羟基、氨基、酰氨基、酮基、醛基、内酰胺基、内酯基、异氰酸酯基、环氧基和硅烷基。带有这些功能基团的烯属不饱和单体是熟知的。优选羟基和环氧基。
合适的非官能单体是例如其醇部分含1到18个C原子的丙烯酸和甲基丙烯酸的酯类、乙烯基芳族化合物、脂族单元羧酸的乙烯酯、丙烯腈和甲基丙烯腈。
共聚物的生产可以根据常规的工艺进行聚合。共聚物的生产优选在有机溶剂中进行。连续共聚或不连续共聚工艺都可以用。
合适的溶剂是芳族化合物、酯、醚和酮。优选乙二醇醚。
共聚是在例如80℃到180℃的温度下使用常用的引发剂例如脂族偶氮化合物、或过氧化物进行的。为调节共聚物的分子量可以用常规的调节剂。共聚完成之后,可将共聚物中和并转化成水溶液或分散体,正如在缩聚树脂中描述的那样,其中的有机溶剂可任选蒸馏掉。碱性中和剂的例子是上文中用于聚酯树脂的中和的那些。
适合于做电泳漆粘合剂的聚氨酯树脂包括例如含有以盐形式存在的羧酸、磺酸、和/或磷酸基团的阴离子聚氨酯树脂。粘合剂是按熟知的方法由多羟基化合物、多异氰酸酯和任选的增链剂制备的。
聚氨酯树脂既可以本体生产也可以在不与异氰酸酯反应的有机溶剂中生产。如在缩聚树脂中描述的那样,在中和了酸性基团之后可以把这些树脂引入水相。也可以用逐步的方法来生产聚氨酯树脂。
因此,就可例如首先在有机溶剂中生产含有酸性基团和端位异氰酸酯基的预聚物,预聚物用叔胺中和酸性基团后,经过链增长,接着引入水相,其间可通过蒸馏去除有机溶剂。
用于生产预聚物的多羟基化合物可以是低分子量和/或高分子量的多羟基化合物且也可包含阴离子基团。
低分子量的多羟基化合物的数均分子量Mn优选为60到400,且可含有脂肪、脂环或芳基基团。它们的用量例如可以占总多羟基化合物组分的30重量%。
适合的低分子量的多羟基化合物包括例如二醇、三元醇和多元醇如乙二醇、二甘醇、三甘醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、1,2-丁二醇、1,6-己二醇、三羟甲基丙烷、蓖麻油或氢化蓖麻油、季戊四醇、1,2-环己二醇、1,4-环己二甲醇、双酚A、双酚F、氢化双酚A以及这些多羟基化合物的混合物。
高分子量的多羟基化合物包括OH数为30到150的直链或支链多羟基化合物。它们的用量例如最高可以占总多羟基化合物组成的97重量%。这些多羟基化合物优选是数均分子量Mn为400到5000的饱和或不饱和聚酯二醇和/或聚醚二醇和/或聚碳酸酯二醇或它们的混合物。
适合的直链或支链聚醚二醇是例如聚氧化乙二醇、聚氧化丙二醇和/或聚氧化丁二醇。
优选聚酯二醇,聚酯二醇是按已知方法通过把二元羧酸或它们的酐与二醇进行酯化来制备的。为制备支链聚酯,也可以少量的应用高官能度的多羟基化合物或多羧酸。
能形成阴离子的基团可以来自聚酯中,或通过共用含有两个可以和异氰酸酯基反应的活性H基且至少一个H基可形成阴离子的化合物引入到预聚物中。与异氰酸酯基反应的合适的基团特别是羟基以及伯和/或仲胺基。可以形成阴离子的基团包括例如羧酸基、磺酸基、和/或磷酸基。此类化合物的例子有二羟基羧酸如二羟基丙酸、二羟基丁酸、二羟基丁二酸、二氨基丁二酸并且优选α,α-二羟甲基链烷酸例如二羟甲基丙酸。
合适的聚异氰酸酯包括每个分子有至少两个异氰酸酯基的脂族、脂环族和/或芳族聚异氰酸酯,与含有熟知的缩二脲-、脲基甲酸-、尿烷-和/或异氰酸酯基的这些二异氰酸酯的衍生物,以及这些聚异氰酸酯的混合物。优选使用有机二异氰酸酯的异构体或异构体混合物。
用于制备预聚物的聚异氰酸酯组分也可包含少量的高官能度聚异氰酸酯。
预聚物的制备可以便利地在催化剂例如有机锡化合物或叔胺存在下进行。
在用碱中和剂中和聚氨酯树脂中的酸基,任选蒸馏掉有机溶剂之后,进行聚氨酯树脂向水相的转移,如聚酯树脂中描述的那样。
碱中和剂的例子如上文聚酯树脂中所述。
用在本发明电泳涂漆中粘合剂的交联过程优选在烘烤下与交联剂进行反应。通常交联剂是分开加的;当然粘合剂也可以含有能导致自交联的活性官能基团。作为交联剂和/或交联组分可以用本领域技术人员普遍知道的那些。例子包括氨基塑料树脂、特别是三聚氰胺甲醛树脂;酚塑料树脂;封端聚异氰酸酯或酯交换交联剂如带有羟烷基酯基的聚酯或聚氨酯、乙酰乙酸或丙二酸的烷基酯衍生物、三(烷氧羰基氨基)三嗪衍生物和这些组分的混合物,它们可以在有催化剂或没催化剂的情况下形成高度交联涂层。优选三聚氰胺树脂和封端聚异氰酸酯。
封端聚异氰酸酯平均每个分子含有多于一个的异氰酸酯基、优选至少两个异氰酸酯基。当储存在pH值为大约中性到弱碱性的水相中时,它们应该能稳定存在,加热到100℃到200℃时离解,且可与树脂结构中有活性的羟基和/或羧基发生交联。
封端聚异氰酸酯是通过聚异氰酸酯与含活性氢的单官能团化合物反应得到的。
作为既可单独又可以封端形式的混合物用作交联剂的聚异氰酸酯合适的是含有脂族、脂环族、芳脂族和/或芳族连接的游离异氰酸酯基的任意有机二异氰酸酯和/或聚异氰酸酯都适合。
优选含有3到36,最好是8到15个碳原子的聚异氰酸酯。适合的聚异氰酸酯的例子有甲代亚苯基二异氰酸酯、二苯甲基二异氰酸酯和、特别是六亚甲基二异氰酸酯、四甲代苯二甲撑二异氰酸酯、异佛尔酮二异氰酸酯、二环己基甲烷二异氰酸酯和环己烷二异氰酸酯。
基于环己烷二异氰酸酯、异佛尔酮二异氰酸酯和/或二环己基甲烷二异氰酸酯的“聚异氰酸酯漆”是最适合的,此外涉及熟知的这些二异氰酸酯的含有缩二脲、氨基甲酸酯基、uretdione、和/或异氰脲酯基的衍生物。
用来封端聚异氰酸酯的含活性氢的单官能团化合物是本领域技术人员熟知的。举例来说可用的有CH酸性化合物如乙酰丙酮;CH酸性酯如乙酰乙酸烷基酯、丙二酸二烷基酯;(环)脂肪醇如正丁醇、2-乙基己醇、环己醇;乙二醇醚类如丁基乙二醇、丁基二甘醇;酚类如甲酚、叔丁基苯酚;二氨基醇类如二甲氨基乙醇;肟类如丁酮肟、丙酮肟、环己酮肟;内酰胺如ε-己内酰胺或吡咯烷酮-2;酰亚胺;羟烷基酯;异羟肟酸及其酯;吡唑类。
聚异氰酸酯可以在一个分子内用相同的或不同的封端剂来封端。也可使用相同或不同的封端的聚异氰酸酯的混合物。
三聚氰胺甲醛树脂例如与聚酯树脂的羟基通过形成醚基交联。这些交联剂例如根据已知的工业方法在醇如甲醇、乙醇、丙醇、丁醇或己醇存在的情况下与醛类、特别是甲醛进行缩合的三嗪类诸如三聚氰胺或苯并胍胺。这些交联剂优选是甲醇醚化的三聚氰胺树脂例如Cymel325、Cymel 327、Cymel 350、Cymel 370、Maprenal MF 927;丁醇醚化的或异丁醇醚化的三聚氰胺树脂例如Setamin US 138或Maprenal MF 610;混合醚化的三聚氰胺树脂、以及特别是六羟甲基三聚氰胺树脂例如Cymel 301或Cymel 303。
常用的颜料、填料、防腐剂和漆助剂都可用来给阳极电泳涂漆染色,只要它们不与弱碱性到中性pH范围的水产生干扰的反应也带入水溶性的干扰杂质离子。对此的颜料和填料是通常用于漆工业中的填料和无机或有机发色的和/或特殊效果颜料。
无机发色颜料的例子包括二氧化钛、微粉二氧化钛、硫化锌、锌钡白、碳酸铅、硫化铅、氧化锡、氧化锑、铁的氧化物、铬黄、镍钛黄、铬橙、钼红、矿物紫、群青紫、群青(蓝)、钴蓝、氧化铬绿和碳黑。发色有机颜料的例子选自由偶氮、酞菁、喹吖啶酮、苝、Perinon、蒽醌、硫靛和二酮吡咯并吡咯颜料。特殊效果颜料的例子有金属颜料、特别是铝、铜或其它金属颜料;光干涉颜料例如带金属氧化膜的金属颜料或带金属氧化膜的云母;珠光颜料和光可变颜料(OVP)。
填料的例子包括碳酸钙、硫酸钡、滑石、二氧化硅、硅酸铝、硅酸镁、云母、氢氧化铝和硅酸。填料还可用有机化合物来改性(涂覆)。这类改性填料的例子有涂覆微粉化氧化铝或涂覆微粉化二氧化硅。
颜料可用本领域技术人员熟知的方法,分散到部分粘合剂中、或分散到常用的树脂浆中。最佳分散系的成分组成是由各分散装置分别决定的。合适的分散装置有例如搅拌板装置、三辊式碾磨机、球磨机或、优选砂磨机或珠磨机。在分散中也可以加入常用的辅助物质例如消泡剂、分散助剂和控制流变能力的助剂。
本发明所用的能在阳极沉积的水溶性电泳涂漆也可包含常用的漆辅助物质和添加剂如杀微生物剂、光稳定剂和均化剂。另外也可共用其它亲水性的和/或憎水性的带有或没有活性基团的聚合物或这些聚合物的混合物。
此类聚合物的例子有饱和或不饱和丙烯酸酯、聚氨酯或聚酯树脂、丙烯酰基改性的丙烯酸酯、聚氨酯或聚酯树脂、环氧树脂、氨基塑料树脂、酚醛树脂、烃树脂、硅改性的丙烯酸酯、聚氨酯或聚酯树脂、丁二烯与丙烯腈的共聚物、和苯乙烯-烯丙醇的共聚物。
用完全去离子水把阳极电泳涂漆稀释转化到工作状态(电浸涂漆液),任选在添加了另外的中和剂之后进行。
在备用的电浸涂漆液中固体含量例如为8~25重量%,优选10~15重量%。MEQ值优选30到150,特别优选40到80。有机溶剂的含量是例如0.1~10重量%,优选小于5重量%。
沉积是以常用的方法进行的,例如通过施加50到500伏直流电压,涂覆时间为0.5到5分钟,电浸涂漆液温度为15℃到35℃。
本发明所述的工艺适合于有导电表面工件的涂覆,特别是给家用器具、和电器设备、钢制家俱、建筑构件、建筑机械和农业机械、汽车车身和汽车的配件和附件上底漆和单层漆。
通过本发明所述的步骤可以提高边缘保护且可以调节无光度、还有良好的操纵性。本发明用的混合酯和阳极粘合剂的相容性很好,由此可以得到跟通常用磷酸环氧酯相比有更高的槽液稳定性以及在装置的清洗区中或在可能故障情况如电源故障下沉积的漆材料再溶解更少,这时已涂基体在电浸涂漆液中静止不动。
实施例1磷酸环氧酯的制备
将26.44重量%的仲丁醇加入到带搅拌器、温度计和回流冷凝器的反应器中,并加热到80°到100℃。向其中撒入38.51重量%的Epikote1001(Shell公司)(双酚A与表氯醇的缩合产物,环氧当量450到500),并在80°到100℃搅拌下完全溶解。将反应混合物冷却到80°,分批加入由1.4重量%的85%的磷酸与0.31重量%的完全去离子水构成的混合物。反应混合物在80°到110℃轻微的回流下加热并保持此温度直到酸值达到22~26mg KOH/g。将反应混合物冷却到80°到90℃之后加入1.87重量%的50%的二甲基乙醇胺并均化30分钟。然后迅速加入30.56重量%的完全去离子水并搅拌30分钟,温度降到25°到35℃。特性数据:固体含量(30分钟,150℃):37到41%MEQ-胺: 35到38毫当量胺/100克固体树脂实施例2用于阳极电浸涂漆的无硬化剂树脂的聚酯树脂水分散体的制备
在100℃下、向装有搅拌器、温度计和回流冷凝器的反应器中的57.00重量份的酸值49、羟基数60的聚酯树脂(由26.17重量份的新戊二醇、5.43重量份的三羟甲基丙烷、10.83重量份的间苯二甲酸、21.45重量份的异癸醇和36.12重量份的偏苯三酸酐制得)中加入1.80重量份的二乙醇胺和3重量份的完全去离子水的混合物,并搅拌10分钟形成均匀混合物,之后加入0.15重量份的商购杀微生物剂同样搅拌10分钟形成均匀混合物。在搅拌下加入38.05重量份的完全去离子水。将该混合物在80℃下搅拌90分钟,然后快速冷却到25℃。特性数据:固体含量(30分钟,180℃):53到57%MEQ-胺: 30到35毫当量胺/100克固体树脂实施例3用于阳极电浸涂漆的含硬化剂树脂的粘合剂水分散体的制备
在搅拌下,将12.10重量份商购三聚氰胺树脂Cymel 303(Cytec公司)加入到87.90重量份的2中所制得的聚酯树脂分散体中,再均化30分钟。特性数据:固体含量(计算):60.4%MEQ-胺: 26到30毫当量胺/100克固体树脂实施例4用于阳极电浸涂漆的含硬化剂树脂和磷酸环氧酯的粘合剂水分散体的制备
在搅拌下,将10.80重量份的商购三聚氰胺树脂Cymel 303(Cytec公司)和11.00重量份的实施例1中制备的磷酸环氧酯加入到78.20重量份的2中制备的聚酯树脂分散体中,再均化30分钟。特性数据:固体含量(计算):58.1%MEQ-胺: 31到35毫当量胺/100克固体树脂实施例5黑颜料水浆的制备
要制备100kg的黑颜料浆,将24.50kg的75%的树脂浆放入溶解器中,用2.18kg的50%二异丙醇胺溶液中和,并用40.90kg的完全去离子水稀释。
然后在搅拌下按顺序加入2.50kg聚丁二烯、2.21kg槽法炭黑、2.21kg炉法炭黑以及25.50kg的氢化硅酸铝(Aluminiumhydrosilikat)。
将由此得到的磨料在40℃搅拌15分钟。经过12小时的溶胀时间后,在指定条件下将磨料在Coball研磨机中分散。特性数据:固体含量(计算):50%MEQ-胺: 12到17毫当量胺/100克固体树脂实施例6含磷酸环氧酯的电浸涂漆液的配制
将1452.50g完全去离子水放入容量2升的烧杯中。搅拌下接连加入5.00g的50%的二异丙醇胺和5.00g二甲基乙醇胺。在搅拌下分批加入385.80g实施例4中制备的含有硬化剂树脂和磷酸环氧酯的分散体。经过10分钟的均化后再在搅拌下缓慢加入151.70g实施例5中制备的颜料浆。
经过大约一个小时的均化后,电浸涂漆液就可以用于涂覆。特性数据:固体含量(计算):15%MEQ-胺: 51.2毫当量胺/100克固体树脂实施例7无磷酸环氧酯的电浸涂漆液的制备
将1467.20g完全去离子水放入容量2升的烧杯。搅拌下接连加入5.00g的50%的二异丙醇胺和5.00g二甲基乙醇胺。在搅拌下分批加入371.1g实施例3中制备的含有硬化树脂的分散体。经过10分钟的均化后,再在搅拌下缓慢加入151.70g实施例5中制备的颜料浆。
经过大约一个小时的均化后,电浸涂漆液就可以用于涂覆。特性数据:固体含量(计算):15%MEQ-胺: 49.0毫当量胺/100克固体树脂实施例8测试规程与测试结果用实施例6和7中配制的电浸涂漆液进行涂覆试片并烘烤。预处理: 铁磷化(Unibond WH/W)电压: 220±40V电极间距: 5厘米涂覆时间: 180秒槽温度: 30℃烘烤条件: 在实验室循环空气炉中180℃处理25分钟涂层厚度: 30±3μm测试: 根据DIN(德国工业标准)67530 60°几何角
进行表面反光率测试
根据DIN 50021 SS做120小时盐雾测试
根据DIN 50021 SS做240小时盐雾测试测试结果:
本发明 对比表面反光率测试 实施例6 实施例7根据DIN 67530 19单位 45单位60°几何角120小时盐雾测试,根据DIN 50021 SS;根据ISO 4628评价表面生锈x 0 0-1边缘生锈xx 0-1 4x 0=无表面生锈5=严重表面生锈xx 0=无边缘生锈5=严重边缘生锈(100%)
Claims (5)
1.一种通过将导电表面浸在水性阳极电浸涂漆液中并连接做阳极来对它进行阳极电浸涂漆的方法,其特征在于所用水性阳极电浸涂漆液基于电浸涂漆液的粘合剂固体含有1~15重量%的一种或多种酸值为10~50的磷酸环氧酯和/或膦酸环氧酯,所述磷酸环氧酯和/或膦酸环氧酯由一种或多种单体的、低聚或聚合环氧化合物与磷酸或膦酸或其酯或其混合物在一种或多种醇存在的情况下反应得到。
2.根据权利要求1所述的方法,其特征在于应用磷酸二乙酯、磷酸三乙酯、磷酸二丁酯、磷酸三丁酯、羟甲基膦酸、羟乙基膦酸、乙烯基膦酸、烯丙基膦酸、苯甲基膦酸二乙酯和/或正磷酸进行反应。
3.根据权利要求1或2所述的方法,其特征在于所用的那些环氧化合物平均每个分子至少含有一个,优选至少两个环氧基,且环氧当量为90到4000克/当量。
4.含有一种或多种成膜粘合剂、以及任选的交联剂、颜料、填料、有机溶剂和/或常用的漆添加剂的水性电浸涂漆液,其特征在于它基于粘合剂固体含有1~15重量%的一种或多种酸值为10~50的磷酸环氧酯和/或膦酸环氧酯,所述磷酸环氧酯和/或膦酸环氧酯由一种或多种单体的、低聚或聚合环氧化合物与磷酸或膦酸或其酯或其混合物在一种或多种醇存在下反应得到的。
5.由一种或多种单体的、低聚或聚合环氧化合物与磷酸或膦酸或其酯或其混合物在一种或多种醇存在下反应得到的酸值10~50的磷酸环氧酯和/或膦酸环氧酯用作电浸涂漆液添加剂的用途。
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- 2000-12-13 EP EP00983309A patent/EP1248823B1/de not_active Revoked
- 2000-12-13 ES ES00983309T patent/ES2213633T3/es not_active Expired - Lifetime
- 2000-12-13 MX MXPA02005958A patent/MXPA02005958A/es active IP Right Grant
- 2000-12-13 AT AT00983309T patent/ATE262012T1/de active
- 2000-12-13 JP JP2001544862A patent/JP2003534395A/ja active Pending
- 2000-12-13 PT PT00983309T patent/PT1248823E/pt unknown
- 2000-12-13 CN CNB008172862A patent/CN1211441C/zh not_active Expired - Fee Related
- 2000-12-13 BR BR0016333-3A patent/BR0016333A/pt not_active IP Right Cessation
- 2000-12-13 CA CA002391883A patent/CA2391883C/en not_active Expired - Fee Related
- 2000-12-13 DK DK00983309T patent/DK1248823T3/da active
- 2000-12-13 US US10/168,208 patent/US7494716B2/en not_active Expired - Fee Related
- 2000-12-13 WO PCT/EP2000/012647 patent/WO2001044382A1/de active IP Right Grant
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CN109679118A (zh) * | 2018-12-02 | 2019-04-26 | 廊坊立邦涂料有限公司 | 一种磷酸酯改性阳离子微凝胶、制备方法及用途 |
CN109504264B (zh) * | 2018-12-02 | 2021-09-17 | 广州立邦涂料有限公司 | 一种边缘防腐电泳涂料组合物、制备方法及用途 |
CN109679118B (zh) * | 2018-12-02 | 2022-02-11 | 廊坊立邦涂料有限公司 | 一种磷酸酯改性阳离子微凝胶、制备方法及用途 |
Also Published As
Publication number | Publication date |
---|---|
US20030004231A1 (en) | 2003-01-02 |
CN1211441C (zh) | 2005-07-20 |
DK1248823T3 (da) | 2004-04-13 |
EP1248823A1 (de) | 2002-10-16 |
PT1248823E (pt) | 2004-06-30 |
DE19960693A1 (de) | 2001-07-19 |
CA2391883C (en) | 2009-06-16 |
ES2213633T3 (es) | 2004-09-01 |
JP2003534395A (ja) | 2003-11-18 |
DE50005745D1 (de) | 2004-04-22 |
MXPA02005958A (es) | 2002-10-23 |
ATE262012T1 (de) | 2004-04-15 |
BR0016333A (pt) | 2002-08-27 |
WO2001044382A1 (de) | 2001-06-21 |
US7494716B2 (en) | 2009-02-24 |
EP1248823B1 (de) | 2004-03-17 |
CA2391883A1 (en) | 2001-06-21 |
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