CN102361835B - 浆料组合物的制造方法 - Google Patents
浆料组合物的制造方法 Download PDFInfo
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- CN102361835B CN102361835B CN201080013393.XA CN201080013393A CN102361835B CN 102361835 B CN102361835 B CN 102361835B CN 201080013393 A CN201080013393 A CN 201080013393A CN 102361835 B CN102361835 B CN 102361835B
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- Prior art keywords
- polyvinyl acetal
- acetal resin
- paste compound
- inorganic
- resin
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 34
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 102
- 239000011354 acetal resin Substances 0.000 claims abstract description 95
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 95
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 94
- 239000000843 powder Substances 0.000 claims abstract description 79
- 239000006185 dispersion Substances 0.000 claims abstract description 54
- 239000003960 organic solvent Substances 0.000 claims abstract description 36
- 229920005989 resin Polymers 0.000 claims abstract description 36
- 239000011347 resin Substances 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 17
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 13
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 8
- 125000000129 anionic group Chemical group 0.000 claims description 7
- 239000012046 mixed solvent Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 description 27
- -1 phenylacetaldehyde acetal Chemical class 0.000 description 19
- 239000003795 chemical substances by application Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N ethyl acetate Substances CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 7
- 239000004840 adhesive resin Substances 0.000 description 6
- 229920006223 adhesive resin Polymers 0.000 description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 6
- 229910002113 barium titanate Inorganic materials 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- 238000007127 saponification reaction Methods 0.000 description 6
- DTUQWGWMVIHBKE-UHFFFAOYSA-N Benzeneacetaldehyde Natural products O=CCC1=CC=CC=C1 DTUQWGWMVIHBKE-UHFFFAOYSA-N 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000003985 ceramic capacitor Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 229940100595 phenylacetaldehyde Drugs 0.000 description 5
- 229920001567 vinyl ester resin Polymers 0.000 description 5
- 229910000859 α-Fe Inorganic materials 0.000 description 5
- 239000005977 Ethylene Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000005481 NMR spectroscopy Methods 0.000 description 4
- 230000000254 damaging effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- UODXCYZDMHPIJE-UHFFFAOYSA-N menthanol Chemical compound CC1CCC(C(C)(C)O)CC1 UODXCYZDMHPIJE-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 description 3
- 239000004711 α-olefin Substances 0.000 description 3
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 2
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910018605 Ni—Zn Inorganic materials 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- XUPYJHCZDLZNFP-UHFFFAOYSA-N butyl butanoate Chemical compound CCCCOC(=O)CCC XUPYJHCZDLZNFP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 2
- 235000019439 ethyl acetate Nutrition 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- SHZIWNPUGXLXDT-UHFFFAOYSA-N ethyl hexanoate Chemical compound CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N itaconic acid Chemical compound OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 2
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 2
- NUKZAGXMHTUAFE-UHFFFAOYSA-N methyl hexanoate Chemical compound CCCCCC(=O)OC NUKZAGXMHTUAFE-UHFFFAOYSA-N 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-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
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 description 1
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 1
- HFZLSTDPRQSZCQ-UHFFFAOYSA-N 1-pyrrolidin-3-ylpyrrolidine Chemical compound C1CCCN1C1CNCC1 HFZLSTDPRQSZCQ-UHFFFAOYSA-N 0.000 description 1
- BQCXFGVWPFXMKD-UHFFFAOYSA-N 2,2-dimethylpropanoic acid;ethenyl acetate Chemical compound CC(=O)OC=C.CC(C)(C)C(O)=O BQCXFGVWPFXMKD-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- ZSDQQJHSRVEGTJ-UHFFFAOYSA-N 2-(6-amino-1h-indol-3-yl)acetonitrile Chemical compound NC1=CC=C2C(CC#N)=CNC2=C1 ZSDQQJHSRVEGTJ-UHFFFAOYSA-N 0.000 description 1
- PTTPXKJBFFKCEK-UHFFFAOYSA-N 2-Methyl-4-heptanone Chemical compound CC(C)CC(=O)CC(C)C PTTPXKJBFFKCEK-UHFFFAOYSA-N 0.000 description 1
- WOYWLLHHWAMFCB-UHFFFAOYSA-N 2-ethylhexyl acetate Chemical group CCCCC(CC)COC(C)=O WOYWLLHHWAMFCB-UHFFFAOYSA-N 0.000 description 1
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical group CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 description 1
- AUZRCMMVHXRSGT-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CC(C)CS(O)(=O)=O AUZRCMMVHXRSGT-UHFFFAOYSA-N 0.000 description 1
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical compound FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 description 1
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 229910017083 AlN Inorganic materials 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- OKJADYKTJJGKDX-UHFFFAOYSA-N Butyl pentanoate Chemical compound CCCCOC(=O)CCCC OKJADYKTJJGKDX-UHFFFAOYSA-N 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 1
- 101100387911 Caenorhabditis elegans dop-2 gene Proteins 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ICMAFTSLXCXHRK-UHFFFAOYSA-N Ethyl pentanoate Chemical compound CCCCC(=O)OCC ICMAFTSLXCXHRK-UHFFFAOYSA-N 0.000 description 1
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- JGFBQFKZKSSODQ-UHFFFAOYSA-N Isothiocyanatocyclopropane Chemical compound S=C=NC1CC1 JGFBQFKZKSSODQ-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 description 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- VFIJBTVGUHVPPW-UHFFFAOYSA-N [Br].C=C Chemical compound [Br].C=C VFIJBTVGUHVPPW-UHFFFAOYSA-N 0.000 description 1
- NYZRMWCPMJEXKL-UHFFFAOYSA-N [Fe].[Cu].[Zn] Chemical compound [Fe].[Cu].[Zn] NYZRMWCPMJEXKL-UHFFFAOYSA-N 0.000 description 1
- RFIJBZKUGCJPOE-UHFFFAOYSA-N [Fe].[Ni].[Zn] Chemical compound [Fe].[Ni].[Zn] RFIJBZKUGCJPOE-UHFFFAOYSA-N 0.000 description 1
- TXDRMFQQROPOKK-UHFFFAOYSA-N [Si+2]=O.[B+]=O.[O-2].[Zn+2] Chemical class [Si+2]=O.[B+]=O.[O-2].[Zn+2] TXDRMFQQROPOKK-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- IYABWNGZIDDRAK-UHFFFAOYSA-N allene Chemical compound C=C=C IYABWNGZIDDRAK-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 description 1
- PWLNAUNEAKQYLH-UHFFFAOYSA-N butyric acid octyl ester Natural products CCCCCCCCOC(=O)CCC PWLNAUNEAKQYLH-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000001460 carbon-13 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- BXKDSDJJOVIHMX-UHFFFAOYSA-N edrophonium chloride Chemical compound [Cl-].CC[N+](C)(C)C1=CC=CC(O)=C1 BXKDSDJJOVIHMX-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- GFJVXXWOPWLRNU-UHFFFAOYSA-N ethenyl formate Chemical compound C=COC=O GFJVXXWOPWLRNU-UHFFFAOYSA-N 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- 239000010931 gold Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
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- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
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- 150000004706 metal oxides Chemical class 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
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- 229910052863 mullite Inorganic materials 0.000 description 1
- UUIQMZJEGPQKFD-UHFFFAOYSA-N n-butyric acid methyl ester Natural products CCCC(=O)OC UUIQMZJEGPQKFD-UHFFFAOYSA-N 0.000 description 1
- HNBDRPTVWVGKBR-UHFFFAOYSA-N n-pentanoic acid methyl ester Natural products CCCCC(=O)OC HNBDRPTVWVGKBR-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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Abstract
本发明提供一种可以以简便的工序实现优异的分散性的浆料组合物的制造方法。另外,提供一种使用该浆料组合物的制造方法制造的浆料组合物。所述方法为含有无机粉末、聚乙烯醇缩醛树脂及有机溶剂的浆料组合物的制造方法,其具有:添加无机粉末、聚乙烯醇缩醛树脂(A)及无机分散用有机溶剂并进行混合而制作无机分散液的工序;添加聚乙烯醇缩醛树脂(B)及树脂溶液用有机溶剂并进行混合而制作树脂溶液的工序;以及;在所述无机分散液中添加树脂溶液的工序,所述聚乙烯醇缩醛树脂(A)的聚合度为200~600,所述聚乙烯醇缩醛树脂(B)的聚合度为800~4000,并且,在制作所述无机分散液的工序中,相对于无机粉末100重量份添加所述聚乙烯醇缩醛树脂(A)0.1~20重量份。
Description
技术领域
本发明涉及一种可以以简便的工序实现优异的分散性的浆料组合物的制造方法。另外,涉及一种使用该浆料组合物的制造方法制造的浆料组合物。
背景技术
聚乙烯醇缩醛树脂由于坚韧性、造膜性、颜料等无机、有机粉体等的分散性、对涂布面的粘接性等优异,例如,可以利用于构成层叠陶瓷电容器的陶瓷生片或导电糊剂、油墨、涂料、烧成用珐琅、洗涤底漆等用途。
其中,层叠陶瓷电容器通常经由如下工序来制造。
首先,在聚乙烯醇缩丁醛树脂等粘合剂树脂中添加陶瓷原料粉末,通过均匀混合得到浆料组合物。将得到的浆料组合物涂布在脱模处理后的支承体面上。通过对其进行加热等蒸馏除去溶剂等挥发成分后,从支承体上剥离而得到陶瓷生片。接着,交替层叠多个在得到的陶瓷生片上通过丝网印刷涂布含有乙基纤维素、聚乙烯醇缩丁醛树脂等作为粘合剂树脂的导电糊剂所得的片材,加热压接而制作层叠体,进行脱脂处理后,在烧成而得到的陶瓷烧成物的端面经由烧结外部电极的工序得到层叠陶瓷电容器。
近年来,要求层叠陶瓷电容器更小型化、高容量化,研究进一步多层化、薄膜化,但这样的层叠陶瓷电容器要求陶瓷生片进一步薄膜化,且伴随其而使用的陶瓷粉末的粒径也小。
通常,作为在浆料组合物中分散陶瓷粉末等的方法,可以使用如下方法:如专利文献1所述,一方面制备由无机粉末、有机溶剂等构成的无机分散液,另一方面制备使粘合剂树脂溶解而形成的树脂溶液后,混合无机分散液和树脂溶液的方法。
但是,在这样的方法中,存在如下问题:如果不经长时间搅拌混合液,则陶瓷粉末不充分分散,搅拌需要过大的能量及时间。
另外,作为确保浆料组合物中的陶瓷粉末的分散性的方法,如专利文献2所述,也可以使用添加分散剂的方法。但是,在这样的方法中,存在如果与粘合剂树脂的相容性差,相反地使分散性变差、或在长时间保存时分散性降低的问题。
先行技术文献
专利文献
专利文献1:日本特开2005-139034号公报
专利文献2:日本特开平6-325971号公报
发明内容
发明要解决的问题
鉴于所述现状,本发明的目的在于提供一种可以以简便的工序实现优异的分散性的浆料组合物的制造方法。另外,其目的在于提供一种使用该浆料组合物的制造方法制造的浆料组合物。
用于解决问题的手段
本发明提供一种浆料组合物的制造方法,其为含有无机粉末、聚乙烯醇缩醛树脂及有机溶剂的浆料组合物的制造方法,其具有:添加无机粉末、聚乙烯醇缩醛树脂(A)及无机分散用有机溶剂并进行混合而制作无机分散液的工序;添加聚乙烯醇缩醛树脂(B)及树脂溶液用有机溶剂并进行混合而制作树脂溶液的工序;以及;在所述无机分散液中添加树脂溶液的工序,所述聚乙烯醇缩醛树脂(A)的聚合度为200~600,所述聚乙烯醇缩醛树脂(B)的聚合度为800~4000,并且,在制作所述无机分散液的工序中,相对于无机粉末100重量份添加所述聚乙烯醇缩醛树脂(A)0.1~20重量份。
以下,对本发明进行详细说明。
本发明人等进行了潜心研究,结果发现,在一方面制备由无机粉末、无机分散用有机溶剂、分散剂等构成的无机分散液,另一方面制备使粘合剂树脂溶解的树脂溶液后,混合无机分散液和树脂溶液的浆料组合物的制造方法中,通过在分散剂中使用聚乙烯醇缩醛树脂,可以大幅改善无机粉末的分散性,同时,能够制造可以得到具有高强度的膜状体的浆料组合物,以至完成了本发明。
本发明具有添加无机粉末、聚乙烯醇缩醛树脂(A)及无机分散用有机溶剂并进行混合而制作无机分散液的工序;添加聚乙烯醇缩醛树脂(B)及树脂溶液用有机溶剂并进行混合而制作树脂溶液的工序;以及;在所述无机分散液中添加树脂溶液的工序。
对本发明而言,在所述制作无机分散液的工序中,使用聚乙烯醇缩醛树脂(A)作为分散剂。在这样制作无机分散液的工序中,通过使用聚乙烯醇缩醛树脂(A)作为分散剂,聚乙烯醇缩醛树脂(A)附着在无机粉末的表面,其结果,可以提高无机粉末的分散性。然后,通过在无机分散液中添加含有聚乙烯醇缩醛树脂(B)的树脂溶液,可以不损伤无机粉末的分散性,可以提高例如制成生片的情况等中得到的片材的强度。
在所述制作无机分散液的工序中,优选预先在无机分散用有机溶剂中混合并溶解聚乙烯醇缩醛树脂(A)后,添加无机粉末。
对本发明而言,在制作无机分散液的工序中,使用聚乙烯醇缩醛树脂(A)作为分散剂。在本发明中,通过使用和粘合剂树脂同种的聚乙烯醇缩醛树脂(A)作为分散剂,不需要考虑如上所述的由分散剂添加引起的不良影响。
另外,在本说明书中,在不需要特别区别聚乙烯醇缩醛树脂(A)和后述的聚乙烯醇缩醛树脂(B)的情况下,也简称为聚乙烯醇缩醛树脂。
所述聚乙烯醇缩醛树脂(A)的聚合度的下限为200,上限为600。所述聚合度如果小于200,则变得难以从工业方面获得,不实用。所述聚合度如果大于600,则凝集力变得过高,难以表达充分的分散性。所述聚合度的优选下限为300、优选上限为500。
所述聚乙烯醇缩醛树脂(A)的羟基量的优选下限为28摩尔%,优选上限为60摩尔%。所述羟基量如果小于28摩尔%,则有时变得难以在无机粉末的表面附着所述聚乙烯醇缩醛树脂(A),对分散性的提高没有帮助,如果大于60摩尔%,则有时不仅该聚乙烯醇缩醛树脂(A)的合成变得困难,而且在溶剂中的溶解性降低。所述羟基量的更优选下限为35摩尔%,更优选上限为55摩尔%。所述羟基量的进一步优选下限为40摩尔%,进一步优选上限为50摩尔%。
所述聚乙烯醇缩醛树脂(A)优选具有阴离子性基团。
通过具有所述阴离子性基团,聚乙烯醇缩醛树脂(A)变得容易附着在无机粉末的表面,可以提高无机粉末的分散性。
作为所述阴离子性基团,只要为阴离子性的改性基团就没有特别限定,例如可以举出:羧基、磺酸基、磷酸基等。
所述阴离子性基团的改性度的优选下限为0.1摩尔%,优选上限为2摩尔%。
所述阴离子性基团的改性度如果小于0.1摩尔%,则有时所述聚乙烯醇缩醛树脂(A)变得难以附着在无机粉末的表面,对分散性的提高没有帮助,如果大于2摩尔%,则有时上述聚乙烯醇缩醛树脂(A)之间产生引力相互作用,变得难以附着在无机粉末的表面。所述改性度的更优选下限为0.2摩尔%,更优选上限为1摩尔%。
另外,所述改性度可以如下算出:将改性聚乙烯醇缩醛树脂溶解在DMSO-d6(二甲基亚砜)中,测定13C-NMR光谱,由来自羧基键合的次甲基的峰面积和来自缩醛化的部分的次甲基的峰面积算出。
对所述聚乙烯醇缩醛树脂(A)而言,用乙醛缩醛化的部分与用丁醛缩醛化的部分的比例优选为20/80~70/30。对所述用乙醛缩醛化的部分而言,起因于醛的烃基的长度变短,立体位阻降低,因此,羟基变得易吸附在无机粉末上。因此,通过将用乙醛缩醛化的部分设为20/80以上,从而使无机粉末的分散性提高。相反地,如果用乙醛缩醛化的部分变得过多,则在无机分散用有机溶剂中的溶解性降低或成型、干燥后的片材变得过硬而易混入裂缝,因此,优选为70/30以下。用乙醛缩醛化的部分与用丁醛缩醛化的部分的比例进一步优选为30/70~60/40。
作为所述无机粉末没有特别的限定,例如可以举出:金属粉体、导电粉末、陶瓷粉末、玻璃粉末等。
在使用导电粉末作为所述无机粉末的情况下,可以用作导电糊剂。
作为所述导电粉末只要为显示充分的导电性的导电粉末就没有特别的限定,例如可以举出:由镍、钯、铂、金、银、铜、这些的合金等形成的粉末。这些导电粉末可以单独使用,也可以将两种以上并用。
在使用陶瓷粉末作为所述无机粉末的情况下,可以用作陶瓷糊剂。作为所述陶瓷粉末没有特别的限定,例如可以举出:由氧化铝、氧化锆、硅酸铝、氧化钛、氧化锌、钛酸钡、氧化镁、赛阿龙(sialon)、尖晶石莫来石(spinelmullite)、碳化硅、氮化硅、氮化铝等形成的粉末。其中,优选由与在使用的陶瓷生片中所含的陶瓷粉末相同的成分形成。这些陶瓷粉末可以单独使用,也可以将两种以上并用。
在使用玻璃粉末作为所述无机粉末的情况下,可以用作玻璃糊剂。作为所述玻璃粉末没有特别的限定,例如可以举出:氧化铅-氧化硼-氧化硅-氧化钙系玻璃、氧化锌-氧化硼-氧化硅系玻璃、氧化铅-氧化锌-氧化硼-氧化硅系玻璃等。这些玻璃粉末可以单独使用,也可以将两种以上并用。另外,在不损伤本发明的目的的范围内,可以并用氧化铝等。
在使用磁性粉末作为所述无机粉末的情况下,可以用作磁性材料糊剂。作为所述磁性粉末没有特别的限定,例如可以举出:锰锌铁素体、镍锌铁素体、铜锌铁素体、钡铁素体、锶铁素体等铁素体类、氧化铬等金属氧化物、钴等金属磁性体、无定形磁性体等。这些磁性粉末可以单独使用,也可以将两种以上并用。
在所述制作无机分散液的工序中的所述聚乙烯醇缩醛树脂(A)的添加量的下限相对无机粉末100重量份为0.1重量份,上限为20重量份。所述聚乙烯醇缩醛树脂(A)的添加量如果小于0.1重量份,则有时例如无机粉末的分散性变得不充分,如果大于20重量份,则有时粘度变得过高,操作性变差。所述添加量的优选下限为0.6重量份,优选上限为15重量份。进而所述添加量的更优选下限为1重量份,更优选上限为10重量份。特别是通过将所述添加量设为0.6重量份以上,可以使聚乙烯醇缩醛树脂(A)充分地吸附在无机粉末的表面,因此,可以使陶瓷浆料中的无机粉末更微细地分散。
在本发明中,接着,进行添加聚乙烯醇缩醛树脂(B)及树脂溶液用有机溶剂并进行混合而制作树脂溶液的工序。
所述聚乙烯醇缩醛树脂(B)的聚合度的下限为800,上限为4000。如果所述聚合度小于800,则在生片中使用的情况下,片材强度变得不充分,如果所述聚合度大于4000,则浆料组合物的粘度变得过高而难以涂布。所述聚合度的优选下限为1200,优选上限为3500。
所述聚乙烯醇缩醛树脂(B)的羟基量的优选下限为22摩尔%,优选上限为42摩尔%。如果所述羟基量小于22摩尔%,则在使用含有该聚乙烯醇缩醛树脂(B)的浆料制作生片的情况下,有时片材强度变得不充分,如果大于42摩尔%,则有时招致无机粉末粒子的凝集。所述羟基量的更优选下限为28摩尔%,更优选上限为40摩尔%。
在所述制作树脂溶液的工序中的所述聚乙烯醇缩醛树脂(B)的添加量的优选下限相对无机粉末100重量份为5重量份,优选上限为20重量份。如果所述聚乙烯醇缩醛树脂(B)的添加量小于5重量份,则有时例如无机粉末的分散性变得不充分或干燥后的涂膜的强度、柔软性及粘接性等变得不充分,如果大于20重量份,则有时粘度变得过高或涂布性降低,操作性变差。
特别是在要求强度的薄层的陶瓷生片中,通过含有相对于聚合度低的聚乙烯醇缩醛树脂(A)、聚合度高的聚乙烯醇缩醛树脂(B),可以制作具有充分的分散性和片材强度的陶瓷生片。
所述聚乙烯醇缩醛树脂是将聚乙烯醇用醛缩醛化而成的。
上述聚乙烯醇例如可以通过将乙烯基酯与乙烯的共聚物进行皂化而得到。作为乙烯基酯,例如可以举出:甲酸乙烯酯、乙酸乙烯酯、丙酸乙烯酯、特戊酸乙烯酯等。其中,从经济性的观点考虑,优选乙酸乙烯酯。
对所述聚乙烯醇而言,在不损伤本发明的效果的范围内,可以为将乙烯性不饱和单体共聚而成的聚乙烯醇。作为所述乙烯性不饱和单体没有特别的限定,例如可以举出:丙烯酸、甲基丙烯酸、(无水)邻苯二甲酸、(无水)马来酸、(无水)衣康酸、丙烯腈、甲基丙烯腈、丙烯酰胺、甲基丙烯酰胺、三甲基-(3-丙烯酰胺-3-二甲基丙基)-氯化铵、丙烯酰胺-2-甲基丙烷磺酸、及其钠盐、乙基乙烯基醚、丁基乙烯基醚、N-乙烯基吡咯烷酮、氯乙烯、溴乙烯、氟乙烯、偏氯乙烯、偏氟乙烯、四氟乙烯、乙烯基磺酸钠、烯丙基磺酸钠等。另外,也可以使用末端改性聚乙烯醇,所述末端改性聚乙烯醇是通过在硫代乙酸、巯基丙酸等硫化合物的存在下,将乙酸乙烯酯等乙烯基酯系单体和乙烯共聚,将其皂化而得到。
上述聚乙烯醇也可以为将共聚物皂化而成的聚乙烯醇,所述共聚物是将所述乙烯基酯和α-烯烃共聚而成。另外,进而也可以将所述乙烯性不饱和单体共聚,制成含有来自乙烯性不饱和单体的成分的聚乙烯醇。另外,也可以使用末端聚乙烯醇,所述末端聚乙烯醇通过在硫代乙酸、巯基丙酸等硫化合物的存在下,将乙酸乙烯酯等乙烯基酯系单体和α-烯烃共聚,将其皂化而得到。作为所述α-烯烃没有特别的限定,例如可以举出:甲撑、乙烯、丙烯、异丙烯、丁烯、异丁烯、戊烯、己烯、环己烯、环己基乙烯、环己基丙烯等。
对所述聚乙烯醇缩醛树脂而言,缩醛化度优选为40~80摩尔%。如果所述缩醛化度小于40摩尔%,则由于在有机溶剂中的溶解性降低,因此,变得难以在浆料组合物中使用。如果所述缩醛化度大于80摩尔%,则变得难以将聚乙烯醇缩醛树脂在工业方面进行制造。优选为50~80摩尔%。
另外,在本说明书中,缩醛化度是指在聚乙烯醇的羟基数中,用丁醛缩醛化的羟基数的比例,作为缩醛化度的计算方法,由于聚乙烯醇缩醛树脂的缩醛基由2个羟基缩醛化而形成,因此,采用计算缩醛化的2个羟基的方法而算出缩醛化度的摩尔%。
在本发明中,接着,进行在所述无机分散液中添加树脂溶液的工序。由此,可以得到浆料组合物。
另外,在本发明的浆料组合物的制造方法中,在不损伤本发明的效果的范围内,也可以含有所述聚乙烯醇缩醛树脂以外的聚乙烯醇缩醛树脂或丙烯酸树脂、乙基纤维素等其它的树脂。但是,在这样的情况下,相对总粘合剂树脂的所述聚乙烯醇缩醛树脂的含量需要为50重量%以上。
作为所述无机分散用有机溶剂及树脂溶液用有机溶剂没有特别的限定,可以使用通常用于浆料组合物的有机溶剂,例如可以举出:丙酮、甲基乙基酮、二丙基酮、二异丁基酮等酮类、甲醇、乙醇、异丙醇、丁醇等醇类、甲苯、二甲苯等芳香族烃类、丙酸甲酯、丙酸乙酯、丙酸丁酯、丁酸甲酯、丁酸乙酯、丁酸丁酯、戊酸甲酯、戊酸乙酯、戊酸丁酯、己酸甲酯、己酸乙酯、己酸丁酯、乙酸2-乙基己酯、丁酸2-乙基己酯等酯类、萜品醇、二氢萜品醇、萜品醇乙酸酯、二氢萜品醇乙酸酯等萜品醇及其衍生物等。这些有机溶剂可以单独使用,也可以将两种以上并用。
作为所述无机分散用有机溶剂及树脂溶液用有机溶剂,特别优选使用包含乙醇及甲苯的混合溶剂。通过使用所述混合溶剂,可以大幅提高浆料组合物的分散性。认为这是因为相对乙醇有助于防止聚乙烯醇缩醛树脂(B)的凝集,甲苯有助于聚乙烯醇缩醛树脂(A)附着在无机粉末表面,通过这些的相辅效果可以大幅提高浆料组合物的分散性。
使用所述混合溶剂的情况中的所述乙醇与甲苯的混合比优选设为5∶5~2∶8。通过设为所述范围内,可以大幅提高浆料组合物的分散性。
所述制造无机分散液的工序中的所述无机分散用有机溶剂的添加量的优选下限相对无机粉末100重量份为20重量份,优选上限为60重量份。如果所述无机分散用有机溶剂的添加量小于20重量份,则有时分散液的粘度变高,陶瓷粉末的运动受限而不能得到充分的分散性,如果大于60重量份,则有时分散液的陶瓷粉末浓度变低,陶瓷粉末之间的碰撞次数减少,因此,不能得到充分的分散性。
另外,所述制作树脂溶液的工序中的所述树脂溶液用有机溶剂的添加量的优选下限相对无机粉末100重量份为70重量份,优选上限为130重量份。如果所述树脂溶液用有机溶剂的添加量小于70重量份,则有时变得难以调整为期望粘度,涂布性降低,如果大于130重量份,则有时陶瓷粉末浓度变低,干燥后的片材不一致。
在本发明的浆料组合物的制造方法中,在不损伤本发明的效果的范围内,也可以适宜添加增塑剂、润滑剂、抗静电剂等。
通过使用本发明的浆料组合物的制造方法,可以实现极高的分散性且可以制造得到的膜状体具有高强度的浆料组合物。这样的浆料组合物也还是本发明之一。
发明效果
本发明可以提供一种可以以简便的工序实现优异的分散性的浆料组合物的制造方法。另外,可以提供一种使用该浆料组合物的制造方法制造的浆料组合物。
具体实施方式
以下,举出实施例对本发明进行更详细的说明,本发明并不仅限于这些实施例。
(聚乙烯醇缩醛树脂(A)[(A1)~(A11)]的合成)
将聚合度320、皂化度99摩尔%的聚乙烯醇350重量份加入到纯水3000重量份中,在90℃的温度下搅拌约2小时使其溶解。将该溶液冷却至40℃,在其中添加浓度35重量%的盐酸230重量份和正丁醛150重量份,将液温降至1℃,保持该温度进行缩醛化反应,析出反应产物。然后,将液温在20℃下保持3小时使反应完成,根据常法经由中和、水洗及干燥而得到聚乙烯醇缩醛树脂(A1)的白色粉末。将得到的聚乙烯醇缩醛树脂溶解在DMSO-d6(二甲亚砜)中,使用13C-NMR(核磁共振光谱)测定丁缩醛化度,结果是丁缩醛化度为51摩尔%。
另外,除设为表1所示的条件以外,与聚乙烯醇缩醛树脂(A1)同样地合成聚乙烯醇缩醛树脂(A2)~(A11)。
(聚乙烯醇缩醛树脂(B)[(B1)~(B6)]的合成)
将聚合度1700、皂化度99摩尔%的聚乙烯醇280重量份加入纯水3000重量份中,在90℃的温度下搅拌约2小时使其溶解。将该溶液冷却至40℃,在其中添加浓度35重量%的盐酸200重量份和正丁醛155重量份,将液温降至1℃,保持该温度进行缩醛化反应,析出反应产物。然后,将液温在40℃下保持3小时使反应完成,根据常规方法经由中和、水洗及干燥而得到聚乙烯醇缩醛树脂(B1)的白色粉末。将得到的聚乙烯醇缩醛树脂溶解在DMSO-d6(二甲亚砜)中,使用13C-NMR(核磁共振光谱)测定丁缩醛化度,结果是丁缩醛化度为66摩尔%。
另外,除设为表2所示的条件以外,与聚乙烯醇缩醛树脂(B1)同样地合成聚乙烯醇缩醛树脂(B2)~(B6)。
(实施例1)
(无机分散液的制作)
将得到的聚乙烯醇缩醛树脂(A1)1重量份添加到甲苯20重量份和乙醇20重量份的混合溶剂中,搅拌使其溶解。接着,将100重量份的钛酸钡的粉末(界化学工业公司制、BT02)添加到得到的溶液中,通过利用珠磨机(Aimex公司制ReadyMill)搅拌180分钟,从而制作无机分散液。
(树脂溶液的制作)
将得到的聚乙烯醇缩醛树脂(B1)8重量份、DOP2重量份加入到乙醇45重量份和甲苯45重量份的混合溶剂中,通过搅拌使其溶解,从而制作树脂溶液。
(浆料组合物的制作)
通过在得到的无机分散液中添加树脂溶液并利用珠磨机搅拌90分钟,从而得到浆料组合物。
(实施例2~20)
使用表3所示的聚乙烯醇缩醛树脂(A)、聚乙烯醇缩醛树脂(B)、及有机溶剂,除此以外,与实施例1同样地得到浆料组合物。
(实施例21~23)
作为无机粉末,使用氮化铝粉代替钛酸钡,使用表3所示的聚乙烯醇缩醛树脂(A)、聚乙烯醇缩醛树脂(B)及有机溶剂,除此以外,与实施例1同样地得到浆料组合物。
(实施例24~26)
作为无机粉末,使用Ni-Zn系铁素体粉代替钛酸钡,使用表3所示的聚乙烯醇缩醛树脂(A)、聚乙烯醇缩醛树脂(B)及有机溶剂,除此以外,与实施例1同样地得到浆料组合物。
(比较例1~4)
不添加聚乙烯醇缩醛树脂(A),使用表4所示的聚乙烯醇缩醛树脂(B)及有机溶剂,除此以外,与实施例1同样地得到浆料组合物。
(比较例5)
如表4所示,在无机分散液中不添加聚乙烯醇缩醛树脂(A),与聚乙烯醇缩醛树脂(B)一起溶解在树脂溶液中,除此以外,与实施例1同样地得到浆料组合物。
(比较例6)
使用表4所示的聚乙烯醇缩醛树脂(B),除此以外,与实施例1同样地得到浆料组合物。
(比较例7)
使聚乙烯醇缩醛树脂(A)的添加量如表4所示,除此以外,与实施例1同样地得到浆料组合物。
(比较例8)
使聚乙烯醇缩醛树脂(A)如表4所示,除此以外,与实施例1同样地得到浆料组合物。
(比较例9)
使用“HypermerKD-2”(Croda公司、在侧链接枝烃的多胺化合物)代替聚乙烯醇缩醛树脂(A),除此以外,与实施例1同样地得到浆料组合物。
(比较例10)
作为无机粉末,使用氮化铝粉代替钛酸钡,不添加聚乙烯醇缩醛树脂(A),使用表4所示的聚乙烯醇缩醛树脂(B)及有机溶剂,除此以外,与实施例1同样地得到浆料组合物。
(比较例11)
作为无机粉末,使用Ni-Zn系铁素体粉代替钛酸钡,不添加聚乙烯醇缩醛树脂(A),使用表4所示的聚乙烯醇缩醛树脂(B)及有机溶剂,除此以外,与实施例1同样地得到浆料组合物。
(评价)
对得到的浆料组合物进行以下的评价。
(1)生片的评价
(生片的制作)
在脱模处理后的聚对苯二甲酸乙二醇酯(PET)膜上以干燥后的膜厚为20μm的方式涂布得到的浆料组合物,并进行干燥制作陶瓷生片。
(1-1)表面粗糙度
依据JISB0601(1994)对得到的陶瓷生片进行表面粗糙度Ra进行测定,评价陶瓷浆料的表面粗糙度。通常,浆料组合物的分散性越高陶瓷生片的表面粗糙度变得越小。
(1-2)拉伸弹性模量
依据JISK7113,使用TENSILON(岛津制作所公司制、AUTOGRAPHAGS-J),在拉伸速度20mm/分钟的条件下进行拉伸弹性模量(MPa)的测定。
(2)分散性评价
(分散性评价溶液的制作)
将得到的浆料组合物0.1重量份添加到乙醇5重量份和甲苯5重量份的混合溶剂中,利用超声波分散机(SND公司制US-303)搅拌10分钟,从而制作分散评价用溶液。
(分散性评价)
对得到的分散评价用溶液,使用激光衍射式粒度分布计(堀场制作所公司制、LA-910)进行粒度分布测定,测定最大粒径峰的位置、及平均粒径。
产业上的可利用性
根据本发明,可以提供一种可以以简便的工序实现优异的分散性的浆料组合物的制造方法。另外,可以提供一种使用该浆料组合物的制造方法制造的浆料组合物。
Claims (4)
1.一种浆料组合物的制造方法,其特征在于,
所述方法是含有无机粉末、聚乙烯醇缩醛树脂及有机溶剂的浆料组合物的制造方法,
其具有:添加无机粉末、聚乙烯醇缩醛树脂(A)及无机分散用有机溶剂并进行混合而制作无机分散液的工序1;添加聚乙烯醇缩醛树脂(B)及树脂溶液用有机溶剂并进行混合而制作树脂溶液的工序2;及在所述无机分散液中添加树脂溶液的工序3,
所述聚乙烯醇缩醛树脂(A)以及聚乙烯醇缩醛树脂(B)是将聚乙烯醇用丁醛缩醛化而成的,
所述聚乙烯醇缩醛树脂(A)的聚合度为200~600,羟基量为28~60摩尔%,缩醛化度为40~80摩尔%,
所述聚乙烯醇缩醛树脂(B)的聚合度为800~4000,羟基量为28~42摩尔%,缩醛化度为40~80摩尔%,并且,
在制作所述无机分散液的工序1中,预先在无机分散用有机溶剂中混合并溶解聚乙烯醇缩醛树脂(A)后,添加无机粉末,
在制作所述无机分散液的工序1中,相对于无机粉末100重量份添加所述聚乙烯醇缩醛树脂(A)0.1~20重量份,
在制作所述树脂溶液的工序2中,相对于无机粉末100重量份添加所述聚乙烯醇缩醛树脂(B)5~20重量份。
2.根据权利要求1所述的浆料组合物的制造方法,其特征在于,
聚乙烯醇缩醛树脂(A)具有阴离子性基团。
3.根据权利要求1或2所述的浆料组合物的制造方法,其特征在于,
无机分散用有机溶剂及树脂溶液用有机溶剂为包含乙醇及甲苯的混合溶剂。
4.一种浆料组合物,其特征在于,
是使用权利要求1、2或3所述的浆料组合物的制造方法来制造的。
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