JP5698750B2 - ポリビニルアセタール樹脂、そのスラリー組成物、セラミックグリーンシート及び積層セラミックコンデンサ - Google Patents
ポリビニルアセタール樹脂、そのスラリー組成物、セラミックグリーンシート及び積層セラミックコンデンサ Download PDFInfo
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- JP5698750B2 JP5698750B2 JP2012529589A JP2012529589A JP5698750B2 JP 5698750 B2 JP5698750 B2 JP 5698750B2 JP 2012529589 A JP2012529589 A JP 2012529589A JP 2012529589 A JP2012529589 A JP 2012529589A JP 5698750 B2 JP5698750 B2 JP 5698750B2
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- Prior art keywords
- mol
- polyvinyl acetal
- acetal resin
- content
- resin
- 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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- 229920002554 vinyl polymer Polymers 0.000 title claims description 128
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 title claims description 127
- 239000011354 acetal resin Substances 0.000 title claims description 121
- 229920006324 polyoxymethylene Polymers 0.000 title claims description 121
- 239000000919 ceramic Substances 0.000 title claims description 85
- 239000000203 mixture Substances 0.000 title claims description 59
- 239000002002 slurry Substances 0.000 title claims description 56
- 239000003985 ceramic capacitor Substances 0.000 title claims description 15
- YGHRJJRRZDOVPD-UHFFFAOYSA-N 3-methylbutanal Chemical compound CC(C)CC=O YGHRJJRRZDOVPD-UHFFFAOYSA-N 0.000 claims description 86
- 229920005989 resin Polymers 0.000 claims description 56
- 239000011347 resin Substances 0.000 claims description 56
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 46
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 46
- 238000006359 acetalization reaction Methods 0.000 claims description 41
- 238000006116 polymerization reaction Methods 0.000 claims description 40
- 229920001567 vinyl ester resin Polymers 0.000 claims description 39
- 150000001299 aldehydes Chemical class 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 27
- 239000003960 organic solvent Substances 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 22
- 125000004185 ester group Chemical group 0.000 claims 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical group OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 53
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 39
- 150000002148 esters Chemical group 0.000 description 35
- -1 polyethylene terephthalate Polymers 0.000 description 32
- 150000003839 salts Chemical class 0.000 description 23
- 239000011230 binding agent Substances 0.000 description 22
- 238000000034 method Methods 0.000 description 22
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 20
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 18
- 238000007127 saponification reaction Methods 0.000 description 17
- 230000032798 delamination Effects 0.000 description 15
- 150000003863 ammonium salts Chemical class 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 14
- 229910052751 metal Chemical class 0.000 description 14
- 239000002184 metal Chemical class 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 239000004014 plasticizer Substances 0.000 description 11
- 238000003860 storage Methods 0.000 description 11
- 238000005238 degreasing Methods 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000178 monomer Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 230000009477 glass transition Effects 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 6
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000004711 α-olefin Substances 0.000 description 6
- 239000003377 acid catalyst Substances 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000004925 Acrylic resin Substances 0.000 description 4
- 229920000178 Acrylic resin Polymers 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N Glycolaldehyde Chemical compound OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 125000003172 aldehyde group Chemical group 0.000 description 4
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 4
- 239000012461 cellulose resin Substances 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 description 4
- DTUQWGWMVIHBKE-UHFFFAOYSA-N phenylacetaldehyde Chemical compound O=CCC1=CC=CC=C1 DTUQWGWMVIHBKE-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 239000001431 2-methylbenzaldehyde Substances 0.000 description 3
- YGCZTXZTJXYWCO-UHFFFAOYSA-N 3-phenylpropanal Chemical compound O=CCCC1=CC=CC=C1 YGCZTXZTJXYWCO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 3
- 150000001241 acetals Chemical class 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- SAOKZLXYCUGLFA-UHFFFAOYSA-N bis(2-ethylhexyl) adipate Chemical compound CCCCC(CC)COC(=O)CCCCC(=O)OCC(CC)CCCC SAOKZLXYCUGLFA-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- BTFQKIATRPGRBS-UHFFFAOYSA-N o-tolualdehyde Chemical compound CC1=CC=CC=C1C=O BTFQKIATRPGRBS-UHFFFAOYSA-N 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 230000000379 polymerizing effect Effects 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- QEGNUYASOUJEHD-UHFFFAOYSA-N 1,1-dimethylcyclohexane Chemical compound CC1(C)CCCCC1 QEGNUYASOUJEHD-UHFFFAOYSA-N 0.000 description 2
- FJJYHTVHBVXEEQ-UHFFFAOYSA-N 2,2-dimethylpropanal Chemical compound CC(C)(C)C=O FJJYHTVHBVXEEQ-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- 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 2
- NMPVEAUIHMEAQP-UHFFFAOYSA-N 2-Bromoacetaldehyde Chemical compound BrCC=O NMPVEAUIHMEAQP-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- LGYNIFWIKSEESD-UHFFFAOYSA-N 2-ethylhexanal Chemical compound CCCCC(CC)C=O LGYNIFWIKSEESD-UHFFFAOYSA-N 0.000 description 2
- IAVREABSGIHHMO-UHFFFAOYSA-N 3-hydroxybenzaldehyde Chemical compound OC1=CC=CC(C=O)=C1 IAVREABSGIHHMO-UHFFFAOYSA-N 0.000 description 2
- GOUHYARYYWKXHS-UHFFFAOYSA-N 4-formylbenzoic acid Chemical class OC(=O)C1=CC=C(C=O)C=C1 GOUHYARYYWKXHS-UHFFFAOYSA-N 0.000 description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
- RGHHSNMVTDWUBI-UHFFFAOYSA-N 4-hydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1 RGHHSNMVTDWUBI-UHFFFAOYSA-N 0.000 description 2
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 description 2
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- KCXZNSGUUQJJTR-UHFFFAOYSA-N Di-n-hexyl phthalate Chemical compound CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCC KCXZNSGUUQJJTR-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- AMIMRNSIRUDHCM-UHFFFAOYSA-N Isopropylaldehyde Chemical compound CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- UUIQMZJEGPQKFD-UHFFFAOYSA-N Methyl butyrate Chemical compound CCCC(=O)OC UUIQMZJEGPQKFD-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- WTWBUQJHJGUZCY-UHFFFAOYSA-N cuminaldehyde Chemical compound CC(C)C1=CC=C(C=O)C=C1 WTWBUQJHJGUZCY-UHFFFAOYSA-N 0.000 description 2
- KSMVZQYAVGTKIV-UHFFFAOYSA-N decanal Chemical compound CCCCCCCCCC=O KSMVZQYAVGTKIV-UHFFFAOYSA-N 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- QWHNJUXXYKPLQM-UHFFFAOYSA-N dimethyl cyclopentane Natural products CC1(C)CCCC1 QWHNJUXXYKPLQM-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- HFJRKMMYBMWEAD-UHFFFAOYSA-N dodecanal Chemical compound CCCCCCCCCCCC=O HFJRKMMYBMWEAD-UHFFFAOYSA-N 0.000 description 2
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 2
- OBNCKNCVKJNDBV-UHFFFAOYSA-N ethyl butyrate Chemical compound CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 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
- 239000010419 fine particle Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 2
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical class OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 2
- FXHGMKSSBGDXIY-UHFFFAOYSA-N heptanal Chemical compound CCCCCCC=O FXHGMKSSBGDXIY-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- BSABBBMNWQWLLU-UHFFFAOYSA-N hydroxypropionaldehyde Natural products CC(O)C=O BSABBBMNWQWLLU-UHFFFAOYSA-N 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 2
- NUKZAGXMHTUAFE-UHFFFAOYSA-N methyl hexanoate Chemical compound CCCCCC(=O)OC NUKZAGXMHTUAFE-UHFFFAOYSA-N 0.000 description 2
- HNBDRPTVWVGKBR-UHFFFAOYSA-N methyl pentanoate Chemical compound CCCCC(=O)OC HNBDRPTVWVGKBR-UHFFFAOYSA-N 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methylcyclopentane Chemical compound CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 description 2
- GYHFUZHODSMOHU-UHFFFAOYSA-N nonanal Chemical compound CCCCCCCCC=O GYHFUZHODSMOHU-UHFFFAOYSA-N 0.000 description 2
- NUJGJRNETVAIRJ-UHFFFAOYSA-N octanal Chemical compound CCCCCCCC=O NUJGJRNETVAIRJ-UHFFFAOYSA-N 0.000 description 2
- FXLOVSHXALFLKQ-UHFFFAOYSA-N p-tolualdehyde Chemical compound CC1=CC=C(C=O)C=C1 FXLOVSHXALFLKQ-UHFFFAOYSA-N 0.000 description 2
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 2
- 229940100595 phenylacetaldehyde Drugs 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920006267 polyester film Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000000425 proton nuclear magnetic resonance spectrum Methods 0.000 description 2
- SMQUZDBALVYZAC-UHFFFAOYSA-N salicylaldehyde Chemical compound OC1=CC=CC=C1C=O SMQUZDBALVYZAC-UHFFFAOYSA-N 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 2
- ISAZDYZOHLBJRO-UHFFFAOYSA-N (4-formylphenyl) dihydrogen phosphate Chemical class OP(O)(=O)OC1=CC=C(C=O)C=C1 ISAZDYZOHLBJRO-UHFFFAOYSA-N 0.000 description 1
- VQROQDIDXQDQLG-UHFFFAOYSA-N (4-formylphenyl) hydrogen sulfate Chemical class OS(=O)(=O)OC1=CC=C(C=O)C=C1 VQROQDIDXQDQLG-UHFFFAOYSA-N 0.000 description 1
- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 description 1
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 description 1
- LAYAKLSFVAPMEL-UHFFFAOYSA-N 1-ethenoxydodecane Chemical compound CCCCCCCCCCCCOC=C LAYAKLSFVAPMEL-UHFFFAOYSA-N 0.000 description 1
- QJJDJWUCRAPCOL-UHFFFAOYSA-N 1-ethenoxyoctadecane Chemical compound CCCCCCCCCCCCCCCCCCOC=C QJJDJWUCRAPCOL-UHFFFAOYSA-N 0.000 description 1
- OVGRCEFMXPHEBL-UHFFFAOYSA-N 1-ethenoxypropane Chemical compound CCCOC=C OVGRCEFMXPHEBL-UHFFFAOYSA-N 0.000 description 1
- HFZLSTDPRQSZCQ-UHFFFAOYSA-N 1-pyrrolidin-3-ylpyrrolidine Chemical compound C1CCCN1C1CNCC1 HFZLSTDPRQSZCQ-UHFFFAOYSA-N 0.000 description 1
- IYEVWHMMOAAJEL-UHFFFAOYSA-N 2,3,4-tribromobenzaldehyde Chemical compound BrC1=CC=C(C=O)C(Br)=C1Br IYEVWHMMOAAJEL-UHFFFAOYSA-N 0.000 description 1
- WMOOOIUXYRHDEZ-UHFFFAOYSA-N 2,3,4-trichlorobenzaldehyde Chemical compound ClC1=CC=C(C=O)C(Cl)=C1Cl WMOOOIUXYRHDEZ-UHFFFAOYSA-N 0.000 description 1
- GEICDMWIZIQEEI-UHFFFAOYSA-N 2,3-dibromobenzaldehyde Chemical compound BrC1=CC=CC(C=O)=C1Br GEICDMWIZIQEEI-UHFFFAOYSA-N 0.000 description 1
- LLMLNAVBOAMOEE-UHFFFAOYSA-N 2,3-dichlorobenzaldehyde Chemical compound ClC1=CC=CC(C=O)=C1Cl LLMLNAVBOAMOEE-UHFFFAOYSA-N 0.000 description 1
- WDBAXYQUOZDFOJ-UHFFFAOYSA-N 2,3-difluorobenzaldehyde Chemical compound FC1=CC=CC(C=O)=C1F WDBAXYQUOZDFOJ-UHFFFAOYSA-N 0.000 description 1
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- OJXOOFXUHZAXLO-UHFFFAOYSA-M magnesium;1-bromo-3-methanidylbenzene;bromide Chemical compound [Mg+2].[Br-].[CH2-]C1=CC=CC(Br)=C1 OJXOOFXUHZAXLO-UHFFFAOYSA-M 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
- 239000011976 maleic acid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000005397 methacrylic acid ester group Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- XJRBAMWJDBPFIM-UHFFFAOYSA-N methyl vinyl ether Chemical compound COC=C XJRBAMWJDBPFIM-UHFFFAOYSA-N 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- BGEHHAVMRVXCGR-UHFFFAOYSA-N methylundecylketone Natural products CCCCCCCCCCCCC=O BGEHHAVMRVXCGR-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- WFKDPJRCBCBQNT-UHFFFAOYSA-N n,2-dimethylprop-2-enamide Chemical compound CNC(=O)C(C)=C WFKDPJRCBCBQNT-UHFFFAOYSA-N 0.000 description 1
- 229940088644 n,n-dimethylacrylamide Drugs 0.000 description 1
- YLGYACDQVQQZSW-UHFFFAOYSA-N n,n-dimethylprop-2-enamide Chemical compound CN(C)C(=O)C=C YLGYACDQVQQZSW-UHFFFAOYSA-N 0.000 description 1
- QQGJWWNPACORPU-UHFFFAOYSA-N n,n-dimethylpropan-1-amine;prop-2-enamide Chemical compound NC(=O)C=C.CCCN(C)C QQGJWWNPACORPU-UHFFFAOYSA-N 0.000 description 1
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 1
- DNTMQTKDNSEIFO-UHFFFAOYSA-N n-(hydroxymethyl)-2-methylprop-2-enamide Chemical group CC(=C)C(=O)NCO DNTMQTKDNSEIFO-UHFFFAOYSA-N 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- ZIWDVJPPVMGJGR-UHFFFAOYSA-N n-ethyl-2-methylprop-2-enamide Chemical compound CCNC(=O)C(C)=C ZIWDVJPPVMGJGR-UHFFFAOYSA-N 0.000 description 1
- SWPMNMYLORDLJE-UHFFFAOYSA-N n-ethylprop-2-enamide Chemical compound CCNC(=O)C=C SWPMNMYLORDLJE-UHFFFAOYSA-N 0.000 description 1
- YPHQUSNPXDGUHL-UHFFFAOYSA-N n-methylprop-2-enamide Chemical compound CNC(=O)C=C YPHQUSNPXDGUHL-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- LIINGNMKNRSOGW-UHFFFAOYSA-N oct-7-enal Chemical compound C=CCCCCCC=O LIINGNMKNRSOGW-UHFFFAOYSA-N 0.000 description 1
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 description 1
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- SQYNKIJPMDEDEG-UHFFFAOYSA-N paraldehyde Chemical compound CC1OC(C)OC(C)O1 SQYNKIJPMDEDEG-UHFFFAOYSA-N 0.000 description 1
- 229960003868 paraldehyde Drugs 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- HVAMZGADVCBITI-UHFFFAOYSA-M pent-4-enoate Chemical compound [O-]C(=O)CCC=C HVAMZGADVCBITI-UHFFFAOYSA-M 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- AAYRWMCIKCRHIN-UHFFFAOYSA-N propane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CCCS(O)(=O)=O AAYRWMCIKCRHIN-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- ADPUQRRLAAPXGT-UHFFFAOYSA-M sodium;2-formylbenzenesulfonate Chemical class [Na+].[O-]S(=O)(=O)C1=CC=CC=C1C=O ADPUQRRLAAPXGT-UHFFFAOYSA-M 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- UIUJIQZEACWQSV-UHFFFAOYSA-N succinic semialdehyde Chemical class OC(=O)CCC=O UIUJIQZEACWQSV-UHFFFAOYSA-N 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000010558 suspension polymerization method Methods 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- AHNWPWARKNOJJM-UHFFFAOYSA-M triethyl-(4-formylphenyl)azanium;iodide Chemical compound [I-].CC[N+](CC)(CC)C1=CC=C(C=O)C=C1 AHNWPWARKNOJJM-UHFFFAOYSA-M 0.000 description 1
- KKDKGWUSNRBBQX-UHFFFAOYSA-M trimethyl(3-oxopropyl)azanium iodide Chemical compound [I-].C[N+](C)(C)CCC=O KKDKGWUSNRBBQX-UHFFFAOYSA-M 0.000 description 1
- KOZCZZVUFDCZGG-UHFFFAOYSA-N vinyl benzoate Chemical compound C=COC(=O)C1=CC=CC=C1 KOZCZZVUFDCZGG-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- C09D129/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
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- C08F16/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F16/38—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an acetal or ketal radical
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- H01G4/00—Fixed capacitors; Processes of their manufacture
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Description
ポリビニルアセタール樹脂をDMSO−d6(ジメチルスルホキシド)に溶解させて、1H−NMRスペクトルを測定し、算出した。
DSC(示差走査熱量計)として、セイコーインスツル株式会社製 EXTAR6000(RD220)を用い、ポリビニルアセタール樹脂を、窒素中で30℃から昇温速度10℃/分で150℃まで昇温させた後、30℃まで冷却し、再度、昇温速度10℃/分で150℃まで昇温させた。再昇温後の測定値をガラス転移点とした。
厚さ0.2mm×10cm×10cmの測定用試料を50℃で減圧下に6日間乾燥し、次いで、乾燥後の試料を20℃の純水中に24時間浸漬したときの質量を測定し、下記式にしたがって吸水率を求めた。
(ポリビニルアセタール樹脂の調製)
還流冷却器、温度計及びイカリ型撹拌翼を備えた内容積2Lのガラス製容器に、イオン交換水1295gと、ポリビニルアルコール(PVA−1:重合度1700、けん化度99.0モル%)105gとを仕込み、全体を95℃に昇温してポリビニルアルコールを完全に溶解させ、ポリビニルアルコール水溶液(濃度7.5質量%)を作製した。作製したポリビニルアルコール水溶液を、回転速度120rpmにて撹拌し続けながら、約30分かけて13℃まで徐々に冷却した後、当該水溶液に、3−メチルブタナール70.5gを添加し、さらにアセタール化触媒である酸触媒として濃度20質量%の塩酸100mLを添加して、ポリビニルアルコールのアセタール化を開始した。アセタール化を15分間行った後、120分かけて全体を47℃まで昇温し、47℃にて180分間保持した後に、室温まで冷却した。冷却によって析出した樹脂をろ過後、イオン交換水(樹脂に対して100倍量のイオン交換水)で10回洗浄した後、中和のために0.3質量%水酸化ナトリウム水溶液を加え、50℃で5時間保持した後、さらに100倍量のイオン交換水で再洗浄を10回繰り返し、脱水したのち、40℃、減圧下で18時間乾燥し、ポリビニルアセタール樹脂(PVIV−1)を得た。得られたポリビニルアセタール樹脂(PVIV−1)は、3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率が69.0モル%(アセタール化度は69.0モル%)、ビニルエステル単位の含有率が1.0モル%、ビニルアルコール単位の含有率が30.0モル%であった。
得られたポリビニルアセタール樹脂10質量部を、トルエン20質量部とエタノール20質量部との混合溶剤に加え、撹拌溶解し、更に、可塑剤としてDOP8質量部を加え、撹拌溶解した。得られた樹脂溶液に、セラミック粉末としてチタン酸バリウム(堺化学工業株式会社製、BT−03(平均粒径0.3μm))100質量部を加え、ボールミルで48時間混合することによりスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−2:重合度800、けん化度99.0モル%)を用い、3−メチルブタナールを73.5g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−2)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は71.2モル%(アセタール化度は71.2モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は27.8モル%であった。次いで、PVIV−2を用いて実施例1と同様にしてスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−3:重合度2400、けん化度99.0モル%)を用い、3−メチルブタナールを70.5g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−3)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は68.4モル%(アセタール化度は68.4モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は30.6モル%であった。次いで、PVIV−3を用いて実施例1と同様にしてスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−4:重合度4300、けん化度99.0モル%)を用い、3−メチルブタナールを75.6g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−4)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は73.8モル%(アセタール化度は73.8モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は25.2モル%であった。次いで、PVIV−4を用いて実施例1と同様にしてスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−5:重合度1700、けん化度88.0モル%)を用い、3−メチルブタナールを64.6g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−5)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は71.2モル%(アセタール化度は71.2モル%)、ビニルエステル単位の含有率は12.0モル%、ビニルアルコール単位の含有率は16.8モル%であった。次いで、PVIV−5を用いて実施例1と同様にしてスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−6:重合度3500、けん化度88.0モル%)を用い、3−メチルブタナールを62.5g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−6)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は69.7モル%(アセタール化度は69.7モル%)、ビニルエステル単位の含有率は12.0モル%、ビニルアルコール単位の含有率は18.3モル%であった。次いで、PVIV−6を用いて実施例1と同様にしてスラリー組成物を得た。
3−メチルブタナールを81.6g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−7)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は79.0モル%(アセタール化度は79.0モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は20.0モル%であった。次いで、PVIV−7を用いて実施例1と同様にしてスラリー組成物を得た。
3−メチルブタナールを66.6g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−8)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は65.0モル%(アセタール化度は65.0モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は34.0モル%であった。次いで、PVIV−8を用いて実施例1と同様にしてスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−7:重合度500、けん化度99.0モル%)を用い、3−メチルブタナールを70.5g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−9)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は69.0モル%(アセタール化度は69.0モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は30.0モル%であった。次いで、PVIV−9を用いて実施例1と同様にしてスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−8:重合度5000、けん化度99.0モル%)を用い、3−メチルブタナールを71.5g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−10)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は70.0モル%(アセタール化度は70.0モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は29.0モル%であった。次いで、PVIV−10を用いて実施例1と同様にしてスラリー組成物を得た。
アルデヒドとして、3−メチルブタナールを44.6g及びブチルアルデヒドを30.5g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−11)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は42.9モル%、ブチルアルデヒドでアセタール化されたビニルアルコール単位の含有率は36.1モル%(アセタール化度は79.0モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は20.0モル%であった。次いで、PVIV−11を用いて実施例1と同様にしてスラリー組成物を得た。
アルデヒドとして、3−メチルブタナールを42.6g及びアセトアルデヒドを20.2g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−12)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は41.0モル%、アセトアルデヒドでアセタール化されたビニルアルコール単位の含有率は38.0モル%(アセタール化度は79.0モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は20.0モル%であった。次いで、PVIV−12を用いて実施例1と同様にしてスラリー組成物を得た。
アルデヒドとしてブチルアルデヒドを65.0g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVB−A)を得た。ブチルアルデヒドでアセタール化されたビニルアルコール単位の含有率は68.8モル%(アセタール化度は68.8モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は30.2モル%であった。次いで、PVB−Aを用いて実施例1と同様にしてスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−9:重合度3500、けん化度99.0モル%)を用い、アルデヒドとして、アセトアルデヒドを25.1g及びブチルアルデヒドを31.0g用いたこと以外は実施例1と同様にしてポリビニルアセトアセタール樹脂(PVB−B)を得た。ブチルアルデヒドでアセタール化されたビニルアルコール単位の含有率は36.0モル%、アセトアルデヒドでアセタール化されたビニルアルコール単位の含有率は44.4モル%(アセタール化度は80.4モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は18.6モル%であった。次いで、PVB−Bを用いて実施例1と同様にしてスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−10:重合度6500、けん化度88.0モル%)を用い、アルデヒドとして3−メチルブタナールを69.0g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−13)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は73.9モル%(アセタール化度は73.9モル%)、ビニルエステル単位の含有率は12.0モル%、ビニルアルコール単位の含有率は14.1モル%であった。次いで、PVIV−13を用いて実施例1と同様にしてスラリー組成物を作製しようとしたが、分散不良のため、スラリー組成物を得ることが出来なかった。
PVA−1に代えてポリビニルアルコール(PVA−11:重合度150、けん化度99.0モル%)を用い、アルデヒドとして3−メチルブタナールを69.0g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−14)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は66.8モル%(アセタール化度は66.8モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は32.2モル%であった。次いで、PVIV−14を用いて実施例1と同様にしてスラリー組成物を得た。
PVA−1に代えてポリビニルアルコール(PVA−12:重合度1700、けん化度69.0モル%)を用い、アルデヒドとして3−メチルブタナールを39.0g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−15)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は50.0モル%(アセタール化度は50.0モル%)、ビニルエステル単位の含有率は31.0モル%、ビニルアルコール単位の含有率は19.0モル%であった。次いで、PVIV−15を用いて実施例1と同様にしてスラリー組成物を得た。
アルデヒドとして3−メチルブタナールを54.0g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVIV−16)を得た。3−メチルブタナールでアセタール化されたビニルアルコール単位の含有率は53.6モル%(アセタール化度は53.6モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は45.4モル%であった。次いで、PVIV−16を用いて実施例1と同様にしてスラリー組成物を得た。
アルデヒドとしてブチルアルデヒドを45.0g用いたこと以外は実施例1と同様にして、ポリビニルアセタール樹脂(PVB−C)を得た。ブチルアルデヒドでアセタール化されたビニルアルコール単位の含有率は78.0モル%(アセタール化度は78.0モル%)、ビニルエステル単位の含有率は1.0モル%、ビニルアルコール単位の含有率は21.0モル%であった。次いで、PVB−Cを用いて実施例1と同様にしてスラリー組成物を得た。
離形処理したポリエステルフィルム上に実施例1〜12又は比較例1〜7で作製したスラリー組成物を、コーターバーを用いて、乾燥後の厚みが1μmとなるように塗工し、常温で1時間風乾した後、熱風乾燥機にて80℃にて3時間、続いて120℃で2時間乾燥させてセラミックグリーンシートを得た。
導電粉末としてのニッケル粉末(三井金属鉱業株式会社製 2020SS)100質量部、エチルセルロース(ダウケミカルカンパニー社製 STD−100)5質量部、及び溶剤としてテルピネオール−C(日本テルペン株式会社製)60質量部を混合した後、3本ロールで混練して導電ペーストを得た。
上記で得られたセラミックグリーンシートの片面に、上記で得られた導電ペーストを、乾燥後の厚みが約1.0μmとなるようにスクリーン印刷法により塗工し、乾燥させて導電層を形成した。この導電層を有するセラミックグリーンシートを5cm角に切断し、100枚積重ねて、温度70℃、圧力150kg/cm2で10分間加熱及び圧着して、積層体を得た。得られた積層体を、窒素雰囲気下、昇温速度3℃/分で400℃まで昇温し、5時間保持した後、昇温速度5℃/分で1350℃まで昇温し、10時間保持することにより、セラミック焼成体を得た。
(機械的強度の評価)
得られたセラミックグリーンシートをポリエステルフィルムから剥離し、シートの状態を観察し、以下に示す3段階で評価した。結果を表1に示す。
A:セラミックグリーンシートに切れや破れが観察されなかったもの。
B:切れや破れがわずかに観察されたもの。
C:切れや破れが観察されたもの。
30cm×30cmのセラミックグリーンシートを23℃、65%RHの恒温恒湿下に静置し、製膜後と10日後の寸法変化率を測定し、以下に示す2段階で評価した。結果を表1に示す。
A:セラミックグリーンシートの寸法変化率が0.1%未満であって、且つ反りが認められないもの。
B:セラミックグリーンシートの寸法変化率が0.1%以上である、及び/又は反りが認められるもの。
得られたセラミック焼成体(常温まで冷却した後のもの)を半分に割り、電子顕微鏡で観察し、セラミック層と導電層とのデラミネーションの有無を観察し、以下に示す3段階で評価した。結果を表1に示す。
A:デラミネーションなし。
B:デラミネーションが僅かに見られる。
C:デラミネーションあり。
Claims (10)
- 重合度が1500を超え、4500以下である請求項1に記載のポリビニルアセタール樹脂。
- 3−メチルブタナールを含むアルデヒドを用いてポリビニルアルコール樹脂をアセタール化することにより得られる請求項1又は2記載のポリビニルアセタール樹脂。
- 化学式(1)で表される構造単位が、全てのアセタール化された構造単位の総モル量に対して、30モル%以上含まれる請求項1〜4のいずれかに記載のポリビニルアセタール樹脂。
- 請求項1〜5のいずれかに記載のポリビニルアセタール樹脂、セラミック粉末及び有機溶剤を含有するスラリー組成物。
- 請求項6に記載のスラリー組成物を用いて得られるセラミックグリーンシート。
- 請求項1〜5のいずれかに記載のポリビニルアセタール樹脂、及び導電性粉末を含有する導電ペースト。
- 請求項7に記載のセラミックグリーンシートを用いて得られる積層セラミックコンデンサ。
- 請求項8に記載の導電ペーストを用いて得られる積層セラミックコンデンサ。
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KR20160124171A (ko) * | 2014-02-17 | 2016-10-26 | 주식회사 쿠라레 | 세라믹 성형용 또는 도전 페이스트용 결합제, 및 이들의 용도 |
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US9758662B2 (en) | 2014-12-08 | 2017-09-12 | Solutia Inc. | Poly(vinyl acetal) resin compositions, layers and interlayers having enhanced properties |
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KR101829788B1 (ko) | 2018-02-19 |
CN105175590B (zh) | 2017-10-03 |
US20160032131A1 (en) | 2016-02-04 |
CN103068859B (zh) | 2015-11-25 |
EP2607390A1 (en) | 2013-06-26 |
US20130148263A1 (en) | 2013-06-13 |
CN103068859A (zh) | 2013-04-24 |
TW201219419A (en) | 2012-05-16 |
US9550909B2 (en) | 2017-01-24 |
EP2607390B1 (en) | 2016-06-22 |
JPWO2012023517A1 (ja) | 2013-10-28 |
WO2012023517A1 (ja) | 2012-02-23 |
EP2607390A4 (en) | 2014-08-13 |
TWI504613B (zh) | 2015-10-21 |
KR20130100132A (ko) | 2013-09-09 |
CN105175590A (zh) | 2015-12-23 |
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