TW201700604A - 黏結劑樹脂組合物 - Google Patents
黏結劑樹脂組合物 Download PDFInfo
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- TW201700604A TW201700604A TW105108701A TW105108701A TW201700604A TW 201700604 A TW201700604 A TW 201700604A TW 105108701 A TW105108701 A TW 105108701A TW 105108701 A TW105108701 A TW 105108701A TW 201700604 A TW201700604 A TW 201700604A
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- resin composition
- aliphatic polycarbonate
- formula
- polycarbonate resin
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- 239000000203 mixture Substances 0.000 title claims abstract description 50
- 239000004840 adhesive resin Substances 0.000 title claims abstract description 5
- 229920006223 adhesive resin Polymers 0.000 title claims abstract description 5
- -1 optical discs Substances 0.000 claims abstract description 72
- 239000011230 binding agent Substances 0.000 claims abstract description 49
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 47
- 229920005668 polycarbonate resin Polymers 0.000 claims abstract description 46
- 239000004431 polycarbonate resin Substances 0.000 claims abstract description 46
- 239000011342 resin composition Substances 0.000 claims abstract description 44
- 239000002002 slurry Substances 0.000 claims abstract description 23
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 125000004185 ester group Chemical group 0.000 claims abstract description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 9
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000000524 functional group Chemical group 0.000 claims abstract description 7
- 125000005843 halogen group Chemical group 0.000 claims abstract description 7
- JOYRKODLDBILNP-UHFFFAOYSA-N urethane group Chemical group NC(=O)OCC JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000004036 acetal group Chemical group 0.000 claims abstract description 5
- 125000005534 decanoate group Chemical group 0.000 claims abstract description 5
- 125000001033 ether group Chemical group 0.000 claims abstract description 5
- 239000010419 fine particle Substances 0.000 claims description 22
- 229920000379 polypropylene carbonate Polymers 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 22
- 125000004432 carbon atom Chemical group C* 0.000 claims description 12
- 125000000217 alkyl group Chemical group 0.000 claims description 11
- 125000003118 aryl group Chemical group 0.000 claims description 11
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 6
- 229920005989 resin Polymers 0.000 abstract description 48
- 239000011347 resin Substances 0.000 abstract description 48
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 15
- 239000000654 additive Substances 0.000 abstract description 9
- 239000000919 ceramic Substances 0.000 abstract description 8
- 230000000996 additive effect Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 229920006167 biodegradable resin Polymers 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 239000002775 capsule Substances 0.000 abstract description 2
- 238000010114 lost-foam casting Methods 0.000 abstract description 2
- 239000012567 medical material Substances 0.000 abstract description 2
- 239000011859 microparticle Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 abstract 1
- 239000013307 optical fiber Substances 0.000 abstract 1
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 30
- 238000000034 method Methods 0.000 description 27
- 238000004519 manufacturing process Methods 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 21
- 238000000354 decomposition reaction Methods 0.000 description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 18
- 229910052725 zinc Inorganic materials 0.000 description 16
- 239000011701 zinc Substances 0.000 description 16
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 15
- 238000006116 polymerization reaction Methods 0.000 description 15
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 14
- 239000002981 blocking agent Substances 0.000 description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 13
- 238000002156 mixing Methods 0.000 description 12
- 229910004298 SiO 2 Inorganic materials 0.000 description 11
- 238000005245 sintering Methods 0.000 description 11
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- 239000011521 glass Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
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- 238000009826 distribution Methods 0.000 description 9
- 238000004898 kneading Methods 0.000 description 9
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- 239000004094 surface-active agent Substances 0.000 description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 7
- 239000012456 homogeneous solution Substances 0.000 description 7
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 229940014800 succinic anhydride Drugs 0.000 description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 5
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- 239000002184 metal Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 150000001335 aliphatic alkanes Chemical group 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 4
- 239000007810 chemical reaction solvent Substances 0.000 description 4
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 4
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 4
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 4
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 239000004014 plasticizer Substances 0.000 description 4
- YKYONYBAUNKHLG-UHFFFAOYSA-N propyl acetate Chemical compound CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 4
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 4
- 239000003381 stabilizer Substances 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 4
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 3
- RBACIKXCRWGCBB-UHFFFAOYSA-N 1,2-Epoxybutane Chemical compound CCC1CO1 RBACIKXCRWGCBB-UHFFFAOYSA-N 0.000 description 3
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000004721 Polyphenylene oxide Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 235000011054 acetic acid Nutrition 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- 229920000570 polyether Polymers 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- DAFHKNAQFPVRKR-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylpropanoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)C DAFHKNAQFPVRKR-UHFFFAOYSA-N 0.000 description 2
- 239000001716 (4-methyl-1-propan-2-yl-1-cyclohex-2-enyl) acetate Substances 0.000 description 2
- VZXTWGWHSMCWGA-UHFFFAOYSA-N 1,3,5-triazine-2,4-diamine Chemical compound NC1=NC=NC(N)=N1 VZXTWGWHSMCWGA-UHFFFAOYSA-N 0.000 description 2
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 description 2
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 2
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 2
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- QJNLUNBGDFUULX-UHFFFAOYSA-N 4-n,4-n'-dimethyl-3h-pyridine-4,4-diamine Chemical compound CNC1(NC)CC=NC=C1 QJNLUNBGDFUULX-UHFFFAOYSA-N 0.000 description 2
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
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- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
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- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
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- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
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- 239000002318 adhesion promoter Substances 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- IGODOXYLBBXFDW-UHFFFAOYSA-N alpha-Terpinyl acetate Chemical compound CC(=O)OC(C)(C)C1CCC(C)=CC1 IGODOXYLBBXFDW-UHFFFAOYSA-N 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
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- QARVLSVVCXYDNA-UHFFFAOYSA-N bromobenzene Chemical compound BrC1=CC=CC=C1 QARVLSVVCXYDNA-UHFFFAOYSA-N 0.000 description 2
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
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- 125000004093 cyano group Chemical group *C#N 0.000 description 2
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- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
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- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
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- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 2
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- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
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- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
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- 150000003021 phthalic acid derivatives Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
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- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 2
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- 229940116411 terpineol Drugs 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 125000004149 thio group Chemical group *S* 0.000 description 2
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- YWWDBCBWQNCYNR-UHFFFAOYSA-N trimethylphosphine Chemical compound CP(C)C YWWDBCBWQNCYNR-UHFFFAOYSA-N 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
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- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
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- 229910052727 yttrium Inorganic materials 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- HEPBQSXQJMTVFI-UHFFFAOYSA-N zinc;butane Chemical compound [Zn+2].CCC[CH2-].CCC[CH2-] HEPBQSXQJMTVFI-UHFFFAOYSA-N 0.000 description 1
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Abstract
本發明係一種包含式(1)所表示之脂肪族聚碳酸酯樹脂與式(2)所表示之末端封端脂肪族聚碳酸酯樹脂之黏結劑樹脂組合物、及含有該樹脂組合物之無機微粒子分散漿料組合物。
□□(式中，X及Y可相同或不同，為於末端具有選自羧基、酯基、胺基甲酸酯基、矽酸酯基、異氰酸酯基、醚基、縮醛基、及鹵素原子中之至少1種官能基之基)
本發明之黏結劑樹脂組合物可用於一般成形物、膜、纖維、光纖、光碟等光學材料、陶瓷黏結劑、消失模鑄造等之熱分解性材料、藥劑膠囊等醫用材料、生物可降解樹脂之添加劑、生物可降解樹脂之主成分等。
Description
本發明係關於一種黏結劑樹脂組合物、及含有該樹脂組合物之無機微粒子分散漿料組合物。
近年來，藉由製造包含導電性粒子、陶瓷、玻璃、螢光體等無機粉末與成形用黏結劑之漿料，使其成型，並且進行燒結，而製造各種各樣之製品。作為成形用黏結劑，使用聚乙烯醇縮丁醛(PVB)、乙基纖維素(EC)、羧甲基纖維素(CMC)、聚乙烯醇(PVA)、丙烯酸系聚合物等。黏結劑成分較佳為於燒結時完全消失，但由於上述黏結劑不易分解，若僅藉由加熱，則成形之陶瓷中會殘留黏結劑殘渣，對陶瓷之性能造成不良影響，故而使用於燒結時供給氧使黏結劑完全燃燒而消失之方法。
然而，若於燒結時之高溫條件下存在氧，則存在無機成分變質，燒結體之性能降低之情形，故而多數情況下需要燒結後於還原氣氛下進而進行燒結之步驟。因此，業界期待於燒結時不供給氧而可消失之黏結劑。
進而，由於上述之黏結劑會發熱分解，故而難以一面控制燒結爐內之溫度，一面一次進行大量燒結。
作為於燒結時無需氧而可吸熱分解之黏結劑，業界正研究聚碳酸丙烯酯及聚碳酸乙烯酯之類的脂肪族聚碳酸酯樹脂。然而，該等樹脂之分解溫度根據製程而存在過低之情形(參照專利文獻1)。因此，
作為其解決方法，已知有藉由將分子鏈末端封端而使分解溫度上升之方法(參照專利文獻2、非專利文獻1)。
[專利文獻1]日本專利特開平6-334282號公報
[專利文獻2]美國專利第4066630號說明書
[非專利文獻1]Shuwen Peng, Yuxian An, Cheng Chen, Bin Fei, Yugang Zhuang, Lisong Dong. Polymer Degradation and Stability, 2003年，vol. 80, p. 141-147
然而，藉由該等方法難以設計以所需之任意之溫度分解之黏結劑，對於製程之應用受限制，故而期望能夠以良好之精度控制分解溫度之黏結劑。
本發明之課題在於提供一種能夠以良好之精度控制分解溫度之黏結劑樹脂組合物、及含有該樹脂組合物之無機微粒子分散漿料組合物。
本發明者等人為了解決上述問題進行努力研究，結果發現，藉由將脂肪族聚碳酸酯樹脂之末端由封端劑(末端封端劑)封端之樹脂與未封端之樹脂以任意之比率混合，可於兩樹脂之分解開始溫度之範圍內大致任意地控制分解開始溫度，並進一步反覆研究，結果完成本發明。
本發明係關於如下者：
[1]一種黏結劑樹脂組合物，其包含式(1)所表示之脂肪族聚碳酸
酯樹脂與式(2)所表示之末端封端脂肪族聚碳酸酯樹脂，
(式中，R1、R2、R3及R4可相同或不同，為氫原子、碳數1~10之烷基或碳數6~20之芳基，m為40~23000之整數)
(式中，R5、R6、R7及R8可相同或不同，為氫原子、碳數1~10之烷基或碳數6~20之芳基，X及Y可相同或不同，為於末端具有選自羧基、酯基、胺基甲酸酯基、矽酸酯基、異氰酸酯基、醚基、縮醛基、及鹵素原子中之至少1種官能基之基，n為40~23000之整數)；及
[2]一種無機微粒子分散漿料組合物，其含有如上述[1]之黏結劑樹脂組合物、無機微粒子、及溶劑。
本發明之黏結劑樹脂組合物發揮可以良好之精度控制分解溫度之優異效果。
圖1係實施例1~5及參考例1、2中所獲得之樹脂組合物之熱分解曲線。
圖2係表示實施例1~5及參考例1、2中所獲得之樹脂組合物之組成比與熱分解開始溫度之關係之圖表。
圖3係表示實施例1~5及參考例1、2中所獲得之樹脂組合物之組成比與50質量%分解溫度之關係之圖表。
本發明之黏結劑樹脂組合物包含式(1)所表示之脂肪族聚碳酸酯樹脂與式(2)所表示之末端封端脂肪族聚碳酸酯樹脂。
(式中，R1、R2、R3及R4可相同或不同，為氫原子、碳數1~10之烷基或碳數6~20之芳基，m為40~23000之整數)
(式中，R5、R6、R7及R8可相同或不同，為氫原子、碳數1~10之烷基或碳數6~20之芳基，X及Y可相同或不同，為於末端具有選自羧基、酯基、胺基甲酸酯基、矽酸酯基、異氰酸酯基、醚基、縮醛基、及鹵素原子中之至少1種官能基之基，n為40~23000之整數)
通常，若將2種樹脂混合並使其熱分解，則各樹脂獨立地進行熱分解，但本發明之黏結劑樹脂組合物根據各樹脂之混合比率，如單一樹脂之熱分解般進行分解，故而可以良好之精度控制黏結劑樹脂組合物之分解溫度。
式(1)及式(2)中，烷基之碳數為1~10，較佳為1~4。作為烷基，較佳為直鏈或支鏈之經取代或未經取代之烷基，例如可列舉甲基、乙
基、正丙基、異丙基、正丁基、第二丁基、第三丁基、正戊基、正己基、正庚基、正辛基、正壬基、正癸基等。烷基亦可經例如選自烷氧基、酯基、矽烷基、硫基、氰基、硝基、磺基、甲醯基、芳基、鹵素原子等中之1種或2種以上之取代基取代。
又，芳基之碳數為6~20，較佳為6~14。作為芳基，例如可列舉苯基、茚基、萘基、四氫萘基等。芳基亦可經例如選自甲基、乙基、正丙基、異丙基、正丁基、第二丁基、第三丁基等烷基、苯基、萘基等其他芳基、烷氧基、酯基、矽烷基、硫基、氰基、硝基、磺基、甲醯基、鹵素原子等中之1種或2種以上之取代基取代。
式(1)及式(2)中，n及m為40~23000之整數，較佳為200~5000。n與m可相同亦可不同，但n與m越接近越佳，n與m之比(n/m)較佳為0.5~2.0，更佳為0.7~1.3。
式(2)中，X及Y之末端為羥基以外之基，為於末端具有選自羧基、酯基、胺基甲酸酯基、矽酸酯基、異氰酸酯基、醚基、縮醛基、及鹵素原子中之至少1種官能基之基，就封端反應之容易性之觀點而言，較佳為於末端具有選自羧基、酯基、胺基甲酸酯基及異氰酸酯基中之至少1種官能基之基。
作為上述脂肪族聚碳酸酯樹脂之製造方法，可列舉使環氧化物與二氧化碳進行聚合反應之方法。
作為用於製造上述脂肪族聚碳酸酯樹脂中式(1)或式(2)所表示之脂肪族聚碳酸酯樹脂之環氧化物並無特別限定，例如可列舉環氧乙烷、環氧丙烷、1,2-環氧丁烷、2,3-環氧丁烷、異環氧丁烷、1-環氧戊烷、2-環氧戊烷、1-環氧己烷、1-環氧辛烷、1-環氧十二烷、環氧環戊烷、環氧環己烷、環氧苯乙烷、乙烯基環氧環己烷、3-苯基環氧丙烷、3,3,3-三氟環氧丙烷、3-萘基環氧丙烷、2-苯氧基環氧丙烷、3-萘氧基環氧丙烷、環氧丁烯、3-乙烯氧基環氧丙烷及3-三甲基矽烷氧
基環氧丙烷等。
上述環氧化物中，就具有較高之反應性之觀點而言，較佳為環氧乙烷、環氧丙烷、及1,2-環氧丁烷，更佳為環氧乙烷及環氧丙烷。因此，式(1)所表示之脂肪族聚碳酸酯樹脂及式(2)所表示之脂肪族聚碳酸酯樹脂分別可相同亦可不同，較佳為選自由聚碳酸乙烯酯、聚碳酸丙烯酯及聚碳酸丁烯酯所組成之群中之至少1種，更佳為聚碳酸乙烯酯及/或聚碳酸丙烯酯。
環氧化物與二氧化碳之聚合反應較佳為於金屬觸媒之存在下進行。
作為金屬觸媒，例如可列舉鋅系觸媒、鋁系觸媒、鉻系觸媒、鈷系觸媒等。該等之中，就於環氧化物與二氧化碳之聚合反應中具有較高之聚合活性之方面而言，較佳為鋅系觸媒及/或鈷系觸媒，就獲得高分子聚體之觀點而言，更佳為鋅系觸媒。
作為鋅系觸媒，例如可列舉乙酸鋅、二乙基鋅、二丁基鋅等有機鋅觸媒；藉由使一級胺、二元酚(苯二酚)、芳香族二羧酸、芳香族羥酸、脂肪族二羧酸、脂肪族單羧酸等化合物與鋅化合物反應而獲得之有機鋅觸媒等。該等有機鋅觸媒之中，就具有更高之聚合活性之方面而言，較佳為使鋅化合物與脂肪族二羧酸及脂肪族單羧酸反應而獲得之有機鋅觸媒，更佳為使氧化鋅與戊二酸及乙酸反應而獲得之有機鋅觸媒。
上述聚合反應所使用之金屬觸媒之使用量相對於環氧化物1莫耳，就促進聚合反應之進行之觀點而言，較佳為0.001莫耳以上，更佳為0.005莫耳以上，就獲得與使用量相稱之效果之觀點而言，較佳為0.2莫耳以下，更佳為0.1莫耳以下。
上述聚合反應中亦可視需要使用反應溶劑。作為反應溶劑並無特別限定，可使用各種有機溶劑。作為有機溶劑，例如可列舉戊烷、
己烷、辛烷、癸烷、環己烷等脂肪族烴系溶劑；苯、甲苯、二甲苯等芳香族烴系溶劑；二氯甲烷、氯仿、四氯化碳、1,1-二氯乙烷、1,2-二氯乙烷、氯乙烷、三氯乙烷、1-氯丙烷、2-氯丙烷、1-氯丁烷、2-氯丁烷、1-氯-2-甲基丙烷、氯苯、溴苯等鹵化烴系溶劑；二甲氧基乙烷、四氫呋喃、2-甲基四氫呋喃、1,4-二烷、1,3-二氧雜環戊烷等醚系溶劑；乙酸乙酯、乙酸正丙酯、乙酸異丙酯等酯系溶劑；N,N-二甲基甲醯胺、N,N-二甲基乙醯胺等醯胺系溶劑；碳酸二甲酯、碳酸甲酯乙酯、碳酸二乙酯、碳酸丙烯酯等碳酸酯系溶劑等。
就使反應順利進行之觀點而言，反應溶劑之使用量相對於環氧化物100質量份較佳為100~10000質量份。
作為使環氧化物與二氧化碳於金屬觸媒之存在下進行聚合反應之方法並無特別限定，例如可列舉向高壓釜中添加環氧化物、金屬觸媒、及視需要之輔觸媒、反應溶劑等，並進行混合，然後壓入二氧化碳而使之反應之方法。
上述聚合反應中所使用之二氧化碳之使用量相對於環氧化物1莫耳，較佳為0.5~10莫耳，更佳為0.6~5莫耳，進而較佳為0.7~3莫耳。
上述聚合反應中所使用之二氧化碳之使用壓力並無特別限定，就使反應順利進行之觀點而言，較佳為0.1MPa以上，更佳為0.2MPa以上，進而較佳為0.5MPa以上，就獲得與使用壓力相稱之效果之觀點而言，較佳為20MPa以下，更佳為10MPa以下，進而較佳為5MPa以下。
上述聚合反應中之聚合反應溫度並無特別限定，就反應時間縮短之觀點而言，較佳為0℃以上，更佳為20℃以上，進而較佳為30℃以上，就抑制副反應，提高產率之觀點而言，較佳為100℃以下，更佳為80℃以下，進而較佳為60℃以下。
聚合反應時間根據聚合反應條件而不同，故而無法一概而定，通常較佳為1~40小時左右。
作為式(2)所表示之結構之末端封端脂肪族聚碳酸酯樹脂之製造方法，可列舉於製造式(1)所表示之脂肪族聚碳酸酯樹脂時繼聚合反應後使其與末端封端劑反應之方法，使單離之式(1)所表示之脂肪族聚碳酸酯樹脂與末端封端劑反應之方法等。
作為末端封端劑，例如可列舉甲酸、乙酸、丙酸、苯甲酸等羧酸；乙酸酐、琥珀酸酐、馬來酸酐、鄰苯二甲酸酐、均苯四甲酸二酐等酸酐；乙醯氯、丙醯氯、苯甲醯氯、對甲苯磺醯氯、乙二醯氯、琥珀醯氯、己二醯氯、對苯二甲醯氯等醯鹵化物；異氰酸甲酯、異氰酸乙酯、異氰酸苯酯、異氰酸苄酯、1,6-六亞甲基二異氰酸酯、4,4'-二苯基甲烷二異氰酸酯、甲苯二異氰酸酯等異氰酸酯化合物；矽酸甲酯、矽酸乙酯、矽酸丙酯等有機矽酸酯化合物；甲基溴、甲基碘、苄基氯、苄基溴等鹵代烷化合物；氯化氫、溴化氫、碘化氫等鹵化氫；甲醛、乙醛、苯甲醛等醛化合物。
作為使脂肪族聚碳酸酯樹脂與末端封端劑反應之方法，可列舉於有機溶劑中使其反應之方法或藉由熔融混練而使其反應之方法等。
作為脂肪族聚碳酸酯樹脂與末端封端劑之反應中所使用之有機溶劑，只要為能夠溶解脂肪族聚碳酸酯樹脂且不與末端封端劑發生反應之溶劑則無特別限定，可列舉苯、甲苯、二甲苯等芳香族烴系溶劑；二氯甲烷(dichloromethane)、氯仿、1,2-二氯乙烷、氯苯等鹵化烴系溶劑；二甲氧基乙烷、四氫呋喃、2-甲基四氫呋喃、1,4-二烷、1,3-二氧雜環戊烷等醚系溶劑；乙酸乙酯、乙酸正丙酯、乙酸異丙酯等酯系溶劑；丙酮、甲基乙基酮、甲基異丁基酮等酮系溶劑；N,N-二甲基甲醯胺、N,N-二甲基乙醯胺等醯胺系溶劑；碳酸二甲酯、碳酸丙烯酯等碳酸酯系溶劑等。
脂肪族聚碳酸酯樹脂與末端封端劑之反應中可使用觸媒，亦可不使用。作為與末端封端劑之反應中所使用之觸媒，可列舉三乙胺、三丙胺、三丁胺、4,4-二甲胺基吡啶等胺化合物；吡啶、N-甲基咪唑等含氮雜環化合物；三甲基膦、三乙基膦、三苯基膦等有機磷化合物；二丁基錫、辛酸錫等有機錫化合物等。觸媒之使用量相對於末端封端劑1莫耳較佳為0.01~1莫耳左右。
作為用於以熔融混練之方式進行脂肪族聚碳酸酯樹脂與末端封端劑之反應之裝置，可列舉輥、擠出機、班布里混合機、Plastomill、布拉本德密煉機(Brabender)等混練機。
脂肪族聚碳酸酯樹脂與末端封端劑之反應溫度並無特別限定，於有機溶劑中使其反應之情形時，例如可以20~120℃左右之溫度進行反應。於以熔融混練之方式使其反應之情形時，例如可以80~200℃左右之溫度進行反應。
關於末端封端劑之使用量，於控制末端之封端量之情形時，可根據末端基之量進行調節，於完全封端之情形時，相對於脂肪族聚碳酸酯樹脂100質量份較佳為0.3質量份以上，就防止因過量之末端封端劑之殘留所致之作為黏結劑之性能降低之觀點而言，較佳為5質量份以下。就該等觀點而言，末端封端劑之使用量相對於脂肪族聚碳酸酯樹脂100質量份，較佳為0.3~5質量份，更佳為0.5~2質量份。
關於上述式(1)或式(2)所表示之脂肪族聚碳酸酯樹脂之質量平均分子量，就於使黏結劑樹脂組合物與無機微粒子混合而用作無機微粒子分散漿料組合物之情形時，使無機微粒子於脂肪族聚碳酸酯樹脂中穩定分散之觀點而言，較佳為5,000以上，更佳為10,000以上，進而較佳為100,000以上，就避免因黏結劑樹脂組合物於溶劑中之溶解性降低所致之操作性降低之觀點而言，較佳為2,000,000以下，更佳為1,000,000以下，進而較佳為500,000以下。
就易於控制黏結劑溶液黏度之觀點而言，上述式(1)或式(2)所表示之脂肪族聚碳酸酯樹脂之分子量分佈(質量平均分子量/數量平均分子量)較佳為1.0~20.0，更佳為1.0~15.0，進而較佳為1.0~10.0。
作為本發明之黏結劑樹脂組合物之製造方法，可列舉將式(1)所表示之脂肪族聚碳酸酯樹脂與式(2)所表示之末端封端脂肪族聚碳酸酯樹脂分別以任意之比率混合之方法。式(1)所表示之脂肪族聚碳酸酯樹脂與式(2)所表示之末端封端脂肪族聚碳酸酯樹脂之調配比率根據作為目標之熱分解溫度而適當確定，就因2種脂肪族聚碳酸酯樹脂之混合而熱分解溫度之變化明確之觀點而言，兩者之質量比(式(1)所表示之脂肪族聚碳酸酯樹脂/式(2)所表示之末端封端脂肪族聚碳酸酯樹脂)較佳為10/90~90/10，更佳為20/80~80/20。
作為混合2種脂肪族聚碳酸酯樹脂之方法，可列舉使其一次溶解於溶劑中進行混合後去除溶劑之方法或使用輥、擠出機、班布里混合機、Plastomill、布拉本德密煉機等進行熔融混練之方法。
本發明之黏結劑樹脂組合物中亦可視需要包含觸變劑、界面活性劑、塑化劑、保存穩定劑等添加劑。
作為觸變劑，可列舉脂肪酸醯胺、二氧化矽微粒子及有機膨潤土等。作為界面活性劑，可列舉聚氧乙烯系界面活性劑、脂肪酸酯系界面活性劑等。作為塑化劑，可列舉聚醚多元醇、鄰苯二甲酸酯等。作為保存穩定劑，可列舉胺化合物、羧酸化合物、磷化合物、硫化合物、三唑系化合物等。
本發明之黏結劑樹脂組合物之添加劑之含量相對於黏結劑樹脂(式(1)所表示之脂肪族聚碳酸酯樹脂與式(2)所表示之末端封端脂肪族聚碳酸酯樹脂之合計)100質量份，較佳為30質量份以下，更佳為20質量份以下。
藉由混合本發明之黏結劑樹脂組合物與溶劑、陶瓷等無機粉
末、及視需要之添加劑等而製造漿料，並進行成型、燒結，藉此可製造所需之形狀之製品。
因此，本發明進而提供一種含有本發明之黏結劑樹脂組合物、無機微粒子、及溶劑之無機微粒子分散漿料組合物。
作為無機微粒子並無特別限定，較佳為選自由導電體粒子、陶瓷粉末、玻璃粉末、及無機螢光體微粒子所組成之群中之至少1種。
作為導電體粒子，例如可列舉銅、鐵、鎳、鈀、鉑、金、銀、鋁、鎢、及包含該等合金等之金屬粒子等。
作為陶瓷粉末，例如可列舉氧化鋁、氧化鋯、氧化鈦、鈦酸鋇、氮氧化鋁、氮化矽、氮化硼、碳化矽等之粉末。又，亦可較佳地使用透明電極材料所使用之奈米ITO(摻錫氧化銦)或染料敏化太陽電池所使用之奈米氧化鈦等。
作為玻璃粉末，例如可列舉CaO-Al2O3-SiO2系、MgO-Al2O3-SiO2系、LiO2-Al2O3-SiO2系等各種矽氧化物、氧化鉍玻璃、矽酸鹽玻璃、鉛玻璃、鋅玻璃、硼玻璃等玻璃粉末等。
又，作為玻璃粉末，亦可使用PbO-B2O3-SiO2混合物、BaO-ZnO-B2O3-SiO2混合物、ZnO-Bi2O3-B2O3-SiO2混合物、Bi2O3-B2O3-BaO-CuO混合物、Bi2O3-ZnO-B2O3-Al2O3-SrO混合物、ZnO-Bi2O3-B2O3混合物、Bi2O3-SiO2混合物、P2O5-Na2O-CaO-BaO-Al2O3-B2O3混合物、P2O5-SnO混合物、P2O5-SnO-B2O3混合物、P2O5-SnO-SiO2混合物、CuO-P2O5-RO混合物、SiO2-B2O3-ZnO-Na2O-Li2O-NaF-V2O5混合物、P2O5-ZnO-SnO-R2O-RO混合物、B2O3-SiO2-ZnO混合物、B2O3-SiO2-Al2O3-ZrO2混合物、SiO2-B2O3-ZnO-R2O-RO混合物、SiO2-B2O3-Al2O3-RO-R2O混合物、SrO-ZnO-P2O5混合物、SrO-ZnO-P2O5混合物、BaO-ZnO-B2O3-SiO2混合物等玻璃粉末。此處，上述R表示選自由Zn、Ba、Ca、Mg、Sr、Sn、Ni、Fe及Mn所組成之群中之元素。
作為無機螢光體微粒子，例如可列舉BaMgAl10O17：Eu、Zn2SiO4：Mn、(Y、Gd)BO3：Eu等。
無機微粒子分散漿料組合物中之黏結劑樹脂組合物之含量相對於上述無機微粒子100質量份，就避免無機微粒子之分散性降低，於成形時因無機微粒子之偏集存在而導致燒結體之性能降低之觀點而言，較佳為0.001質量份以上，更佳為0.01質量份以上，進而較佳為0.1質量份以上，就於燒結無機微粒子分散漿料組合物時，減少因脂肪族聚碳酸酯樹脂之過度分解而生成之分解物，獲得緻密之燒結體之觀點而言，較佳為20質量份以下，更佳為15質量份以下，進而較佳為10質量份以下。
作為溶劑並無特別限定，例如可列舉甲苯、乙酸乙酯、乙酸丁酯、異丙醇、甲基異丁基酮、甲基乙基酮、N-甲基-2-吡咯啶酮、乙二醇乙醚、乙二醇單丁醚、乙二醇單乙醚乙酸酯、二乙二醇單乙醚、二乙二醇單甲醚、二乙二醇單異丁醚、三甲基戊二醇單異丁酸酯、乙基卡必醇、丁基卡必醇、乙基卡必醇乙酸酯、丁基卡必醇乙酸酯、松油醇、松油醇乙酸酯、二氫松油醇、二氫松油醇乙酸酯、酯醇-12(TEXANOL)、異佛爾酮、乳酸丁酯、鄰苯二甲酸二辛酯、己二酸二辛酯、苄醇、苯基丙二醇、甲酚、N,N-二甲基甲醯胺、碳酸丙烯酯等。其中，就沸點適度高，燒結時易於均勻揮發之觀點而言，較佳為N-甲基-2-吡咯啶酮、松油醇、松油醇乙酸酯、乙基卡必醇乙酸酯、丁基卡必醇乙酸酯、酯醇-12(TEXANOL)、及碳酸丙烯酯。再者，該等有機溶劑可單獨使用，亦可併用2種以上。
無機微粒子分散漿料組合物中之溶劑之含量相對於無機微粒子100質量份，就無機微粒子之分散性之觀點而言，較佳為0.001質量份以上，更佳為0.01質量份以上，進而較佳為0.1質量份以上，就調整無機微粒子分散漿料組合物之黏度之觀點而言，較佳為100質量份以
下，更佳為80質量份以下，進而較佳為50質量份以下。
本發明之無機微粒子分散漿料組合物亦可視需要含有添加劑。
作為添加劑，可列舉密接促進劑、界面活性劑、塑化劑、保存穩定劑、消泡劑等。
作為密接促進劑，可列舉胺系矽烷偶合劑、縮水甘油基系矽烷偶合劑等。作為界面活性劑，可列舉聚氧乙烯系界面活性劑、脂肪酸酯系界面活性劑等。作為塑化劑，可列舉聚醚多元醇、鄰苯二甲酸酯等。作為保存穩定劑，可列舉胺化合物、羧酸化合物、磷化合物、硫化合物、三唑系化合物等。作為消泡劑，可列舉疏水性二氧化矽、聚伸烷基衍生物、聚醚衍生物等。
無機微粒子分散漿料組合物中之添加劑之含量相對於無機微粒子100質量份，較佳為50質量份以下，更佳為30質量份以下。
作為本發明之無機微粒子分散漿料組合物之製造方法並無特別限定，可列舉使用先前公知之攪拌方法將脂肪族聚碳酸酯樹脂、溶劑、無機微粒子、及視需要之添加劑進行混合、攪拌之方法等。
作為上述公知之攪拌方法，例如可列舉使用球磨機、布拉本德密煉機、三輥研磨機等裝置進行混練之方法，使用研缽進行混練之方法等。
以下，藉由實施例具體地說明本發明，但本發明不受該等實施例之任何限定。脂肪族聚碳酸酯樹脂之物性係藉由以下之方法進行測定。
[脂肪族聚碳酸酯樹脂之質量平均分子量(Mw)及分子量分佈(Mw/Mn)]
使用凝膠滲透層析儀(日本Waters製造、Waters 2695Separation Module)，於30mmol/L之N,N-二甲基甲醯胺溴化鋰溶液中以40℃進行
測定，以標準聚苯乙烯為基準，算出質量平均分子量(Mw)及數量平均分子量(Mn)，求出分子量分佈(Mw/Mn)。
觸媒製造例1[有機鋅觸媒之製造]
向具備攪拌機、氮氣導入管、溫度計、迪安-斯塔克管、及回流冷卻管之1L容積之四口燒瓶中添加氧化鋅77.3g(0.95mol)、戊二酸123g(1mol)、乙酸1.14g(0.02mol)及甲苯760g。其次，一面以50mL/min之流量向反應系統內通入氮氣，一面升溫至55℃並於該溫度下攪拌4小時而使其進行反應。其後，升溫至110℃，進而於該溫度下攪拌2小時而使其進行共沸脫水，去除水分後冷卻至室溫，獲得包含有機鋅觸媒之漿料液。
樹脂製造例1[琥珀酸酐封端聚碳酸丙烯酯之製造]
將具備攪拌機、氣體導入管、及溫度計之1L容積之高壓釜之系統內預先置換為氮氣環境後，添加藉由觸媒製造例1所獲得之包含有機鋅觸媒之漿料液117.3g(包含135mmol之有機鋅觸媒)、碳酸二甲酯577.2g、及環氧丙烷78.3g(1.35mol)。其次，於攪拌下添加二氧化碳，填充二氧化碳直至反應系統內成為1MPa。其後，升溫至60℃，一面補給因反應而消耗之二氧化碳一面進行8小時聚合反應。二氧化碳之消耗量為1.17mol。反應結束後，冷卻高壓釜並進行釋壓，此時添加琥珀酸酐0.7g(相對於假設全部單體已反應之情形之樹脂100質量份為0.5質量份)，於40℃下攪拌1小時。過濾反應溶液後，進行減壓乾燥，而獲得利用琥珀酸酐將末端以羧基進行封端之聚碳酸丙烯酯樹脂(A)120g。所獲得之聚碳酸丙烯酯之質量平均分子量(Mw)為236,000，分子量分佈(Mw/Mn)為10.0。
樹脂製造例2[末端未封端之聚碳酸丙烯酯之製造]
反應結束後，冷卻高壓釜並進行釋壓，然後不添加琥珀酸酐，過濾反應溶液，進行減壓乾燥，除此以外，以與樹脂製造例1相同之
方式獲得聚碳酸丙烯酯樹脂(B)123g。所獲得之聚碳酸丙烯酯之質量平均分子量為315,000，分子量分佈(Mw/Mn)為9.74。
樹脂製造例3[異氰酸酯封端聚碳酸丙烯酯之製造]
將聚碳酸丙烯酯樹脂(B)40g與4,4'-二苯基甲烷二異氰酸酯0.4g投入混練機(東洋精機製作所製造、Laboplastomill 4C150)中，以混練溫度160℃、轉數40r/min熔融混練5分鐘，而獲得末端由異氰酸酯基封端之聚碳酸丙烯酯樹脂(C)。所獲得之聚碳酸丙烯酯之質量平均分子量為323,000，分子量分佈(Mw/Mn)為8.82。
樹脂製造例4[琥珀酸酐封端聚碳酸乙烯酯之製造]
將聚碳酸乙烯酯樹脂(D)(Empowermaterials公司製造、商品名QPAC25、Mw：198,000、Mw/Mn：3.48)40g與琥珀酸酐0.3g投入混練機(東洋精機製作所製造、Laboplastomill 4C150)中，以混練溫度100℃、轉數40r/min熔融混練5分鐘，而獲得利用琥珀酸酐將末端以羧基進行封端之聚碳酸乙烯酯樹脂(E)。所獲得之聚碳酸乙烯酯之質量平均分子量為197,000，分子量分佈(Mw/Mn)為3.49。
樹脂製造例5[末端未封端之聚碳酸丁烯酯之製造]
將具備攪拌機、氣體導入管、及溫度計之1L容積之高壓釜之系統內預先置換為氮氣環境後，添加藉由觸媒製造例1所獲得之包含有機鋅觸媒之漿料液117.3g(包含135mmol之有機鋅觸媒)、碳酸二甲酯577.2g、及1,2-環氧丁烷97.3g(1.35mol)。其次，於攪拌下添加二氧化碳，填充二氧化碳直至反應系統內成為1MPa。其後，升溫至60℃，一面補給因反應而消耗之二氧化碳一面進行8小時聚合反應。二氧化碳之消耗量為1.02mol。反應結束後，冷卻高壓釜並進行釋壓，過濾後進行減壓乾燥而獲得聚碳酸丁烯酯樹脂(F)118g。所獲得之聚碳酸丁烯酯之質量平均分子量為273,000，分子量分佈(Mw/Mn)為12.2。
樹脂製造例6[乙酸酐封端聚碳酸丁烯酯之製造]
使樹脂製造例5中所獲得之聚碳酸丁烯酯樹脂(F)11.6g(100mmol)溶解於二氯甲烷120g中，並添加乙酸酐0.51g(5.0mmol)、三乙胺0.3g(3.25mmol)及4,4-二甲基胺基吡啶0.2g(1.63mmol)，於25℃下攪拌24小時。去除揮發分，將殘留物注入甲醇200mL中，並將析出之白色聚合物加以乾燥，藉此獲得利用乙酸酐將末端以酯基進行封端之聚碳酸丁烯酯樹脂(G)。所獲得之聚碳酸丁烯酯之質量平均分子量為290,000，分子量分佈(Mw/Mn)為10.4。
實施例1
於50mL體積玻璃小瓶中稱取樹脂製造例1中所獲得之聚碳酸丙烯酯樹脂(A)0.2g與樹脂製造例2中所獲得之聚碳酸丙烯酯樹脂(B)0.8g，並使其溶解於丙酮10g中，而製備均勻之溶液。將該溶液加以乾燥而獲得黏結劑樹脂組合物1.0g。所獲得之黏結劑樹脂組合物之熱分解開始溫度為215.5℃，50質量%分解溫度為217.2℃。
實施例2~5
以表1所記載之比率使用聚碳酸丙烯酯樹脂(A)與聚碳酸丙烯酯樹脂(B)，除此以外，以與實施例1相同之方式而獲得黏結劑樹脂組合物1.0g。
參考例1、2
使聚碳酸丙烯酯樹脂(A)或聚碳酸丙烯酯樹脂(B)1.0g溶解於丙酮10g中，而製備均勻之溶液。將該溶液加以乾燥而獲得黏結劑樹脂組合物1.0g。
藉由下述之方法測定各實施例、參考例中所獲得之黏結劑樹脂組合物之熱分解溫度(Td)及50質量%分解溫度(Td50)。將結果示於表1。
[黏結劑樹脂組合物之熱分解溫度(Td)及50質量%分解溫度(Td50)]
使用精工電子奈米科技公司製造之TG/DTA7220，一面於氮氣環境下以10℃/min之升溫速度自室溫升溫至500℃，一面測定熱重量之變化。熱分解開始溫度(Td)係設為和通過試驗加熱開始前之質量之橫軸平行之線與以分解曲線之臨界點間之斜率成為最大之方式引出之切線之交點。50質量%分解溫度(Td50)係讀取樣品之熱重量變為試驗加熱開始前之質量之一半(50%)時之溫度。
將實施例1~5及參考例1、2中所獲得之樹脂組合物之熱分解曲線示於圖1。又，將表示實施例1~5及參考例1、2中所獲得之樹脂組合物之組成比與熱分解開始溫度(Td)之關係之圖表示於圖2，將表示樹脂組合物之組成比與50質量%分解溫度(Td50)之關係之圖表示於圖3。再者，表1所記載之確定係數R2係自1減去藉由最小平方法進行圖1及圖2之圖表之線性近似時之殘差方差與合計方差之比而獲得者，顯示出越接近1而與近似曲線之一致性越佳。
實施例6~8
以表2所記載之比率使用聚碳酸丙烯酯樹脂(B)與聚碳酸丙烯酯樹脂(C)，除此以外，以與實施例1相同之方式而獲得黏結劑樹脂組合物
1.0g。
參考例3
使聚碳酸丙烯酯樹脂(C)1.0g溶解於丙酮10g中，而製備均勻之溶液。將該溶液加以乾燥而獲得黏結劑樹脂組合物1.0g。
實施例9~11
以表3所記載之比率使用聚碳酸乙烯酯樹脂(D)與聚碳酸乙烯酯樹脂(E)，除此以外，以與實施例1相同之方式而獲得黏結劑樹脂組合物1.0g。
參考例4、5
使聚碳酸乙烯酯樹脂(D)或聚碳酸乙烯酯樹脂(E)1.0g溶解於丙酮10g中，而製備均勻之溶液。將該溶液加以乾燥而獲得黏結劑樹脂組合物1.0g。
實施例12~14
以表4所記載之比率使用聚碳酸丁烯酯樹脂(F)與聚碳酸丁烯酯樹脂(G)，除此以外，以與實施例1相同之方式而獲得黏結劑樹脂組合物1.0g。
參考例6、7
使聚碳酸丁烯酯樹脂(F)或聚碳酸丁烯酯樹脂(G)1.0g溶解於丙酮10g中，而製備均勻之溶液。將該溶液加以乾燥而獲得黏結劑樹脂組合物1.0g。
藉由上述方法測定實施例6~14及參考例3~7中所獲得之黏結劑樹脂組合物之熱分解溫度(Td)及50質量%分解溫度(Td50)，而求出確定係數R2。將結果示於表2~4。
根據以上之結果可知，本發明之黏結劑樹脂組合物具有2種樹脂之混合比與熱分解溫度之關係接近1之確定係數，藉由調整混合比能夠於混合前之各樹脂之分解溫度之範圍內任意調整。
實施例15
無機微粒子分散漿料之製造例
於10mL體積之玻璃小瓶中稱取實施例1中所獲得之黏結劑樹脂組合物0.12g，並使其溶解於N-甲基-2-吡咯啶酮0.88g中，而製備均勻之溶液。於研缽中稱取銀粒子4.0g，一面添加所製備之溶液，一面混練20分鐘直至潤滑，而獲得銀粒子分散漿料5.0g。
實施例16
於10mL體積之玻璃小瓶中稱取實施例1中所獲得之黏結劑樹脂組合物0.12g，並使其溶解於N-甲基-2-吡咯啶酮0.88g中，而製備均勻之溶液。使該溶液全部量與氧化鋁粒子4.0g混合，使用自轉公轉攪拌機進行混練使其漿料化後，進而使用三輥研磨機進行混練，而獲得氧化鋁分散漿料5.0g。
本發明之黏結劑樹脂組合物可用於一般成形物、膜、纖維、光
纖、光碟等光學材料、陶瓷黏結劑、消失模鑄造等之熱分解性材料、藥劑膠囊等醫用材料、生物可降解樹脂之添加劑、生物可降解樹脂之主成分等。
Claims (4)
- 一種黏結劑樹脂組合物，其包含式(1)所表示之脂肪族聚碳酸酯樹脂與式(2)所表示之末端封端脂肪族聚碳酸酯樹脂，
- 如請求項1之黏結劑樹脂組合物，其中於式(2)中，X及Y為於末端具有選自羧基、酯基、胺基甲酸酯基及異氰酸酯基中之至少1種官能基之基。
- 如請求項1或2之黏結劑樹脂組合物，其中式(1)所表示之脂肪族聚碳酸酯樹脂及/或式(2)所表示之脂肪族聚碳酸酯樹脂為選自由聚碳酸乙烯酯、聚碳酸丙烯酯及聚碳酸丁烯酯所組成之群中之至少1種。
- 一種無機微粒子分散漿料組合物，其含有如請求項1至3中任一項之黏結劑樹脂組合物、無機微粒子、及溶劑。
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