CN114729145B - Release film and preparation method thereof - Google Patents
Release film and preparation method thereof Download PDFInfo
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- CN114729145B CN114729145B CN202180002509.8A CN202180002509A CN114729145B CN 114729145 B CN114729145 B CN 114729145B CN 202180002509 A CN202180002509 A CN 202180002509A CN 114729145 B CN114729145 B CN 114729145B
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- release film
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- 238000002360 preparation method Methods 0.000 title abstract description 25
- -1 fluorosilane compound Chemical class 0.000 claims abstract description 79
- 239000011242 organic-inorganic particle Substances 0.000 claims abstract description 62
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims description 53
- 239000010954 inorganic particle Substances 0.000 claims description 44
- 229920001296 polysiloxane Polymers 0.000 claims description 38
- 150000001875 compounds Chemical class 0.000 claims description 34
- 229910052731 fluorine Inorganic materials 0.000 claims description 34
- 239000011737 fluorine Substances 0.000 claims description 31
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 24
- 239000000758 substrate Substances 0.000 claims description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 229920001577 copolymer Polymers 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 13
- 229920000642 polymer Polymers 0.000 claims description 12
- 229910000077 silane Inorganic materials 0.000 claims description 11
- 125000001153 fluoro group Chemical group F* 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 125000006374 C2-C10 alkenyl group Chemical group 0.000 claims description 9
- 125000004429 atom Chemical group 0.000 claims description 9
- 125000003860 C1-C20 alkoxy group Chemical group 0.000 claims description 7
- 238000002329 infrared spectrum Methods 0.000 claims description 6
- 229920001774 Perfluoroether Polymers 0.000 claims description 5
- 239000003377 acid catalyst Substances 0.000 claims description 5
- 125000003342 alkenyl group Chemical group 0.000 claims description 5
- 125000003709 fluoroalkyl group Chemical group 0.000 claims description 5
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 125000003837 (C1-C20) alkyl group Chemical group 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 150000001242 acetic acid derivatives Chemical class 0.000 claims description 3
- 150000001642 boronic acid derivatives Chemical class 0.000 claims description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 3
- 150000004820 halides Chemical class 0.000 claims description 3
- 150000004677 hydrates Chemical class 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 150000004679 hydroxides Chemical class 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 235000021317 phosphate Nutrition 0.000 claims description 3
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 claims description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 3
- 150000004760 silicates Chemical class 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 3
- 150000003568 thioethers Chemical class 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 2
- 239000010408 film Substances 0.000 description 83
- 239000010410 layer Substances 0.000 description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 50
- 239000000377 silicon dioxide Substances 0.000 description 25
- 239000002245 particle Substances 0.000 description 20
- 229920005989 resin Polymers 0.000 description 15
- 239000011347 resin Substances 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 229920000728 polyester Polymers 0.000 description 13
- 239000002904 solvent Substances 0.000 description 12
- 125000000217 alkyl group Chemical group 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 125000004432 carbon atom Chemical group C* 0.000 description 8
- 239000002390 adhesive tape Substances 0.000 description 7
- 150000002430 hydrocarbons Chemical group 0.000 description 7
- 239000000376 reactant Substances 0.000 description 7
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 6
- 125000000524 functional group Chemical group 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
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- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
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- 125000003545 alkoxy group Chemical group 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 3
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
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- 125000003118 aryl group Chemical group 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 229920006267 polyester film Polymers 0.000 description 3
- 239000004645 polyester resin Substances 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- OJVAMHKKJGICOG-UHFFFAOYSA-N 2,5-hexanedione Chemical compound CC(=O)CCC(C)=O OJVAMHKKJGICOG-UHFFFAOYSA-N 0.000 description 2
- QQZOPKMRPOGIEB-UHFFFAOYSA-N 2-Oxohexane Chemical compound CCCCC(C)=O QQZOPKMRPOGIEB-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 2
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 2
- 125000004491 isohexyl group Chemical group C(CCC(C)C)* 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 2
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-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
- 230000000704 physical effect Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 2
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- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GETTZEONDQJALK-UHFFFAOYSA-N (trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=CC=C1 GETTZEONDQJALK-UHFFFAOYSA-N 0.000 description 1
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 1
- XXZOEDQFGXTEAD-UHFFFAOYSA-N 1,2-bis(trifluoromethyl)benzene Chemical group FC(F)(F)C1=CC=CC=C1C(F)(F)F XXZOEDQFGXTEAD-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- DFUYAWQUODQGFF-UHFFFAOYSA-N 1-ethoxy-1,1,2,2,3,3,4,4,4-nonafluorobutane Chemical compound CCOC(F)(F)C(F)(F)C(F)(F)C(F)(F)F DFUYAWQUODQGFF-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
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- 125000000094 2-phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- FNUBKINEQIEODM-UHFFFAOYSA-N 3,3,4,4,5,5,5-heptafluoropentanal Chemical compound FC(F)(F)C(F)(F)C(F)(F)CC=O FNUBKINEQIEODM-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
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- RGMZNZABJYWAEC-UHFFFAOYSA-N Methyltris(trimethylsiloxy)silane Chemical compound C[Si](C)(C)O[Si](C)(O[Si](C)(C)C)O[Si](C)(C)C RGMZNZABJYWAEC-UHFFFAOYSA-N 0.000 description 1
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- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
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- QHIWVLPBUQWDMQ-UHFFFAOYSA-N butyl prop-2-enoate;methyl 2-methylprop-2-enoate;prop-2-enoic acid Chemical compound OC(=O)C=C.COC(=O)C(C)=C.CCCCOC(=O)C=C QHIWVLPBUQWDMQ-UHFFFAOYSA-N 0.000 description 1
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- 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
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- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 1
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- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 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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- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- VNRWTCZXQWOWIG-UHFFFAOYSA-N tetrakis(trimethylsilyl) silicate Chemical compound C[Si](C)(C)O[Si](O[Si](C)(C)C)(O[Si](C)(C)C)O[Si](C)(C)C VNRWTCZXQWOWIG-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
- C08K5/5445—Silicon-containing compounds containing nitrogen containing at least one Si-N bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
- C09J7/401—Adhesives in the form of films or foils characterised by release liners characterised by the release coating composition
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to a release film and a preparation method thereof. In the release film, a base material and a release layer are sequentially positioned, the surface energy of the release layer is 24dyne/cm or less, the release layer includes organic-inorganic particles in which a portion (mole) including a fluorosilane compound is introduced onto the surface thereof, the organic-inorganic particles can satisfy the content ratio (M) of F/Si elements represented by the following formula 1 F /M Si ) The range is as follows: [ 1 ] M is 0.1.ltoreq.M F /M Si In the formula, M is less than or equal to 1.0 F Content of F element (atomic%) M Si The content of Si element (at%).
Description
Technical Field
The invention relates to a release film and a preparation method thereof.
Background
Generally, a silicone-based adhesive (hereinafter, this is meant to include a pressure-sensitive adhesive) has characteristics of heat resistance, weather resistance, flexibility, chemical resistance, and the like, and recently, IT is widely used not only for general industrial tapes but also for IT fields of mobile phones, semiconductors, displays, and the like.
However, since the silicone release film using the silicone adhesive is completely laminated to the adhesive and is not peeled off, a film coated with a release agent of a fluorine-containing resin is generally used. After curing, the release agent containing the fluorine-based resin is extremely prone to interlayer curing due to the residual curing agent, and the peeling force and residual adhesion rate are liable to be lowered.
In order to solve these problems, there is still a need for a release film excellent in light peelability, residual adhesion and coating appearance, and a method for preparing the same.
Disclosure of Invention
Technical problem
In one aspect, the present invention provides a release film having excellent light peelability, residual adhesion and coating appearance.
The invention further provides a preparation method of the release film.
Technical proposal
In one aspect, the present invention provides a release film, wherein,
the base material and the release layer are positioned in sequence,
the surface energy of the release layer is below 24dyne/cm,
the release layer comprises organic-inorganic particles,
in the organic-inorganic particles, a moiety (mole) including a fluorosilane compound is introduced onto the surface thereof,
the organic-inorganic particles can satisfy the content ratio (M) of F/Si element represented by the following formula 1 F /M Si ) The range is as follows:
[ 1 ]
0.1≤M F /M Si ≤1.0
In the formula (I), the compound (II) is a compound (III),
M F can be the content (atomic%) of the F element, M Si The content (atomic%) of Si element may be set.
The fluorosilane compound moiety may include a fluorosilane compound represented by the following chemical formula 1.
[ chemical formula 1 ]
*-OSi(R a )(R b )(R c )
In the formula (I), the compound (II) is a compound (III),
R a and R is b C1-C20 alkoxy which may be substituted or unsubstituted;
R c as can be seen from the following chemical formula 2,
* May be a binding site to the surface of the organic-inorganic particles.
[ chemical formula 2 ]
In the formula (I), the compound (II) is a compound (III),
R d may be a hydrogen atom or a substituted or unsubstituted C1-C20 alkyl group;
R a and R is b C1-C20 alkoxy which may be substituted or unsubstituted;
R f may be a C4-C20 alkyl group substituted with fluorine;
n 1 may be an integer of 1 to 10;
* May be a binding site to a Si atom.
The weight ratio of the organic-inorganic particles to the fluorosilane compound may be 1:1 to 20:1.
at the distance ofIn the layer, 1064cm of infrared spectrum is compared with the organic-inorganic particles whose surface does not include the part of the fluorine-containing silane compound -1 To 1066cm -1 Peaks in the wavenumber range may be shifted to the right.
The organic-inorganic particles may include natural minerals; oxides, hydroxides, sulfides, nitrides or halides of group 1 to group 4, group 11 to group 12, group 14 and group 16 to group 18 elements; carbonates, sulphates, acetates, phosphates, phosphites, carboxylates, silicates, titanates, borates or hydrates thereof; and inorganic particles selected from its complex compounds.
The release layer may further comprise a polymer or copolymer comprising a fluorine-containing polysiloxane.
The fluorine-containing polysiloxane may include an organopolysiloxane represented by the following chemical formula 3.
< chemical formula 3>
< chemical formula 4>
< chemical formula 5>
In the formula (I), the compound (II) is a compound (III),
R 1 may be a substituted or unsubstituted C1-C10 monovalent hydrocarbon group, or a substituted or unsubstituted C2-C10 alkenyl group;
R 2 may be a substituted or unsubstituted C1-C10 monovalent hydrocarbon group, a substituted or unsubstituted C2-C10 alkenyl group, or hydrogen;
R 3 can be a fluoroalkyl group represented by the chemical formula 4 and a fluoroalkyl group represented by the chemical formula 5A fluoroether group, or a combination thereof;
n may be an integer from 1 to 8, and m may be an integer from 1 to 5;
p may be an integer from 1 to 5, q may be 0 or 1, r may be 0, 1 or 2, and v may be an integer from 1 to 5;
a can be an oxygen atom or a single bond;
x, y and z may each be an integer of 1 or more;
* May be a binding site to an adjacent atom;
wherein R is 1 And R is 2 At least one of them may be a substituted or unsubstituted C2-C10 alkenyl group.
The release layer may further include at least one of a hydrogen polysiloxane (hydrogen polysiloxane) and an acid catalyst.
The release film may have a peel force of 23gf/25mm or less.
The release film may have a residual adhesion rate of 90% or more.
In another aspect, the present invention provides a method for preparing a release film, comprising:
preparing a base material;
adding and stirring the inorganic particles, the fluorosilane compound and the aminosilane-based coreactant, and then heating to prepare organic-inorganic particles; and
a composition for forming a release layer comprising a polymer or copolymer comprising a fluorine-containing polysiloxane, and organic-inorganic particles is coated on at least one side of the substrate and dried to form a release layer to prepare the above release film,
the weight ratio of the inorganic particles to the fluorine-containing silane compound is 4:1 to 20:1.
the heating may be performed at 60 ℃ or higher under an air atmosphere.
The weight ratio of the inorganic particles to the fluorosilane compound may be 1:1 to 20:1.
advantageous effects
In the release film according to one aspect, the surface energy of the release layer is 24dyne/cm or less, and the release layer comprisesComprises organic-inorganic particles in which a portion (mole) including a fluorosilane compound is introduced onto the surface thereof, the organic-inorganic particles being capable of satisfying the content ratio (M) of F/Si elements represented by the formula 1 F /M Si ) Range. The release film can provide a release film excellent in light peelability, residual adhesion and coating appearance.
Drawings
Fig. 1 is a cross-sectional view of a release film according to an embodiment of the present invention.
Fig. 2 is an infrared spectrum result of three kinds of silica inorganic particles, wherein the first kind of silica inorganic particles is a starting material of the release film prepared according to example 1, the second kind of silica inorganic particles is an intermediate reactant for introducing aminosilane at the surface, and the third kind of silica inorganic particles is a final result of introducing aminosilane and a fluorine-containing silane compound at the surface.
Detailed Description
The release film and the method of preparing the same will be described in detail below with reference to examples of the present invention and the accompanying drawings. It will be understood by those of ordinary skill in the art that these embodiments are given by way of example only to more specifically describe the present invention, and that the scope of the present invention is not limited by these embodiments.
Unless defined otherwise, all technical and scientific terms used in this specification have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
All methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, with suitable methods and materials being described herein.
In this specification, unless stated to the contrary, the term "comprising" means that other components may be further included without excluding other components.
In this specification, the term "combination thereof" refers to a mixture or combination with at least one of the described components.
In this specification, the term "and/or" is intended to include any and all combinations of one or more of the items associated with the description thereof. In this specification, the term "or" means "and/or". In this specification, the expression "at least one" or "more than one" preceding an element means that a list of all elements can be supplemented but does not mean that the individual elements of the description can be supplemented.
In this specification, when an element is referred to as being disposed "on" or "over" another element, it can be directly on the other element or intervening elements may be present. On the other hand, when referring to an element as being "directly on" or "directly over" another element, there may be no intervening elements present.
In the present specification, "-system resin", "-system polymer" or/and "," -system copolymer "is a broad concept including", "-resin", "-polymer", "-copolymer" or/and "," -resin, polymer or derivative of copolymer ".
In the present specification, the term "polymer or copolymer crosslinked with a resin thereof" means "polymer or copolymer crosslinked with the above-mentioned resin".
In the present specification, "aminosilane-based coreactant" is a broad concept including "aminosilane-based coreactant" or "coreactant comprising aminosilane".
According to an embodiment of the present invention, a release film, a substrate and a release layer are sequentially positioned, the release layer having a surface energy of 24dyne/cm or less, the release layer comprising organic-inorganic particles in which a portion (mole) including a fluorosilane compound is introduced onto the surface thereof, the organic-inorganic particles being capable of satisfying a content ratio (M) of F/Si element represented by the following formula 1 F /M Si ) The range is as follows:
[ 1 ]
0.1≤M F /M Si ≤1.0
In the formula (I), the compound (II) is a compound (III),
M F for the content of F element (originalSub%) M Si The content of Si element (at%).
The release film according to an embodiment of the present invention has blocking resistance, and can provide a release film excellent in light peelability, residual adhesion rate, and coating appearance.
The substrate constituting the release film, the release layer, the release film, and the method of preparing the same will be described in detail below.
< substrate >
As the substrate used in the present invention, a known substrate film or substrate sheet can be used as the substrate of the release film. For example, a polyester resin film can be used as the base material. As the polyester resin, a known base film commonly used in the field of release films can be used. For example, as the polyester-based resin base film, polyester-based base films disclosed in korean registered patent nos. 10-1268584, 2012-45213, 2012-99546, and the like can be used. However, in an embodiment of the present invention, in order to describe only the features of the present invention, description of the polyester-based substrate film is not limited, but should be understood to include technical features related to known polyester-based substrate films.
The polyester base film may include polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, or the like.
As the polyester-based resin forming the base film, a polyester obtained by polycondensing an aromatic dicarboxylic acid or an aliphatic dicarboxylic acid with an aliphatic diol may be used, and among them, isophthalic acid, phthalic acid, terephthalic acid, 2, 6-naphthalenedicarboxylic acid, adipic acid, sebacic acid, hydroxycarboxylic acid (for example, ρ -oxybenzoic acid or 4-oxybenzoic acid) and the like may be used, and as the aliphatic diol, ethylene glycol, diethylene glycol, propylene glycol, butanediol, 1, 4-cyclohexanedimethanol, neopentyl glycol and the like may be used. As such a polyester resin, two or more of the dicarboxylic acid component and the diol component may be used in combination, or a copolymer including a third component may be used.
Further, as the polyester base film, a uniaxially or biaxially oriented film having high transparency and excellent productivity and processability can be used. As the polyester base film, polyethylene terephthalate (PET), poly (vinyl 2, 6-naphthalate) (PEN), or the like can be used.
In addition, the polyester-based substrate film may include particles to provide excellent inter-Roll running characteristics, and may be used without limitation as long as the added particles can exhibit excellent sliding characteristics.
Examples of such particles may include particles of silica, calcium carbonate, calcium sulfate, calcium phosphate, magnesium carbonate, magnesium phosphate, barium carbonate, kaolin, alumina, titanium oxide, and the like, and the shape of the particles used is not limited, but any of spherical, bulk, rod-like, and plate-like particles may be used, for example.
In addition, although the hardness, specific gravity and color of the particles are not limited, two or more kinds may be used in parallel as required, and the average particle diameter of the particles used may be 0.1 to 5 μm, for example, particles in the range of 0.1 to 2 μm may be used. At this time, when the average particle diameter of the particles is less than 0.1 μm, an aggregation phenomenon between the particles may occur, resulting in poor dispersion, and when the average particle diameter of the particles is more than 5 μm, coating defects may occur during post-treatment because the surface roughness characteristics of the thin film are deteriorated.
Further, when the polyester-based substrate film includes particles, the content of the particles may be 0.01 to 5 wt%, for example, 0.01 to 3 wt%, based on the total weight of the polyester-based substrate film. When the content of the particles is less than 0.01 wt%, the sliding property of the polyester film may be deteriorated, resulting in deterioration of the running property between the rolls, and when the content of the particles is more than 5 wt%, the surface smoothness of the film may be deteriorated.
The thickness of the polyester base film is not limited, but may be 30 μm to 125 μm.
When the polyester-based substrate is too thin to 30 μm or less, heat treatment during processing may cause deformation, and when the polyester-based substrate is too thick to 125 μm or more, curing may be problematic due to insufficient heat transfer.
< Release layer >
The release layer of the release film according to an embodiment of the present invention may have a surface energy of 24dyne/cm or less. Due to such low surface energy, the release film can achieve light peelability with low peeling force.
The release layer includes organic-inorganic particles, a portion (mole) including a fluorine-containing silane compound is introduced onto the surface of the organic-inorganic particles, and the organic-inorganic particles may satisfy a content ratio (M) of F/Si element represented by the following chemical formula 1 F /M Si ) The range is as follows:
[ 1 ]
0.1≤M F /M Si ≤1.0
In the formula (I), the compound (II) is a compound (III),
M F can be the content (atomic%) of the F element, M Si The content (atomic%) of Si element may be set.
The organic-inorganic particles can prevent blocking. The organic-inorganic particles include a fluorosilane compound on the surface thereof and satisfy the F/Si element content ratio (M) F /M Si ) The range, thereby not only improving light peelability but also improving residual adhesion and coating appearance.
The fluorosilane compound moiety may include a fluorosilane compound represented by the following chemical formula 1.
[ chemical formula 1 ]
*-OSi(R a )(R b )(R c )
In the formula (I), the compound (II) is a compound (III),
R a and R is b C1-C20 alkoxy which may be substituted or unsubstituted;
R c as can be seen from the following chemical formula 2,
* May be a binding site to the surface of the organic-inorganic particles.
[ chemical formula 2 ]
In the formula (I), the compound (II) is a compound (III),
R d may be a hydrogen atom or a substituted or unsubstituted C1-C20 alkyl group;
R a and R is b C1-C20 alkoxy which may be substituted or unsubstituted;
R f may be a C4-C20 alkyl group substituted with fluorine;
n 1 may be an integer of 1 to 10;
* May be a binding site to a Si atom.
For example, in the chemical formula 1 and chemical formula 2, R a 、R b 、R e And R is g May be, independently of one another, a substituted or unsubstituted C1-C20 alkoxy group, a substituted or unsubstituted C1-C5 alkoxy group, or an unsubstituted C1-C5 alkoxy group.
For example, in the chemical formula 2, n 1 May be an integer of 1 to 10, or an integer of 1 to 5.
For example, in the chemical formula 2, R f Can be a C4-C20 alkyl group substituted with fluorine, a C4-C15 alkyl group substituted with fluorine or a C4-C10 alkyl group substituted with fluorine. When R in the chemical formula 2 f In the case of having the alkyl group of the carbon number substituted with fluorine, the peeling force can be reduced to achieve excellent light peelability.
The weight ratio of the organic-inorganic particles to the fluorosilane compound may be 1:1 to 20:1. when the weight ratio of the organic-inorganic particles to the fluorosilane compound is within the range, the peeling force can be further reduced to achieve excellent light peelability.
In the release layer, 1064cm in the infrared spectrum is compared with the organic-inorganic particles whose surface does not include the part of the fluorine-containing silane compound -1 To 1066cm -1 Peaks in the wavenumber range may be shifted to the right.
The organic-inorganic particles may include natural minerals; oxides, hydroxides, sulfides, nitrides or halides of group 1 to group 4, group 11 to group 12, group 14 and group 16 to group 18 elements; carbonates, sulphates, acetates, phosphates, phosphites, carboxylates, silicates, titanates, borates or hydrates thereof; and inorganic particles selected from its complex compounds.
The organic-inorganic particles may include organic particles selected from the group consisting of fluorine-based resins, melamine-based resins, styrene-based resins, acrylic-based resins, silicone-based resins, styrene-divinylbenzene-based copolymer resins, and polymers or copolymers crosslinked with the resins thereof, as required.
The shape of the organic-inorganic particles used is not particularly limited, and may be spherical, block-shaped, rod-shaped, flat, or the like. In addition, the hardness, specific gravity, color, etc. of the organic-inorganic particles are not limited, and these organic-inorganic particles may be used alone or in combination of two or more kinds, if necessary.
The release layer may further comprise a polymer or copolymer comprising a fluorine-containing polysiloxane.
The fluorine-containing polysiloxane may include an organopolysiloxane represented by the following chemical formula 3.
< chemical formula 3>
< chemical formula 4>
< chemical formula 5>
In the formula (I), the compound (II) is a compound (III),
R 1 may be a substituted or unsubstituted C1-C10 monovalent hydrocarbon group, or a substituted or unsubstituted C2-C10 alkenyl group;
R 2 can be a substituted or unsubstituted C1-C10 monovalent hydrocarbon radical, a substituted or unsubstituted C2-C10 alkenyl radicalOr hydrogen;
R 3 may be a fluoroalkyl group represented by the chemical formula 4, a fluoroether group represented by the chemical formula 5, or a combination thereof;
n may be an integer from 1 to 8, and m may be an integer from 1 to 5;
p may be an integer from 1 to 5, q may be 0 or 1, r may be 0, 1 or 2, and v may be an integer from 1 to 5;
a can be an oxygen atom or a single bond;
x, y and z may each be an integer of 1 or more;
* May be a binding site to an adjacent atom;
wherein R is 1 And R is 2 At least one of them may be a substituted or unsubstituted C2-C10 alkenyl group.
The fluorine-containing polysiloxane may be a blend of the organopolysiloxane represented by the chemical formula 3 and the organopolysiloxane represented by the following chemical formula 6, or may be a copolymer obtained by linking the organopolysiloxane represented by the chemical formula 3 and the organopolysiloxane represented by the following chemical formula 6, according to need:
< chemical formula 6>
< chemical formula 7>
In the formula (I), the compound (II) is a compound (III),
R' 1 may be a substituted or unsubstituted C1-C10 monovalent hydrocarbon group, or a substituted or unsubstituted C2-C10 alkenyl group;
R' 2 may be a fluoroether group represented by the chemical formula 7;
n 'may be an integer of 1 to 8, and m' may be an integer of 3 to 17;
* May be a binding site to an adjacent atom.
For example, the weight ratio of the organopolysiloxane represented by the chemical formula 3 to the organopolysiloxane represented by the chemical formula 6 may be 10:1 to 1:10.
the release layer may further include at least one of a hydrogen polysiloxane (hydrogen polysiloxane) and an acid catalyst.
The hydrogen polysiloxane may include at least one of an addition reaction type siloxane resin, a condensation reaction type siloxane resin, and an ultraviolet curing type siloxane resin. The hydrogen polysiloxane may be one of linear, branched or cyclic, or may be in the form of a mixture thereof. The hydrogen polysiloxane is not limited in viscosity and molecular weight, but must have good compatibility with the above-mentioned organopolysiloxane, and may not include a fluorine group. However, the hydrogen polysiloxane may also include the same fluoroalkyl groups and/or fluoroether groups as the organopolysiloxane described above.
The hydrogen polysiloxane may be present in an amount of 1.0 to 10.0 wt% based on the total weight of the composition for forming the release layer.
As the acid catalyst, at least one metal or amphoteric element selected from group 4 to group 14 elements may be used, and for example, at least one selected from Rh, pt, sn, ti, pd, ir, W and Co may be used. For example, the acid catalyst may include a platinum chelate catalyst.
The release layer may further include additives for imparting various functions such as a reaction modifier, an antistatic agent, and the like, if necessary.
The thickness of the release layer may be 0.03 to 3.0 μm. When the thickness of the release layer is less than 0.01um, the coverage of the release layer is poor, and when the thickness of the release layer is more than 3um, thermal deformation of the substrate film may be caused due to a large amount of heat required during curing.
< Release film >
Fig. 1 is a cross-sectional view of a release film 100 according to an embodiment of the present invention.
Referring to fig. 1, a release film 120 according to an embodiment of the present invention has a structure in which a substrate 100 and a release layer 110 are sequentially positioned.
The release film 120 according to an embodiment of the present invention can provide a release film excellent in light peelability, residual adhesion rate, and coating appearance.
The release film may have a peel force of 23gf/25mm or less.
The release film may have a residual adhesion rate of 90% or more.
When the residual adhesion rate of the release film is less than 90%, the release agent is transferred to the adhesive layer due to insufficient curing of the release layer, thereby causing a problem that the adhesion of the adhesive is deteriorated.
< preparation method of Release film >
The preparation method of the release film according to the embodiment of the invention comprises the following steps: preparing a base material; adding and stirring the inorganic particles, the fluorosilane compound and the aminosilane-based coreactant, and then heating to prepare organic-inorganic particles; and coating a composition for forming a release layer including a polymer or copolymer including a fluorine-containing polysiloxane, and organic-inorganic particles on at least one side of the substrate and drying to form a release layer to prepare the release film, wherein the weight ratio of the inorganic particles to the fluorine-containing silane compound may be 4:1 to 20:1.
the release film prepared by the preparation method of the release film according to an embodiment of the present invention can provide a release film excellent in light peelability, residual adhesion rate and coating appearance.
In this case, as the solvent used in the composition for forming a release layer, a solvent used is not limited as long as the solid content in the composition for forming a release layer can be dispersed and coated on the substrate. When the total solid content of the composition for forming a release layer is less than 0.5 wt%, a uniform release layer cannot be formed, so that problems such as poor peeling between the silicone-based adhesive layer and the release film may occur, and when the total solid content of the composition for forming a release layer is more than 10 wt%, the high viscosity of the composition for forming a release layer may cause uneven leveling, so that thickness uniformity of the release layer may be deteriorated.
As the solvent used in the composition for forming a release layer, an aromatic hydrocarbon-based solvent such as toluene, xylene, or the like can be used; aliphatic hydrocarbon solvents such as hexane, heptane, n-octane, isooctane, decane, cyclohexane, methylcyclohexane, isoparaffin and the like; hydrocarbon solvents such as industrial gasoline (rubber gasoline, etc.), petroleum benzene, solvent oil, etc.; ketone solvents such as acetone, methyl ethyl ketone, 2-pentanone, 3-pentanone, 2-hexanone, 2-heptanone, 4-heptanone, methyl isobutyl ketone, diisobutyl ketone, acetonylacetone, cyclohexanone, and the like; ester solvents such as ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate, and the like; ether solvents such as diethyl ether, dipropyl ether, diisopropyl ether, dibutyl ether, 1, 2-dimethoxyethane, 1, 4-dioxane, etc.; solvents having ester and ether moieties such as ethyl 2-methoxyacetate, ethyl 2-ethoxyacetate, propylene glycol monomethyl ether acetate, and ethyl 2-butoxyacetate, and the like; siloxane solvents such as hexamethyldisiloxane, octamethyltrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, tris (trimethylsiloxy) methylsilane, tetrakis (trimethylsiloxy) silane, and the like; fluorine-based solvents such as benzotrifluoride, hexafluoroxylene, methyl nonafluorobutyl ether, ethyl nonafluorobutyl ether, and the like; or a mixed solvent thereof, and the like. For example, as the solvent used in the composition for forming a release layer, a mixed solvent of heptane and methyl isobutyl ketone may be used.
As a method of coating the composition for forming the release layer on the substrate, an off-line coating method available in the art, such as bar coating, gravure coating, die coating, and the like, may be used. The energy source for curing the composition for forming the release layer is not particularly limited, but heat treatment, ultraviolet irradiation, or electron beam irradiation may be used, which may be used alone or in combination, and heat treatment alone or a combination of heat treatment and ultraviolet irradiation may be used.
The heating may be performed at 60 ℃ or higher under an air atmosphere. For example, the heating may be performed at 60 ℃ or above for 24 hours under an air atmosphere. When the heating is performed at less than 60 ℃, it is difficult to introduce a portion including the fluorosilane compound to the particle surface.
The weight ratio of the inorganic particles to the fluorosilane compound may be 1:1 to 20:1. when the weight ratio of the inorganic particles to the fluorosilane compound is within the range, the peeling force can be further reduced to achieve excellent light peelability.
In the present specification, "substitution" is induced by replacing at least one hydrogen in an unsubstituted parent group (mother group) with another atom or functional group. Unless otherwise indicated, when a certain functional group is considered to be "substituted", this means that the functional group is substituted with at least one substituent selected from the group consisting of an alkyl group having 1 to 40 carbon atoms, an alkenyl group having 2 to 40 carbon atoms, an alkynyl group having 2 to 40 carbon atoms, a cycloalkyl group having 3 to 40 carbon atoms, a cycloalkenyl group having 3 to 40 carbon atoms, and an aryl group having 7 to 40 carbon atoms. When a functional group is described as "optionally substituted", this means that the functional group may be substituted with the substituents described above.
In the present specification, the monovalent hydrocarbon group of C1 to C10 means, for example, a linear alkyl group such as methyl, ethyl, n-hexyl, n-octyl, n-decyl, or the like; branched alkyl groups such as isopropyl, t-butyl, neopentyl, isohexyl and the like; cyclic alkyl groups such as cyclopentyl or cyclohexyl, and the like; alkenyl groups such as vinyl and allyl; aryl groups such as phenyl or tolyl, and the like; or aralkyl groups such as benzyl or phenethyl, and the like. Wherein when considering the availability of raw materials, it may be an alkyl group, and when considering the usefulness of the product, it may also be a methyl group or an ethyl group.
In the present specification, the C1-C20 alkyl group may include, for example, a linear alkyl group such as methyl, ethyl, n-hexyl, n-octyl, n-decyl, etc.; isopropyl, tert-butyl, neopentyl, isohexyl and the like. Wherein when considering the availability of raw materials, it may be an alkyl group, and when considering the usefulness of the product, it may also be a methyl group or an ethyl group.
In the present specification, a C2-C10 alkenyl group means a branched or unbranched hydrocarbon having at least one carbon-carbon double bond. Non-limiting examples of alkenyl groups may include vinyl, allyl, butenyl, isopropenyl, or isobutenyl, and the like.
In the present specification, the alkoxy group of C1 to C20 means an alkyl group bonded to oxygen. Non-limiting examples of alkoxy groups may include methoxy, ethoxy, and the like.
The constitution of the present invention and its effects will be described in more detail below by examples and comparative examples. It is, however, apparent that these examples are used to explain the present invention in more detail, and the scope of the present invention is not limited to these examples.
[ example ]
(preparation of organic-inorganic particles)
Preparation example 1: organic-inorganic particles
Silica inorganic particles (prepared by ABC Nanotech, SILNOS 160) and Triethoxy-1h, 2 h-tridecyl-fluoro-n-octylsilane (prepared by TCI) as a fluorosilane compound were mixed in a ratio of 4:1 to 100g of ethanol and stirred for 15 minutes to obtain a mixture. While heating the mixture to 60 ℃, aminosilane (manufactured by ShinEtsu, KBP-90) was slowly added as a co-reactant in an amount of 1/4 of the weight of the silica inorganic particles, followed by a reaction for 24 hours to obtain a reactant. Next, organic-inorganic particles are prepared by removing the solvent from the reactants through a filter.
Preparation example 2: organic-inorganic particles
Organic-inorganic particles were produced in the same manner as in production example 1 except that silica inorganic particles (produced by ABC Nanotech, SILNOS 160) and Triethoxy-1h, 2 h-tridecafluoron-octylsilane (produced by TCI) as a fluorosilane compound were produced in the same manner as in production example 1 in the following manner: 1 in a weight ratio of 100g of ethanol.
Preparation example 3: organic-inorganic particles
Organic-inorganic particles were produced in the same manner as in production example 1 except that silica inorganic particles (produced by ABC Nanotech, SILNOS 160) and Triethoxy-1h, 2 h-tridecafluoron-octylsilane (produced by TCI) as a fluorosilane compound were produced in the same manner as in production example 1, with the exception that the silica inorganic particles were produced by Triethoxy-1h, 2 h-tridecafluoro-n-octyilane in the following ratio of 20:1 in a weight ratio of 100g of ethanol.
Preparation example 4: organic-inorganic particles
Organic-inorganic particles were produced in the same manner as in production example 1 except that silica inorganic particles (produced by ABC Nanotech, SILNOS 160) and Triethoxy-1h, 2h-nonafluorohexylsilane (produced by TCI) as a fluorosilane compound were produced in the following manner as described in 4:1 in a weight ratio of 100g of ethanol.
Comparative preparation 1: organic-inorganic particles
Silica inorganic particles (prepared by ABC Nanotech, e540+) were prepared.
Comparative preparation 2: organic-inorganic particles
Organic-inorganic particles were produced in the same manner as in production example 1 except that silica inorganic particles (produced by ABC Nanotech, SILNOS 160) and Triethoxy-1h, 2 h-tridecafluoron-octylsilane (produced by TCI) as a fluorosilane compound were produced in the same manner as in production example 1, with the exception that the silica inorganic particles were produced by Triethoxy-1h, 2 h-tridecafluoro-n-octyilane in an amount of 40:1 in a weight ratio of 100g of ethanol.
Comparative preparation 3: organic-inorganic particles
Organic-inorganic particles were produced in the same manner as in production example 1 except that silica inorganic particles (produced by ABC Nanotech, SILNOS 160) and Trimethoxy-3, 3-trifluoropropyl silane (produced by TCI) as a fluorosilane compound were produced in the following manner as described in 4:1 in a weight ratio of 100g of ethanol.
Comparative preparation 4: organic-inorganic particles
Organic-inorganic particles were produced in the same manner as in production example 1 except that silica inorganic particles (produced by ABC Nanotech, SILNOS 160) and Trimethoxy-3, 3-trifluoropropyl silane (produced by TCI) as a fluorosilane compound were produced in the following manner as 1:1 in a weight ratio of 100g of ethanol.
(Release film)
Example 1: release film
A38 μm thick polyester film (DONGLI advanced material, XD 500P) was prepared.
Separately therefrom, 100 parts by weight of an organopolysiloxane (prepared by Dow Chemical, Q2-7785) represented by the following Chemical formula 3,3 parts by weight of a hydrogen polysiloxane (prepared by Dow Chemical, Q2-7560), 1 part by weight of a platinum chelate catalyst (prepared by Dow Chemical, SYL-OFF 4000) were diluted in a mixed solvent (weight ratio; 5:1) of heptane and methyl isobutyl ketone to prepare a composition having a total solid content of 5% by weight, and then a composition for forming a release layer was prepared by mixing the organic-inorganic particles prepared in preparation example 1 in the composition in an amount of 1% by weight based on the total solid content.
A release film was prepared by coating the composition for forming a release layer on one side of the polyester film and heat-treating in a hot air dryer at 150 ℃ for 2 minutes to form a release layer 0.3 μm thick.
< chemical formula 3>
< chemical formula 4>
In the formula (I), the compound (II) is a compound (III),
R 1 is vinyl, R 2 Is methyl, R 3 Is a fluorine-containing compound represented by the chemical formula 4An alkyl group;
n=4, m is 2, and is the binding site to the adjacent atom.
Examples 2 to 4: release film
A release film was prepared in the same manner as in example 1 except that the organic-inorganic particles prepared in preparation examples 2 to 4 were used instead of the organic-inorganic particles prepared in preparation example 1.
Comparative examples 1 to 4: release film
A release film was prepared in the same manner as in example 1 except that the (organic) inorganic particles prepared in comparative preparation examples 2 to 4 were used instead of the organic-inorganic particles prepared in preparation example 1.
Analytical example 1: infrared spectrum
Infrared spectroscopic analysis was performed on three kinds of silica inorganic particles, wherein the first silica inorganic particle is a starting material of the release film prepared according to example 1, the second silica inorganic particle is an intermediate reactant in which aminosilane is introduced at the surface, and the third silica inorganic particle is a final result in which aminosilane and a fluorosilane compound are introduced at the surface. Wherein the infrared spectroscopic analysis is performed using Fourier transform infrared spectroscopy (FT-IR) of Perkinelmer company. The infrared spectrum analysis result is shown in fig. 2.
Referring to FIG. 2, in the silica inorganic particles as the final result, 1064cm was confirmed as compared with the silica inorganic particles as the starting material and the silica inorganic particles as the intermediate reactant -1 To 1066cm -1 The peaks in the wavenumber range are shifted to the right, wherein the end result is silica inorganic particles incorporating aminosilane and a fluorosilane compound at the surface and the intermediate reactant is silica inorganic particles incorporating aminosilane at the surface.
Evaluation example 1: evaluation of physical Properties
The physical properties of the (organic) inorganic particles prepared in preparation examples 1 to 4 and comparative preparation examples 1 to 4 and the release films prepared in examples 1 to 4 and comparative examples 1 to 4 were evaluated in the following manner, and the results thereof are shown in table 1 below.
(1) X-ray photoelectron spectroscopy (XPS) analysis of (organic) inorganic particles
For each (organic) inorganic particle, the composition of Si, F, C and O atoms was analyzed using an X-ray photoelectron spectroscopy (ThermoFisher, K-ALPHA) in terms of atomic%, and the content ratio of F/Si element (M F /M Si )。
(2) Energy dispersive spectrometer (EDAX) analysis of (organic) inorganic particles
For each (organic) inorganic particle, the composition of Si, F, C and O atoms was analyzed using an energy dispersive spectrometer (EDAX) (Hitachi, S-4800), expressed in atomic%, and the content ratio of F/Si element (M F /M Si )。
(3) Release film peel force measurement
Each release film was cut to a size of 500mm×1500mm to prepare a sample. The samples were stored at 25℃and 65% RH for 24 hours. Next, at 50℃and 20g/cm 2 Silicone-based adhesive tape (Nitto, 903 UL) was pressed onto the release layer of the sample for 24 hours, and then the peel force of 250mm x 1500mm dimensions was measured using a peel force tester AR-2000 apparatus manufactured by cheminc. At this time, the peel force was obtained by calculating an average value after 5 measurements.
(4) Residual adhesion analysis of release film
Each release film was cut to a size of 500mm×1500mm to prepare a sample. The samples were stored at 25℃and 65% RH for 24 hours. At room temperature and 20g/cm 2 After pressing the adhesive tape (Nitto, 31B) on the release layer of the sample for 24 hours under the load, the adhesive tape adhered to the release layer was collected without contamination. The adhesive tape was adhered to a polyethylene terephthalate film side having a flat and clean surface. The adhesive tape adhered to the polyethylene terephthalate film surface was repeatedly pressure-bonded once with a 2kg tape roll (ASTMD-1000-55T) using a chemistry companyThe peel force test apparatus AR-2000 was manufactured to measure the peel force of 250mm x 1500mm size at 180 ° and 0.3mpm speed, and then the residual adhesion rate was obtained by substituting the following formula 2.
[ 2 ]
Residual adhesion ratio (%) = [ (peel force of adhesive tape peeled after adhering to release layer)/(peel force of adhesive tape not adhered to release layer) ×100]
(5) Evaluation of appearance of Release layer
Each release film was prepared as an A4-sized sample, which was placed on a black bottom evaluation plate, and shrinkage cavity (crazing) and appearance defects of the release layer were confirmed and recorded under a fluorescent lamp.
O: less than 2 shrinkage cavities
Delta: 3 to 5 shrinkage cavities
X: more than 5 shrinkage cavities
[ Table 1 ]
Referring to table 1, it was confirmed that the release films prepared in examples 1 to 4 were more excellent in peel force (light peelability) than the release films prepared in comparative examples 1 to 4 in the content ratio of F/Si element in the range of 0.1 to 1.0 among the organic-inorganic particles prepared in examples 1 to 4 included in the release films prepared in examples 1 to 4. In addition, it was confirmed that the release films prepared in examples 1 to 4 were excellent in residual adhesion and coating appearance. In contrast, it was confirmed that the release films prepared in comparative examples 1 and 2 had higher peel force than the release films prepared in examples 1 to 4. It was confirmed that the organic-inorganic particles prepared from comparative preparation examples 3 to 4 included in the release films prepared from comparative examples 3 to 4 had an F/Si element content ratio of less than 0.1 and a high peeling force.
Claims (11)
1. A release film, wherein, a base material and a release layer are positioned in sequence,
the surface energy of the release layer is below 24dyne/cm,
the release layer comprises organic-inorganic particles,
in the organic-inorganic particles, a portion including a fluorosilane compound is introduced onto the surface thereof, the organic-inorganic particles can satisfy the content ratio M of F/Si element represented by the following formula 1 F /M Si The range is as follows: [ 1 ]
0.1≤M F /M Si ≤1.0
In the formula (I), the compound (II) is a compound (III),
M F in atomic percent of F element, M Si The content of Si element in atomic%,
the fluorosilane compound moiety includes a fluorosilane compound represented by the following chemical formula 1:
[ chemical formula 1 ]
*-OSi(R a )(R b )(R c )
In the formula (I), the compound (II) is a compound (III),
R a and R is b A C1-C20 alkoxy group which is substituted or unsubstituted;
R c as shown in the following chemical formula 2,
* To be binding sites to the surface of the organic-inorganic particles,
[ chemical formula 2 ]
In the formula (I), the compound (II) is a compound (III),
R d is a hydrogen atom or a substituted or unsubstituted C1-C20 alkyl group;
R e and R is g A C1-C20 alkoxy group which is substituted or unsubstituted;
R f is C4-C20 alkyl substituted by fluorine;
n 1 an integer of 1 to 10;
* In order to be a binding site with the Si atom,
in the organic-inorganic particles, the weight ratio of the inorganic particles to the fluorosilane compound is 1:1 to 20:1.
2. The release film according to claim 1, wherein,
in the release layer, 1064cm in the infrared spectrum is compared with the organic-inorganic particles whose surface does not include the part of the fluorine-containing silane compound -1 To 1066cm -1 Peaks in the wavenumber range move to the right.
3. The release film according to claim 1, wherein,
the organic-inorganic particles include natural minerals; oxides, hydroxides, sulfides, nitrides or halides of group 1 to group 4, group 11 to group 12, group 14 and group 16 to group 18 elements; carbonates, sulphates, acetates, phosphates, phosphites, carboxylates, silicates, titanates, borates or hydrates thereof; and inorganic particles selected from its complex compounds.
4. The release film according to claim 1, wherein,
the release layer further comprises a polymer or copolymer comprising a fluorine-containing polysiloxane.
5. The release film according to claim 4, wherein,
the fluorine-containing polysiloxane includes an organopolysiloxane represented by the following chemical formula 3:
< chemical formula 3>
< chemical formula 4>
< chemical formula 5>
In the formula (I), the compound (II) is a compound (III),
R 1 a monovalent hydrocarbon group of C1-C10 which is substituted or unsubstituted, or an alkenyl group of C2-C10 which is substituted or unsubstituted;
R 2 a monovalent hydrocarbon group of substituted or unsubstituted C1-C10, an alkenyl group of substituted or unsubstituted C2-C10, or hydrogen;
R 3 a fluoroalkyl group represented by the chemical formula 4, a fluoroether group represented by the chemical formula 5, or a combination thereof;
n is an integer from 1 to 8, m is an integer from 1 to 5;
p is an integer from 1 to 5, q is 0 or 1, r is 0, 1 or 2, v is an integer from 1 to 5;
a is an oxygen atom or a single bond;
x, y and z are integers of 1 or more respectively;
* Is a binding site to an adjacent atom;
wherein R is 1 And R is 2 At least one of them is a substituted or unsubstituted C2-C10 alkenyl group.
6. The release film according to claim 1, wherein,
the release layer further includes at least one of a hydrogen polysiloxane and an acid catalyst.
7. The release film according to claim 1, wherein,
the release film has a peel force of 23gf/25mm or less.
8. The release film according to claim 1, wherein,
the residual adhesion rate of the release film is more than 90%.
9. A method of preparing a release film comprising: preparing a base material;
adding and stirring the inorganic particles, the fluorosilane compound and the aminosilane-based coreactant, and then heating to prepare organic-inorganic particles; and
a release film according to claim 1 is prepared by coating a composition for forming a release layer comprising a polymer or copolymer including a fluorine-containing polysiloxane, and organic-inorganic particles on at least one side of the substrate and drying to form a release layer,
the weight ratio of the inorganic particles to the fluorine-containing silane compound is 1:1 to 20:1.
10. the method for preparing a release film according to claim 9, wherein,
the heating is performed at 60 ℃ or higher under an air atmosphere.
11. The method for preparing a release film according to claim 9, wherein,
the weight ratio of the inorganic particles to the fluorine-containing silane compound is 4:1 to 20:1.
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| CN114729145A (en) | 2022-07-08 |
| KR20220061777A (en) | 2022-05-13 |
| WO2022097872A1 (en) | 2022-05-12 |
| KR102531723B1 (en) | 2023-05-11 |
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