CN116284925A - 一种含水性氟素离型剂的pet膜材料及其合成工艺 - Google Patents
一种含水性氟素离型剂的pet膜材料及其合成工艺 Download PDFInfo
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 52
- 239000011737 fluorine Substances 0.000 title claims abstract description 52
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 30
- 229920002799 BoPET Polymers 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 24
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 17
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 14
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 13
- LCPUCXXYIYXLJY-UHFFFAOYSA-N 1,1,2,4,4,4-hexafluorobutyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(F)(F)C(F)CC(F)(F)F LCPUCXXYIYXLJY-UHFFFAOYSA-N 0.000 claims abstract description 12
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 12
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 claims abstract description 11
- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical compound CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-UHFFFAOYSA-N 0.000 claims abstract description 10
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 5
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- 230000035484 reaction time Effects 0.000 claims description 16
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- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 229920006267 polyester film Polymers 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 239000003995 emulsifying agent Substances 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 238000001723 curing Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
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- 230000032683 aging Effects 0.000 abstract description 3
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- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- JTHZUSWLNCPZLX-UHFFFAOYSA-N 6-fluoro-3-methyl-2h-indazole Chemical compound FC1=CC=C2C(C)=NNC2=C1 JTHZUSWLNCPZLX-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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Abstract
本发明涉及PET技术领域，且公开了一种含水性氟素离型剂的PET膜材料及其合成工艺，以十三氟‑8‑碘辛烷和70mmol的2‑(二甲氨基)丙烯酸乙酯作为反应原理，合成一种新型的丙烯酸酯基全氟季铵盐。与丙烯酸、甲基丙烯酸六氟丁酯、丙烯酸十八酯进行共聚，从而将亲水性的季铵盐官能团接枝到氟素离型剂聚合物的侧链，得到新型的水性氟素离型剂。通过热固化附着中PET膜材料表面，得到含水性氟素离型剂的PET膜材料具有杂色点邵，剥离力高，耐老化性好、剩余粘着率大的优点。
Description
技术领域
本发明涉及PET技术领域，具体为一种含水性氟素离型剂的PET膜材料及其合成工艺。
背景技术
含氟离型剂是一种用于复合材料与模具之间的隔离膜，可以避免制品黏着在模具上，是材料可以方便地从模具上取下来，保持材料和模具的完整性；含氟离型剂主要有聚四氟乙烯类、氟碳化合物、氟硅离型剂、氟素离型剂等，其中氟素离型膜主要应用在聚酯薄膜基材上，可以提供稳定的易离型力，还可以保持良好的后续黏着强度，使薄膜表面具有平整光洁，无折皱等性能。开发新型氟素离型膜，应用于PET聚酯材料中具有重要的应用。如申请号为CN201310085616.9的专利《一种氟素离型膜的制作工艺》，公开了将氟素涂料主剂和正庚烷溶剂混合，然后加入架桥剂和锚固剂，再加入催化剂并搅拌，最后涂覆在PET原膜上，加热进行固化反应，使产品具有离型力稳定，耐老化效果好等优点。本发明旨在合成新型的含水性氟素离型剂，应用于PET膜材料中。
发明内容
(一)解决的技术问题
本发明提供了一种含水性氟素离型剂的PET膜材料及其合成工艺，PET膜材料具有剥离力高，剩余粘着率大的优点。
(二)技术方案
一种含水性氟素离型剂的PET膜材料的合成工艺：
(1)将十三氟-8-碘辛烷和2-(二甲氨基)丙烯酸乙酯溶解到溶剂中，然后搅拌进行反应，反应后减压蒸馏，产物用正己烷洗涤后，得到丙烯酸酯基全氟季铵盐。
(2)将丙烯酸、丙烯酸酯基全氟季铵盐、甲基丙烯酸六氟丁酯、丙烯酸十八酯加入到水中，然后加入乳化剂十二烷基硫酸钠和OP-10，在氮气气氛中滴加偶氮二异丁腈，反应后得到含水性氟素离型剂的乳液。
(3)将含水性氟素离型剂的乳液涂覆在PET聚酯膜表面，加热固化，得到含水性氟素离型剂的PET膜材料。
优选的，所述(1)中十三氟-8-碘辛烷和2-(二甲氨基)丙烯酸乙酯的反应摩尔比为1:1-1.4。
优选的，所述(1)中溶剂包括正丙醇、正丁醇、乙腈、N,N-二甲基甲酰胺或N,N-二甲基乙酰胺。
优选的，所述(1)中控制反应温度为60-100℃，反应时间为24-48h。
优选的，所述(2)中丙烯酸、丙烯酸酯基全氟季铵盐、甲基丙烯酸六氟丁酯、丙烯酸十八酯、偶氮二异丁腈的摩尔比为0.05-0.2:0.1-0.5:1:0.8-1.5:0.02-0.035。
优选的，所述(2)中控制反应温度为60-80℃，反应时间为3-6h。
优选的，所述(3)中加热固化的工艺为先在60℃下热固化1-2h，然后在80℃下热固化2-3h，最后在100℃下热固化1-2h。
(三)有益的技术效果
以十三氟-8-碘辛烷和70mmol的2-(二甲氨基)丙烯酸乙酯作为反应原理，合成一种新型的丙烯酸酯基全氟季铵盐。与丙烯酸、甲基丙烯酸六氟丁酯、丙烯酸十八酯进行共聚，从而将亲水性的季铵盐官能团接枝到氟素离型剂聚合物的侧链，得到新型的水性氟素离型剂。通过热固化附着中PET膜材料表面，得到含水性氟素离型剂的PET膜材料具有杂色点邵，剥离力高，耐老化性好、剩余粘着率大的优点。
具体实施方式
实施例1
(1)将50mmol的十三氟-8-碘辛烷和70mmol的2-(二甲氨基)丙烯酸乙酯溶解到正丁醇溶剂中，然后搅拌进行反应，控制反应温度为80℃，反应时间为24h，反应后减压蒸馏，产物用正己烷洗涤后，得到丙烯酸酯基全氟季铵盐。
(2)将2mmol的丙烯酸、10mmol的丙烯酸酯基全氟季铵盐、20mmol的甲基丙烯酸六氟丁酯、22mmol的丙烯酸十八酯加入到水中，然后加入乳化剂十二烷基硫酸钠和OP-10，在氮气气氛中滴加0.5mmol的偶氮二异丁腈，控制反应温度为80℃，反应时间为4h，反应后得到含水性氟素离型剂的乳液。
(3)将含水性氟素离型剂的乳液涂覆在PET聚酯膜表面，先加热至60℃热固化2h，然后在80℃下热固化2h，最后在100℃下热固化2h，得到含水性氟素离型剂的PET膜材料。
实施例2
(1)将50mmol的十三氟-8-碘辛烷和65mmol的2-(二甲氨基)丙烯酸乙酯溶解到N,N-二甲基乙酰胺溶剂中，然后搅拌进行反应，控制反应温度为100℃，反应时间为48h，反应后减压蒸馏，产物用正己烷洗涤后，得到丙烯酸酯基全氟季铵盐。
(2)将2mmol的丙烯酸、8mmol的丙烯酸酯基全氟季铵盐、20mmol的甲基丙烯酸六氟丁酯、16mmol的丙烯酸十八酯加入到水中，然后加入乳化剂十二烷基硫酸钠和OP-10，在氮气气氛中滴加0.5mmol的偶氮二异丁腈，控制反应温度为80℃，反应时间为3h，反应后得到含水性氟素离型剂的乳液。
(3)将含水性氟素离型剂的乳液涂覆在PET聚酯膜表面，先加热至60℃热固化1h，然后在80℃下热固化3h，最后在100℃下热固化2h，得到含水性氟素离型剂的PET膜材料。
实施例3
(1)将50mmol的十三氟-8-碘辛烷和70mmol的2-(二甲氨基)丙烯酸乙酯溶解到N,N-二甲基甲酰胺溶剂中，然后搅拌进行反应，控制反应温度为100℃，反应时间为24h，反应后减压蒸馏，产物用正己烷洗涤后，得到丙烯酸酯基全氟季铵盐。
(2)将1mmol的丙烯酸、10mmol的丙烯酸酯基全氟季铵盐、20mmol的甲基丙烯酸六氟丁酯、16mmol的丙烯酸十八酯加入到水中，然后加入乳化剂十二烷基硫酸钠和OP-10，在氮气气氛中滴加0.5mmol的偶氮二异丁腈，控制反应温度为70℃，反应时间为6h，反应后得到含水性氟素离型剂的乳液。
(3)将含水性氟素离型剂的乳液涂覆在PET聚酯膜表面，先加热至60℃热固化1h，然后在80℃下热固化2h，最后在100℃下热固化2h，得到含水性氟素离型剂的PET膜材料。
实施例4
(1)将50mmol的十三氟-8-碘辛烷和50mmol的2-(二甲氨基)丙烯酸乙酯溶解到正丙醇溶剂中，然后搅拌进行反应，控制反应温度为60℃，反应时间为36h，反应后减压蒸馏，产物用正己烷洗涤后，得到丙烯酸酯基全氟季铵盐。
(2)将4mmol的丙烯酸、2mmol的丙烯酸酯基全氟季铵盐、20mmol的甲基丙烯酸六氟丁酯、30mmol的丙烯酸十八酯加入到水中，然后加入乳化剂十二烷基硫酸钠和OP-10，在氮气气氛中滴加0.7mmol的偶氮二异丁腈，控制反应温度为70℃，反应时间为5h，反应后得到含水性氟素离型剂的乳液。
(3)将含水性氟素离型剂的乳液涂覆在PET聚酯膜表面，先加热至60℃热固化2h，然后在80℃下热固化3h，最后在100℃下热固化1h，得到含水性氟素离型剂的PET膜材料。
实施例5
(1)将50mmol的十三氟-8-碘辛烷和60mmol的2-(二甲氨基)丙烯酸乙酯溶解到乙腈溶剂中，然后搅拌进行反应，控制反应温度为80℃，反应时间为24h，反应后减压蒸馏，产物用正己烷洗涤后，得到丙烯酸酯基全氟季铵盐。
(2)将2mmol的丙烯酸、5mmol的丙烯酸酯基全氟季铵盐、20mmol的甲基丙烯酸六氟丁酯、25mmol的丙烯酸十八酯加入到水中，然后加入乳化剂十二烷基硫酸钠和OP-10，在氮气气氛中滴加0.7mmol的偶氮二异丁腈，控制反应温度为70℃，反应时间为3h，反应后得到含水性氟素离型剂的乳液。
(3)将含水性氟素离型剂的乳液涂覆在PET聚酯膜表面，先加热至60℃热固化2h，然后在80℃下热固化2h，最后在100℃下热固化2h，得到含水性氟素离型剂的PET膜材料。
实施例6
(1)将50mmol的十三氟-8-碘辛烷和50mmol的2-(二甲氨基)丙烯酸乙酯溶解到N,N-二甲基甲酰胺溶剂中，然后搅拌进行反应，控制反应温度为100℃，反应时间为36h，反应后减压蒸馏，产物用正己烷洗涤后，得到丙烯酸酯基全氟季铵盐。
(2)将3mmol的丙烯酸、10mmol的丙烯酸酯基全氟季铵盐、20mmol的甲基丙烯酸六氟丁酯、16mmol的丙烯酸十八酯加入到水中，然后加入乳化剂十二烷基硫酸钠和OP-10，在氮气气氛中滴加0.7mmol的偶氮二异丁腈，控制反应温度为70℃，反应时间为6h，反应后得到含水性氟素离型剂的乳液。
(3)将含水性氟素离型剂的乳液涂覆在PET聚酯膜表面，先加热至60℃热固化2h，然后在80℃下热固化2h，最后在100℃下热固化1h，得到含水性氟素离型剂的PET膜材料。
含水性氟素离型剂的PET膜材料性能测试
Claims (7)
1.一种含水性氟素离型剂的PET膜材料的合成工艺，其特征在于：所述合成工艺为：
(1)将十三氟-8-碘辛烷和2-(二甲氨基)丙烯酸乙酯溶解到溶剂中，然后搅拌进行反应，反应后减压蒸馏，产物用正己烷洗涤后，得到丙烯酸酯基全氟季铵盐；
(2)将丙烯酸、丙烯酸酯基全氟季铵盐、甲基丙烯酸六氟丁酯、丙烯酸十八酯加入到水中，然后加入乳化剂十二烷基硫酸钠和OP-10，在氮气气氛中滴加偶氮二异丁腈，反应后得到含水性氟素离型剂的乳液；
(3)将含水性氟素离型剂的乳液涂覆在PET聚酯膜表面，加热固化，得到含水性氟素离型剂的PET膜材料。
2.根据权利要求1所述的含水性氟素离型剂的PET膜材料的合成工艺，其特征在于：所述(1)中十三氟-8-碘辛烷和2-(二甲氨基)丙烯酸乙酯的反应摩尔比为1:1-1.4。
3.根据权利要求1所述的含水性氟素离型剂的PET膜材料的合成工艺，其特征在于：所述(1)中溶剂包括正丙醇、正丁醇、乙腈、N,N-二甲基甲酰胺或N,N-二甲基乙酰胺。
4.根据权利要求1所述的含水性氟素离型剂的PET膜材料的合成工艺，其特征在于：所述(1)中控制反应温度为60-100℃，反应时间为24-48h。
5.根据权利要求1所述的含水性氟素离型剂的PET膜材料的合成工艺，其特征在于：所述(2)中丙烯酸、丙烯酸酯基全氟季铵盐、甲基丙烯酸六氟丁酯、丙烯酸十八酯、偶氮二异丁腈的摩尔比为0.05-0.2:0.1-0.5:1:0.8-1.5:0.02-0.035。
6.根据权利要求1所述的含水性氟素离型剂的PET膜材料的合成工艺，其特征在于：所述(2)中控制反应温度为60-80℃，反应时间为3-6h。
7.根据权利要求1所述的含水性氟素离型剂的PET膜材料的合成工艺，其特征在于：所述(3)中加热固化的工艺为先在60℃下热固化1-2h，然后在80℃下热固化2-3h，最后在100℃下热固化1-2h。
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