CN112442201A - 一种聚酰亚胺光学反射膜的制备方法 - Google Patents
一种聚酰亚胺光学反射膜的制备方法 Download PDFInfo
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- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims abstract description 50
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 45
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 41
- 150000004985 diamines Chemical class 0.000 claims abstract description 41
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 41
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 48
- 239000000463 material Substances 0.000 claims description 14
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
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- IIQLVLWFQUUZII-UHFFFAOYSA-N 2-amino-5-(4-amino-3-carboxyphenyl)benzoic acid Chemical compound C1=C(C(O)=O)C(N)=CC=C1C1=CC=C(N)C(C(O)=O)=C1 IIQLVLWFQUUZII-UHFFFAOYSA-N 0.000 claims description 4
- UENRXLSRMCSUSN-UHFFFAOYSA-N 3,5-diaminobenzoic acid Chemical compound NC1=CC(N)=CC(C(O)=O)=C1 UENRXLSRMCSUSN-UHFFFAOYSA-N 0.000 claims description 4
- GPXCORHXFPYJEH-UHFFFAOYSA-N 3-[[3-aminopropyl(dimethyl)silyl]oxy-dimethylsilyl]propan-1-amine Chemical compound NCCC[Si](C)(C)O[Si](C)(C)CCCN GPXCORHXFPYJEH-UHFFFAOYSA-N 0.000 claims description 4
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical group CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 4
- QHHKLPCQTTWFSS-UHFFFAOYSA-N 5-[2-(1,3-dioxo-2-benzofuran-5-yl)-1,1,1,3,3,3-hexafluoropropan-2-yl]-2-benzofuran-1,3-dione Chemical group C1=C2C(=O)OC(=O)C2=CC(C(C=2C=C3C(=O)OC(=O)C3=CC=2)(C(F)(F)F)C(F)(F)F)=C1 QHHKLPCQTTWFSS-UHFFFAOYSA-N 0.000 claims description 4
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 4
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- GGZRCTWHSWYCFR-UHFFFAOYSA-N 2,4-diaminopyrimidine-5-carboxylic acid Chemical compound NC1=NC=C(C(O)=O)C(N)=N1 GGZRCTWHSWYCFR-UHFFFAOYSA-N 0.000 claims description 3
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 claims description 2
- KOOBYHRLTYIPTH-UHFFFAOYSA-N methyl 3,5-diamino-6-chloropyrazine-2-carboxylate Chemical compound COC(=O)C1=NC(Cl)=C(N)N=C1N KOOBYHRLTYIPTH-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
一种聚酰亚胺光学反射膜的制备方法,包括以下步骤:①、将含氟二酐和含羧基二胺溶解于有机溶剂中,将溶液置于冰水浴中,再加入甲醇,在40‑60℃下离心提纯后,在110‑130℃真空干燥得到白色中间产物;②、在20‑40℃条件下,白色中间产物溶于极性溶剂和二氯亚砜中,升温至60‑80℃,然后在溶液加入氨基硅氧烷、聚对苯二甲酸乙二酯、乙酸酐和三乙胺,将反应混合物在80‑120℃搅拌2‑4h,反应结束将混合物先后用乙醇和水离心洗涤,得到粘稠溶液;③、在步骤②所得粘稠溶液中加入聚乙二醇、无机粒子充分混合,经真空干燥后,通过T形模头挤压流涎于钢辊上,再经纵向和横向的拉伸从而获得聚酰亚胺光学反射膜,该薄膜能够在较高温度下长期使用且保持尺寸稳定。
Description
技术领域
本发明涉及一种光学反射膜的制备方法。
背景技术
反射膜是位于光学模组底部非常重要一种光学膜,其将漏出导光板底部的光线高效率且无损耗的反射,从而降低光损耗,降低能耗。但反射膜紧贴导光板,背光源中的LED灯条会在反射膜一侧,局部高温会导致反射膜热收缩,从而影响背光模组的光学效果。因此耐热且形状稳定反射膜的制备是一个亟待解决的问题。
发明内容
为了克服现有光学反射膜的上述不足,本发明提供一种聚酰亚胺光学反射膜的制备方法,制备得到的光学反射膜耐热稳定性好。
本发明解决其技术问题的技术方案是:一种聚酰亚胺光学反射膜的制备方法,包括以下步骤:
①、在氮气氛围中将含氟二酐和含羧基二胺充分溶解于有机溶剂中,在160-250℃下加入甲苯搅拌6-12h,然后将溶液置于冰水浴中,再加入甲醇,静置1-3h,在40-60℃ 下离心提纯后,在110-130℃ 真空干燥10-14h得到白色中间产物;
②、在20-40℃ 条件下,步骤①得到的白色中间产物溶于极性溶剂和二氯亚砜中,搅拌1-3h,升温至60-80℃ 静置10-30min,然后在溶液加入氨基硅氧烷、聚对苯二甲酸乙二酯、乙酸酐和三乙胺,将反应混合物在80-120℃ 搅拌2-4h,反应结束将混合物先后用乙醇和水离心洗涤,得到粘稠溶液;
③、在步骤②所得粘稠溶液中加入聚乙二醇、无机粒子充分混合,经真空干燥后,通过T形模头挤压流涎于钢辊上,再经纵向和横向的拉伸从而获得聚酰亚胺光学反射膜。
优选的,在步骤①中,含氟二酐和含羧基二胺摩尔比为0.8-1.2:1。
优选的,在步骤①中,所述的含氟二酐为4,4′-(六氟异丙烯)二酞酸酐,或4,4′-(2-(3′-三氟甲基-苯基)-1,4-苯氧基)-邻苯二甲酸酐,或4, 4′-(2-(3′,5′-二三氟甲基-苯基)-1,4-苯氧基)-邻苯二甲酸酐。
优选的,在步骤①中,所述的含羧基二胺为3,5-二氨基苯甲酸,或4,4'-二氨基-1,1'-联苯-3,3'-二羧酸,或2,4-二氨基-5-羧基嘧啶,或3,5-二氨基-6-氯吡嗪-2-羧酸甲酯。
优选的,在步骤①中,所述的有机溶剂为苯酚,或甲苯酚,或甲酚,用量为每克含氟二酐和含羧基二胺用4-8mL。
优选的,在步骤①中,所述甲苯的用量为每克含氟二酐和含羧基二胺用1.6-2.3mL。
优选的,在步骤②中,所述白色中间产物与极性溶剂和二氯亚砜的质量体积比为0.1-0.5g/ml;所述极性溶剂与二氯亚砜体积比2-3:1。
优选的,在步骤②中,所述的极性溶剂为二甲基甲酰胺,或1,3-二甲基-2-咪唑啉酮,或二甲基亚砜,或六甲基磷酰三胺。
优选的,在步骤②中,所述的氨基硅氧烷为3-氨基丙基三甲氧基硅烷,或1,3-二(3-氨基丙基)-1,1,3,3-四甲基二硅氧烷,或N-(β-氨乙基)-γ-氨丙基甲基,或γ-氨丙基三乙氧基硅烷二甲氧基硅烷中的一种,用量为每克白色中间产物用150-300mL;
聚对苯二甲酸乙二酯用量为:使其质量百分含量为15-30%;
乙酸酐用量为为每克白色中间产物用2-4mL;
三乙胺用量为为每克白色中间产物用10-20mL。
优选的,在步骤③中,聚乙二醇用量为:使其质量百分含量为5-10%;无机粒子为二氧化硅、二氧化钛、氧化锌及钛酸钡中的一种,用量为:使其质量百分含量为2-6%。
本发明的有益效果在于:本发明采用氨基硅氧烷作为交联剂将聚酰亚胺树脂和聚酯树脂结合在一起,使获得的反射膜兼具聚酰亚胺的耐热稳定性与聚酯树脂优异的光学性能。该薄膜能够在较高温度下长期使用且保持尺寸稳定,能够用于OLED/Mini-LED等耐高温的背光模组中,满足多种领域对高性能聚酰亚胺光学反射膜的应用要求,取得较好的技术效果。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明。
实施例一,一种聚酰亚胺光学反射膜的制备方法,包括以下步骤:
①、在氮气氛围中将含氟二酐和含羧基二胺充分溶解于有机溶剂苯酚中,机溶剂用量为每克(含氟二酐和含羧基二胺)用6mL,在160-250℃温度范围下加入甲苯搅拌10h,甲苯的用量为每克(含氟二酐和含羧基二胺)用2mL,然后将溶液置于冰水浴中,再加入甲醇(甲醇的加入量并不做具体限定,其只是作为有机容积的补充,故加入量的多少并不影响本发明的实施),静置2h,在40-60℃ 温度范围下离心提纯后,在110-130℃ 温度范围下真空干燥12h得到白色中间产物。
其中,含氟二酐和含羧基二胺摩尔比为1:1,所述的含氟二酐为4,4′-(六氟异丙烯)二酞酸酐,所述的含羧基二胺为3,5-二氨基苯甲酸。
②、在20-40℃ 条件下,步骤①得到的白色中间产物溶于极性溶剂和二氯亚砜中,搅拌1-3h,升温至60-80℃ 静置10-30min,然后在溶液加入氨基硅氧烷、聚对苯二甲酸乙二酯、乙酸酐和三乙胺,将反应混合物在80-120℃ 搅拌2-4h,反应结束将混合物先后用乙醇和水离心洗涤,得到粘稠溶液。
其中,白色中间产物与极性溶剂和二氯亚砜的质量体积比为0.3g/ml,所述极性溶剂与二氯亚砜体积比2.5:1。所述的极性溶剂为二甲基甲酰胺。所述的氨基硅氧烷为3-氨基丙基三甲氧基硅烷,用量为每克白色中间产物用200mL。聚对苯二甲酸乙二酯用量为:使其质量百分含量为20%。乙酸酐用量为每克白色中间产物用3mL。三乙胺用量为为每克白色中间产物用15mL。
③、在步骤②所得粘稠溶液中加入聚乙二醇、无机粒子充分混合,经真空干燥后,通过T形模头挤压流涎于钢辊上,再经纵向和横向的拉伸从而获得聚酰亚胺光学反射膜。
其中聚乙二醇用量为:使其质量百分含量为8%;无机粒子为二氧化硅粒子,其用量为:使其质量百分含量为5%。
实施例二,一种聚酰亚胺光学反射膜的制备方法,包括以下步骤:
①、在氮气氛围中将含氟二酐和含羧基二胺充分溶解于有机溶剂甲苯酚中,机溶剂用量为每克(含氟二酐和含羧基二胺)用8mL,在160-250℃温度范围下加入甲苯搅拌12h,甲苯的用量为每克(含氟二酐和含羧基二胺)用1.6mL,然后将溶液置于冰水浴中,再加入甲醇(甲醇的加入量并不做具体限定,其只是作为有机容积的补充,故加入量的多少并不影响本发明的实施),静置3h,在40-60℃ 温度范围下离心提纯后,在110-130℃ 温度范围下真空干燥10h得到白色中间产物。
其中,含氟二酐和含羧基二胺摩尔比为1.1:1,所述的含氟二酐为4,4′-(2-(3′-三氟甲基-苯基)-1,4-苯氧基)-邻苯二甲酸酐,所述的含羧基二胺为4,4'-二氨基-1,1'-联苯-3,3'-二羧酸。
②、在20-40℃ 条件下,步骤①得到的白色中间产物溶于极性溶剂和二氯亚砜中,搅拌1-3h,升温至60-80℃ 静置10-30min,然后在溶液加入氨基硅氧烷、聚对苯二甲酸乙二酯、乙酸酐和三乙胺,将反应混合物在80-120℃ 搅拌2-4h,反应结束将混合物先后用乙醇和水离心洗涤,得到粘稠溶液。
其中,白色中间产物与极性溶剂和二氯亚砜的质量体积比为0.2g/ml,所述极性溶剂与二氯亚砜体积比2.8:1。所述的极性溶剂为1,3-二甲基-2-咪唑啉酮。所述的氨基硅氧烷为1,3-二(3-氨基丙基)-1,1,3,3-四甲基二硅氧烷,用量为每克白色中间产物用220mL。聚对苯二甲酸乙二酯用量为:使其质量百分含量为25%。乙酸酐用量为每克白色中间产物用2.5mL。三乙胺用量为为每克白色中间产物用20mL。
③、在步骤②所得粘稠溶液中加入聚乙二醇、无机粒子充分混合,经真空干燥后,通过T形模头挤压流涎于钢辊上,再经纵向和横向的拉伸从而获得聚酰亚胺光学反射膜。
其中聚乙二醇用量为:使其质量百分含量为6%;无机粒子为二氧化钛粒子,其用量为:使其质量百分含量为4%。
实施例三,一种聚酰亚胺光学反射膜的制备方法,包括以下步骤:
①、在氮气氛围中将含氟二酐和含羧基二胺充分溶解于有机溶剂甲酚中,机溶剂用量为每克(含氟二酐和含羧基二胺)用4mL,在160-250℃温度范围下加入甲苯搅拌8h,甲苯的用量为每克(含氟二酐和含羧基二胺)用2.3mL,然后将溶液置于冰水浴中,再加入甲醇(甲醇的加入量并不做具体限定,其只是作为有机容积的补充,故加入量的多少并不影响本发明的实施),静置1.5h,在40-60℃ 温度范围下离心提纯后,在110-130℃ 温度范围下真空干燥11h得到白色中间产物。
其中,含氟二酐和含羧基二胺摩尔比为0.9:1,所述的含氟二酐为4, 4′-(2-(3′,5′-二三氟甲基-苯基)-1,4-苯氧基)-邻苯二甲酸酐,所述的含羧基二胺为2,4-二氨基-5-羧基嘧啶。
②、在20-40℃ 条件下,步骤①得到的白色中间产物溶于极性溶剂和二氯亚砜中,搅拌1-3h,升温至60-80℃ 静置10-30min,然后在溶液加入氨基硅氧烷、聚对苯二甲酸乙二酯、乙酸酐和三乙胺,将反应混合物在80-120℃ 搅拌2-4h,反应结束将混合物先后用乙醇和水离心洗涤,得到粘稠溶液。
其中,白色中间产物与极性溶剂和二氯亚砜的质量体积比为0.5g/ml,所述极性溶剂与二氯亚砜体积比2:1。所述的极性溶剂为二甲基亚砜。所述的氨基硅氧烷为N-(β-氨乙基)-γ-氨丙基甲基,用量为每克白色中间产物用160mL。聚对苯二甲酸乙二酯用量为:使其质量百分含量为15%。乙酸酐用量为每克白色中间产物用2mL。三乙胺用量为为每克白色中间产物用18mL。
③、在步骤②所得粘稠溶液中加入聚乙二醇、无机粒子充分混合,经真空干燥后,通过T形模头挤压流涎于钢辊上,再经纵向和横向的拉伸从而获得聚酰亚胺光学反射膜。
其中聚乙二醇用量为:使其质量百分含量为10%;无机粒子为氧化锌粒子,其用量为:使其质量百分含量为4.5%。
实施例四,一种聚酰亚胺光学反射膜的制备方法,包括以下步骤:
①、在氮气氛围中将含氟二酐和含羧基二胺充分溶解于有机溶剂苯酚中,机溶剂用量为每克(含氟二酐和含羧基二胺)用5mL,在160-250℃温度范围下加入甲苯搅拌6h,甲苯的用量为每克(含氟二酐和含羧基二胺)用1.7mL,然后将溶液置于冰水浴中,再加入甲醇(甲醇的加入量并不做具体限定,其只是作为有机容积的补充,故加入量的多少并不影响本发明的实施),静置1h,在40-60℃ 温度范围下离心提纯后,在110-130℃ 温度范围下真空干燥14h得到白色中间产物。
其中,含氟二酐和含羧基二胺摩尔比为1.2:1,所述的含氟二酐为4,4′-(六氟异丙烯)二酞酸酐,所述的含羧基二胺为3,5-二氨基-6-氯吡嗪-2-羧酸甲酯。
②、在20-40℃ 条件下,步骤①得到的白色中间产物溶于极性溶剂和二氯亚砜中,搅拌1-3h,升温至60-80℃ 静置10-30min,然后在溶液加入氨基硅氧烷、聚对苯二甲酸乙二酯、乙酸酐和三乙胺,将反应混合物在80-120℃ 搅拌2-4h,反应结束将混合物先后用乙醇和水离心洗涤,得到粘稠溶液。
其中,白色中间产物与极性溶剂和二氯亚砜的质量体积比为0.1g/ml,所述极性溶剂与二氯亚砜体积比3:1。所述的极性溶剂为六甲基磷酰三胺。所述的氨基硅氧烷为γ-氨丙基三乙氧基硅烷二甲氧基硅烷,用量为每克白色中间产物用150mL。聚对苯二甲酸乙二酯用量为:使其质量百分含量为30%。乙酸酐用量为每克白色中间产物用3.5mL。三乙胺用量为为每克白色中间产物用10mL。
③、在步骤②所得粘稠溶液中加入聚乙二醇、无机粒子充分混合,经真空干燥后,通过T形模头挤压流涎于钢辊上,再经纵向和横向的拉伸从而获得聚酰亚胺光学反射膜。
其中聚乙二醇用量为:使其质量百分含量为9%;无机粒子为钛酸钡粒子,其用量为:使其质量百分含量为3%。
实施例五,一种聚酰亚胺光学反射膜的制备方法,包括以下步骤:
①、在氮气氛围中将含氟二酐和含羧基二胺充分溶解于有机溶剂甲苯酚中,机溶剂用量为每克(含氟二酐和含羧基二胺)用7mL,在160-250℃温度范围下加入甲苯搅拌11h,甲苯的用量为每克(含氟二酐和含羧基二胺)用1.8mL,然后将溶液置于冰水浴中,再加入甲醇(甲醇的加入量并不做具体限定,其只是作为有机容积的补充,故加入量的多少并不影响本发明的实施),静置2.5h,在40-60℃ 温度范围下离心提纯后,在110-130℃ 温度范围下真空干燥13h得到白色中间产物。
其中,含氟二酐和含羧基二胺摩尔比为0.8:1,所述的含氟二酐为4,4′-(2-(3′-三氟甲基-苯基)-1,4-苯氧基)-邻苯二甲酸酐,所述的含羧基二胺为3,5-二氨基苯甲酸。
②、在20-40℃ 条件下,步骤①得到的白色中间产物溶于极性溶剂和二氯亚砜中,搅拌1-3h,升温至60-80℃ 静置10-30min,然后在溶液加入氨基硅氧烷、聚对苯二甲酸乙二酯、乙酸酐和三乙胺,将反应混合物在80-120℃ 搅拌2-4h,反应结束将混合物先后用乙醇和水离心洗涤,得到粘稠溶液。
其中,白色中间产物与极性溶剂和二氯亚砜的质量体积比为0.4g/ml,所述极性溶剂与二氯亚砜体积比2.1:1。所述的极性溶剂为二甲基甲酰胺。所述的氨基硅氧烷为3-氨基丙基三甲氧基硅烷,用量为每克白色中间产物用300mL。聚对苯二甲酸乙二酯用量为:使其质量百分含量为22%。乙酸酐用量为每克白色中间产物用4mL。三乙胺用量为为每克白色中间产物用12mL。
③、在步骤②所得粘稠溶液中加入聚乙二醇、无机粒子充分混合,经真空干燥后,通过T形模头挤压流涎于钢辊上,再经纵向和横向的拉伸从而获得聚酰亚胺光学反射膜。
其中聚乙二醇用量为:使其质量百分含量为5%;无机粒子为二氧化硅粒子,其用量为:使其质量百分含量为6%。
实施例六,一种聚酰亚胺光学反射膜的制备方法,包括以下步骤:
①、在氮气氛围中将含氟二酐和含羧基二胺充分溶解于有机溶剂甲酚中,机溶剂用量为每克(含氟二酐和含羧基二胺)用6.5mL,在160-250℃温度范围下加入甲苯搅拌9h,甲苯的用量为每克(含氟二酐和含羧基二胺)用2.1mL,然后将溶液置于冰水浴中,再加入甲醇(甲醇的加入量并不做具体限定,其只是作为有机容积的补充,故加入量的多少并不影响本发明的实施),静置2.2h,在40-60℃ 温度范围下离心提纯后,在110-130℃ 温度范围下真空干燥12.5h得到白色中间产物。
其中,含氟二酐和含羧基二胺摩尔比为0.95:1,所述的含氟二酐为4, 4′-(2-(3′,5′-二三氟甲基-苯基)-1,4-苯氧基)-邻苯二甲酸酐,所述的含羧基二胺为4,4'-二氨基-1,1'-联苯-3,3'-二羧酸。
②、在20-40℃ 条件下,步骤①得到的白色中间产物溶于极性溶剂和二氯亚砜中,搅拌1-3h,升温至60-80℃ 静置10-30min,然后在溶液加入氨基硅氧烷、聚对苯二甲酸乙二酯、乙酸酐和三乙胺,将反应混合物在80-120℃ 搅拌2-4h,反应结束将混合物先后用乙醇和水离心洗涤,得到粘稠溶液。
其中,白色中间产物与极性溶剂和二氯亚砜的质量体积比为0.25g/ml,所述极性溶剂与二氯亚砜体积比2.2:1。所述的极性溶剂为1,3-二甲基-2-咪唑啉酮。所述的氨基硅氧烷为1,3-二(3-氨基丙基)-1,1,3,3-四甲基二硅氧烷,用量为每克白色中间产物用280mL。聚对苯二甲酸乙二酯用量为:使其质量百分含量为28%。乙酸酐用量为每克白色中间产物用3.2mL。三乙胺用量为为每克白色中间产物用16mL。
③、在步骤②所得粘稠溶液中加入聚乙二醇、无机粒子充分混合,经真空干燥后,通过T形模头挤压流涎于钢辊上,再经纵向和横向的拉伸从而获得聚酰亚胺光学反射膜。
其中聚乙二醇用量为:使其质量百分含量为7%;无机粒子为二氧化钛粒子,其用量为:使其质量百分含量为2%。
Claims (10)
1.一种聚酰亚胺光学反射膜的制备方法,其特征在于包括以下步骤:
①、在氮气氛围中将含氟二酐和含羧基二胺充分溶解于有机溶剂中,在160-250℃下加入甲苯搅拌6-12h,然后将溶液置于冰水浴中,再加入甲醇,静置1-3h,在40-60℃ 下离心提纯后,在110-130℃ 真空干燥10-14h得到白色中间产物;
②、在20-40℃ 条件下,步骤①得到的白色中间产物溶于极性溶剂和二氯亚砜中,搅拌1-3h,升温至60-80℃ 静置10-30min,然后在溶液加入氨基硅氧烷、聚对苯二甲酸乙二酯、乙酸酐和三乙胺,将反应混合物在80-120℃ 搅拌2-4h,反应结束将混合物先后用乙醇和水离心洗涤,得到粘稠溶液;
③、在步骤②所得粘稠溶液中加入聚乙二醇、无机粒子充分混合,经真空干燥后,通过T形模头挤压流涎于钢辊上,再经纵向和横向的拉伸从而获得聚酰亚胺光学反射膜。
2.如权利要求1所述的聚酰亚胺光学反射膜的制备方法,其特征在于:在步骤①中,含氟二酐和含羧基二胺摩尔比为0.8-1.2:1。
3.如权利要求2所述的聚酰亚胺光学反射膜的制备方法,其特征在于:在步骤①中,所述的含氟二酐为4,4′-(六氟异丙烯)二酞酸酐,或4,4′-(2-(3′-三氟甲基-苯基)-1,4-苯氧基)-邻苯二甲酸酐,或4, 4′-(2-(3′,5′-二三氟甲基-苯基)-1,4-苯氧基)-邻苯二甲酸酐。
4.如权利要求2所述的聚酰亚胺光学反射膜的制备方法,其特征在于:在步骤①中,所述的含羧基二胺为3,5-二氨基苯甲酸,或4,4'-二氨基-1,1'-联苯-3,3'-二羧酸,或2,4-二氨基-5-羧基嘧啶,或3,5-二氨基-6-氯吡嗪-2-羧酸甲酯。
5.如权利要求2所述的聚酰亚胺光学反射膜的制备方法,其特征在于:在步骤①中,所述的有机溶剂为苯酚,或甲苯酚,或甲酚,用量为每克含氟二酐和含羧基二胺用4-8mL。
6.如权利要求2所述的聚酰亚胺光学反射膜的制备方法,其特征在于:在步骤①中,所述甲苯的用量为每克含氟二酐和含羧基二胺用1.6-2.3mL。
7.如权利要求2所述的聚酰亚胺光学反射膜的制备方法,其特征在于:在步骤②中,所述白色中间产物与极性溶剂和二氯亚砜的质量体积比为0.1-0.5g/ml;所述极性溶剂与二氯亚砜体积比2-3:1。
8.如权利要求7所述的聚酰亚胺光学反射膜的制备方法,其特征在于:在步骤②中,所述的极性溶剂为二甲基甲酰胺,或1,3-二甲基-2-咪唑啉酮,或二甲基亚砜,或六甲基磷酰三胺。
9.如权利要求7所述的聚酰亚胺光学反射膜的制备方法,其特征在于:在步骤②中,所述的氨基硅氧烷为3-氨基丙基三甲氧基硅烷,或1,3-二(3-氨基丙基)-1,1,3,3-四甲基二硅氧烷,或N-(β-氨乙基)-γ-氨丙基甲基,或γ-氨丙基三乙氧基硅烷二甲氧基硅烷,用量为每克白色中间产物用150-300mL;
聚对苯二甲酸乙二酯用量为:使其质量百分含量为15-30%;
乙酸酐用量为为每克白色中间产物用2-4mL;
三乙胺用量为为每克白色中间产物用10-20mL。
10.如权利要求2所述的聚酰亚胺光学反射膜的制备方法,其特征在于:在步骤③中,聚乙二醇用量为:使其质量百分含量为5-10%;无机粒子为二氧化硅、二氧化钛、氧化锌及钛酸钡中的一种,用量为:使其质量百分含量为2-6%;
在步骤③中,聚乙二醇用量为:使其质量百分含量为5-10%;无机粒子为二氧化硅、二氧化钛、氧化锌及钛酸钡中的一种,用量为:使其质量百分含量为2-6%。
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US6646060B1 (en) * | 1999-05-10 | 2003-11-11 | Teijin Limited | Resin composition containing crystalline polyimide |
CN105143309A (zh) * | 2013-05-14 | 2015-12-09 | 三井化学株式会社 | 透明聚酰亚胺及其前体 |
CN107454910A (zh) * | 2015-02-03 | 2017-12-08 | 沙特基础全球技术有限公司 | 用于电容器膜的聚醚酰亚胺混溶聚合物共混物 |
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US6646060B1 (en) * | 1999-05-10 | 2003-11-11 | Teijin Limited | Resin composition containing crystalline polyimide |
CN105143309A (zh) * | 2013-05-14 | 2015-12-09 | 三井化学株式会社 | 透明聚酰亚胺及其前体 |
CN107454910A (zh) * | 2015-02-03 | 2017-12-08 | 沙特基础全球技术有限公司 | 用于电容器膜的聚醚酰亚胺混溶聚合物共混物 |
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