Low-thermal-expansion transparent polyimide film and preparation method thereof
A technology of transparent polyimide and polyimide film, which is applied in the direction of instruments, identification devices, etc., and can solve the problems of device display accuracy reduction, layer-to-layer peeling, etc.
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[0119] The present invention also provides a method for preparing the above-mentioned transparent polyimide film with high strength and low thermal expansion, comprising the following steps:
[0120] The dianhydride monomer and the diamine monomer are polycondensed and then imidized to obtain polyimide;
[0121] The dianhydride monomer has a structure shown in formula VII:
[0122]
[0123] in At least one selected from the following amide-containing structural groups:
[0124]
[0125] R 1 , R 2 , R 3 , R 4 independently selected from hydrogen, alkyl, cycloalkyl, fluoroalkyl, ester or halo; preferably -H, -F, CH 3 or -CF 3 ;
[0126] The diamine monomer has a structure shown in formula VIII:
[0127] h 2 N-Ar 2 -NH 2 Formula VIII
[0128] —Ar 2 - selected from one of the structural groups shown in formula II to formula IV:
[0129]
[0130] In formula II, R 5 for
[0131] R 6 selected from hydrogen, alkyl, cycloalkyl, fluoroalkyl, ester or halo;...
Embodiment 1
[0192] Add 2.27g of diamine compound (1), 3.20g of 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl, 80.0g of dimethylacetamide to the reaction vessel, at 20°C, Stir to dissolve. Add 2.34g of dianhydride compound (8) and 6.66g of 2,2-bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride in sequence, polymerize for 24 hours, and test the rotational viscosity to reach 4.0×10 4 mPa / s, forming the precursor solution of transparent polyimide. Test its logarithmic viscosity.
[0193] Add 10.20 g of acetic anhydride and 5.05 g of triethylamine to this precursor solution, and carry out chemical imidization reaction for 2 h. After imidization is completed, a polyimide solution is obtained. This solution was slowly poured into ethanol. A white filamentary precipitate precipitated. The filamentous precipitate was filtered off and dried. Obtain transparent polyimide resin, test its number average molecular weight and weight average molecular weight.
[0194] Dissolve this resin in N-...
Embodiment 2
[0196] Add 4.14 g of diamine compound (2), 10.02 g of 2,2-bis(4-aminophenyl)hexafluoropropane, and 90 g of N-methylpyrrolidone into the reaction vessel, stir and dissolve at 20°C. Add 3.43g of dianhydride compound (7) and 6.72g of cyclohexanetetracarboxylic dianhydride in sequence, polymerize for 24 hours, and test the rotational viscosity to reach 4.2×10 4 mPa / s, forming the precursor solution of transparent polyimide. Test its logarithmic viscosity.
[0197] Add 20.0 g of acetic anhydride and 10.1 g of triethylamine to this precursor solution, and carry out chemical imidization reaction for 2 h. After imidization is completed, a polyimide solution is obtained. This solution was slowly poured into ethanol. A white filamentary precipitate precipitated. The filamentous precipitate was filtered off and dried. Obtain transparent polyimide resin, test its number average molecular weight and weight average molecular weight.
[0198] Dissolve this resin in N-methylpyrrolidone ...
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