High-adhesion-property low-linear-expansion-coefficient polyimide film material and preparation method thereof
A technology of polyimide film and linear expansion coefficient, which is applied in the field of polymer material synthesis, can solve the problems of poor adhesion, oligoimide, and can only be reached, and achieves improved adhesion performance and low thermal expansion coefficient. , the effect of good dimensional stability
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[0052] Example 1
[0053] 1) Preparation of nitro compounds
[0054] In a 500ml three-necked flask equipped with an electric stirring device, a condenser, a water device, and a nitrogen protection device, 18.6207g (0.1mol) of biphenol and 38.3384g of 2-chloro-5-nitrobenzonitrile ( 0.21mol), anhydrous K2CO 3 16.5847g (0.12mol), 141ml DMF (the percentage of the total weight of the raw material monomer to the weight of the whole material is 30%, that is, the solid content) and 20ml of toluene, the initial reaction temperature is 135~140℃, with water for 2~3h, gradually heating up When the reaction temperature is 150~155℃, continue the reaction for 4~6h, filter while hot and discharge into ice ethanol to obtain a large amount of bright yellow precipitate. After filtering, wash the crude product in deionized water 3~4 times until the filtrate is basically Until clarification, reflux in hot ethanol for 2 to 3 hours to remove organic impurities, recrystallize in DMSO solvent, filter, coo...
Example Embodiment
[0060] Example 2
[0061] According to the operation of preparing the nitro compound in Example 1, the anhydrous K 2 CO 3 The input amount increased to 20.7g (0.15mol), and the other conditions remained unchanged, the product 1,4-bis(4-nitro-2cyanophenoxy)biphenyl was obtained. The characterization results of the product were the same as those of the nitro compound in Example 1. The characterization results are consistent.
Example Embodiment
[0062] Example 3
[0063] According to the operation of preparing the nitro compound in Example 1, only the amount of DMF added was changed to 112ml (the solid content of the system was increased from 30% to 35%) to obtain the product 1,4-bis(4-nitro-2 cyano The characterization result of phenoxy)biphenyl is consistent with the characterization result of the nitro compound in Example 1.
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