Bisphenol f tetraacid dianhydride and preparation method thereof
A tetraacid dianhydride and double substitution technology, applied in the field of polyimide, can solve the problems of high cost, difficult to realize industrialized production, low yield, etc., and achieve low cost, good solvent resistance and processability, and raw materials. simple effect
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[0040] The present invention also provides a kind of preparation method of bisphenol F tetraacid dianhydride, comprises the following steps:
[0041] a) Under the action of a basic compound, bisphenol F reacts with phthalimide having a structure of formula (IV) and / or formula (V) in a polar aprotic solvent to obtain N, N-bis Substituted bisphenol F bisphthalimide:
[0042]
[0043] Among them, R 1 is halogen or nitro, R 2 is phenyl, substituted phenyl or alkyl with 1 to 6 carbon atoms;
[0044] b) After the N,N-disubstituted bisphenol F bisphthalimide is sequentially hydrolyzed, acidified and dehydrated, bisphenol F tetraacid dianhydride is obtained.
[0045] The present invention prepares bisphenol F tetraacid dianhydride with bisphenol F and phthalimide having the structure of formula (IV) and / or formula (V) as raw materials. The method raw materials provided by the invention are simple and easy to obtain, and the process The process is simple, no complicated post-tre...
Embodiment 1
[0068] Add 20.02g (0.1mol) of bisphenol F, 8.0g (0.2mol) of sodium hydroxide, 80g of dimethyl sulfoxide and 40g of benzene into a 500mL dry round-bottomed flask, blow nitrogen into it, and reflux at 100°C with water for 4h. After distilling off the benzene, cool to room temperature; then add 39.12g (0.2mol) N-methyl-4-chlorophthalimide to it, heat up to 50°C for 10h, and cool to room temperature; The reaction mixture was slowly poured into 400 mL of water, and the resulting solid was washed with water and ethanol to obtain 41.48 g of 4,4'-(4,4'-methylenebisphenoxy)bis(N-methylphthalimide) ) with a melting point of 191°C to 193°C and a yield of 80%.
Embodiment 2
[0070] Add 20.02g (0.1mol) of bisphenol F, 41.46g (0.3mol) of anhydrous potassium carbonate, 200g of sulfolane and 100g of toluene into a 500mL dry round-bottomed flask, pass nitrogen gas into it, reflux with water at 150°C for 10h, and distill it off Then, 48.9g (0.25mol) of N-methyl-3-chlorophthalimide was added thereto, and the temperature was raised to 200°C for 4h, and then cooled to room temperature; the obtained reaction mixture was Slowly poured into 400mL water, the obtained solid was washed with water and ethanol to obtain 46.66g 3,3'-(4,4'-methylenebisphenoxy)bis(N-methylphthalimide), the melting point It is 180°C to 182°C, and the yield is 90%.
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