Dianhydride and polyimide
A dianhydride and polyimide technology, applied in the field of polyimide, can solve problems such as affecting usability, changes in structure and thermal properties, and reducing heat resistance of polymers.
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Embodiment 1
[0023] Embodiment 1 (phenyl fluorene monomer synthesis)
[0024] 1,2,4-Trimellitic anhydride chloride (120 mmol) was dissolved in 60 mL of anhydrous THF. Bisphenol fluorene (60 mmol) and pyridine (14.5 ml) were dissolved in 100 ml of anhydrous THF, then slowly added dropwise to the 1,2,4-trimellitic anhydride chloride solution under nitrogen, and reacted at 40°C 12 hours. The reaction result was then filtered to remove salts, and the filtrate was concentrated to obtain a solid. Wash the solid with n-hexane and recrystallize twice with acetic anhydride to obtain a white solid product (yield 75%), and its hydrogen spectrum is as follows: 1 HNMR (CDCl 3 , 400MHz, ppm): 8.77 (s, 2H), 8.69 (d, 2H), 8.14 (d, 2H), 7.82 (d, 2H), 7.43 (m, 4H). The above reaction is shown in formula 7.
[0025]
Embodiment 2
[0026] Embodiment 2 (naphthyl fluorene monomer synthesis)
[0027] Synthesis of compound I: After adding fluorene (0.54 moles), 2-naphthol (1.2 moles), 3-thiol propionic acid (0.0377 moles) and 300 milliliters of toluene into a 1-liter reaction flask, slowly drop 10 grams of sulfuric acid into In a reaction flask, it was heated to 80°C and reacted at 80°C for 10 hours. Then, 100 grams of toluene and 30 grams of water were added to the reaction product, and then the pH was adjusted to about 7 with 10% aqueous sodium hydroxide solution, and the filter cake was obtained after filtration. After washing the filter cake 5 times with water, drying the filter cake and recrystallizing twice with petroleum ether, a white solid compound I was obtained (yield 78%). The hydrogen spectrum of white solid compound I is as follows: 1 HNMR (CDCl 3 , 400MHz, ppm): 7.94 (d, 2H), 7.62 (m, 8H), 7.37 (m, 6H), 7.10 (m, 4H). The above reaction is shown in formula 8.
[0028] Chlorine was reacte...
Embodiment 3
[0030] Embodiment 3 (spirocyclyl fluorene monomer synthesis)
[0031] Synthesis of compound II: Mix 9-fluorenone (60 mmol), 1,3-benzenediol (240 mmol) and zinc chloride (27.01 mmol), heat to 140°C and maintain at 140°C for 3 hours, Slowly add 150 ml of concentrated hydrochloric acid in molten state and then reflux for 2 hours. Then pour into 1 liter of ice water and reprecipitate. After filtration, the filter cake was taken, washed with n-hexane and then recrystallized twice with petroleum ether to obtain white solid compound II (yield 70%), and its hydrogen spectrum was as follows: 1 HNMR (CDCl 3 , 400MHz, ppm): 7.90(d, 2H), 7.42(dd, 2H), 7.23(dd, 2H), 7.08(d, 2H), 6.68(d, 2H), 6.31(d, 2H), 6.13( d, 2H). The above reaction is shown in formula 10.
[0032]
[0033] Then, with the reaction steps similar to Example 1, compound II was reacted with 1,2,4-trimellitic anhydride acid chloride to obtain a white solid (yield 82%), and its hydrogen spectrum was as follows: 1 HN...
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