Modified maleimide end-sealed type polyimide resin composite and application thereof
A technology of polyimide resin and maleimide, which is applied in the direction of layered products, metal layered products, chemical instruments and methods, etc., can solve the problem of not meeting the requirements of large-scale industrial production, equipment and environmental conditions Too high, harsh condition control and other problems, to achieve low production costs, lower requirements for equipment and environmental conditions, and good stability
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Embodiment 1
[0038] Under the protection of nitrogen, 32.265 g (0.10 mol) of 3,3',4,4'-benzophenone tetracarboxylic dianhydride was refluxed in 250 ml of methanol for 1 to 5 hours to obtain the corresponding diacid diester. Distilled off, the remaining methanol was removed under reduced pressure, 27.338g (0.11mol) of 1,3-bis(3-aminopropyl)tetramethyldisiloxane, 31ml of chlorobenzene and 123ml of N- Methyl-2-pyrrolidone is dissolved and added to the diester of diacid. After fully stirring, react at 164°C for 6 hours to form an amino-terminated polyimide resin solution. After it is naturally cooled, add maleic acid 1.961 g (0.02 mol) of dianhydride, after reacting at room temperature for 8 hours, add 205 ml of chlorobenzene, reflux and separate water at 132°C for 32 hours, after cooling, pour the reaction solution into high-speed stirring absolute ethanol to obtain a precipitate After fully washing the obtained precipitate with absolute ethanol and anhydrous ether successively, and vacuum drying...
Embodiment 2
[0041] Under the protection of nitrogen, 24.851 g (0.08 mol) of 3,3',4,4'-diphenyl ether tetraacid dianhydride was refluxed in 174 ml of ethanol for 1 to 5 hours to obtain the corresponding diacid diester. The ethanol was evaporated After removing the remaining ethanol under reduced pressure, 20.369 g (0.09 mol) of 3,3′-dimethyl-4,4′-diaminodiphenylmethane was used, 20 ml of chlorobenzene and 98 ml of N-methane were used. After dissolving the 2-pyrrolidone, add it to the diacid diester. After fully stirring, react at 168°C for 10 hours to form an amino-terminated polyimide resin solution. After it cools naturally, add maleic acid 1.961 g (0.02 mol) of dianhydride, react at room temperature for 12 hours, add 274 ml of chlorobenzene, reflux and separate water at 130°C for 36 hours, after cooling, pour the reaction solution into high-speed stirring absolute ethanol to obtain a precipitate After fully washing the obtained precipitate with anhydrous ethanol and anhydrous ether successi...
Embodiment 3
[0044] Under the protection of nitrogen, 8.827 g (0.03 moles) of 3,3',4,4'-bipyromellitic dianhydride and 19.359 g of 3,3',4,4'-benzophenonetetracarboxylic dianhydride ( 0.06 mol) was refluxed in 230 ml of methanol for 1 to 5 hours to obtain the corresponding diacid diester. The methanol was distilled off, and the remaining methanol was removed under reduced pressure to remove 1.4-bis(4-aminophenoxy)-2 -Tert-butylbenzene 13.938g (0.04mol), 1.4-bis(4-aminophenoxy)-2.5-di-tert-butylbenzene 24.273g (0.06mol), use 25ml chlorobenzene and 150ml N-methyl After the -2-pyrrolidone is dissolved, it is added to the diacid diester. After fully stirring, it is reacted at 172°C for 16 hours to form an amino-terminated polyimide resin solution. After it is naturally cooled, add the maleic acid Acid anhydride 1.961 g (0.02 mol), after reacting at room temperature for 24 hours, add 425 ml of chlorobenzene, reflux and separate water at 130°C for 29 hours, after cooling, pour the reaction solution i...
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