Method for synthesizing polyimino-alcohol
A technology of polyiminool and synthesis method, which is applied in the field of polymers, can solve the problems of high cost, and achieve the effects of low cost, high thermal decomposition temperature, and wide range of rubber states
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Embodiment 1
[0021] Example 1. A method for synthesizing polyiminoalcohol. Include the following steps:
[0022] (1) Add dihalogenated aromatic ketone, sodium tert-butoxide NaO to a three-necked flask with nitrogen gas t -Bu, 1.1′-binaphthyl-2.2′-diphenylphosphine BINAP, aromatic diamine and Pd 2 (dba) 3 , the molar ratio is 1:1:2.8:0.03:0.01;
[0023] (2) Add N,N-dimethylacetamide (DMAc) to keep the monomer concentration between 0.5 and 0.65mol / L;
[0024] (3) Raise the system from 20°C to 100°C and keep it for 4-6 hours, then raise the temperature from 100°C to 200°C and keep it for 20 hours;
[0025] (4) Slowly cool the system to 20°C, pour it into a mixed solution of ammonia water and methanol, wherein ammonia water / methanol=1:4 (L / L), stir, and let stand for 1h;
[0026] (5) wash 3 times with ammonia water and methanol mixed solution, filter;
[0027] (6) Vacuum drying at 100° C. for 6 hours to obtain polyimide ketone.
Embodiment 2
[0033] Example 2. A polycondensation synthesis method of polyiminool. Equipped with a water condensing device, an oil bath, and a magnetic stirring device, add 1.776 g (4 mmol) of 1,4-bis-(4'bromobenzoyl)benzene, sodium tert-butoxide NaOt -Bu1.076g (11.2mmol), 1.1'-binaphthyl-2.2'-diphenylphosphine (BINAP) 74.8mg (0.12mmol), 4-[(4'aminophenyl)diazenyl]aniline 1.368g (4mmol ) and tris(dibenzylideneacetone)dipalladium (Pd2(dba)3) 36.6mg (0.04mmol). 6 mL of N,N-dimethylacetamide (DMAc) was added. The system was raised from room temperature 20°C to 100°C and kept for 5h, then raised from 100°C to 150°C and kept for 20h. Slowly cool to room temperature 20°C, pour into a mixed solution of ammonia water and methanol, wherein ammonia water / methanol=100mL / 400mL, stir, and let stand for 1h. Wash 3 times with a mixed solution of ammonia water and methanol, and filter. Vacuum-dried under nitrogen for 6 h. The obtained polyiminoketone-3 (PIK-3) was a yellow-green solid. The obtained...
Embodiment 3
[0035] Example 3. A polycondensation synthesis method of polyiminool. Include the following steps:
[0036] (1) Add dihalogenated aromatic ketone, sodium tert-butoxide NaO to a three-necked flask with nitrogen gas t -Bu, 1.1′-binaphthyl-2.2′-diphenylphosphine BINAP, aromatic diamine and Pd 2 (dba) 3 , the molar ratio is 1:1:2.8:0.03:0.01;
[0037] (2) Add N,N-dimethylacetamide DMAc to keep the monomer concentration between 0.5 and 0.65mol / L;
[0038] (3) Raise the system from 20°C to 100°C and keep it for 4-6 hours, then raise the temperature from 100°C to 150°C and keep it for 22 hours;
[0039] (4) Slowly cool the system to 20°C, pour it into a mixed solution of ammonia water and methanol, wherein ammonia water / methanol=1:4 (L / L), stir, and let stand for 1h;
[0040] (5) wash 3 times with ammonia water and methanol mixed solution, filter;
[0041] (6) Vacuum drying at 100°C for 6 hours to obtain polyimide ketone;
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