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

Inactive Publication Date: 2008-05-28
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, some traditional polyimide synthesis methods use expensive aromatic difluorides as synthetic monomers, so the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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.

[0028] (7) Add polyiminoketone, lithium benzene and tetr...

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;

[0042] (7) Add polyiminoketone, lithium benzene and ...

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Abstract

The invention relates to a synthesis method of polyuralcohol, belonging to polymer technical field, which comprises that adds dihalide aromatic ketone, sodium tert-butoxide NaOt-Bu, 1, 1'-dinaphthalene-2, 2'-diphenylphosphino BINAP, aromatic diamine and Pd2(dba)3 into a three-mouth flask with nitrogen gas feeding in turn, wherein the mole ratio is 1:1:2.8:0.03:0.01, adds N, N-dimethylacetamide until the monomer density is 0.5-0.65mol / L, increases temperature from 20DEG C to 100DEG C, keeps for 4-6h, increases temperature from 100DEG C to 150-200DEG C, keeps for 20-24h, cools to 20DEG C, adds the mixture of ammonia and methanol at the ratio of 1:4(L / L), mixes, stands for 1h, washes via the mixture of ammonia and methanol for three times, filters, dries at vacuum for 6h, mixes and dissolves poly(imino ketone) and benzoyl chloride in tetrahydrofuran for 2-12h at 1-3DEG C, to obtain polyuralcohol to be dried. The synthesized polyuralcohol Tg is higher than 190DEG C and TD is higher than 450DEG C, with better heat stability and dynamic mechanical stability.

Description

technical field [0001] The invention belongs to the technical field of polymers, and more specifically relates to the improvement and innovation of the synthesis method of polyiminoalcohol. Background technique [0002] High-performance polymers are extremely valuable and often have special applications. Due to its unique physical, chemical and mechanical properties, it can be used in industries such as automobiles, aircraft, aerospace, and medicine. However, due to their high production costs, only a few have been commercialized. As a new high-performance polymer material, polyimide has been successfully synthesized and characterized, and it has good heat resistance (T g >180°C, T D >450°C) and good solubility properties. However, some traditional synthesis methods of polyimide ketones use expensive aromatic difluorides as synthetic monomers, resulting in high costs. The main chain of the polyimide ketone molecule contains a carbonyl group, which is a very active...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/40
Inventor 林润雄常冠军王莹崔轶焦文秀
Owner QINGDAO UNIV OF SCI & TECH
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