Bisphenols monomer with imide structure and its synthesis

A technology containing imides and monomers, applied in the field of polymer chemistry, can solve the problems of polyamic acid solution instability and water vapor sensitivity

Inactive Publication Date: 2005-10-12
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The two-step method is to obtain the precursor polyamic acid first, and then generate PI through heating or chemical methods, intramolecular dehydration and ring closure. The process is mature and practical. It is a method widely used in actual production, but the polyamic acid solution is unstable. , is sensitive to moisture and often decomposes during storage

Method used

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  • Bisphenols monomer with imide structure and its synthesis
  • Bisphenols monomer with imide structure and its synthesis
  • Bisphenols monomer with imide structure and its synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 200mlDMF to the there-necked flask equipped with mechanical stirring, thermometer and reflux condenser, put 21.8g (0.1mol) pyromellitic dianhydride (a) and 21.8g (0.2mol) p-aminophenol into it, at room temperature Stir vigorously for 2 hours, when the system becomes a clear solution, add toluene as a water-carrying agent, continue heating and stirring under the protection of nitrogen, and reflux with water at 110°C-120°C for 3 to 4 hours, the clear solution becomes a suspension Liquid, distill toluene at 140°C-150°C and continue to reflux at this temperature, cool down and discharge the material after 4 to 5 hours, wash with ethanol three times to remove the organic solvent in the mixed system, then boil and wash with water for 3 to 4 times, After suction filtration with a Buchner funnel, the solid product was dried in an oven at 80°C-100°C to obtain a light yellow powdery solid (38g, yield 87%), which was pure isophthalic imide bisphenol mono body.

Embodiment 2

[0028] Add 200ml NMP to the three-necked flask equipped with mechanical stirring, thermometer and reflux condenser, put 21.8g (0.1mol) pyromellitic dianhydride (a) and 21.8g (0.2mol) p-aminophenol into it, at room temperature Stir vigorously for 2 hours, when the system becomes a clear solution, add toluene as a water-carrying agent, continue heating and stirring under the protection of nitrogen, and reflux with water at 110°C-120°C for 3 to 4 hours, the clear solution becomes a suspension Liquid, distill toluene at 140°C-150°C and continue to reflux at this temperature, cool down and discharge the material after 4 to 5 hours, wash with ethanol three times to remove the organic solvent in the mixed system, then boil and wash with water for 3 to 4 times, After suction filtration with a Buchner funnel, the solid product was dried in an oven at 80°C-100°C, and the obtained light yellow powdery solid (33g, yield rate 77%) was pure isophthalic imide bisphenol monomer.

[0029] 2. ...

Embodiment 3

[0031] Add 205mlDMF in the there-necked flask equipped with mechanical stirring, thermometer and reflux condenser, mix 26.8g (0.1mol) naphthalene-1,4,5,8-dianhydride (b) with 21.8g (0.2mol) p-aminophenol Put it into it and stir vigorously at room temperature for 2 hours. When the system becomes a clear solution, add toluene as a water-carrying agent, continue heating and stirring under the protection of nitrogen, and reflux with water at 110°C-120°C for 3 to 4 hours. The clarified solution becomes a suspension, steam the toluene at 140°C-150°C and continue to reflux at this temperature, cool down and discharge the material after 4 to 5 hours, wash with ethanol three times to remove the organic solvent in the mixed system, and boil with water After washing 3 to 4 times, and suction filtering with a Buchner funnel, the solid product was dried in an oven at 80°C-100°C to obtain a yellow powdery solid (44g, yield 90%) which was pure naphthalene-1,4 , 5,8-diimide bisphenol monomer....

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Abstract

Bisphenol monomer with acid imide structure and its synthesis are disclosed. It is carried out by taking 1,2,4,5-benzenetetracarboxylic acid dianhydride or naphthyl-1,4,5,8-dianhydride or p-aminophenol as material, taking DMF as reacting solvent, agitating for 2-3 hrs at room temperature, clarifying the system into solution, adding methylbenzene or dimethyl benzene with volume ratio 1 / 3-1 / 2 of solvent, continuous heating and agitating under nitrogen protecting, back-flowing with water for 3-4 hrs at 110-120deg.C, the light liquid changing into suspensoid, evaporating out methylbenzene, back-flowing for 4-5 hrs at 140-150deg.C, lowering temperature, discharging, washing for 3-4 times by alcohol, removing organic solvent in mixed system, boiling for 3-4 times by water, drying the solid products in oven at 80-100deg.C, and obtaining powdered solid pure products. It achieves high productivity.

Description

technical field [0001] The invention belongs to the field of polymer chemistry, and in particular relates to a bisphenol monomer containing an imide structure and a synthesis method of the monomer. Background technique [0002] Polyimide is a kind of polymer with imide ring as the characteristic structure. It has outstanding heat resistance and can maintain its excellent mechanical properties and dielectric properties between 200°C and 260°C. In aerospace, It is widely used in communication, electronic technology, mechanization and chemical industry and other fields. [0003] The common synthetic method of polyimide has one-step method and two-step method, and one-step method is that dianhydride and diamine carry out solution polymerization in high boiling point solvent to directly generate polyimide (PI), and the reaction condition of this method is higher than Heat treatment is much milder, but the reaction cycle is long, and the requirements for solvents are relatively h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/00C07D471/04C07D487/04
Inventor 那辉窦志宇
Owner JILIN UNIV
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