Preparation method of phenolic hydroxyl group containing polyimide powder

A technology of phenolic hydroxyl polyimide containing phenolic hydroxyl groups, which is applied in the field of preparation of high-temperature-resistant high-performance aromatic heterocyclic polymer powders, can solve the problems of difficult wastewater treatment, strong pungent odor, and high production costs, and achieve effective Conducive to environmental protection, easy solvent recovery, and product cost reduction effects

Inactive Publication Date: 2007-03-14
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The shortcoming of this method is: (1) use triethylamine / acetic anhydride system to carry out imidization reaction, production cost height, pungent smell is big, brings inconvenience to operation, also pollutes environment; (2) organic solvent separation , It is difficult to recycle and reuse, and the treatment cost is high; (3) Operations such as adding water for precipitation and washing produce a large amount of wastewater, and the treatment of wastewater is difficult and expensive
This will undoubtedly increase the cost and the three wastes and other issues

Method used

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  • Preparation method of phenolic hydroxyl group containing polyimide powder
  • Preparation method of phenolic hydroxyl group containing polyimide powder
  • Preparation method of phenolic hydroxyl group containing polyimide powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 25.8 grams (0.1 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) propane (B3A4HPP) into the polymerization bottle, add 400 milliliters of N-methyl-2-pyrrolidone (NMP), and feed Nitrogen, cooled to 5°C in an ice-water bath, stirred to make it completely dissolved, then added 21.8 grams (0.1 moles) of pyromellitic dianhydride (PMDA) powder, stirred and reacted for 3 hours, and viscous poly-o-hydroxyamide was obtained acid solution. Subsequently, nitrogen gas was introduced, 40 ml of toluene was added, the temperature was raised to reflux, and the temperature was maintained at 140° C. for 18 hours. A yellow solid powder was precipitated in the reaction flask, the heating system was turned off, stirred rapidly, cooled to room temperature naturally, filtered and washed to obtain polyimide powder containing phenolic hydroxyl groups. There is an obvious OH absorption peak in the infrared spectrum absorption spectrum (3400cm -1 ), the characteristic absorption peak of the imine...

Embodiment 2

[0031] Add 25.8 grams (0.1 moles) of 2,2-bis(3-amino-4-hydroxyphenyl)propane (B3A4HPP) into the polymerization bottle, add 450 milliliters of N-methyl-2-pyrrolidone (NMP), and feed Nitrogen, ice-water bath cooling to 5 ° C, stirring, to make it completely dissolved, add 10.9 grams (0.05 moles) pyromellitic dianhydride (PMDA) powder and 14.7 grams (0.05 moles) 3,3',4,4' - Tetraformic acid biphenyl dianhydride (BPDA) powder, after stirring and reacting for 3 hours, a viscous poly-o-hydroxyamic acid solution was obtained. Subsequently, nitrogen gas was introduced, 500 ml of toluene was added, the temperature was raised to reflux at 160°C, and after keeping for 5 hours, part of the toluene was distilled off. A yellow solid powder was precipitated in the reaction flask, the heating system was turned off, stirred rapidly, cooled to room temperature naturally, filtered and washed to obtain polyimide powder containing phenolic hydroxyl groups.

Embodiment 3

[0033] 12.9 g (0.05 mol) of 2,2-bis(3-amino-4-hydroxyphenyl)propane (B3A4HPP) and 18.3 g (0.05 mol) of 2,2-bis(3-amino-4-hydroxyphenyl) -1,1,1,3,3,3-hexafluoropropane (B3A4HPFP) was added to the polymerization bottle, 400 ml of N,N-dimethylacetamide (DMAc) was added, nitrogen gas was introduced, and the ice-water bath was cooled to 0 ℃, stirring, after making it completely dissolved, add 10.9 (0.05 mol) gram of pyromellitic dianhydride (PMDA) powder and 14.7 gram (0.05 mol) of 3,3',4,4'-tetracarboxylic biphenyl dianhydride (BPDA) powder, after stirring and reacting for 12 hours, a viscous poly-o-hydroxyamic acid solution was obtained. Subsequently, nitrogen gas was introduced, 600 ml of toluene was added, the temperature was raised to reflux, and after being kept at 120° C. for 5 hours, part of the toluene was distilled off. A yellow solid powder was precipitated in the reaction flask, the heating system was turned off, stirred rapidly, cooled to room temperature naturally, f...

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Abstract

The preparation process of phenolic hydroxyl group-containing polyimide powder includes the following steps: 1. reaction of phenolic hydroxyl group-containing aromatic diamine compound or its mixture with other diamine compound and aromatic binary anhydride in the molar ratio of 1 to 1 in strong polar non-protonic organic solvent under protection of nitrogen at 0-30 deg.c for 3-12 hr to obtain transparent ropy polyhydroxy amido acid solution; and 2. adding azeotropic dewatering agent in nitrogen atmosphere and heating to 120-160 deg.c to reflux, azeotropically dewater and imidize for 5-18 hr, cooling to room temperature, washing and vacuum drying to obtain phenolic hydroxyl group-containing polyimide powder. The industrial production process has environment friendship, simple operation, low cost and easy solvent recovery.

Description

technical field [0001] The invention relates to a preparation method of a high-temperature-resistant high-performance aromatic heterocyclic polymer powder containing active phenolic hydroxyl reactive groups, in particular to a preparation method of a phenolic hydroxyl-containing polyimide powder. Background technique [0002] Polyimide is a class of polymers with excellent comprehensive properties. It has excellent heat resistance, low temperature resistance, solvent resistance, self-lubrication, radiation resistance and flame retardancy. At the same time, it also has very good mechanical and dielectric properties. Therefore, it is widely used in high-temperature and radiation-resistant materials such as spacecraft, satellites or space vehicles; advanced structural composite materials in aerospace, automotive, electromechanical, etc., C-level or 200-level electrical insulation materials, high-temperature resistant adhesives etc.; and FPC or PCB base materials in the field o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J3/12
Inventor 虞鑫海赵炯心徐永芬
Owner DONGHUA UNIV
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