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A kind of synthetic method of flower-like structure polyimide

A technology of polyimide and flower-like structure is applied in the field of synthesis of flower-like structure polyimide, which can solve the problems of uneven structure, high cost of raw materials, small specific surface area of ​​polyimide materials, etc., and achieve uniform structure. , low price, less effect of three wastes

Active Publication Date: 2020-02-11
ZHUZHOU TIMES NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2012, Japanese scientist Shinji Watanabe et al first prepared diethyl pyromellitic acid by reacting pyromellitic dianhydride (PMDA) and ethanol, and then neutralized with aliphatic diamine to form nylon salt, which was passed through ethylene glycol The flower-shaped polyimide powder with a particle size of 15 μm was prepared by thermal imidization at 130°C, but its structure was not uniform, and the specific surface area of ​​the obtained polyimide material was also small
However, this method can only prepare a small amount of polyimide with a flower-like structure. In addition, the aromatic dianhydride monomers used in this research are all dianhydride monomers with special structures. The cost of raw materials is high, and it is difficult to implement in the industrial process.

Method used

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  • A kind of synthetic method of flower-like structure polyimide
  • A kind of synthetic method of flower-like structure polyimide
  • A kind of synthetic method of flower-like structure polyimide

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Experimental program
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Effect test

Embodiment 1

[0030] Such as figure 1 Shown, a kind of synthetic method of flower-like structure polyimide comprises the following steps:

[0031] (1) dissolving pyromellitic dianhydride monomer in ethanol through dewatering treatment, and reflux esterification to obtain pyromellitic acid diethyl;

[0032] (2) Keep the stirring rate at 80r / min, and slowly add 1,6-hexanediamine dropwise to the reaction solution in step (1), and react to obtain the carboxylic acid amine salt of the dibasic ester of 1,6-hexanediamine, Wherein, the addition amount of 1,6-hexanediamine is based on the molar ratio of 1,6-hexanediamine to pyromellitic dianhydride of 1.02:1;

[0033] (3) The carboxylic acid amine salt of the dibasic ester of 1,6-hexanediamine obtained in step (2) is spray-dried, and the process conditions of spray-drying are: the inlet air temperature is 80°C, and the outlet air temperature is 70°C. ℃, the amount of evaporating medium is 1800ml / h, and the maximum feeding amount is 200ml / h, and a ...

Embodiment 2

[0038] Such as figure 1 Shown, a kind of synthetic method of flower-like structure polyimide comprises the following steps:

[0039] (1) Dissolve 3,3',4,4'-benzophenone tetra-acid dianhydride monomer in ethanol that has been treated with water removal, and reflux esterification reaction to obtain 3'3,4'4-benzophenone tetra Acid diethyl ester solution;

[0040] (2) Keep the stirring rate at 70r / min, and slowly add 1,4-butanediamine dropwise to the reaction solution in step (1), and react to obtain the carboxylic acid amine salt of the dibasic ester of 1,4-butanediamine, Wherein, the addition amount of 1,4-butanediamine is based on the molar ratio of 1,4-butanediamine to 3'3,4'4-benzophenone tetraacid dianhydride is 1.02:1;

[0041] (3) The carboxylic acid amine salt of the dibasic ester of 1,4-butanediamine obtained in step (2) is spray-dried, and the process conditions of spray-drying are: the inlet air temperature is 80°C, and the outlet air temperature is 70°C. ℃, the amo...

Embodiment 3

[0046] Such as figure 1 Shown, a kind of synthetic method of flower-like structure polyimide comprises the following steps:

[0047] (1) dissolving the pyromellitic dianhydride monomer in ethanol through dewatering treatment, reflux esterification reaction to obtain pyromellitic acid diethyl ester solution;

[0048] (2) Keep the stirring rate at 75r / min, and slowly add 1,2-ethylenediamine dropwise to the reaction solution in step (1), and react to obtain the carboxylic acid amine salt of the dibasic ester of 1,2-ethylenediamine, Among them, the amount of 1,2-ethylenediamine added is based on the molar ratio of 1,2-ethylenediamine to pyromellitic dianhydride being 1.05:1;

[0049] (3) The carboxylic acid amine salt of the dibasic ester of 1,2-ethylenediamine obtained in step (2) is spray-dried, and the process conditions of spray-drying are: the inlet air temperature is 80°C, and the outlet air temperature is 70°C. ℃, the amount of evaporating medium is 1800ml / h, and the maxi...

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Abstract

The invention discloses a synthesis method of flower-like structure polyimide. The method comprises the following steps of (1) carrying out esterification reaction on a dianhydride monomer and alcohol to obtain aromatic tetrabasic acid dibasic ester; (2) obtaining a pyrazinecarboxamide salt of dibasic ester from a dianhydride monomer and the aromatic tetrabasic acid dibasic ester; (3) carrying out spray drying on the pyrazinecarboxamide salt of the dibasic ester to obtain a white powder solid; (4) adding the white powder solid to dihydric alcohol, raising the temperature and carrying out heat preservation reaction in a nitrogen atmosphere to obtain a product a; (5) centrifugally separating the product a, and washing the solid product by adopting an eluent; and (6) drying the washed solid product in the nitrogen atmosphere to obtain the flower-like structure polyimide. The method is a novel method and way for simply, efficiently and quickly preparing the flower-like structure polyimide, and the method has important application value.

Description

technical field [0001] The invention belongs to the field of polymer materials, in particular to a method for synthesizing polyimide with a flower-like structure. Background technique [0002] In recent years, the synthesis of multidimensional structural materials has become a research hotspot in the field of material synthesis technology, especially the shape control during the synthesis process has become the core technology in the key issues of functional material synthesis. Due to its extremely high specific surface area and unique physical and chemical properties, the flower-like structure has potential applications in high and low temperature adsorption materials, catalyst supports, biosensors, energy storage and other fields, especially in new catalyst materials. The research and development aspect has been highly valued by relevant scientific and technological workers at home and abroad. [0003] Polyimide material is one of the polymers with the highest temperature...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10
CPCC08G73/1028C08G73/1082
Inventor 王进高敬民王文志彭博胡天辉姜其斌李鸿岩
Owner ZHUZHOU TIMES NEW MATERIALS TECH