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Prepn process of polyimide microsphere

A technology of polyimide microspheres and polyamic acid, which is applied in the field of preparing polyimide microspheres from monomers in solution by dispersion polymerization, can solve the problem of poor control of particle shape and particle size distribution. Easy to degrade imide, high cost, low solubility of polyimide, etc., to achieve the effect of mild implementation conditions, increased yield, and simple operation method

Inactive Publication Date: 2007-12-19
NANJING UNIV OF TECH
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Problems solved by technology

However, the amount of microspheres obtained by this method is controlled, because the solubility of polyimide in organic solvents is extremely small, and the cost is high
[0009] Therefore, in order to overcome the disadvantages that the particle shape and particle size distribution cannot be well controlled and the polyimide is easy to degrade in the above-mentioned technology, the present invention develops a simple method for synthesizing polyimide microspheres, which improves the polyimide at high temperature. Solubility of imide Polyimide is directly synthesized in the solution, and polyimide is precipitated from the system in the form of microspheres by adding a poor solvent to the system, which can improve the solubility and degree of polymerization of polyimide, and increase the yield and cost reduction

Method used

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  • Prepn process of polyimide microsphere

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example 1

[0037] Example 1: In a 1 L three-necked flask, 19 g of 1,3-bis(3-aminophenoxy)benzene BAPB (commercially available) was dissolved in 160 g of NMP, and stirred until completely dissolved. Add about 20g of PVA into this homogeneous solution, stir and dissolve evenly. Add 21 g of triphenyl ether tetra-acid dianhydride HQDPA (commercially available) in three times, add 0.2 g of phthalic anhydride after polymerization, and polymerize at 60°C for four hours to obtain a polyamide with a solid content of 20%. Acid solution 200g. Then according to the process conditions, 2.37 g of triethylamine catalyst and 10.6 g of dehydrating agent acetic anhydride were sequentially added for chemical imidization. After the stirring reaction is complete, 400 g of an aqueous solution of PVA with a mass concentration of 10% is prepared and added dropwise to the imidized reaction system. The aqueous solution of the dispersant needs to be added after the previous solution is completely dissolved, unti...

example 2

[0038] Example 2: In a 500 mL open beaker, 35 g of diaminotriphenylamine DATPA (commercially available) was dissolved in 90 g of DMAc, and stirred until completely dissolved. Add about 5g of PVA into this homogeneous solution, stir and dissolve evenly. Add 5.12 g of 3,3,4,4,-biphenyltetracarboxylic dianhydride (commercially available) BPDA (commercially available) in four times, and polymerize for four hours in a water bath at 70°C to obtain 100 g of a polyamic acid solution with a solid content of 10%. . Then, 1.4 g of pyridine catalyst and 3.6 g of dehydrating agent acetic anhydride were sequentially added according to the process conditions for chemical imidization. After complete stirring, 300 g of an aqueous solution of PVA with a mass fraction of 3% was prepared and added dropwise to the imidized reaction system. The aqueous solution of the dispersant needs to be added after the previous solution is completely dissolved, until the precipitate no longer disappears, cont...

example 3

[0039] Example 3: In a 1 L three-necked flask, 19 g of 1,3-bis(3-aminophenoxy)benzene BAPB (commercially available) was dissolved in 160 g of NMP, and stirred until completely dissolved. Add about 10g of PVP into this homogeneous solution, stir and dissolve evenly. Add 21g of triphenyl ether tetra-acid dianhydride HQDPA (commercially available) in three times, add 0.2g of phthalic anhydride after polymerization, and polymerize at 60°C for five hours to obtain a polyamide with a solid content of 20%. Acid solution 200g. Then, 4.2 g of pyridine catalyst and 10.6 g of dehydrating agent acetic anhydride were sequentially added according to the process conditions for chemical imidization. Stir to complete the reaction. Prepare 400 g of an aqueous solution of PVP with a mass fraction of 10%, and add it dropwise into the imidized reaction system. The aqueous solution of the dispersant needs to be added after the previous solution is completely dissolved, until the precipitate no l...

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Abstract

The present invention relates to dispersive polymerization process of preparing polyimide microsphere in monomer solution. The process includes the following steps: dissolving monomer diamine and dispersant in organic solvent through stirring; stage adding monomer diamine and heating for polymerizing to prepare polyamic acid solution; adding catalyst and dewatering agent successively for chemical imination; dropping water solution of dispersant to separate out solid grains, centrifugally filtering, washing and stoving to obtain polyimide microsphere. Thus prepared polyimide microsphere has glass transition temperature Tg of 200-300 deg.c, and grain size of 0.1-100 micron. The process has high polyimide yield, low cost and controllable grain shape and size distribution.

Description

technical field [0001] The invention relates to the technical field of preparing polyimide microspheres, in particular to a method for preparing polyimide microspheres from monomers in solution by adopting a dispersion polymerization method. Background technique [0002] Polymer microsphere is a new type of functional material with excellent performance. It has the characteristics of large specific surface area, strong adsorption, large cohesion and strong surface reaction ability. The field shows good application prospects and can be used as a chromatographic filler for chromatographic analysis. Polyimide not only has good mechanical properties, but also has outstanding heat resistance, chemical resistance, and excellent overall performance; therefore, it is widely used as electronic materials, automotive parts materials, substitutes for metals and ceramics, and other application. Utilizing the heat resistance of polyimide, heat-resistant polyimide microspheres with bette...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J3/12
Inventor 黄培王晓东朱鹏蒋远媛
Owner NANJING UNIV OF TECH
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