Application of 3D printing in cross-linked polyimide, preparation of porous polyimide and preparation of polyimide composite material
A 3D printing and polyimide technology, which is applied in application, additive processing, household appliances, etc., can solve the problem of high heat-resistant cross-linked polyimide 3D printing, which has less research on 3D printing and thermosetting polyimide. Reduced thermal performance of parts, difficult to melt and high temperature resistant cross-linked polyimide, etc., to achieve the effect of rich pores, excellent dimensional stability, and enhanced van der Waals force
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[0036] The invention provides a preparation method of direct writing 3D printing cross-linked porous polyimide, comprising the following steps:
[0037] Mix polyamic acid, organic solvent and porogen to obtain polyamic acid ink;
[0038] Carrying out direct writing 3D printing with the polyamic acid ink to obtain 3D printing components;
[0039] The 3D printing component is heat-treated to obtain a cross-linked porous polyimide.
[0040] In the present invention, unless otherwise specified, the required preparation materials are commercially available products well known to those skilled in the art.
[0041] The invention mixes polyamic acid, organic solvent and porogen to obtain polyamic acid ink. In the present invention, the number average molecular weight of the polyamic acid corresponding to the polyimide is preferably 5000-50000 g / mol, more preferably 10000-30000 g / mol; the polyamic acid is preferably:
[0042]
[0043] In the present invention, there is no special l...
Embodiment 1
[0078] (1) Preparation of polyamic acid powder: under a nitrogen atmosphere, dissolve 4.9199g of 4,4'-diaminodiphenyl ether in 70mL of N,N-dimethylformamide, and add 10.4707 g 4,4'-(hexafluoroisopropene) diphthalic anhydride, remove the ice bath after 1 hour of reaction, and after 5 hours of reaction at room temperature, add 0.4965g of 4-phenylethynylphthalic anhydride and add 20mL of N,N-dimethylformamide , continue to react for 24h to obtain a polyamic acid solution with a solid content of 15%, the polyamic acid solution is poured into a mixed solution of water and ethanol (4:1 by volume) under excessive stirring conditions, and then the resulting white Soak the solid in the mixed solution of water and ethanol for 12 hours, filter and wash with water, dry at 80°C for 12 hours, pulverize the obtained solid with a pulverizer, and sieve with a 100-mesh sieve to obtain polyamic acid powder, corresponding to the number of polyimide The average molecular weight is 18700g / mol;
[...
Embodiment 2
[0084] Mix 6 parts of polyamic acid powder prepared in Example 1, 4 parts of N,N-dimethylformamide and 15 parts of sodium chloride with a particle size of less than 300 mesh at room temperature for ball milling, the ball milling time is 30min, and the ball milling rate is 3000r / min, the resulting mixed material is pumped and centrifuged to remove air bubbles to obtain polyamic acid ink;
[0085] Direct writing 3D printing and heat treatment were carried out in the same method as in Example 1, and the obtained article was soaked in deionized water for 12 hours, then taken out, washed with deionized water, and dried to obtain a cross-linked porous polyimide.
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