Diamine compound, polyimide fiber and preparation method thereof
A polyimide fiber and amine compound technology, which is applied in the field of functional polymer fibers, can solve the problems of ineffective effects of ultraviolet radiation and electron beam radiation, and achieve excellent atomic oxygen resistance and improved structure
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[0089] In order to ensure the performance of the polyimide fiber, the present invention clearly describes the overall technical solution, and the present invention also provides a preparation method of the polyimide fiber, comprising the following steps:
[0090] 1) After the polyamic acid solution described in any one of the above technical solutions is subjected to a wet spinning forming process or a dry spinning forming process, polyamic acid fibers are obtained;
[0091] 2) After the polyamic acid fibers obtained in the above steps are imidized and thermally drawn, polyimide fibers are obtained.
[0092] In the present invention, firstly, the polyamic acid solution (polyamic acid solution) described in any one of the above technical solutions is subjected to a wet spinning forming process or a dry spinning forming process to obtain a polyamic acid fiber;
[0093] The present invention has no special limitation on the concentration of the polyamic acid solution, it can be pre...
Embodiment 1
[0121] Preparation of 3-[4-(POSS-methylene-oxy)benzoyl]-1,5-diaminobenzene
[0122] The synthetic route is shown in the following formula:
[0123] in,
[0124] 1), the synthesis of 3-[4-(POSS-methylene-oxy)benzoyl]-1,5-dinitrobenzene:
[0125] A, 3-(4-hydroxybenzoyl)-1,5-dinitrobenzene (2.882 g, 0.01 mol), monochloromethyl POSS (10.82 g, 0.01 mol) and 100 ml tetrahydrofuran were added to the reaction vessel. Stir at room temperature to dissolve. Sodium hydride (0.288 g, 0.012 mol) was added in portions. The reaction was continued for 6 hours. The reaction solution was poured into 250ml of water, and a white solid was precipitated, which was filtered and vacuum-dried at room temperature.
[0126] Finally, 9.8 g of the product was obtained, and the calculated yield was 73.4%. The 3-[4-(POSS-methylene-oxyl)-benzoyl]-1,5-dinitrobenzene prepared by the above steps of the present invention was characterized by NMR. The H NMR spectrum data are as follows:
[0127] 1H NMR (...
Embodiment 2
[0154] Dissolve 637.40g (0.5mol) of 3-[4-(POSS-methylene-oxy)benzoyl]-1,5-diaminobenzene and 54.07g (0.5mol) of p-phenylenediamine in 3500ml N , in N-dimethylacetamide, add 294.23g (1mol) 4,4'-biphenyl dianhydride under stirring, and react at 30°C for 24 hours to obtain a light yellow viscous polyamic acid spinning solution. After the solution is filtered Directly used as spinning slurry.
[0155] The above-mentioned polyamic acid slurry is spun and formed by dry-jet wet spinning technology, and the spinning slurry at room temperature is accurately measured by a metering pump, and then extruded from the spinneret hole and enters the N,N-dimethyl In a coagulation bath of methyl formamide and water (1:3 volume ratio). The spinneret has 30 holes, the hole diameter is Φ0.12mm, the spray ratio is 2.5 times, the spinning speed is 40m / min, and the air layer height is 15mm. The as-spun fibers were washed with water and then dried in a hot nitrogen tunnel to obtain polyamic acid fibe...
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