Preparation method of polyimide fiber
A technology of polyimide fiber and nascent fiber, which is applied in fiber treatment, spinning solution preparation, fiber chemical characteristics, etc., can solve the problems of unstable spinning, unstable viscosity of polyamic acid solution, difficult filtration, etc. The effect of controlling the molecular weight and viscosity of the system and improving the spinnability
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Embodiment 1
[0029] 1. Stock solution preparation: mix p-phenylenediamine with 3,3′,4,4′-biphenyltetraacid dianhydride at a total molar ratio of 1:0.99, and mix 10.0807g (0.1mol) of terephthalic Add amine, 203.3g N,N-dimethylacetamide and 22.3g 1-methyl-2-pyrrolidone into a four-neck flask (water content 410ppm), stir at room temperature and under nitrogen protection, after completely dissolving, stir at 20°C Add 29.1080g (0.099mol) 3,3′,4,4′-biphenyltetraacid dianhydride powder at a speed of 250 rpm, and continue stirring for 0.5 hours to obtain the desired polyamic acid solution with a solid content of 14.8%. . Then the spinning solution was left to stand under reduced pressure to remove air bubbles, and then filtered through an 8 μm filter material to obtain a polyamic acid spinning stock solution. The solution was tested by filtration without gel generation, the apparent viscosity of the solution was 108 Pa·s at 25°C, and the intrinsic viscosity was 1.43dL / g at 25°C.
[0030] 2. Coag...
Embodiment 2
[0037] 1. Stock solution preparation: mix 4,4′-diphenyl ether diamine with 3,3′,4,4′-biphenyltetraacid dianhydride at a total molar ratio of 1:1.005, mix 20.0090g (0.1 mol) of 4,4′-diphenyl ether diamine, 100.5g of N,N-dimethylacetamide and 15.1g of 1-methyl-2-pyrrolidone into a four-necked flask (water content 700ppm), stirred at room temperature and Under nitrogen protection, after complete dissolution, adjust the temperature to 40°C, add 29.5470g (0.1005mol) of 3,3′,4,4′-biphenyltetraacid dianhydride powder at a stirring speed of 250 rpm, and continue stirring After 10 hours, the desired polyamic acid solution with a solid content of 30% was obtained. Then the spinning solution was left to stand under reduced pressure to remove air bubbles, and then filtered through an 8 μm filter material to obtain a polyamic acid spinning stock solution. The solution was tested by filtration without gel formation, the apparent viscosity of the solution was 269 Pa·S at 25°C, and the intri...
Embodiment 3
[0041] 1. Stock solution preparation: mix 4,4′-diphenyl ether diamine with 3,3′,4,4′-biphenyltetraacid dianhydride at a total molar ratio of 1:0.98, mix 20.0090g (0.1 mol) of 4,4′-diphenyl ether diamine, 773.0g N,N-dimethylacetamide and 154.6g 1-methyl-2-pyrrolidone into a four-necked flask (water content 450ppm), stirred at room temperature and Under the protection of nitrogen, after completely dissolving, cool in an ice-water bath to -10°C, add 28.8120g (0.098mol) of 3,3′,4,4′-biphenyltetraacid dianhydride powder at a stirring speed of 250 rpm, Stirring was continued for 8 hours to obtain the desired polyamic acid solution with a solid content of 5%. Then the spinning solution was left to stand under reduced pressure to remove air bubbles, and then filtered through an 8 μm filter material to obtain a polyamic acid spinning stock solution. The solution was filtered and tested to have no gel. The apparent viscosity of the solution was 53 Pa·S at 25° C., and the intrinsic visc...
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