A kind of preparation method of polyamideimide precipitated fiber
A technology of polyamide-imide and polyamide-imide stock solution, which is applied in the field of fiber preparation, can solve the problems of difficult removal of catalyst and instability of trimellitic anhydride chloride in water, etc., and achieve easy control of shape and size and rich hairiness , the effect of simple operation
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Embodiment 1
[0023] Under the protection of nitrogen deoxygenation, add 3L of N-methylpyrrolidone, 35.5g of lithium chloride, 56.7g of 2,6-diaminotoluene, and 105.6g of 4,4'-diaminobenzoanilide into a 5L polymerization kettle After completely dissolving, add 299.5 g of benzophenone tetra-acid dianhydride and react at 0°C for 5-10 hours. Under the protection of nitrogen, 17.76 g of the chemical cyclization catalyst isoquinoline was added dropwise, and then under the condensing and reflux device, the temperature was raised step by step, stirred, and polymerized at 100 ° C for 3 h, 120 ° C for 3 h, and 185 ° C for 3 h, and the solid content was obtained. 13% polyamideimide spinning dope with intrinsic viscosity of 3.2dl / g.
[0024] Dilute the spinning stock solution to 3% and inject it into the sedimentation solution to prepare the precipitation fiber. The injection speed is 5ml / min, the temperature of the precipitation solution is 20-30°C, and 10ml of the polyamide-imide solution is added to...
Embodiment 2
[0026] Under the protection of nitrogen deoxygenation, add 3L of dimethylacetamide, 32.3g of lithium chloride, 51.9g of 2,4-diaminotoluene, and 95.9g of 4,4'-diaminobenzanilide into a 5L polymerization kettle After completely dissolving, add 272.3 g of benzophenone tetra-acid dianhydride and react at 0°C for 5-10 hours. Under the protection of nitrogen, 16.1 g of the chemical cyclization catalyst isoquinoline was added dropwise, and then under the condensing and reflux device, the temperature was raised step by step, stirred, and polymerized at 100 ° C for 3 h, 130 ° C for 3 h, and 150 ° C for 5 h, and the solid content was obtained. 14% polyamideimide spinning dope with intrinsic viscosity of 3.5dl / g.
[0027] Dilute the spinning stock solution to 5% and inject it into the sedimentation solution to prepare the precipitation fiber. The injection speed is 5ml / min, the temperature of the precipitation solution is 20-30°C, and 10ml of the polyamide-imide solution is added to the ...
Embodiment 3
[0029] Under the protection of nitrogen deoxygenation, 3L of dimethylformamide, 32.6g of lithium chloride, 78.4g of 4,4'-diaminodiphenylmethane, 4,4'-diaminobenzoyl For aniline 89.9g, after completely dissolving, add 255.1g of benzophenone tetra-acid dianhydride and react at 0°C for 5-10h. Under the protection of nitrogen, 16.3 g of the chemical cyclization catalyst isoquinoline was added dropwise, and then under the condensing and reflux device, the temperature was raised in stages, stirred, and polymerized at 100 ° C for 3 h, 120 ° C for 3 h, and 150 ° C for 5 h, and the solid content was obtained. 15% polyamideimide spinning dope with intrinsic viscosity of 2.8dl / g.
[0030] Dilute the spinning stock solution to 4% and inject it into the sedimentation solution to prepare the precipitation fiber. The injection speed is 5ml / min, the temperature of the precipitation solution is 20-30°C, and 10ml of the polyamide-imide solution is added to the In the precipitation solution of ...
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