Preparation method of poly-p-phenylene ben-zobisthiazole fiber
A technology of benzobisoxazole and polyparaphenylene, which is applied in the directions of fiber processing, fiber chemical characteristics, dry spinning method, etc., can solve the problems of good spinnability, poor processing performance, difficult synthesis of PBO spinning system, and the like, Achieve the effect of good spinnability, strong dissolving ability, and solvent recyclability
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Embodiment 1
[0037] A preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the steps of:
[0038] (1) Add 2L of solvent DMAC to a polymerization kettle with nitrogen gas, add 179.4g of 4,6-diaminoresorcinol, stir for 30min, add 6.6g of catalyst isoquinoline, and add part of terephthaloyl dichloride 121.1g , add 1.65g of stannous chloride, stir for 30min, then add remaining 30.2g of terephthaloyl chloride, stir and react at 0°C for 24 hours to obtain the precursor PHA spinning solution;
[0039] (2) After the above PHA solution is filtered and degassed, it is extruded through a spinneret and then dry-spun. The hot air temperature in the spinning tunnel is 250°C, and the spinning air volume is 8m 3 / min, the line speed of the first roll is 500m / min, to obtain PHA as-spun fibers. The solvent volatilized during the fiber forming process is taken out by the hot air and then enters the solvent recovery device, where it is separated by multi-stage tray vacuum distillation to...
Embodiment 2
[0044] A preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the steps of:
[0045] (1) In a nitrogen-filled polymerization kettle, add 2L solvent NMP, add 223.1g of 4,6-diaminoresorcinol, stir for 60min, add catalyst pyridine 0.41g, add part of terephthaloyl dichloride 150.4g, add 0.71g of stannous chloride, stirred for 30min, then added the remaining 37.6g of terephthaloyl chloride, stirred and reacted at 20°C for 24 hours, and the precursor PHA spinning solution was obtained;
[0046] (2) After the above PHA solution is filtered and degassed, it is extruded through a spinneret and then dry-spun. The hot air temperature in the spinning tunnel is 200°C, and the spinning air volume is 30m 3 / min, the line speed of the first roll is 800m / min, to get PHA as-spun fibers. The solvent volatilized during the fiber forming process is taken out by the hot air and then enters the solvent recovery device, where it is separated by multi-stage tray vacuum distillati...
Embodiment 3
[0051] A preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the steps of:
[0052] (1) Add 2L of solvent DMAC to a polymerization kettle with nitrogen gas, add 338.8g of 4,6-diaminoresorcinol, stir for 50min, add 0.62g of catalyst isoquinoline, and add part of terephthaloyl dichloride 228.6g , add 12.4g of stannous chloride, stir for 30min, then add remaining 57.1g of terephthaloyl chloride, stir and react at 10°C for 24 hours to obtain the precursor PHA spinning solution;
[0053] (2) After the above PHA solution is filtered and degassed, it is extruded through a spinneret and then dry-spun. The hot air temperature in the spinning tunnel is 150°C, and the spinning air volume is 15m 3 / min, the line speed of the first roll is 1000m / min, to get PHA as-spun fibers. The solvent volatilized during the fiber forming process is taken out by the hot air and then enters the solvent recovery device, where it is separated by multi-stage tray vacuum distillation t...
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