Method for preparing para-aramid pulp by ultrasonic induction

A para-aramid fiber pulp and ultrasonic technology, applied in spinning solution preparation, wet spinning, single-component polyamide rayon, etc., can solve the problems of serious environmental pollution, difficulty in solvent recovery, high investment cost, etc. , to achieve the effect of improving specific surface area, good fiber shape, simple and stable process

Inactive Publication Date: 2015-11-25
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to solve the problems of high equipment investment cost and complex process in the traditional preparation of para-aramid pulp; the general low-temperature solution direct polycondensation method adds an acid-binding agent, which is expensive, serious environmental pollution, and difficult to recover solvents. , and provide a method for preparing para-aramid pulp by ultrasonic induction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] in N 2 Under the protective effect of preparation 100mlN-methylpyrrolidone-calcium chloride (NMP-CaCl 2 ) solvent system, wherein the quality of calcium chloride is 8.95g; 3.78g of PPDA powder is added while stirring; after it is completely dissolved, the reaction system is cooled to 5°C with an ice-salt bath, and 7.10g of PPDA powder is added in two times TPC powder, after adding 3.55g of TPC powder for the first time, stir at a high speed at a stirring rate of 500r / min; after 3 minutes, add the remaining 3.55g of TPC powder, turn off the stirring device, and turn on the ultrasonic wave for polycondensation reaction at the same time, the ultrasonic frequency is 78kHz , the reaction time is 1h, obtains pale yellow PPTA slurry; The prepared PPTA slurry is diluted with 50mlNMP, and the slurry is sprayed into the coagulation solution composed of high-speed shear NMP (40ml) and water (10ml), and the stirring rate is 3000r / min, cut for 10 minutes to form chopped fiber-like...

Embodiment 2

[0028] in N 2 Under the protective effect of preparation 100mlN-methylpyrrolidone-calcium chloride (NMP-CaCl 2 ) solvent system, wherein the quality of calcium chloride is 8.95g; 3.78g of PPDA powder is added while stirring; after it is completely dissolved, the reaction system is cooled to 0°C with an ice-salt bath, and 7.10g of PPDA is added in two times TPC powder, after adding 0.71g of TPC powder for the first time, stir at a high speed at a stirring rate of 1000r / min; after 3 minutes, add the remaining 6.39g of TPC powder, turn off the stirring device, and turn on the ultrasonic wave for polycondensation reaction at the same time, the ultrasonic frequency is 78kHz , the reaction time is 1h, obtains pale yellow PPTA slurry; The prepared PPTA slurry is diluted with 50mlNMP, and the slurry is sprayed into the coagulation solution composed of high-speed shear NMP (50ml) and water (10ml), and the stirring speed is 2500r / min, cut for 15 minutes to form chopped fiber-like pulp...

Embodiment 3

[0032] in N 2 Under the protective effect of preparation 100mlN-methylpyrrolidone-calcium chloride (NMP-CaCl 2 ) solvent system, wherein the quality of calcium chloride is 8.95g; 2.70g of PPDA powder is added while stirring; after it is completely dissolved, the reaction system is cooled to -10°C with an ice-salt bath, and 5.08g of PPDA is added in two times After adding 2.54g of TPC powder for the first time, stir at a high speed at a stirring rate of 1500r / min; after 4 minutes, add the remaining 2.54g of TPC powder, turn off the stirring device, and turn on the ultrasonic wave for polycondensation reaction at the same time. The ultrasonic frequency is 68kHz, the reaction time is 0.5h, obtains pale yellow PPTA slurry; The prepared PPTA slurry is diluted with 40mlNMP, and the slurry is sprayed into the coagulation solution composed of high-speed shear NMP (60ml) and water (10ml), stirring speed 2000r / min, cut for 10min to form chopped fiber-like pulp fibers, and after suction...

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Abstract

The invention discloses a method for preparing PPTA-pulp by ultrasonic induction, and belongs to the field of chemical fiber preparation. The method comprises the following steps: completely dissolving p-phenylenediamine powder into a calcium chloride-contained solvent; then, adding paraphthaloyl chloride at twice, wherein the mass ratio of the paraphthaloyl chloride at twice is (1:9) to (9:1), and the time interval is 2-5 minutes, and starting an ultrasonic device after the paraphthaloyl chloride is added at the second time to obtain a faint yellow PPTA slurry liquid, wherein the ultrasonic frequency is 28-120 kHz, and the condensation polymerization is 0.2-2 hours; diluting the prepared faint yellow PPTA slurry liquid by using N-methyl pyrrolidone, adding the diluted faint yellow PPTA slurry liquid into a solidification liquid composed of the N-methyl pyrrolidone and water with a volume ratio of (2:1) to (4:1), chopping at high speed to form a chopped fiber-shaped pulp fiber, washing and drying after suction filtration to obtain the PPTA-pulp. The prepared PPTA-pulp has good fiber morphology, and high specific surface area; the feather-shaped structure feature of the pulp is obvious; meanwhile, excellent high temperature resistance is achieved.

Description

technical field [0001] The invention relates to a method for preparing para-aramid pulp by ultrasonic induction, and belongs to the field of chemical fiber preparation. Background technique [0002] Para-aramid pulp (PPTA-pulp) is a differentiated product of para-aramid fiber (PPTA) developed in the past 20 years. It is a highly dispersed fibrillation product first developed by DuPont in the United States in 1984. The chemical structure of aramid pulp is the same as that of PPTA. It retains most of the excellent properties of aramid, such as heat resistance, wear resistance, and dimensional stability, but it also has some physical properties that distinguish it from PPTA long fibers. The density of aramid pulp is 1.41-1.42, which is slightly smaller than that of PPTA long fibers. The surface is fuzzy and microfibrous, rich in hairiness, and rough like wood pulp. [0003] The emergence and rise of aramid pulp is mainly as an ideal substitute fiber for asbestos and competes ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/32C08G69/28D01F6/90D01F1/10D01D1/02D01D5/06
Inventor 刘吉平刘珂嘉
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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