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Method for synthetizing high-density and high-viscosity polyphenylene terephthalamide

A technology for poly(p-phenylene terephthalamide) and terephthaloyl chloride is applied in the field of polymer synthesis, and can solve the problems of poor solubility, unfavorable industrial production efficiency, low monomer concentration and the like, and achieves improved stability, Reduced stress, improved efficiency

Inactive Publication Date: 2011-07-20
AFCHINA CORP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction speed is fast, and gelation can occur within a few minutes, and the solubility of the PPTA polymer in the solvent system is poor, so the monomer concentration in the current polymerization process is very low, mostly 0.2-0.4mol / L, which is not good for improving industrial production efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: Add 10g of calcium chloride to 100ml of N-methylpyrrolidone under nitrogen protection and stirring, heat to dissolve it, and after it is completely dissolved, let it cool to about 15°C, add 7.570g of p-phenylenediamine to it, After it dissolves, cool the reaction system to 0°C, then add 7.141g of terephthaloyl chloride to it, increase the stirring speed to 1000r / min, add 7.141g of terephthaloyl chloride after 11 minutes of reaction, and then add 11ml of pyridine, Increase the stirring speed to 2500r / min, stop stirring after 30 minutes of reaction, and transfer the reaction product to a crusher after 4 hours of standing, add hot water to stir and crush, then wash twice with water, then soak in ethanol for 12 hours, filter and place in Dry at 120° C. for 8 hours to obtain terephthalamide p-phenylene terephthalamide resin powder with a logarithmic reduced viscosity of 5.88.

Embodiment 2

[0016] Example 2: First, the solvent N-methylpyrrolidone is dehydrated, and the co-solvent calcium chloride needs to be heated at 400° C. for 4 hours before use. Then add 10g of calcium chloride to 100ml of N-methylpyrrolidone under nitrogen protection and stirring, heat to dissolve it, and after it is completely dissolved, let it cool to about 10°C, add 4.326g of p-phenylenediamine to it, and wait for it to dissolve After cooling the reaction system to 5°C, add 4.089g terephthaloyl chloride to it, increase the stirring speed to 1200r / min, add 4.089g terephthaloyl chloride after 10 minutes of reaction, increase the stirring speed to 2400r / min, cool After 5 minutes, continue to react for 20 minutes and then stop stirring. After standing still for 5 hours, transfer the reaction product to a crusher, add hot water, stir and crush, then wash twice with water, then soak in ethanol for 16 hours, filter and place at 120°C Drying at a lower temperature for 18 hours gave terephthalamid...

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PUM

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Abstract

The invention relates to a method for synthetizing high-density and high-viscosity polyphenylene terephthalamide by virtue of high monomer density, comprising the following steps: under the protection of nitrogen, adding calcium chloride into a solvent while stirring; heating to 70-110DEG C; dissolving and cooling to 0-15DEG C; while stirring, adding 0.5-0.7mol / L terephthalamide; dissolving and cooling to minus 15-15DEG C; adding paraphthaloyl chloride; quickening stirring for reaction, and then adding residual paraphthaloyl chloride to improve the stirring rate; adding an acid absorbent; breaking a reaction product; stirring and breaking the obtained product in hot water; washing with hot water; dipping in ethanol; and drying at 110-130DEG C for 8-24 hours to obtain the polyphenylene terephthalamide. The stability of a PPTA (polyphenylene terephthalamide) polymer molecule in solvent is improved by increasing the solvent salt dosage and delaying the adding time of the acid absorben, thus a high-density monomer is polymerized, a high-viscosity polymer is obtained, the polymerization production efficiency is effectively improved, and the pressure of subsequent washing and solvent recovery is lightened.

Description

technical field [0001] The invention relates to a method for synthesizing high-concentration and high-viscosity poly-p-phenylene terephthalamide in the technical field of polymer synthesis. Background technique [0002] Polyparaphenylene terephthalamide (PPTA) fibers have many excellent properties, such as high strength, high modulus, high temperature resistance and solvent resistance, etc. PPTA fiber is made by dissolving PPTA polymer in concentrated sulfuric acid to form a liquid crystal solution, and then through dry spray wet spinning. The performance of the PPTA polymer has a direct impact on the final performance of the PPTA fiber. To obtain high-performance fibers, the PPTA polymer must first have a high molecular weight. It is generally believed that the logarithmic viscosity must be above 5.5dl / g. [0003] There are many ways to prepare PPTA polymers, and the low-temperature solution polycondensation method is widely used at present. This method uses a polar amide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/28
Inventor 庹新林崔庆海周凯
Owner AFCHINA CORP CO LTD