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Production technology of poly (p-phenytene terephthalamide) resin

A technology of poly-p-phenylene terephthalamide and terephthaloyl chloride is applied in the field of preparing poly-p-phenylene terephthalamide resin, and can solve the requirements of particle size, extremely high environmental humidity, and high operating environment. Unfriendly and other problems, to avoid adverse effects, increase product molecular weight, and reduce costs

Active Publication Date: 2010-08-11
SINOCHEM HIGH PERFORMANCE FIBER MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the shortcoming of this method is: adopt terephthaloyl chloride powder to feed, its particle size requirement and environmental humidity requirement are extremely high; Continuously pass dry liquid ammonia as acid absorbent, although relative aza compound toxicity is less, but The operating environment is still not friendly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A kind of production technology of PPTA resin, specifically as follows: in the stainless steel reactor that 250L has jacket, inject and be dissolved with 7% calcium chloride (CaCl 2 ) 200 kg of N-methylpyrrolidone (NMP) solution, add 8.020 kg of p-phenylenediamine (PPDA) at 15 °C to fully dissolve it, and make NMP-CaCl 2- After the PPDA solution, cool to -15°C, slowly add 12.060 kg of terephthaloyl chloride (TPC), and react for 20 minutes to form a prepolymer; the -10°C prepolymer and 50wt% NMP-TPC solution were respectively Simultaneously pump 1000g / min and 27.40g / min into a counter-rotating twin-screw extruder with a diameter of φ50, an aspect ratio of 15, and a rotational speed of 200rpm, and control the precondensation reaction temperature at 15-25°C. After extruding into a co-rotating twin-screw extruder with a diameter of φ65, an aspect ratio of 50, and a rotational speed of 90rpm for polycondensation, the temperature of the co-rotating twin-screw extruder is cont...

Embodiment 2

[0035] A kind of production technology of PPTA resin, specifically as follows: in the stainless steel reactor that 250L has jacket, inject and be dissolved with 7% calcium chloride (CaCl 2 ) 200 kg of N-methylpyrrolidone (NMP) solution, add 8.020 kg of p-phenylenediamine (PPDA) at 15 °C to fully dissolve it, and make NMP-CaCl 2 - After the PPDA solution, cool to -15°C, slowly add 7.575 kg of terephthaloyl chloride (TPC), react for 20 minutes to form a prepolymer, continue to reduce the temperature of the reaction material to -10°C, and mix the prepolymer and The NMP-TPC solution of 50wt% is pumped into the diameter simultaneously with 898.3g / min and 62.5g / min respectively and is that phi 50, aspect ratio is 15, and rotating speed is to carry out pre-condensation reaction in the counter-rotating twin-screw extruder of 200rpm, control pre-condensation The polycondensation reaction temperature is 15-25°C. After high-speed mixing and pre-condensation, it is extruded into a co-rota...

Embodiment 3

[0037] In a 250L jacketed stainless steel reactor, inject 7% calcium chloride (CaCl 2 ) 200 kg of N-methylpyrrolidone (NMP) solution, add 8.020 kg of p-phenylenediamine (PPDA) at 15 °C to fully dissolve it, and make NMP-CaCl 2 After -PPDA solution, cool to -15°C, slowly add 12.060 kg of terephthaloyl chloride (TPC), react for 20 minutes to form a prepolymer, continue to reduce the temperature of the reaction material to -10°C, and mix the prepolymer and The TPC solution is simultaneously pumped at 1000g / min and 13.5g / min respectively into a counter-rotating twin-screw extruder with a diameter of φ50, an aspect ratio of 15, and a rotational speed of 200rpm. After mixing and precondensation, extrude into a co-rotating intermeshing twin-screw extruder with a diameter of φ65, an aspect ratio of 50, and a rotational speed of 90 rpm. The middle section of the intermeshing twin-screw extruder and the machine head are installed with an exhaust barrel filled with fillers at a height o...

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Abstract

The invention relates to a production technology of poly (p-phenytene terephthalamide) resin, including the steps that: (1) p-phenylenediamine and 50-95% of paraphthaloyl chloride are subject to condensation polymerization at the temperature of minus 15 to 10 DEG C in solvent system containing cosolvent, so as to obtain precursor polymer; (2) the rest 5-50% of paraphthaloyl chloride and the precursor polymer are pumped into a first screw extruder for carrying out condensation polymerization, so as to obtain prepolymer; (3) the prepolymer is extruded into a second screw extruder for carrying out condensation polymerization, so as to obtain polymer, wherein the middle piece position and nose position of the second screw extruder are connected with an air extractor, so that at least 50% of hydrogen chloride produced in the condensation polymerization can be removed from the second screw extruder; (4) the obtained polymer is sequentially subject to washing at the temperature of minus 10 to 10 DEG C, dewatering and drying, thus obtaining the poly (p-phenytene terephthalamide) resin. The invention does not require to add acid absorbent, production environment is friendly, technology is simple, and reaction is stable.

Description

technical field [0001] The invention relates to a method for preparing poly(p-phenylene terephthalamide) resin. Background technique [0002] Poly(p-phenylene terephthalamide) (PPTA) resin is the raw material for the preparation of high-strength, high-modulus, high-temperature-resistant special fiber para-aramid and aramid pulp with high friction resistance and high dispersibility. It can be used to produce para-aramid fibers with a specific strength 5-6 times that of steel wire, a specific modulus 2-3 times that of steel wire, and a high temperature resistance of 350 ° C, as well as aramid pulp, which is an ideal substitute for asbestos. Insulating paper with high temperature resistance and friction resistance is widely used in aerospace, transportation and communication, chemical industry and other departments. [0003] In the prior art, the preparation method of poly-p-phenylene terephthalamide resin usually has the following types: [0004] 1. Batch polymerization [...

Claims

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Application Information

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IPC IPC(8): C08G69/32C08G69/28
Inventor 曹煜彤刘兆峰周助胜张浩
Owner SINOCHEM HIGH PERFORMANCE FIBER MATERIALS CO LTD
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