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Novel preparation technique for poly (p-phenylene terephthalamide)

A technology of poly-p-phenylene terephthalamide and terephthaloyl chloride, which is applied in the field of manufacturing poly-p-phenylene terephthalamide resin, can solve the requirements of particle size and environmental humidity requirements, and operation Unfriendly to the environment and other issues, to achieve the effect of fresh color, friendly production environment, and good solubility

Active Publication Date: 2012-03-14
SINOCHEM HIGH PERFORMANCE FIBER MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] 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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  • Novel preparation technique for poly (p-phenylene terephthalamide)
  • Novel preparation technique for poly (p-phenylene terephthalamide)

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 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 the PPDA solution, cool to below 0°C, slowly add 12.060 kg of terephthaloyl chloride (TPC), react for 20 minutes to form a prepolymer, and prepolymer and 50wt% NMP-TPC solution are respectively mixed at 1000g / min and 27.40g / min are simultaneously pumped into a twin-screw extruder with a diameter of Φ50, an aspect ratio of 15, and a rotational speed of 200rpm, and the temperature of the precondensation reaction is controlled at 15-25°C. , length-to-diameter ratio is 50, rotating speed is in the twin-screw extruder of 90rpm, and in its third section, drop 50% NMP-PVP (polyvinylpyrrolidone) with 8g / min, control main polycondensation reaction screw extruder The temperature is 60-80°C, about 20 minutes, extrude the light yellow powder polycondensation...

Embodiment 2

[0037] In a 250L jacketed stainless steel reactor, inject 6% 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 below 0°C, slowly add 7.575 kg of terephthaloyl chloride (TPC), react for 20 minutes to form a prepolymer, and prepolymer and 50wt% NMP-TPC solution are respectively mixed with 898.3g / min and 62.5g / min are simultaneously pumped into a twin-screw extruder with a diameter of Φ50, an aspect ratio of 15, and a rotational speed of 200rpm. The temperature of the precondensation reaction is controlled at 15-25°C. In the twin-screw extruder with Φ65, aspect ratio of 50 and rotating speed of 90rpm, add 50% NMP-PVP (polyvinylpyrrolidone) dropwise at 10g / min in the third section to control the main polycondensation reaction screw extrusion The temperature of the machine is 60-80°C, about 20 minutes, extrude the light yellow powder...

Embodiment 3

[0039] In a 250L jacketed stainless steel reactor, inject 6% 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 below 0°C, slowly add 12.060 kg of terephthaloyl chloride (TPC), react for 20 minutes to form a prepolymer, and prepolymer and 30wt% NMP-TPC solution are respectively mixed at 1000g / min and 45.67g / min are simultaneously pumped into a twin-screw extruder with a diameter of Φ50, an aspect ratio of 15, and a rotational speed of 200rpm, and the temperature of the precondensation reaction is controlled at 15-25°C. , length-to-diameter ratio is 50, rotating speed is in the twin-screw extruder of 90rpm, and in its third section, drop 50% NMP-PVP (polyvinylpyrrolidone) with 10g / min, control main polycondensation reaction screw extruder The temperature is 60-80°C, for about 20 minutes, extrude the light yellow powder polycondensa...

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Abstract

The invention discloses a new technique used for manufacturing poly(p-phenytene terephthalamide) resin, which comprises steps that: (1) para-phenylenediamine and 50-95 percent of terephthaloyl chloride are treated with pre-polycondensation in a solution system at low temperature; (2) the left 5-50 percent of the terephthaloyl chloride is made into a solution with 30-70 percent of content in N-methyl pyrrolidone, and the solution is pumped into a pre-polycondensation screw extruder together with prepolymer; (3) the reaction mixture is intruded into a main reaction screw extruder and a macromolecule addictive, polyvinyl pyrrolidone-N-methyl pyrrolidone solution is dripped in; (4) the extruded polymer is washed with ice water and neutralized by the cleaning solution of calcium carbonate andpotassium hydroxide and the solvent is recycled; (5) the washed polymer is dehydrated and dried, then light yellow polymer powder of the poly(p-phenytene terephthalamide) with logarithmic viscosity number of 4-7.5dl / g is obtained. The poly (p-phenytene terephthalamide) resin which is manufactured by adopting the technique of the invention has simple technology, being convenient for uninterrupted production, and the prepared polymer powder has fresh color and luster and stable capacities, and the resin has good spinnability, the spun fiber has good color and luster, high strength and high modulus.

Description

technical field [0001] The invention relates to a method for producing poly-p-phenylene terephthalamide resin, in particular to a method for precondensation polymerization using counter-rotating twin-screw extruders or reciprocating single-screw extruders, co-meshing twin-screw extruders The screw extruder is the main reactor, adopts the continuous feeding method of terephthaloyl chloride and polymer additive solution, and adopts a new process of washing the extruded polymer with cold water to produce poly-p-phenylene terephthalamide resin. Background technique [0002] Poly-p-phenylene terephthalamide 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 wear resistance and high dispersibility. The specific strength is 5-6 times that of steel wire, the specific modulus is 2-3 times that of steel wire, para-aramid fiber that can withstand high temperatures of 350 ° C, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/32B29C47/60B29C47/92B29C48/625B29C48/92
CPCB29C48/625
Inventor 曹煜彤周助胜尤秀兰刘兆峰
Owner SINOCHEM HIGH PERFORMANCE FIBER MATERIALS CO LTD
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