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Method for continuously preparing poly p phenylene diamine terephthalamide resin

A technology of poly-p-phenylene terephthalamide and p-phenylene diamine, which is applied in the field of continuous preparation of poly-p-phenylene terephthalamide resin, and can solve the problem of harsh operating environment, easy blockage, and difficult molar ratio and other problems, to achieve the effect of good solubility, good fiber color and stable performance

Inactive Publication Date: 2005-10-26
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method not only avoids the carcinogenic hexamethylphosphoramide (HMPA) as reported in patents such as USP 3850888 as a solvent, but also solves the problem of easy blockage of jet mixer mixing as reported in USP 3884881, which affects the smooth polycondensation proceeding and other issues
[0012] However, the disadvantage of this method is that it uses malodorous azobenzene compounds such as pyridine as acid absorbents during the polymerization process, which makes solvent recovery more complicated and the operating environment is harsh, and terephthaloyl chloride is melted The state is added to the mixer through a metering pump, and it is very difficult to achieve an equimolar ratio with p-phenylenediamine

Method used

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  • Method for continuously preparing poly p phenylene diamine terephthalamide resin

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Add 100Kg of anhydrous N-methylpyrrolidone (NMP) into a 150L jacketed stainless steel reaction kettle, add 6Kg of anhydrous calcium chloride (CaCl) activated by high temperature 2 ), after completely dissolving, add 4.32Kg p-phenylenediamine (PPDA), make it dissolve fully, and make NMP-CaCl 2 - PPDA solution, cooled to 0°C for later use. The NMP-CaCl 2 -PPDA solution and terephthaloyl chloride (TPC) powder are added at a speed of 1838.67g / min and 135.33g / min to be Φ65, the aspect ratio is 60, and the rotating speed is in the twin-screw reaction extruder of 200rpm. The third section of the screw extruder passes dry liquid ammonia at a speed of 22.67g / min to neutralize the hydrogen chloride gas generated by the reaction, and controls the temperature inside the twin-screw extruder to 60°C for about 20 minutes to extrude The polycondensation product in the form of light yellow corn powder was left to stand for 2 hours. After removing the solvent, it was crushed, washed wi...

Embodiment 2

[0032] Add 100Kg of anhydrous N,N-dimethylacetamide into a 150L jacketed stainless steel reaction kettle, add 6Kg of anhydrous lithium chloride activated by high temperature, and after completely dissolving, add 4.32Kg of p-phenylenediamine (PPDA) , make it fully dissolved, make a solution, and cool to -20°C for later use. The prepared solution and terephthaloyl chloride (TPC) powder are added at a rate of 1838.67g / min and 135.33g / min by using a liquid metering feeding system and a high-precision loss-in-weight continuous metering electronic scale, respectively. 35, rotating speed is in the twin-screw reaction extruder of 200rpm, add polyvinylpyrrolidone (PVP) with the speed of 10g / min in the sixth section of twin-screw extruder, control the temperature in the twin-screw extruder to be 75 ℃, about 15 minutes, you can extrude the polycondensation product of light yellow corn flour, let it stand for 2 hours, remove the solvent, grind, wash and dry to obtain light yellow poly-p-p...

Embodiment 3

[0034]Add 100Kg of anhydrous hexamethyl triamine phosphate into a 150L jacketed stainless steel reaction kettle, add 6Kg of anhydrous magnesium chloride activated by high temperature, after completely dissolving, add 4.32Kg of p-phenylenediamine (PPDA) to fully dissolve , dubbed into a solution, cooled to -15 ℃ for later use. The prepared solution and terephthaloyl chloride (TPC) powder are added at a rate of 1838.67g / min and 135.33g / min by using a liquid metering feeding system and a high-precision loss-in-weight continuous metering electronic scale, respectively. 50, rotating speed is in the twin-screw reaction extruder of 200rpm, adds polyvinylpyrrolidone (PVP) with the speed of 10g / min in the sixth section of twin-screw extruder, and the temperature in the control twin-screw extruder is 30 ℃, about 25 minutes, the light yellow corn flour-like polycondensation product can be extruded, stand for 2 hours, after removing the solvent, pulverize, wash with water, and dry to obta...

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Abstract

The present invention discloses a method for continuously preparing poly(p-phenylene terephthalamide) resin, said method includes the following steps: (1). after the p-benzenediol powder is completely dissolved in the solvent containing cosolvent, adding P-benzenediol solid and terephthaloyl powder into extruder according to the ratio of 1:1-1.01; (2). feeding the solvent contaiing P-benzenediol and cosolvent into extruder adopting low-temperature medium cooling, its temperature is -20-5 deg.C, the residence time of reaction system in reactor is 2-25 min, polycondensation temp. is 30-90 deg.C, after the reaction is completed, extruding the above-mentioned material; and (3). making the extruded polymer body undergo the processes of standing still, washing, dewatering and drying so as to obtain light yellow polymer body powder.

Description

technical field [0001] The invention relates to a method for continuously preparing poly-p-phenylenediamine terephthalamide resin, in particular to a method using a twin-screw extruder as a reactor and adding dissolved p-phenylenediamine and The invention relates to a method for continuously preparing poly-p-phenylene terephthalamide resin by metering and adding powdered terephthaloyl chloride to a solvent of a co-solvent and a high-precision weight loss type continuous metering electronic balance. Background technique [0002] Poly(p-phenylene terephthalamide) resin is the raw material for preparing high-strength, high-modulus, high-temperature-resistant special fiber para-aramid and aramid pulp with high friction 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, aramid fiber that can withstand high temperatures of 350 ° C, and as an ideal substitute for asbestos, it can be made i...

Claims

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Application Information

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IPC IPC(8): C08G69/26
Inventor 尤秀兰刘兆峰胡祖明潘婉莲于俊荣
Owner DONGHUA UNIV
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