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Industrial method and polycondensation reactor for continuously preparing poly-p-phenylene terephthamide resin with high viscosity

A technology of poly-p-phenylene terephthalamide and terephthaloyl chloride, which is applied in the field of continuous preparation of high-viscosity poly-p-phenylene terephthalamide resin, can solve the problem of low viscosity and environmental protection Unfavorable solvent recovery and other problems, to achieve the effect of purifying the workshop environment, simplifying the recovery process and equipment requirements, and increasing the viscosity

Active Publication Date: 2009-10-07
中国平煤神马控股集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent is in the preparation of NMP-CaCl 2 Solvent is also solid industrial CaCl 2 It is added to NMP after burning, so the logarithmic viscosity of the resin is not high (the highest is only 5.5). In addition, because liquid ammonia is used to neutralize hydrochloric acid, liquid ammonia is flammable, explosive, and has a pungent odor. The volatile liquid is not good for environmental protection and solvent recovery

Method used

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  • Industrial method and polycondensation reactor for continuously preparing poly-p-phenylene terephthamide resin with high viscosity

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Experimental program
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Effect test

Embodiment 1

[0030] The industrial method for continuously preparing high-viscosity poly-p-phenylene terephthalamide resin of the present invention comprises the following steps: adding 650L of pure water in the dissolving kettle, adding 800Kg calcium chloride dihydrate, 25Kg aluminum chloride, dissolving in Prepare an aqueous solution of about 40% calcium chloride in water. After settling and filtering, take 730Kg of calcium chloride / water solution and mix it with 3500Kg of 10% water-containing NMP to obtain NMP / calcium chloride aqueous solution; preheat it to 120°C with a pump The water-containing solvent is sent into the vacuum rectification tower (feeding in the tower) at a speed of 600kg / h, and the temperature of the tower bottom is 100°C, and the pressure of the tower bottom is rectification to remove water under the condition of -50kpa, and the refined solvent system , after inspection, the calcium chloride content is 8.4%, the water content is 85PPm, the temperature is about 50°C, a...

Embodiment 2

[0034] The industrial method for continuously preparing high-viscosity poly-p-phenylene terephthalamide resin of the present invention comprises the following steps: adding 650L of pure water in the dissolving kettle, adding 800Kg calcium chloride dihydrate, 25Kg aluminum chloride, dissolving in Prepare about 40% calcium chloride aqueous solution in water; after settling and filtering, take 830Kg of additive aqueous solution and mix with 3500Kg of 5% water-containing NMP to obtain NMP / calcium chloride aqueous solution. The speed of the solvent 1000kg / h is sent into the vacuum distillation tower (feeding in the tower), and the temperature of the tower bottom is controlled at 200°C, and the pressure of the tower bottom is controlled at -90kpa to rectify and remove water. The refined solvent system is passed through Inspection, calcium chloride content is 10%, water content is 100PPm, at 3.5m 3 Add 2600.0L of solvent to the p-phenylenediamine dissolution kettle, stir and cool dow...

Embodiment 3

[0036] The industrial method for continuously preparing high-viscosity poly-p-phenylene terephthalamide resin of the present invention comprises the following steps: adding 650L of pure water in the dissolving kettle, adding 800Kg calcium chloride dihydrate, 25Kg aluminum chloride, dissolving in Prepare about 40% calcium chloride aqueous solution in water; after settling and filtering, take 675Kg of additive aqueous solution and mix with 3500Kg of 5% water-containing NMP to obtain NMP / calcium chloride aqueous solution. The speed of the solvent 1000kg / h is sent into the vacuum distillation tower (feeding in the tower), and the temperature of the tower bottom is controlled at 200°C, and the pressure of the tower bottom is controlled at -90kpa to rectify and remove water. The refined solvent system is passed through Inspection, the refined solvent system has a calcium chloride content of 7.5%, a water content of 150PPm, a temperature of about 50°C, and a temperature of 3.5m 3 Add...

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Abstract

The invention relates to an industrial method and a polycondensation reactor for continuously preparing poly-p-phenylene terephthamide resin with high viscosity, comprising the following steps: (1) compounding a flux into an aqueous solution, then mixing with solvent to remove water by refinement and continuously and stably obtaining a solvent system with the water content conforming to the requirement, wherein the weight percentage of the flux in the solvent system is from 6 percent to 15 percent; (2) performing the polycondensation reaction of para-phenylene diamine (PPD) and terephthalyl chloride (TPC) in the mol ratio of 1.01-1 to 1-1.01 in the solvent system prepared in the step (1), and obtaining a polymer after reaction; and (3) obtaining the poly-p-phenylene terephthamide resin in yellow powder after pulverizing, neutralizing, washing and drying the polymer. By utilizing the method, the adverse effects of weather and operation on the polymerized solvent system water is overcome, and continuous, closed and clean production is realized.

Description

technical field [0001] The present invention relates to a kind of industrial method for continuously preparing high-viscosity poly-p-phenylene terephthalamide resin (PPTA), especially relate to the aqueous solution of a kind of co-solvent mixed with water-containing NMP to prepare anhydrous NMP / co-solvent solution, then The industrialized method of polymerizing PPD and TPC in anhydrous solvent to prepare high-viscosity poly-p-phenylene terephthalamide resin. Background technique [0002] Polyparaphenylene terephthalamide resin (PPTA) is the raw material for preparing aramid 1414 fiber and pulp. Because of their high strength, high modulus, high temperature resistance, flame retardant and other excellent comprehensive properties, they have been widely used in military, aerospace, sports, communication, chemical and other fields. At present, in the relevant reports of continuous preparation of poly-p-phenylene terephthalamide resin, the early patent USP3850888, 3884881 adopts...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/28C08G69/46C08G69/32
Inventor 李磊潘育英吕清海马源王良赵辉王建民魏建毅罗亚利冯立伟
Owner 中国平煤神马控股集团有限公司
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