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Method and device for preparing polypara-phthaloyl para-phenylene diamine resin

The technology of poly-p-phenylene terephthalamide and p-phenylenediamine is applied in the field of preparation of poly-p-phenylene terephthalamide resin, and can solve the problem of low product quality, difficult reaction control, and easy generation Gel and other problems, to achieve the effect of high surface renewal rate, high heat transfer capacity, and avoiding fouling residues

Active Publication Date: 2008-09-17
SINOPEC YIZHENG CHEM FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the problems of difficult reaction control in the existing preparation method of poly-p-phenylene terephthalamide resin, low product quality, low yield, and easy gel generation due to difficulty in heat dissipation, and provide a replacement Preparation method of polyparaphenylene terephthalamide resin with rapid heating, precise control and high product quality

Method used

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  • Method and device for preparing polypara-phthaloyl para-phenylene diamine resin
  • Method and device for preparing polypara-phthaloyl para-phenylene diamine resin
  • Method and device for preparing polypara-phthaloyl para-phenylene diamine resin

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Embodiment 1

[0035] The structure of the three-axis self-cleaning pre-reactor is shown in the figure. The three shafts 2 are connected to the driving device 4 in the shape of a pin, and several blades 1 are respectively staggeredly installed on the shaft 2 and sealed in the cylinder 7 by the shaft seal 3. Among them The vane 1 and the shaft 2 are hollow and interpenetrated; there is a cavity between the outer wall of the cylinder and the inner wall of the cylinder; the support 8 is connected to the cylinder 7; the material inlet 5 connects the upper part of the cylinder 7 with the inner wall of the cylinder and the shaft The reaction chamber formed by the seal 3 communicates, and the material outlet 6 communicates with the reaction chamber from the bottom of the cylinder 7 . There are small gaps between the blades 1 on the three shafts and between the blades and the inner wall of the cylinder 7, so that materials on the blades and the inner wall of the cylinder can be scraped when stirring ...

Embodiment 2

[0037] Add 30Kg of anhydrous N-N dimethylacetamide into a 50L jacketed stainless steel pre-reaction kettle, add 2Kg of anhydrous magnesium chloride activated by high temperature, after the dissolution is completed, add 1.3Kg of p-phenylenediamine to fully dissolve it into solution, cooled to -15°C for later use. Continuously add 2.5Kg of powdered terephthaloyl chloride at 20.8g / min by using a weight-loss type continuous metering electronic balance, and pass through the stirring equipment of the heat transfer medium with the help of specially designed blades, shafts and jackets (three-axis self-cleaning pre-reaction device) to keep the temperature of the system at -15 to 35°C, the inherent viscosity of the prepolymer is controlled at 1.67dl / g, and the prepolymer and α-picoline are controlled at 290g / min and 7g / min respectively The flow is fed into a twin-screw extruder with a diameter of ∮35, an aspect ratio of 48, and a speed of 150rpm at the same time by a metering pump. The ...

Embodiment 3

[0039] Add 30Kg of anhydrous N-methylpyrrolidone (NMP) in a 50L stainless steel pre-reaction kettle with a jacket, add 2Kg of anhydrous calcium chloride activated by high temperature, after completing the dissolution, add 1.3Kg of p-phenylenediamine to make it Fully dissolved to form a solution, cooled to -15°C for later use. Continuously add 2.5Kg of powdered terephthaloyl chloride at 14.8g / min by using a weight-loss type continuous metering electronic balance, and pass through the stirring equipment of the heat transfer medium with the help of specially designed blades, shafts and jackets (three-axis self-cleaning pre-reaction The heat exchange method of the device) keeps the system temperature at -15~35°C, the inherent viscosity of the prepolymer is controlled within the range of 1.86dl / g, and the flow rates of the prepolymer and pyridine are 150g / min and 3g / min respectively. The metering pump is added to the twin-screw extruder with a diameter of ∮35, an aspect ratio of 48...

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Abstract

The invention discloses a method for preparing poly(p-phenytene terephthalamide)resin, p-phenylenediamine is firstly dissolved and added in a three-shaft self-cleaning type pre-reactor, terephthaloyl chloride and the p-phenylenediamine are added into the pre-reactor in the molar ratio of 1: 1 to 1.01: 1 for carrying out the pre-polycondensation; a prepolymer is added in a double-screw-rod extruder, a pyridine acid absorbent is further added for carrying out the reaction and is extruded after the complete reaction; the extruded polymer undergoes standing, washing, dehydration and drying to obtain the poly(p-phenytene terephthalamide)resin. The invention also discloses the three-shaft self-cleaning type pre-reactor device. The method can precisely control the generated heat of the prepolymerization reaction at unit time and better realize the control of the whole prepolymerization process; the special designs of a stirring shaft and a blade of the pre-reactor can allow the reaction heat to obtain the rapid exchange and avoid the generation of gel; and the obtained resin has good spinnability, good luster of the obtained fiber, high strength and stable performance.

Description

technical field [0001] The invention relates to the field of high molecular polymers, and specifically relates to a preparation method and equipment for poly-p-phenylene terephthalamide resin. 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 fiber) and aramid pulp with high friction resistance and high dispersibility. It can be used to make aramid fiber whose specific strength is 5 to 6 times that of steel wire, specific modulus 2 to 3 times that of steel wire, and can withstand high temperatures of 350 ° C. As an ideal substitute for asbestos, it can be made into high temperature resistant and friction resistant Insulating paper is widely used in aerospace, defense, automobile, optical cable and industrial fields. [0003] There are many patent reports on the preparation method of poly-p-phenylene terephthalamide, USP3,850,888; 3,884,881 ...

Claims

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Application Information

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IPC IPC(8): C08G69/32
Inventor 陈昂朱福和章寅李海明邓飞
Owner SINOPEC YIZHENG CHEM FIBER
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