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,

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

Examples

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Example Embodiment

[0034] Example 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 drive device 4 in a product shape. A number of blades 1 are staggered installed on the shaft 2 and enclosed in the cylinder 7 by the shaft seal 3, wherein The blade 1 and the shaft 2 are hollow structures and penetrate each other; there is a cavity between the outer wall of the barrel and the inner wall of the barrel; the support 8 is connected to the barrel 7; the material inlet 5 is from the upper part of the barrel 7 and the inner wall of the barrel and the shaft The reaction cavity formed by the seal 3 is in communication, and the material outlet 6 is in communication with the reaction cavity from the lower part 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 ...

Example Embodiment

[0036] Example 2:

[0037] Add 30Kg of anhydrous NN dimethylacetamide into a 50L jacketed stainless steel pre-reactor, and add 2Kg of anhydrous magnesium chloride activated at high temperature. After the dissolution is complete, add 1.3Kg of p-phenylenediamine to make it fully dissolved. The solution is cooled to -15°C for later use. Use a weightless continuous metering electronic scale to continuously add 2.5Kg of powdered terephthaloyl chloride at 20.8g / min, and use specially designed blades, shafts and jackets to pass through the mixing equipment of the heat transfer medium (three-axis self-cleaning pre-reaction The heat exchange method of the prepolymer keeps the system temperature at -15~35℃, the inherent viscosity of the prepolymer is controlled at 1.67dl / g, and the prepolymer and α-picoline are at 290g / min and 7g / min respectively. The flow rate is added to a twin-screw extruder with a diameter of ∮35, a length-to-diameter ratio of 48, and a speed of 150 rpm by a metering pu...

Example Embodiment

[0038] Example 3:

[0039] Add 30Kg of anhydrous N-methylpyrrolidone (NMP) into a 50L jacketed stainless steel pre-reactor, and add 2Kg of anhydrous calcium chloride activated at high temperature. After the dissolution is complete, add 1.3Kg of p-phenylenediamine to make it Fully dissolve and prepare a solution, and cool to -15℃ for later use. Using a weightless continuous metering electronic balance to continuously add 2.5Kg of powdered terephthaloyl chloride at 14.8g / min, and with the help of specially designed blades, shafts and jackets to pass through the mixing equipment of the heat transfer medium (three-axis self-cleaning pre-reaction Keep the system temperature at -15~35℃, the inherent viscosity of the prepolymer is controlled in the range of 1.86dl / g, and the flow rate of the prepolymer and pyridine is 150g / min and 3g / min respectively. The metering pump is simultaneously fed into a twin-screw extruder with a diameter of ∮35, a length-to-diameter ratio of 48, and a rotatin...

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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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