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Para-aramid precipitation fiber and continuous production method thereof

A production method, para-aramid technology, applied in the field of para-aramid precipitated fiber and its continuous production, can solve the problem of long process flow

Active Publication Date: 2019-08-16
CHAMBROAD CHEM IND RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese Patent Publication No. CN1187393C completely dissolves aramid resin with a certain intrinsic viscosity in concentrated sulfuric acid to make a slurry, and directly precipitates it in the coagulation liquid under vigorous stirring to obtain aramid pulp. This process cannot avoid the impact of concentrated sulfuric acid on the equipment. Strong corrosion problem, and need to use the aramid fiber resin obtained by polymerization, washing and drying as raw material, the process flow is long
However, it also needs to use the aramid resin prepared by polymerization, washing and drying as raw material, and then prepare the polymer stock solution, and the process is relatively long

Method used

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  • Para-aramid precipitation fiber and continuous production method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] (1) Under the condition of nitrogen protection, through the transfer pump to 1m 3 Put dehydrated NMP750L into the dissolution kettle, then add 46.26kg of calcium chloride under stirring, dissolve at 93°C, and obtain a calcium chloride solution after dissolving for 35min, then lower the temperature in the dissolution kettle to 0°C; then Add 16.23kg p-phenylenediamine (PPD) under stirring, stir and dissolve for 45min to obtain p-phenylenediamine solution;

[0068] (2) The p-phenylenediamine solution and the terephthaloyl chloride melt kept at 105°C are precisely metered by a metering pump, and then directly transported to a twin-screw reactor by a delivery pump for polymerization, wherein the precise control is carried out by a metering pump The molar ratio of terephthaloyl chloride and p-phenylenediamine into the screw reactor is (1.00~1.005):1;

[0069] The length-to-diameter ratio of the twin-screw reactor is 40:1, the rotation speed is 200 rpm, and the outlet tempera...

Embodiment 2

[0075] (1) Under the condition of nitrogen protection, through the transfer pump to 1m 3 Put dehydrated NMP750L into the dissolution kettle, then add 30.84kg magnesium chloride under stirring, dissolve at 90°C, and obtain a magnesium chloride solution after dissolving for 40min, then lower the temperature in the dissolution kettle to 5°C; then add 32.45kg p-phenylenediamine (PPD), stirring and dissolving 40min, obtains p-phenylenediamine solution;

[0076] The p-phenylenediamine solution and the terephthaloyl chloride melt kept at 107°C are accurately metered by a metering pump, and then directly transported to the twin-screw reactor by a delivery pump for polymerization. The molar ratio of formyl chloride and p-phenylenediamine added to the screw reactor is (1.00~1.003):1;

[0077] The length-to-diameter ratio of the twin-screw reactor is 50:1, the rotation speed is 150 rpm, and the outlet temperature at the end of the screw is kept below 70°C. The twin-screw reactor has tw...

Embodiment 3

[0082] (1) Under the condition of nitrogen protection, through the transfer pump to 1m 3 Put 750L of dehydrated DMAc into the dissolution kettle, then add 61.68kg of aluminum chloride under stirring, dissolve at 94°C, and obtain a lithium chloride solution after dissolving for 35min, then lower the temperature in the dissolution kettle to -3°C; Then add 48.65kg p-phenylenediamine (PPD) under stirring, stir and dissolve for 50min to obtain p-phenylenediamine solution;

[0083] (2) The p-phenylenediamine solution and the terephthaloyl chloride melt kept at 103°C are accurately metered by a metering pump, and then directly transported to a twin-screw reactor by a delivery pump for polymerization. The molar ratio of terephthaloyl chloride and p-phenylenediamine into the screw reactor is (1.00~1.008):1;

[0084] The length-to-diameter ratio of the twin-screw reactor is 55:1, the rotation speed is 80 rpm, and the outlet temperature at the end of the screw is kept below 70°C. The t...

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Abstract

The invention provides a continuous production method of para-aramid precipitation fiber. A p-phenylenediamine solution and a terephthaloyl dichloride melt are polymerized in a double-screw reactor, aproduct is mixed with a pre-coagulation agent, and pre-precipitation is performed; an obtained aramid product and a coagulating bath are precipitated in a mixing pump to form fiber, and the para-aramid precipitation fiber is obtained, wherein the pre-coagulation agent comprises a first solvent, a second solvent and an aid; the length-diameter ratio of the twin-screw reactor is (30:1)-(60:1), therotating speed is 60-500 rpm, and a discharging port at the tail end of the screws is kept at 70 DEG C or below; a first adding port and a second adding port are formed in the twin-screw reactor; thefirst adding port is located in the initial position of screws; the p-phenylenediamine solution and the terephthaloyl dichloride melt are added via the first adding port; the second adding port is located in the 1 / 2-6 / 7 position of the screws in the discharging direction; the pre-coagulation agent is added via the second adding port. The method comprises a simple technological process, equipment selection is reasonable, the method is accurate and controllable, and the product structure is easy to adjust. The fiber is on the micrometer-millimeter scale.

Description

technical field [0001] The invention belongs to the technical field of new polymer materials, and in particular relates to a para-aramid fibrid fiber and a continuous production method thereof. Background technique [0002] Para-aramid fiber is one of the most important high-performance fiber materials at present. Its chemical structure is mainly polyparaphenylene terephthalamide. It is widely used in aerospace due to its excellent performance of high strength, high modulus and high temperature resistance. , high-performance composite materials and electrical insulation and other fields. Among them, para-aramid fibrid fiber is a kind of aramid fiber with special structure developed in the past 30 years. The most important feature is that it has rich fibrillation structure. It is easy to compound with other materials, so it has broad application prospects in the fields of electrical insulating paper, honeycomb paper, high-temperature resistant filter materials, and special m...

Claims

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Application Information

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IPC IPC(8): D01F6/60C08G69/28C08G69/32
CPCC08G69/28C08G69/32D01F6/605
Inventor 姚坤承刘振学张云奎庄锐高立花张另见
Owner CHAMBROAD CHEM IND RES INST CO LTD
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