A micro-reaction system and method for preparing p-/meta-aramid fibers

A micro-reaction and micro-reactor technology, which is applied in the field of micro-reaction systems for preparing para/meta-aramid fibers, can solve the problems of poor repeatability of product properties, affecting the dissolution spinning process, and poor controllability of the preparation process. Improves process stability and repeatability, improves product performance, and suppresses side reactions

Active Publication Date: 2017-01-25
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to keep the temperature of the reaction system near 0°C, but the viscosity of the system is high, which makes it very difficult to transfer heat; at the same time, the polymerization product generated in the twin-screw reactor has local inhomogeneity, which affects the subsequent dissolution spinning process
Due to the complexity of the system in the process of preparing para / meta-aramid fibers, the heat transfer and mixing problems of the low-temperature solution polycondensation method make the preparation process poorly controllable, and the properties of the obtained products are not repeatable.

Method used

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  • A micro-reaction system and method for preparing p-/meta-aramid fibers
  • A micro-reaction system and method for preparing p-/meta-aramid fibers
  • A micro-reaction system and method for preparing p-/meta-aramid fibers

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Embodiment 1

[0038] The invention discloses a preparation method of para-aramid fiber, which specifically comprises the following steps:

[0039] (1) calcium chloride is dissolved in nitrogen methyl pyrrolidone to obtain calcium chloride solution, the concentration of calcium chloride is 10%, p-phenylenediamine is dissolved in calcium chloride solution, and pyridine is added, wherein, p-phenylenediamine Concentration is 0.600mol / L, and the concentration ratio of pyridine and p-phenylenediamine is 5, obtains reaction solution A; Dissolves terephthaloyl dichloride in calcium chloride solution, and the concentration of terephthaloyl dichloride is 0.606mol / L, obtains reaction Liquid B;

[0040] (2) Mix reaction solution A and reaction solution B in the microreactor and cause polycondensation reaction to obtain reaction solution C; there is a microstructure distribution plate with a diameter of 0.04mm mesh in the microreactor; The reaction temperature is 0°C, and the time is 100s;

[0041] (3...

Embodiment 2

[0045] The invention discloses a preparation method of para-aramid fiber, which specifically comprises the following steps:

[0046] (1) Calcium chloride is dissolved in dimethylacetamide to obtain calcium chloride solution, the concentration of calcium chloride is 0.01%, p-phenylenediamine is dissolved in calcium chloride solution, and pyridine is added, wherein, p-phenylenediamine The concentration of pyridine and p-phenylenediamine is 0.01mol / L, and the concentration ratio of pyridine and p-phenylenediamine is 0.1 to obtain reaction solution A; terephthaloyl chloride is dissolved in calcium chloride solution, and the concentration of terephthaloyl chloride is 0.01mol / L to obtain Reaction solution B;

[0047] (2) Mix reaction solution A and reaction solution B in a microreactor and cause polycondensation reaction to obtain reaction solution C; there is a microstructure distribution plate with a width of 0.03 mm and a length of 2 mm in the microreactor ; The reaction tempera...

Embodiment 3

[0052] The invention discloses a preparation method of para-aramid fiber, which specifically comprises the following steps:

[0053] (1) Calcium chloride is dissolved in nitrogen ethyl pyrrolidone to obtain calcium chloride solution, the concentration of calcium chloride is 4%, p-phenylenediamine is dissolved in calcium chloride solution, and pyridine is added, wherein, p-phenylenediamine Concentration is 0.5mol / L, and the concentration ratio of pyridine and p-phenylenediamine is 0.2, obtains reaction solution A; Dissolves terephthaloyl chloride in calcium chloride solution, and the concentration of terephthaloyl chloride is 0.505mol / L, obtains reaction Liquid B;

[0054] (2) Mix reaction solution A and reaction solution B in a microreactor and cause polycondensation reaction to obtain reaction solution C; there is a microstructure distribution plate with a width of 0.05 mm and a length of 5 mm in the microreactor ; The reaction temperature in the microreactor is 25°C, and th...

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Abstract

The invention relates to a micro-reaction system and a micro-reaction method for preparing para / meta-aramid. The micro-reaction system is composed of a micro-reactor and a stirring kettle, wherein the micro-reactor is internally provided with a microstructure distribution plate or a micro-channel; and sieve pores or through grooves are formed in the microstructure distribution plate. The method comprises the steps of dissolving p / m-phenylenediamine into a calcium chloride solution, and adding pyridine to obtain a reaction solution A; dissolving isophthaloyl dichloride / paraphthaloyl chloride into the calcium chloride solution to obtain a reaction solution B; mixing the reaction solutions A and B in the micro-reactor, and triggering condensation polymerization reaction to obtain a reaction solution C; enabling the reaction solution C to enter the stirring kettle, and reacting under stirring to produce a product D; and washing the product D to obtain para / meta-aramid. The material mixing effect is enhanced through the micro-reactor, so that reaction heat can be rapidly removed, and the process stability is improved; and due to the further reaction in the stirring kettle, the polymerization degree is further increased, the pressure drop in the reaction process is reduced, and the safety is improved.

Description

technical field [0001] The invention belongs to the technical field of fiber preparation, and relates to a micro-reaction system and method for preparing p- / meta-aramid fibers. Background technique [0002] The scientific name of p- / meta-aramid fiber is poly p- / isophthalamide p- / m-phenylenediamine. Both fiber materials have excellent properties such as high strength, high modulus, high temperature resistance, acid and alkali resistance, and light weight. . In particular, the ultra-high strength and other excellent properties of para-aramid fiber make it widely used in the fields of spacecraft, rocket structural materials, bulletproof materials, rubber reinforcement materials, building structure reinforcement materials and asbestos replacement materials. Para-aramid, carbon fiber, and ultra-high molecular polyethylene fiber are collectively referred to as the three major high-performance fibers in the world today. At present, the para-aramid market is mainly monopolized by ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/00B01J19/18C08G69/32C08G69/28
Inventor 骆广生王佩坚王凯
Owner TSINGHUA UNIV
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