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Poly(m-phenylene isophthalamide) resin liquid, preparation method thereof, poly(m-phenylene isophthalamide) resin and poly(m-phenylene isophthalamide) fibrid

A kind of technology of aramid fiber and polymerization solution, applied in the direction of fiber chemical characteristics, single-component synthetic polymer rayon, single-component polyamide rayon, etc., can solve the problem of insufficient fiber tensile breaking strength, polymer Problems such as wide molecular weight distribution and difficulty in controlling the addition of raw materials can achieve the effect of improving material dispersibility and fluidity, high product quality, and avoiding unstable polymer viscosity.

Inactive Publication Date: 2017-12-29
HUNAN CHEM RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese patents such as CN 100455706C, CN 1195909C, CN 1162572C, CN 100398707C, JP484661 and other patents all provide synthetic methods for preparing aramid resin polymers by low-temperature methods, but all have the following disadvantages: the reaction adopts a "one-pot method" and the reaction temperature is unstable , The addition of raw materials is difficult to control and easy to block the pipe, the heat of reaction is difficult to control, the neutralizer is added too much, the molecular weight distribution of the polymer is wide, the viscosity of the resin is unstable, the content of fiber salt is high, the obtained fiber structure is not uniform, and the fiber stretches Insufficient breaking strength

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A kind of preparation method of meta-aramid fiber resin polymerization liquid of the present invention, comprises the following steps:

[0040] (1) In a reactor with a stirrer, dissolve 109g (1.01mol) of refined m-phenylenediamine in 1090g of freshly distilled dry N,N-dimethylacetamide (DMAc), and stir well , to obtain an organic solution of m-phenylenediamine, cooled to 5°C, and stored; similarly, 203g (1.0mol) of refined isophthaloyl chloride was dissolved in 207g of freshly distilled dry toluene, and stirred evenly to obtain isophthaloyl dichloride Acid chloride organic solution, cooled to 5 ° C, stored.

[0041] (2) Turn on the microreactor (LFR15-328-1A), cool down to 5°C, and at the same time, prepare 599.5g of m-phenylenediamine organic solution and 410g of isophthaloyl organic solution at a rate of 10g / min and 6.8 g / min is pumped into the microreactor for prepolymerization reaction, the feeding is completed within 60 minutes, and the reaction temperature is kep...

Embodiment 2

[0052] (1) In a reactor with a stirrer, dissolve 109g (1.01mol) of refined m-phenylenediamine in 1090g of freshly distilled dry DMAc, stir well to obtain an organic solution of m-phenylenediamine, and cool to Store at 5°C; also dissolve 203g (1.0mol) of refined isophthaloyl chloride in 207 g of freshly distilled dry dichloroethane, stir well to obtain an organic solution of isophthaloyl chloride, cool to 5 ℃, save.

[0053] (2) Turn on the microreactor (LFR15-328-1A), cool down to 5°C, and at the same time, prepare 599.5g m-phenylenediamine organic solution and 410g isophthaloyl organic solution at a rate of 10g / min and 6.8g / min is pumped into the microreactor, the feeding is completed within 60 minutes, and the reaction temperature is kept at 5°C to obtain the prepolymerization mixture;

[0054] (3) After the prepolymerization is completed, 1009.5g of the obtained prepolymerization mixture and the remaining 599.5g m-phenylenediamine organic solution are pumped into the micro...

Embodiment 3

[0059] (1) In a reactor with a stirrer, dissolve 109 g (1.01 mol) of refined m-phenylenediamine in 1090 g of freshly distilled dry N-methyl-pyrrolidone (NMP), and stir well to obtain Organic solution of m-phenylenediamine, cooled to 5°C, and stored; similarly, 203 g (1.0 mol) of refined isophthaloyl chloride was dissolved in 207 g of freshly distilled dry toluene, stirred evenly, and isophthaloyl chloride The organic solution was cooled to 5°C and stored.

[0060] (2) Turn on the microreactor (LFR15-328-1A), cool down to 5°C, and at the same time, prepare 599.5g of m-phenylenediamine organic solution and 410g of isophthaloyl organic solution at a rate of 10g / min and 6.8 g / min is pumped into the microreactor, the feeding is completed within 60 minutes, and the reaction temperature is kept at 5°C to obtain the prepolymerization mixture;

[0061] (3) After the prepolymerization is completed, 1009.5g of the obtained prepolymerization mixture and the remaining 599.5g m-phenylenedi...

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PUM

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Abstract

The invention discloses a poly(m-phenylene isophthalamide) resin liquid, a preparation method thereof, a poly(m-phenylene isophthalamide) resin and a poly(m-phenylene isophthalamide) fibrid. The preparation method of the poly(m-phenylene isophthalamide) resin liquid comprises (1) preparing m-phenylenediamine solution and m-phthaloyl dichloride organic solution; (2) mixing the m-phenylenediamine solution and a part of the m-phthaloyl dichloride organic solution for pre-polymerization; (3) mixing pre-polymerized mixture solution with the rest part of the m-phthaloyl dichloride for polymerization to obtain the poly(m-phenylene isophthalamide) resin liquid. The poly(m-phenylene isophthalamide) resin and the poly(m-phenylene isophthalamide) fibrid are both prepared through precipitation of the poly(m-phenylene isophthalamide) resin liquid. The preparation method of the poly(m-phenylene isophthalamide) resin liquid has the advantages of being controllable in reaction heat, small in influence of by-products, free from of neutralization of acid-binding agent, capable of avoiding moisture absorption of m-phthaloyl dichloride and formation of intermediates, and low in content of low-molecular polymers during reaction. Therefore, the prepared poly(m-phenylene isophthalamide) resin is high and stable in logarithmic viscosity number, and the prepared poly(m-phenylene isophthalamide) fibrid is uniform in fiber structure and high in tensile breaking strength.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, and in particular relates to a meta-aramid resin polymer solution and a preparation method thereof, meta-aramid resin and meta-aramid fibril. Background technique [0002] Aramid 1313 is also called meta-aramid, and its chemical name is poly(m-phenyleneisophthalamide), PMIA. The meta-aramid molecule is a linear macromolecule composed of amide groups connected to meta-phenyl groups. In its crystal, hydrogen bonds exist on two planes, arranged like a grid, thus forming a three-dimensional structure of hydrogen bridges. Due to the strong hydrogen bond, the meta-aramid fiber has a stable chemical structure and has the following superior properties: excellent heat resistance, super flame retardancy, outstanding electrical insulation, excellent chemical stability, good mechanical properties. [0003] As a special fiber, PMIA has excellent properties unmatched by other common mat...

Claims

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Application Information

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IPC IPC(8): C08G69/32C08J3/09D01F6/60
CPCC08G69/32C08J3/09C08J2377/06D01F6/605
Inventor 刘国文罗先福李萍徐健高云英周锦萍黄炜周亮王燕周勇臧阳陵
Owner HUNAN CHEM RES INST
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