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A kind of preparation method of aromatic amide

An aromatic amide, p-phenylenediamine technology, applied in the direction of one-component copolyamide rayon, textile and papermaking, one-component synthetic polymer rayon, etc., can solve the problem of aramid fiber surface active groups less , poor resistance to ultraviolet radiation, low fatigue resistance, etc., to achieve the effect of low polymerization equipment and control requirements, narrow molecular weight distribution, and resistance to erosion damage

Active Publication Date: 2021-11-16
ZHUZHOU TIMES NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to improve problems such as less active groups on the surface of aramid fiber, weak binding force with resin, low compressive strength, low fatigue strength, and poor resistance to ultraviolet radiation. Preparation method of spinning aromatic amides with silk equipment requirements and easy operation

Method used

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  • A kind of preparation method of aromatic amide
  • A kind of preparation method of aromatic amide
  • A kind of preparation method of aromatic amide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The preparation method of aromatic amide of the present invention, its process flow chart is as figure 1 shown, including the following steps:

[0043] (1) Under the environment of dry nitrogen protection, dissolve the p-phenylenediamine powder in N-methylpyrrolidone (NMP) at room temperature, so that the concentration of p-phenylenediamine is 0.8mol / L. After it is completely dissolved, add a certain amount of 4,4'-diaminodiphenyl sulfide and stir until it is completely dissolved, so that the concentration is 0.3mol / L, cool to -10°C with an ice-salt bath, add calcium hydride powder and stir evenly , the concentration of calcium hydride in the solution is 0.2mol / L;

[0044] (2) First, add 2,5-dihydroxyterephthaloyl chloride in an amount of p-phenylenediamine addition of 85% to the solution after step (1) to react for 40 minutes, and control the reaction temperature at 25° C.; then add p-phenylenediamine in three batches Add 2,5-dihydroxyterephthaloyl chloride in an amo...

Embodiment 2

[0052] The preparation method of aromatic amide of the present invention, its process flow chart is as figure 1 shown, including the following steps:

[0053] (1) Under the environment of dry nitrogen protection, dissolve the p-phenylenediamine powder in N-methylpyrrolidone (NMP) at room temperature, so that the concentration of p-phenylenediamine is 0.5mol / L. After it is completely dissolved, add a certain amount of 4,4'-diaminodiphenyl sulfide and stir until it is completely dissolved, so that the concentration is 0.25mol / L, cool to -5°C with an ice-salt bath, add calcium hydride powder and stir evenly , the concentration of calcium hydride in the solution is 0.2mol / L;

[0054] (2) First add 2,5-dihydroxyterephthaloyl chloride in an amount of 50% p-phenylenediamine to the solution after step (1) to react for 1 hour, and control the reaction temperature at 20°C; then add p-phenylenediamine in five batches Add 2,5-dihydroxyterephthaloyl dichloride in an amount of 50% of phen...

Embodiment 3

[0062] The preparation method of aromatic amide of the present invention, its process flow chart is as figure 1 shown, including the following steps:

[0063] (1) Under the environment of dry nitrogen protection, dissolve the p-phenylenediamine powder in N-methylpyrrolidone (NMP) at room temperature, so that the concentration of p-phenylenediamine is 0.6mol / L. After it is completely dissolved, add a certain amount of 4,4'-diaminodiphenyl sulfide and stir until it is completely dissolved, so that the concentration is 0.3mol / L, cool to -10°C with an ice-salt bath, add calcium hydride powder and stir evenly , the concentration of calcium hydride in the solution is 0.2mol / L;

[0064] (2) First, add 2,5-dihydroxyterephthaloyl chloride in an amount of 75% p-phenylenediamine addition to the solution after step (1) to react for 50 minutes, and control the reaction temperature at 30° C.; then add p-phenylenediamine in four batches Add 2,5-dihydroxyterephthaloyl chloride in an amount ...

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Abstract

The invention discloses a preparation method of an aromatic amide, which comprises the following steps: under the protection of an inert gas, adding 4,4'-diaminodiphenyl sulfide to a p-phenylenediamine solution and stirring until dissolved, cooling, adding Calcium hydride powder; (add 2,5-dihydroxyterephthaloyl chloride in batches to react; then add lithium hydroxide powder, stir, and the pH value of the reaction system is at 6 to 7 when the reaction ends; finally the reaction product Freezing, crushing, washing, and drying obtain the aromatic amide. In the preparation method process of the present invention, the viscosity of the polymer system is low, which is beneficial to the growth of molecular weight, and the polymerization reaction conditions are mild, and the polymerization equipment and control requirements are relatively high. Low, can obtain polymers with narrow molecular weight distribution and high molecular weight, high industrial feasibility; the generated aromatic amide not only has similar properties to aramid fibers, but also makes up for its shortcomings such as bending and torsional fatigue, and poor UV aging resistance .

Description

technical field [0001] The invention belongs to the field of polymer materials, in particular to a preparation method of aromatic amides. Background technique [0002] Poly(p-phenylene terephthalamide) is mainly used for high-performance aramid fibers and films. It has a series of excellent properties such as high strength and high modulus, heat resistance, chemical corrosion resistance, low density, and stable size. It is used in the aerospace industry, It has been widely used in many fields such as the automobile industry. However, the current aramid fibers have fewer active groups on the surface and are more inert, resulting in defects such as low compressive strength and weak bonding force between the surface and the resin, resulting in potential constraints on the application of aramid fibers; The end of the polymer chain on the surface is oxidized in the air, and the crystal structure on the fiber surface is rearranged, causing the fiber surface to erode. This effect ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/42D01F6/80
CPCC08G69/42D01F6/805
Inventor 曹凯凯李忠良高敬民伍威曹卓杨佑宋志成袁锋甘顺昌
Owner ZHUZHOU TIMES NEW MATERIALS TECH
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