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Flame-retardant polyamide fiber

A technology of flame-retardant polyamide and polyamide, which is applied in the field of flame-retardant polyamide fiber, can solve the problems of large amount of added flame retardant, reduced flame-retardant durability, general flame-retardant performance, etc., and meets the requirements of industrial production , low cost, simple operation

Inactive Publication Date: 2021-05-07
马海社
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the limiting oxygen index of polyamide 6 fiber is only about 21%, which belongs to combustible fiber. The research on flame-retardant polyamide 6 fiber has become an urgent problem to be solved.
[0003] Chlorinated paraffin is a chlorinated derivative of paraffin. It has the advantages of low volatility, flame retardancy, good barrier property, and low price. It can be used as additives such as plasticizers and flame retardants. It has been widely used in flame retardant materials. Medium, but the amount of added flame retardant is relatively large, and the flame retardant performance is average
Added flame retardants tend to migrate out of the polymer network with extended use time, reducing the durability of flame retardancy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Preparation of carboxyl-containing chlorinated paraffin 42: Dissolve 20 g of chlorinated paraffin 42 in 210 mL of acetone, stir to dissolve, add 20 g of p-hydroxybenzoic acid and 28 g of potassium carbonate, and react at 55° C. for 30 h under nitrogen protection. After the reaction, the pH was adjusted to 3.0 with hydrochloric acid, and then extracted with ethanol, and the product was vacuum-dried at 100° C. for 5 h to obtain carboxyl-containing chlorinated paraffin 42.

[0039] (2) Preparation of chlorinated paraffin 42 containing acid chloride: add 70mol carboxyl-containing chlorinated paraffin 42 to the reaction kettle, add dropwise 85mol phosphorus trichloride, stir and heat up to 70°C, react for 4h, cool to room temperature, and stand to separate Layer to obtain chlorinated paraffin 42 containing acid chloride.

[0040] (3) Preparation of chlorinated paraffin 42 modified 5-hydroxyisophthalic acid: add 100mol5-hydroxyisophthalic acid and an appropriate amount of...

Embodiment 2

[0048] (1) Preparation of carboxyl-containing chlorinated paraffin 52: Dissolve 20 g of chlorinated paraffin 52 in 220 mL of acetone, stir to dissolve, add 20 g of p-hydroxybenzoic acid and 29 g of potassium carbonate, and react at 80° C. for 10 h under nitrogen protection. After the reaction, the pH was adjusted to 3.0 with hydrochloric acid, and then extracted with ethanol. The product was vacuum-dried at 100° C. for 5 h to obtain carboxyl-containing chlorinated paraffin 52.

[0049] (2) Preparation of chlorinated paraffin 52 containing acid chloride: add 70 mol of chlorinated paraffin 52 containing carboxyl to the reaction kettle, dropwise add 85 mol of phosphorus trichloride, stir and heat up to 50°C, react for 6 hours, cool to room temperature, let stand to separate layer to obtain chlorinated paraffin 52 containing acid chloride.

[0050] (3) Preparation of chlorinated paraffin 52 modified 5-hydroxyisophthalic acid: add 100mol5-hydroxyisophthalic acid and an appropriate ...

Embodiment 3

[0058] (1) Preparation of carboxyl-containing chlorinated paraffin 70: Dissolve 20 g of chlorinated paraffin 70 in 200 mL of acetone, stir to dissolve, add 20 g of p-hydroxybenzoic acid and 30 g of potassium carbonate, and react at 65° C. for 24 h under nitrogen protection. After the reaction, the pH was adjusted to 3.0 with hydrochloric acid, and then extracted with ethanol, and the product was vacuum-dried at 100°C for 5 hours to obtain carboxyl-containing chlorinated paraffin 70.

[0059] (2) Preparation of chlorinated paraffin 70 containing acid chloride: add 70 mol of carboxyl-containing chlorinated paraffin 70 to the reaction kettle, add dropwise 85 mol of phosphorus trichloride, stir and heat up to 60° C., react for 5 hours, cool to room temperature, and stand to separate layer to obtain chlorinated paraffin 70 containing acid chloride.

[0060] (3) Preparation of chlorinated paraffin 70 modified 5-hydroxyisophthalic acid: add 100mol5-hydroxyisophthalic acid and an appr...

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Abstract

The invention discloses a flame-retardant polyamide fiber. The flame-retardant polyamide fiber is obtained by melt spinning of a polyamide copolymer. A preparation method of the polyamide copolymer comprises the following steps that chlorinated paraffin reacts with p-hydroxybenzoic acid to prepare carboxyl-containing chlorinated paraffin, the carboxyl-containing chlorinated paraffin is acylated and reacts with 5-hydroxyisophthalic acid or 2,5-dihydroxy terephthalic acid to prepare chlorinated paraffin modified binary acid through esterification reaction, then acylation is carried out, chlorinated paraffin modified 2,5-dihydroxy terephthaloyl chloride reacts with 1,3-propane diamine to prepare chlorinated paraffin modified diamine, then the chlorinated paraffin modified diamine reacts with chlorinated paraffin modified 2,5-dihydroxy terephthaloyl chloride to prepare a polyamide low polymer, finally, the polyamide low polymer and polyamide prepolymer are copolymerized to obtain the chlorinated paraffin modified polyamide copolymer, and the prepared flame-retardant fiber has good mechanical properties and flame retardance and heat resistance.

Description

technical field [0001] The invention relates to a flame-retardant polyamide fiber, which belongs to the field of organic fiber materials. Background technique [0002] Polyamide 6 fiber has excellent strength, abrasion resistance, moisture absorption and resilience, and plays a pivotal role in civil and industrial fields. However, the limiting oxygen index of polyamide 6 fiber is only about 21%, which is a combustible fiber. The research on flame-retardant polyamide 6 fiber has become an urgent problem to be solved. [0003] Chlorinated paraffin is a chlorinated derivative of paraffin. It has the advantages of low volatility, flame retardancy, good barrier property, and low price. It can be used as additives such as plasticizers and flame retardants. It has been widely used in flame retardant materials. Medium, but the amount of added flame retardant is relatively large, and the flame retardant performance is average. With the prolongation of use time, the additive flame r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/60C08G69/48
CPCC08G69/48D01F6/60
Inventor 马海社
Owner 马海社