Flame-retarded polyamide 6 and preparation method thereof

A technology for flame retardant polyamide and polyamide, which is applied in the field of flame retardant polyamide 6 and its preparation, can solve the problems of poor mechanical properties and poor flame retardant performance of polyamide 6, and achieves excellent flame retardant performance and good flame retardant effect. , the effect of easy operation

Active Publication Date: 2017-05-17
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of poor flame retardancy or poor mechanical properties of polyamide 6 pre

Method used

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  • Flame-retarded polyamide 6 and preparation method thereof
  • Flame-retarded polyamide 6 and preparation method thereof
  • Flame-retarded polyamide 6 and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A preparation method of flame retardant polyamide 6, the steps are as follows:

[0045] 1) Mix the DOPO-based reactive phosphorus-based flame retardant, diamine and water at a stirring speed of 50 r / min, and conduct a salt-forming reaction at 60 °C for 2 h to obtain a flame retardant salt. Among them, DOPO-based reactive phosphorus The molar ratio of flame retardant and diamine is 1:1, and the mass ratio of DOPO-based reactive phosphorus-based flame retardant and water is 1:1; the structural formula of DOPO-based reactive phosphorus-based flame retardant is:

[0046]

[0047] The structural formula of the diamine is NH 2 -(CH 2 ) 3 -NH 2 ;

[0048] 2) In parts by weight, 3 parts of aluminum diethylphosphinate, 100 parts of caprolactam and 2 parts of water were added to the reaction kettle, stirred and heated to 250° C. The stirring rate was 50r / min, and when the pressure reached 0.8MPa , heat preservation and pressure holding reaction for 3h, and then release th...

Embodiment 2

[0057] A preparation method of flame retardant polyamide 6, the steps are as follows:

[0058] 1) Mix and stir DOPO-based reactive phosphorus-based flame retardant, diamine and ethanol at a stirring rate of 80 r / min and conduct a salt-forming reaction at 63 °C for 2 h to obtain a flame retardant salt. Among them, DOPO-based reactive phosphorus The molar ratio of flame retardant and diamine is 1:1, the mass ratio of DOPO-based reactive phosphorus-based flame retardant and ethanol is 1:1.1; the structural formula of DOPO-based reactive phosphorus-based flame retardant is:

[0059]

[0060] The structural formula of the diamine is NH 2 -(CH 2 ) 10 -NH 2 ;

[0061] 2) In parts by weight, add 3 parts of zinc diethylphosphinate, 1 part of zinc stannate, 99 parts of caprolactam, 0.1 part of adipic acid and 2 parts of water to the reaction kettle, stir and heat up to 251 ° C, stir The rate is 100r / min. When the pressure reaches 0.9MPa, the reaction is kept under pressure for 2...

Embodiment 3

[0070] A preparation method of flame retardant polyamide 6, the steps are as follows:

[0071] 1) Mix the DOPO-based reactive phosphorus-based flame retardant, diamine and water at a stirring rate of 100 r / min, and conduct a salt-forming reaction at 66 °C for 3 hours to obtain a flame retardant salt. Among them, DOPO-based reactive phosphorus The molar ratio of flame retardant and diamine is 1:1.1, and the mass ratio of DOPO-based reactive phosphorus-based flame retardant and water is 1:1.2; the structural formula of DOPO-based reactive phosphorus-based flame retardant is:

[0072]

[0073] The structural formula of the diamine is NH 2 -(CH 2 ) 5 -NH 2 ;

[0074] In parts by weight, 5 parts of aluminum methyl butyl phosphinate, 97 parts of caprolactam, 1 part of adipic acid and 3 parts of water were added to the reaction kettle, stirred and heated to 252 ° C, and the stirring rate was 200 r / min. When the pressure reaches 1MPa, the reaction is kept under pressure for 3h...

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Abstract

The invention relates to flame-retarded polyamide 6 and a preparation method thereof. The preparation method comprises the steps of firstly obtaining flame retardant salt through reaction between a DOPO-based reaction type phosphorus-based flame retardant and diamine; then adding an addition type phosphorus-based flame retardant, the flame retardant salt and other components during a process of polymerizing caprolactam into polyamide 6 so as to prepare the flame-retarded polyamide 6, wherein a molecular chain of the flame-retarded polyamide 6 is formed by a polyamide chain segment and a DOPO-based reaction type phosphorus-based flame retardant chain segment; the content of phosphorus in the molecular chain is 0.4 to 0.8 percent by weight; and the molecular chain contains 3 to 9 percent by weight of the addition type phosphorus-based flame retardant. The flame-retarded polyamide 6 prepared through the invention has the limit oxygen index being larger than 29 percent, the tensile strength ranging from 55 to 69MPa, the elongation at break ranging from 40 to 110 percent, can become gears, bearings, automobile parts and other products through injection molding and other methods, and can also be prepared into polyamide 6 fiber so as to be further processed to be textile, military fabrics, equipment and the like.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant polyamide synthesis, and relates to a flame-retardant polyamide 6 and a preparation method thereof, in particular to a flame-retardant polyamide 6 with excellent comprehensive performance prepared by introducing a phosphorus-based flame retardant and a preparation method thereof. Background technique [0002] Polyamide, commonly known as nylon, has the characteristics of many varieties, large output and wide application. It is one of the five major engineering plastics. Polyamide 6 is the most widely used variety of polyamides. It has excellent properties such as high mechanical strength, wear resistance, oil resistance, weak acid resistance, and alkali resistance. It can be processed into plastics, fibers, and films, but the limiting oxygen index of polyamide 6 is limited. It is only about 21%, and the phenomenon of molten droplets is serious when burning, which seriously limits the appli...

Claims

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Application Information

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IPC IPC(8): C08L77/02C08K5/5313C08G69/42
CPCC08G69/42C08K5/5313C08L2201/02C08L2201/22C08L77/02
Inventor 肖茹刘可李圆圆李桃桃王华平
Owner DONGHUA UNIV
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