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Organophosphorus copolymeric flame-retarded polyamide and preparation method thereof

A technology for copolymerizing flame retardant and organic phosphorus, which is applied in the field of flame retardant polymer synthesis

Inactive Publication Date: 2017-03-15
CHENGDU TALY TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the relative viscosity of the prepared polyamide material is only 0.78-0.82, and there is still a lot of room for improvement in the mechanical properties and other properties of the material samples

Method used

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  • Organophosphorus copolymeric flame-retarded polyamide and preparation method thereof
  • Organophosphorus copolymeric flame-retarded polyamide and preparation method thereof
  • Organophosphorus copolymeric flame-retarded polyamide and preparation method thereof

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preparation example Construction

[0062] The preparation method of the organophosphorus copolymerized flame-retardant polyamide of the present invention specifically comprises the following steps:

[0063] (A) reacting an organophosphorus flame retardant monomer with a diamine, preferably making the amino group excessive, to generate a salt solution;

[0064] (B) reacting the reaction product of step (A) with diacid, diamine or dibasic amide salt and lactam to produce organophosphorus copolymerized flame-retardant polyamide.

[0065] In step (A), preferably, the diamine monomer is slightly excessive, so that the pH of the salt solution is 7-9. The reaction temperature rose from room temperature to 40-70°C within 5-20 minutes.

[0066] Preferably, the diamine monomers used in step (A) are hexamethylenediamine, decanediamine, nonanediamine, undecanediamine, dodecanediamine, aliphatic C 6 -C 20 One or more of iminodiamine, aromatic diamine, and alicyclic diamine.

[0067] In step (B), preferably, the polymeri...

Embodiment 1

[0081] Stir and react the flame retardant monomer and hexamethylenediamine in an aqueous solution at a molar ratio of 1:1.2 at 60°C for 0.5 h, adjust the pH of the solution to 7.2, and dry to form a salt. Nylon 66 salt (hexamethylene adipamide salt) solution and caprolactam with a molar ratio of 1:1, the above-mentioned salt that accounts for 6.0% of the total mass of the two, catalyst sodium hypophosphite, antioxidant The agent p-phenylenediamine and 40% deionized water were added to the reactor, vacuumed and filled with nitrogen for 5 times, and finally the internal pressure of the reactor was kept at 0.2MPa. Heat the reactor, keep stirring at a high speed, and when the temperature of the reactor reaches 220°C and the pressure is 1.8 MPa, keep the temperature and pressure constant for 1.5 hours. Then the temperature was raised to 250°C, and the pressure was released to normal pressure within 1 hour. Vacuumize to -0.05MPa. After the stirring speed drops to a certain value an...

Embodiment 2

[0084] Stir and react the flame retardant monomer and hexamethylenediamine in an aqueous solution at a molar ratio of 1:1.3 at 45°C for 1 hour, adjust the pH of the solution to 7.8, and dry to form a salt. Adipic acid and hexamethylenediamine are configured according to a mass ratio of 1:1.2, and caprolactam with adipic acid molar ratio of 1:0.6 and 7% of the total weight of adipic acid, hexamethylenediamine and caprolactam The salt obtained above, the catalyst toluenesulfonic acid each accounting for 1‰, the antioxidant 2,6-di-tert-butyl-4-methylphenol, and the deionized water accounting for 35% were added to the reactor, Vacuumize, fill with nitrogen 3 times, and finally keep the pressure in the reactor at 0.3MPa. Heat the reactor, keep stirring at a high speed, and when the temperature of the reactor reaches 215°C and the pressure is 1.7 MPa, keep the temperature and pressure constant for 1.6 hours. Then the temperature was raised to 240°C, and the pressure was released to...

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Abstract

The invention discloses organophosphorus copolymeric flame-retarded polyamide and a preparation method thereof. The preparation method particularly comprises the following steps that 1 an organophosphorus flame-retarded monomer reacts with a diamine monomer, and salt is prepared; 2, diacid, diamine and / or binary amide salt, lactam, the salt prepared in the step 1, an antioxidant, a catalyst and deionized water are added into a reaction kettle, and the needed organophosphorus copolymeric flame-retarded polyamide material is prepared in situ in a nitrogen atmosphere by regulating and controlling the reaction temperature and pressure. According to the organophosphorus polyamide material prepared through the method, a little amount of reaction flame retardant is added, a synergistic flame retardant does not need to be added, the viscosity is controllable in the preparation process, and the obtained product is excellent in mechanical property and outstanding in flame retardance. Meanwhile, the preparation method has the advantages that the technology is environmentally friendly and simple, the cost is low, and operation is easy to learn.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant polymer synthesis, and relates to a preparation method of copolymerized flame-retardant polyamide, in particular to a polymer material containing a phosphorus-containing reactive flame retardant copolymerized and embedded in polyamide molecular chains and a preparation method thereof. Background technique [0002] Polyamide is widely used in construction, chemical industry, transportation and military fields because of its excellent properties, such as high strength, heat resistance, wear resistance, solvent resistance, etc. However, polyamide itself is not flame retardant and may cause or aggravate fires. Therefore, how to modify and prepare polyamides with good flame retardant properties has been researched by industry personnel. [0003] There are usually two ways to modify the flame retardant polyamide material: one is to add a reactive flame retardant to introduce a functional group ...

Claims

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Application Information

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IPC IPC(8): C08G69/42C08G69/36C08G69/04
CPCC08G69/36C08G69/42
Inventor 马永梅陶云峰吕文涛方辉张京楠陈群跃张程夕易丹青郑鲲
Owner CHENGDU TALY TECH CO LTD
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