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Organic phosphorus copolymerized flame-retardant polyamide and preparation method thereof

A technology of copolymerization of flame retardant and organophosphorus, which is applied in the field of flame retardant polymer synthesis to achieve the effect of controllable viscosity

Pending Publication Date: 2021-11-16
CHENGDU TALY TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Organic phosphorus copolymerized flame-retardant polyamide and preparation method thereof
  • Organic phosphorus copolymerized flame-retardant polyamide and preparation method thereof
  • Organic phosphorus copolymerized flame-retardant polyamide and preparation method thereof

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preparation example Construction

[0063] The preparation method of the organophosphorus copolymerized flame-retardant polyamide of the present invention specifically comprises the following steps:

[0064] (A) reacting an organophosphorus flame retardant monomer with a diamine, preferably making the amino group excessive, to generate a salt solution;

[0065] (B) reacting the reaction product of step (A) with diacid, diamine or dibasic amide salt and lactam to produce organophosphorus copolymerized flame-retardant polyamide.

[0066] 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.

[0067] 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.

[0068] In step (B), preferably, the polymeri...

Embodiment 1

[0082] 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

[0085] 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 organic phosphorus copolymerized flame-retardant polyamide and a preparation method thereof. The preparation method specifically comprises the following steps: (A) reacting an organic phosphorus flame-retardant monomer with a diamine monomer to form salt; (B) adding diacid and diamine and / or binary amide salt, lactam, the salt prepared in the step (A), an antioxidant, a catalyst and deionized water into a reaction kettle, and preparing the required organic phosphorus copolymerized flame-retardant polyamide in situ by regulating and controlling the reaction temperature and pressure in a nitrogen atmosphere. According to the prepared organic phosphorus polyamide material, the addition amount of the reaction flame retardant is small, 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 excellent in flame retardant property. Meanwhile, the preparation method also has the characteristics of environment-friendly and simple process, low cost and easiness in operation and learning.

Description

[0001] This case is a divisional application of the patent application with application number 201610932353.4 and the title of the invention "An organophosphorus-based copolymerized flame-retardant polyamide and its preparation method". technical field [0002] 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 [0003] 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 w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42C08G69/36
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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