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In-situ polymerization type N-P synergistic flame-retardant nylon and preparation method thereof

A synergistic flame-retardant, polymeric technology, applied in the field of in-situ polymerized N-P synergistic flame-retardant nylon and its preparation, to achieve the effect of controllable viscosity

Inactive Publication Date: 2021-05-18
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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  • In-situ polymerization type N-P synergistic flame-retardant nylon and preparation method thereof
  • In-situ polymerization type N-P synergistic flame-retardant nylon and preparation method thereof
  • In-situ polymerization type N-P synergistic flame-retardant nylon and preparation method thereof

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preparation example Construction

[0071] The preparation method of in-situ polymerized N-P synergistic flame-retardant nylon of the present invention specifically comprises the following steps:

[0072] (A) Reaction of organophosphorus flame retardant monomers with diamines, preferably with excess amino groups, to form salts;

[0073] (B) make the reaction product of step (A) and diacid and diamine or dibasic amide salt in the presence of 1-10wt% relative to the total weight of all polymerized monomers, preferably 3-6wt% nitrogen-based flame retardant The following reaction is used to prepare in-situ polymerized N-P synergistic flame-retardant nylon.

[0074] 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.

[0075] Preferably, the diamine monomers described in step (A) are hexamethylenediamine, decanediamine, nonanediamine, undecanediamine, dodecanediamine, aliph...

Embodiment 1

[0091] Stir the flame retardant monomer and hexamethylenediamine in an aqueous solution at 40°C for 0.5h at a molar ratio of 1:1.2, adjust the pH of the solution to 7.2, and obtain a salt solution.

[0092] High-speed shear emulsification of 4% MCA accounting for the total mass of polymerized monomers (including the above-mentioned salt solution and the following nylon 66 salt) in a certain amount of water for 10 minutes to obtain a uniformly dispersed MCA emulsion.

[0093] Mix the nylon 66 salt (hexamethylene adipamide salt) solution with the salt solution obtained above, the MCA emulsion, and the catalyst hypophosphorous acid each accounting for 1‰ Sodium, antioxidant p-phenylenediamine, and 40% deionized water were added to the reactor, vacuumed, filled with nitrogen for 5 times, and finally the internal pressure of the reactor was kept at 0.2 MPa. 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...

Embodiment 2

[0096] Stir and react the flame retardant monomer and hexamethylenediamine in an aqueous solution at a molar ratio of 1:1.3 at 50°C for 1 hour, and adjust the pH of the solution to 7.8.

[0097] 3% MCA accounting for the total mass of polymerized monomers was emulsified in a certain amount of water at high speed for 6 minutes to obtain a uniformly dispersed MCA emulsion.

[0098] Adipic acid and hexamethylenediamine are configured according to a mass ratio of 1:1.3, and the above-mentioned salt solution, MCA emulsion, catalyst toluenesulfonic acid and antioxidant Agent 2, 6-di-tert-butyl-4-methylphenol, and 35% deionized water were added to the reactor, vacuumed and filled with nitrogen for 3 times, and finally the internal pressure of the reactor was kept at 0.3 MPa. 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 ...

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Abstract

The invention discloses in-situ polymerization type N-P synergistic flame-retardant nylon 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 a salt; (B) emulsifying and dispersing a nitrogen flame retardant to obtain a nitrogen flame retardant emulsion; and (C) adding diacid and diamine or binary amide salt or a solution thereof, the prepared salt or a solution thereof, the nitrogen flame retardant emulsion, an antioxidant and a catalyst into a reaction kettle, and carrying out in-situ polymerization in an inert atmosphere by regulating and controlling the reaction temperature and pressure to prepare the required N-P synergistic flame-retardant nylon material. According to the prepared in-situ polymerization type flame-retardant nylon, due to the synergistic effect, the total amount of the flame retardant needing to be added is reduced. The viscosity in the whole preparation process is controllable, a product with excellent mechanical property and flame retardant property can be obtained, the vertical combustion test can reach UL-94V-0 level, and the limit oxygen index is 28% or above.

Description

[0001] This case is a divisional application with the application number: 201610932376.5 and the title of the invention: an in-situ polymerized N-P synergistic flame-retardant nylon and its preparation method. technical field [0002] The invention belongs to the technical field of flame-retardant polymer synthesis, and relates to an in-situ polymerized N-P synergistic flame-retardant nylon and a preparation method thereof. Background technique [0003] Nylon (PA) plays an important role in the fields of machinery, transportation, electronics, military, aerospace and other fields due to its high mechanical strength, good thermal stability, wear resistance, and excellent solvent resistance. However, nylon, which is a self-extinguishing polymer material, generally has a limiting oxygen index value of no more than 23%, and its vertical combustion test level is V-2. The fire caused great loss to the preparation and life, and could not meet the flame retardant requirements in pra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L77/06C08K5/3492C08K5/52C08G69/42
CPCC08G69/42C08K5/34928C08L2201/02C08K5/5205C08L77/06
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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