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

A synergistic flame retardant and polymerized technology, applied in the field of in-situ polymerized N-P synergistic flame retardant nylon and its preparation

Inactive Publication Date: 2017-02-22
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

[0069] The preparation method of in-situ polymerized N-P synergistic flame-retardant nylon of the present invention includes the following steps:

[0070] (A) Reacting an organophosphorus flame-retardant monomer or its derivative with a diamine monomer to make the amino group excessive to prepare a salt or salt solution;

[0071] (B) Let the reaction product of step (A) and the lactam be 1-10wt%, preferably 3-6wt% of the nitrogen-based flame retardant (for example, melamine cyanurate emulsion) relative to the total weight of all polymerized monomers In the presence of the reaction, the in-situ polymerized NP synergistic flame retardant nylon is formed.

[0072] In step (A), preferably, the flame retardant and the diamine monomer are reacted in a molar ratio of 1:0.1-20, preferably 1:0.5-10, more preferably 1:1-2.

[0073] In step (A), preferably, the diamine monomer is slightly excessive, so that the pH of the prepared salt solution is 7-9. The reaction temperature rose from room tem...

Embodiment 1

[0090] The flame-retardant monomer and hexamethylenediamine were stirred and reacted in a small amount of water at a molar ratio of 1:1.3 at 42°C for 0.5h, and the pH of the solution was adjusted to 7.5 to obtain a salt solution.

[0091] MCA accounting for 4% of the total mass of polymerized monomers (including the above-mentioned salts and the following lactam monomers) is emulsified at a high-speed shear in a certain amount of water for 10 minutes to obtain a uniformly dispersed MCA emulsion.

[0092] The caprolactam monomer, the salt solution obtained above (accounting for 4% of the total mass of the caprolactam monomer, excluding the solvent, the same below), the MCA emulsion, the catalyst sodium hypophosphite each accounting for 1‰, and the antioxidant terephthalic acid Amine and molecular weight regulator benzoic acid are added to the reactor, evacuated and filled with nitrogen three times, and finally the pressure in the reactor is maintained at 0.25 MPa. Heat the reaction ...

Embodiment 2

[0095] The flame-retardant monomer and hexamethylene diamine were stirred and reacted in a small amount of water at a molar ratio of 1:1.3 at 50° C. for 0.5 h, and the pH of the solution was adjusted to 7.5 to obtain a salt solution.

[0096] Melamine phosphate, which accounts for 4% of the total mass of polymerized monomers (including the above-mentioned salt and the following lactam monomers), is emulsified at high speed for 10 minutes in a certain amount of water to obtain a uniformly dispersed melamine phosphate aqueous dispersion.

[0097] The caprolactam monomer, the salt solution obtained above (accounting for 4% of the total mass of the caprolactam monomer), the melamine phosphate aqueous dispersion, the catalyst sodium hypophosphite each accounting for 1‰, the antioxidant p-phenylenediamine, the molecular weight adjustment Add benzoic acid to the reactor, evacuated, and filled with nitrogen three times, and finally kept the pressure in the reactor at 0.25MPa. Heat the reac...

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Abstract

The invention discloses an in-situ polymerization type N-P synergistic flame-retardant nylon and a preparation method thereof. The preparation method comprises the following steps: (1) reacting an organophosphorus flame-retardant monomer with a diamine monomer to form salt; (2) emulsifying and dispersing a nitrogen flame retardant, so as to obtain a nitrogen flame retardant emulsion; and (3) adding a lactam monomer, the salt prepared in the step (1), an antioxidant, the nitrogen flame retardant, a catalyst and a molecular weight adjusting agent into a reaction kettle, and performing in-situ polymerization by regulating reaction temperature and pressure under inert atmosphere, so as to obtain the needed N-P synergistic flame-retardant nylon material. According to the prepared in-situ polymerization type flame-retardant nylon, the content of the flame retardant needing to be added is reduced due to the synergistic effect, the viscosity during the whole preparation process is controllable, the product with both excellent mechanical performance and flame-retardant performance can be obtained, the vertical burning test can achieve the UL94 V-0 grade, and the limiting oxygen index is more than 28%.

Description

Technical field [0001] The invention relates to an in-situ polymerized N-P synergistic flame-retardant nylon and a preparation method thereof, belonging to the field of polymer flame-retardant materials. Background technique [0002] Nylon (PA) plays an important role in machinery, transportation, electronics, military, aerospace and other fields due to its high mechanical strength, good thermal stability, abrasion resistance, and excellent solvent resistance. However, nylon, which is a self-extinguishing polymer material, generally has a limiting oxygen index value of not more than 23%. The vertical combustion test level is V-2. Once it is ignited, it will be promoted by high heat generation, fast burning speed, and serious dripping. The fire caused heavy losses to the preparation and life, and could not meet the flame retardant requirements in practical applications. Therefore, the development of flame-retardant nylon with excellent comprehensive performance is of great signif...

Claims

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Application Information

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IPC IPC(8): C08L77/00C08K5/3492C08G69/36C08G69/04
CPCC08K5/34928C08G69/04C08G69/36C08L77/00
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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