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Black phosphorus flame retardant coated by in-situ polymerization of cast nylon 6 and preparation method and application of flame retardant

A technology of casting nylon and in-situ polymerization, which is applied in the field of flame retardant materials, can solve the problems of poor compatibility and achieve good compatibility

Active Publication Date: 2019-09-10
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention mainly aims at the shortcomings of the existing black phosphorus flame retardants, which are easy to degrade and have poor compatibility with the polymer matrix, and provides a cast nylon 6 in-situ polymerization-coated black phosphorus flame retardant. The flame retardant uses cast nylon 6 In-situ polymerization coating nano-scale or micron-scale black phosphorus, so that the flame retardant is dispersed in the material matrix at the nanoscale, which can not only improve the flame retardant performance of the material, but also improve the mechanical properties of the material, and broaden the scope of the flame retardant. field of application

Method used

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  • Black phosphorus flame retardant coated by in-situ polymerization of cast nylon 6 and preparation method and application of flame retardant
  • Black phosphorus flame retardant coated by in-situ polymerization of cast nylon 6 and preparation method and application of flame retardant

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Embodiment 1

[0039]The preparation method of the cast nylon 6 in-situ polymerization coated black phosphorus flame retardant in this embodiment comprises the following steps:

[0040] S1. Add anhydrous and oxygen-free N-methylpyrrolidone (NMP) into the reactor, and place 1mol two-dimensional black phosphorus and 10mol caprolactam monomers with a particle diameter of 100nm in pre-storage tanks connected to the reactor respectively. The reaction kettle and the pre-storage tank system are circulated with nitrogen gas to remove air and a small amount of moisture in the system;

[0041] S2. In the pre-storage tank of black phosphorus, add 0.3% TDI promoter of caprolactam monomer weight, in the pre-storage tank of caprolactam monomer, add 0.2% sodium hydroxide catalyst of caprolactam monomer weight, be warming up to 130 ~ 140°C, use circulating inert gas or vacuum to remove the moisture generated in the system;

[0042] S3. Add the pretreated body of black phosphorus and cocatalyst, the pretrea...

Embodiment 2

[0046] The preparation method of the cast nylon 6 in-situ polymerization coated black phosphorus flame retardant in this embodiment comprises the following steps:

[0047] S1. Anhydrous and oxygen-free dimethylformamide (DMF) is added in the reactor, 1mol two-dimensional black phosphorus of 50nm and 0.01mol laurolactam monomer are respectively placed in the pre-storage tank communicated with the reactor, The entire reaction kettle and pre-storage tank system are circulated with nitrogen gas to remove air and a small amount of moisture in the system;

[0048] S2. In the pre-storage tank of black phosphorus, add 0.5% MDI cocatalyst of laurolactam monomer weight, add 0.2% of laurolactam monomer weight in the pre-storage tank of laurolactam monomer Sodium hydroxide catalyst, heat up to 130~140°C, use circulating inert gas or vacuum to remove the moisture generated in the system;

[0049] S3. Put the black phosphorus in the two pre-storage tanks, the pretreated body of the cocatal...

Embodiment 3

[0053] The preparation method of the cast nylon 6 in-situ polymerization coated black phosphorus flame retardant in this embodiment comprises the following steps:

[0054] S1. Add anhydrous and oxygen-free dimethylacetamide (DMAC) into the reactor, and place 10 mol black phosphorus and 30 mol caprolactam monomers of 1 μm in pre-storage tanks connected to the reactor respectively. The entire reactor and pre-storage The tank system is circulated with nitrogen gas to remove air and a small amount of moisture in the system;

[0055] S2. In the pre-storage tank of black phosphorus, add the HDI promoter of 0.8% of caprolactam monomer weight, add the 0.3% sodium hydroxide catalyst of caprolactam monomer weight in the pre-storage tank of caprolactam monomer, be warming up to 130~140 °C, use circulating inert gas or vacuum to remove the moisture generated in the system;

[0056] S3. Add the pretreated body of black phosphorus and cocatalyst, the pretreated body of caprolactam monomer ...

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Abstract

The invention discloses a black phosphorus flame retardant coated by in-situ polymerization of cast nylon 6. The flame retardant is prepared by coating black phosphorus by in-situ polymerization of cast nylon 6 under inert gas protection, wherein the black phosphorus comprises massive black phosphorus and low-dimensional black phosphorus, the massive black phosphorus is obtained by conversion fromwhite phosphorus or red phosphorus under high temperature and high pressure conditions, and the low-dimensional black phosphorus is prepared by massive black phosphorus through a mechanical peeling method or liquid phase peeling method. Innovatively, cast nylon 6 is introduced into an aprotic polar solvent or a polar protic solvent containing black phosphorus to carry out surface modification orcoating of black phosphorus, and a novel flame retardant is prepared by selecting a cast nylon 6 monomer, a catalyst and a co-catalyst and combining the selection of a black phosphorus size. The flameretardant utilizes in-situ polymerization of cast nylon 6 to coat nano- or micro-scale black phosphorus, so that the flame retardant is dispersed in a material matrix in nano-scale, flame retardancyof a material can be improved, various mechanical properties of the material can be also enhanced, and the application field of the flame retardant is broadened.

Description

technical field [0001] The invention relates to the field of flame retardant materials, more specifically, to a cast nylon 6 in-situ polymerization-coated black phosphorus flame retardant and its preparation method and application. Background technique [0002] A large number of studies have shown that both halogen and phosphorus will produce harmful substances during combustion, so ideal green flame-retardant products should not contain halogen and phosphorus. At present, the most economical green flame retardants are inorganic flame retardants, especially aluminum hydroxide and magnesium hydroxide. For nylon, melamine cyanurate flame-retardant nylon is a representative green flame-retardant material today. Melamine cyanurate is widely used in unfilled nylon, while melamine polyphosphate is mostly used in flame retardancy of glass fiber reinforced nylon. However, on the basis of the existing technology, it is still difficult to use a halogen-free and phosphorus-free flame...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/10C08K3/02C08G69/14C08G69/16D01F1/07
CPCC08G69/14C08G69/16C08K3/02C08K9/10C08K2003/026D01F1/07
Inventor 赖登旺李玉华
Owner HUNAN UNIV OF TECH