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Novel organic silicon cladded black phosphorus flame retardant as well as preparation method and application thereof

A technology of organosilicon and flame retardant, which is applied in the field of flame retardant materials and can solve the problems of poor flame retardant effect of flame retardants

Inactive Publication Date: 2019-07-23
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 poor flame retardant effect of the existing organosilicon flame retardants, and provides a new type of organosilicon-coated black phosphorus flame retardant. Combining the synergistic flame retardant effect of the two, the flame retardant is dispersed in the material matrix at a 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 application field of the flame retardant

Method used

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Examples

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preparation example Construction

[0031] The novel silicone-coated black phosphorus flame retardant disclosed by the invention is prepared by the following method: under the protection of an inert gas, the black phosphorus is coated with organic silicon in an aprotic polar solvent or a polar protic solvent.

[0032] Aprotic polar solvents are anhydrous acetonitrile, N-methylpyrrolidone, dimethylformamide, dimethylacetamide, 1,3-dimethyl-2-imidazolidinone, dimethyl sulfoxide, hexa At least one of methylphosphoric triamide and N,N-dimethylacrylurea.

[0033] The polar protic solvent is at least one of methanol, ethanol, isopropanol, ethylene glycol, and n-butanol.

[0034] The silicone is at least one of silane coupling agent, silicone rubber, polysiloxane, and organosilanolamide. Among them, the silane coupling agent is 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, Propylmethyldimethoxysilane, Phenyltriethoxysilane, Trid...

Embodiment 1

[0037] The preparation method of the organosilicon-coated black phosphorus novel flame retardant in the present embodiment comprises the following steps:

[0038] S1. Add anhydrous and oxygen-free N-methylpyrrolidone (NMP) into the reactor, and two-dimensional black phosphorus and 3-aminopropyltriethoxysilane with a particle size of 100nm are respectively placed in the pre-heating tank connected to the reactor. In the storage tank, the whole 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;

[0039] S2. Add 10mol of black phosphorus and 0.001mol of 3-aminopropyltriethoxysilane to the solvent in the reaction kettle in proportion, keep the temperature of the solvent in the kettle at 60°C, and react for 15 minutes while stirring;

[0040] S3. Finally, the material is cooled and discharged, filtered, and dried to obtain a new type of organic silicon-coated black phosphorus flame retardant. ...

Embodiment 2

[0042] The preparation method of the organosilicon-coated black phosphorus novel flame retardant in the present embodiment comprises the following steps:

[0043] S1. Anhydrous and oxygen-free dimethylformamide (DMF) is added to the reactor, and 50nm two-dimensional black phosphorus and tridecafluorooctyltrimethoxysilane are respectively placed in pre-storage tanks connected to 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;

[0044] S2. Add 1 mol of black phosphorus and 0.01 mol of tridecafluorooctyltrimethoxysilane to the solvent in the reaction kettle in proportion, keep the temperature of the solvent in the kettle at 80°C, and react for 30 minutes while stirring;

[0045] S3. Finally, the material is cooled and discharged, and stored in the form of a solution.

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Abstract

The invention discloses a novel organic silicon cladded black phosphorus flame retardant. The novel organic silicon cladded black phosphorus flame retardant is obtained by cladding black phosphorus with organic silicon in an aprotic polar solvent or a polar proton solvent under the protection of inert gas. A micron-grade or nano-grade flame-retarding raw material such as the black phosphorus or low-dimension black phosphorus is creatively subjected to organic silicon cladding and dispersion in the aprotic polar solvent or the polar proton solvent to prepare the micron-grade or nano-grade novelflame retardant; the novel flame retardant can improve various mechanical properties of a base material and can improve the flame-retarding grade of the material very well. According to the flame retardant disclosed by the invention, the micron-grade or nano-grade black phosphorus is cladded by the organic silicon and synergistic flame-retarding effects of the micron-grade or nano-grade black phosphorus and the organic silicon are combined, so that the flame retardant is dispersed into a base body of the material in a nano-grade manner; the flame-retarding performance of the material can be improved and the various mechanical properties of the material also can be improved; an application field of the flame retardant is expanded.

Description

technical field [0001] The invention relates to the field of flame retardant materials, more specifically, to a novel flame retardant coated with organosilicon black phosphorus 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 retardant ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/10C08K3/02
CPCC08K3/02C08K9/10C08K2003/026
Inventor 赖登旺李玉华龙双李笃信姜其斌杨军刘跃军
Owner HUNAN UNIV OF TECH
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