Phosphorus-nitrogen-silicon-containing titanium dioxide hybrid nanoparticle flame retardant as well as preparation method and application thereof

A technology of hybrid nanoparticles and titanium dioxide, applied in the field of flame retardants, can solve the problems of low flame retardant efficiency and poor dispersion, and achieve the effects of improving flame retardant performance, increasing mechanical properties and suppressing combustion.

Active Publication Date: 2021-03-19
XIAMEN UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the existing polymer titanium dioxide flame retardant system, there

Method used

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  • Phosphorus-nitrogen-silicon-containing titanium dioxide hybrid nanoparticle flame retardant as well as preparation method and application thereof
  • Phosphorus-nitrogen-silicon-containing titanium dioxide hybrid nanoparticle flame retardant as well as preparation method and application thereof
  • Phosphorus-nitrogen-silicon-containing titanium dioxide hybrid nanoparticle flame retardant as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] ①Preparation of VP3: Put 2.6g of vanillin in 50mL of analytically pure first solvent chloroform, then add 2mL of triethylamine and slowly add 0.90g of phosphorus oxychloride dropwise, stir for 2h, then heat up to 50°C for 9 hours , after cooling to room temperature, pour 200mL of petroleum ether, stir for half an hour after the white precipitate is precipitated, wash with ethanol several times, and then filter to obtain a white solid; the obtained solid is vacuum-dried at 70°C to constant weight to obtain a white powder, which is The resulting phosphorous-containing VP3;

[0044] ②Preparation of DPASi: Dissolve 2g of dichlorodiphenylsilane in 30mL of the second solvent acetone, slowly add it dropwise to 50mL of 2.18g of K 2 CO 3 and 2.32g of p-nitrophenol in acetone, the second solvent, reflux, condense and heat to 45°C, react for 48h, filter the reaction solution with suction to obtain a solid filter cake, wash the filter cake with deionized water and the second solve...

Embodiment 2

[0048] ①Preparation of VP3: Put 2.6g of vanillin in 50mL of analytically pure first solvent chloroform, then add 2mL of triethylamine and slowly add 0.90g of phosphorus oxychloride dropwise, stir for 2h, then heat up to 50°C for 9 hours , after cooling to room temperature, pour 200mL of petroleum ether, stir for half an hour after the white precipitate is precipitated, wash with ethanol several times, and then filter to obtain a white solid; the obtained solid is vacuum-dried at 70°C to constant weight to obtain a white powder, which is The resulting phosphorous-containing VP3;

[0049] ②Preparation of DPASi: Dissolve 2g of dichlorodiphenylsilane in 30mL of the second solvent acetone, slowly add it dropwise to 50mL of 2.18g of K 2 CO 3 and 2.32g of p-nitrophenol in acetone, the second solvent, reflux, condense and heat to 45°C, react for 48h, filter the reaction solution with suction to obtain a solid filter cake, wash the filter cake with deionized water and the second solve...

Embodiment 3

[0053] ①Preparation of VP3: Put 2.6g of vanillin in 50mL of analytically pure first solvent chloroform, then add 2mL of triethylamine and slowly add 0.90g of phosphorus oxychloride dropwise, stir for 2h, then heat up to 50°C for 9 hours , after cooling to room temperature, pour 200mL of petroleum ether, stir for half an hour after the white precipitate is precipitated, wash with ethanol several times, and then filter to obtain a white solid; the obtained solid is vacuum-dried at 70°C to constant weight to obtain a white powder, which is The resulting phosphorous-containing VP3;

[0054] ②Preparation of DPASi: Dissolve 2g of dichlorodiphenylsilane in 30mL of the second solvent acetone, slowly add it dropwise to 50mL of 2.18g of K 2 CO 3 and 2.32g of p-nitrophenol in acetone, the second solvent, reflux, condense and heat to 45°C, react for 48h, filter the reaction solution with suction to obtain a solid filter cake, wash the filter cake with deionized water and the second solve...

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Abstract

The invention discloses a phosphorus-nitrogen-silicon-containing titanium dioxide hybrid nanoparticle flame retardant as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) reacting vanillic aldehyde, triethylamine and phosphorus oxychloride in a first solvent to obtain a product VP3; (2) enabling dichlorodiphenyl silane, K2CO3 and p-nitrophenol to react in a second solvent to obtain a product DPNSi, dissolving the DPNSi in a third solvent, then adding palladium-carbon super, and carrying out a reduction reaction with an ethanol solution of hydrazine hydrate to obtain DPASi; and (3) adding the VP3 and the DPASi into the ethyl acetate solution in which the titanium dioxide nanoparticles are dispersed, and carrying out condensationpolymerization reaction to obtain the titanium dioxide hybrid nanoparticle flame retardant VPASi containing phosphorus, nitrogen and silicon.

Description

technical field [0001] The invention belongs to the technical field of flame retardant materials, in particular to flame retardants. Background technique [0002] As a material with a wide range of application prospects, polymer materials have the advantages of good physical and chemical stability, easy modification, easy processing, and good optical properties. They are used in automobile manufacturing, electronic devices, coatings, and construction. . However, polymer materials are prone to stress relaxation and creep in terms of strength, and have certain limitations in high temperature performance, poor fire resistance and are very flammable. [0003] It is very necessary for polymer materials to improve their fire and flame retardancy without reducing their mechanical properties. However, in the existing polymer titanium dioxide flame retardant system, there are still problems such as poor dispersion and low flame retardant efficiency. Therefore, it is necessary to i...

Claims

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Application Information

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IPC IPC(8): C08K9/10C08K3/22C08L63/02C08G12/08C07F7/18C07F9/09
CPCC07F7/188C07F7/1892C07F9/091C08G12/08C08K3/22C08K9/10C08K2003/2241C08K2201/003C08K2201/011C08L2201/02C08L63/00
Inventor 戴李宗纪荣彬卢伟彭超华曾珊妮李伟航许一婷
Owner XIAMEN UNIV
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