Graphene hybrid particle flame-retardant agent and preparation method and application thereof

A flame retardant, graphene technology, applied in the field of graphene hybrid particle flame retardant, to achieve the effect of easy control and simple operation

Active Publication Date: 2018-03-20
TAIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to further exert the flame retardant effects of POSS, ionic liquids and graphene, we prepared a new type of hybrid graphene flame retardant by using the π-π and π-cation interactions between POSS-based ionic liquids and graphene. Flame retardants have high stability and structural controllability, and can achieve high-efficiency flame retardant systems. This kind of flame retardants has not been reported at home and abroad.

Method used

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  • Graphene hybrid particle flame-retardant agent and preparation method and application thereof
  • Graphene hybrid particle flame-retardant agent and preparation method and application thereof
  • Graphene hybrid particle flame-retardant agent and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 9.70 grams (0.01mol) of one-armed chlorobenzylethylisobutyl polyhedral oligomeric silsesquioxane (POSS) and dissolve it in 300ml of acetonitrile, then add 2.02 grams (0.02mol) of triethylamine and 0.75 grams of ( 0.005mol) sodium iodide (NaI), stirred and reacted at 80°C for 24 hours, and then added 3.68 grams (0.02mol) potassium hexafluorophosphate (KPF 6 ), stirred and reacted at 20~30°C for 16 hours. After the reaction, the resulting reaction solution was poured into 300ml of water to precipitate a solid product. The resulting mixed solution was suction filtered, washed, and the filter cake was vacuum-dried to obtain 9.34 grams of POSS-based amine salt ionic liquid , abbreviated as POSS-[TEA][PF 6 ], yield 79.1%, the prepared product structure is confirmed, 1 H NMR spectrum see attached figure 1 As shown, the FIIR spectrum of the prepared product is shown in the attached figure 2 shown. Take 4 grams of POSS-[TEA][PF 6 ] and 2 grams of graphene oxide (GO) w...

Embodiment 2

[0039] Take 9.70 g (0.01 mol) of single-arm chlorobenzyl ethyl isobutyl polyhedral oligomeric silsesquioxane (POSS) and dissolve it in 200 ml of acetonitrile, then add 1.18 g (0.02 mol) of trimethylamine and 0.75 g (0.005 mol) sodium iodide (NaI), stirred and reacted at 82°C for 16 hours, and then added 2.20 grams (0.02mol) sodium tetrafluoroborate (NaBF 4 ), stirred and reacted at 20~30°C for 24 hours. After the reaction, the obtained reaction solution was poured into 500ml of water to precipitate a solid product. The obtained mixed solution was suction filtered, washed, and the filter cake was vacuum-dried to obtain 7.80 grams of POSS-based amine salt ions Liquid, abbreviated as POSS-[TMA][BF 4 ], productive rate 72.2%. Take 4 grams of POSS-[TMA][BF 4 ] and 2 grams of graphene oxide (GO) were dissolved in 150ml of propylene carbonate (PC), stirred and reacted at 150°C for 6 hours. After the reaction, the obtained reaction solution was decompressed, distilled, and the filte...

Embodiment 3

[0043] Take 9.70 g (0.01 mol) of one-armed chlorobenzyl ethyl isobutyl polyhedral oligomeric silsesquioxane (POSS) and dissolve it in 500 ml of acetonitrile, then add 2.87 g (0.02 mol) of triethylamine and 0.83 g of ( 0.005mol) potassium iodide (KI), stirred and reacted at 82°C for 20 hours, and added 5.74g (0.02mol) lithium bis(trifluoromethanesulfonyl)imide (LiNTF) to the reaction solution after the reaction 2 ), stirred and reacted at 20~30°C for 20 hours. After the reaction, the resulting reaction solution was poured into 400ml of water to precipitate a solid product. The resulting mixed solution was suction filtered, washed, and the filter cake was vacuum-dried to obtain 7.89 grams of POSS-based amine salt ionic liquid , abbreviated as POSS-[TEA][NTF 2 ], productive rate 60.2%. Take 3 grams of POSS-[TEA][NTF 2 ] and 3 grams of graphene oxide (GO) were dissolved in 200ml of propylene carbonate (PC), stirred and reacted at 150°C for 9 hours. After the reaction, the result...

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Abstract

The invention discloses a graphene hybrid particle flame-retardant agent and a preparation method and application thereof. The preparation method comprises the following steps of enabling active POSS(polyhedral oligomeric silsesquioxane) and N-alkylamine to react, so as to realize ionizing; performing ion exchange reaction, so as to prepare a POSS-based quaternary ammonium salt ion liquid; enabling the POSS-based quaternary ammonium salt ion liquid to mutually react with phi-phi and phi-cations of graphene, so as to obtain the graphene hybrid particle flame-retardant agent. The prepared graphene hybrid particle flame-retardant agent is a halogen-free environment-friendly flame-retardant agent, and has the advantages that POSS, the ion liquid and graphene have different flame-retardant elements and mechanisms, and can generate the synergistic action; by adding 5% of synthesized flame-retardant agent, the limit oxygen index of PS (polystyrene) is increased to 26.5%; by adding 5% of synthesized flame-retardant agent, the limit oxygen index of PP (polypropylene) is increased to 25.9%; the effect is obviously better than the effect of organosilicone flame-retardant agent on market; thegraphene hybrid particle flame-retardant agent can be used as an additive to be applied into a polyolefin type polymer flame-retardant agent, the operation is simple and convenient, and the control is easy.

Description

technical field [0001] The invention relates to a graphene hybrid particle flame retardant and a preparation method and application thereof. Background technique [0002] Graphene is a two-dimensional carbon nanoparticle with a unique structure and good thermal conductivity and flame retardancy. In recent years, graphene has gradually developed into a new type of flame retardant system, which has revolutionized the development of flame retardants. influences. Compared with traditional flame retardant materials, a small amount of graphene can significantly reduce the maximum decomposition rate of polymer materials, delay the combustion process, and reduce the rate of smoke generation, thereby improving the flame retardant properties of the material. However, when graphene is used as a single flame retardant system, the flame retardant efficiency is not high. Therefore, in order to improve the flame retardant efficiency of graphene, graphene must be compounded with other flam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L83/04C08K3/04C08L25/06C08L23/12C08G77/04
CPCC08G77/045C08K3/04C08L23/12C08L25/06C08L2201/02C08L83/04
Inventor 何志才
Owner TAIZHOU UNIV
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