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Phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant and preparation method thereof

A technology containing a phosphorus oxychloride compound and montmorillonite is applied in the field of flame retardants, which can solve the problems of unfavorable industrial production, poor dispersion and high cost, and achieve the effects of simplifying the synthesis process route, simple process route and reducing the preparation cost.

Active Publication Date: 2015-12-16
浙江超盛汽车零部件有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the preparation of phosphorus-nitrogen-silicon-based compound-loaded montmorillonite flame retardants, since montmorillonite is an inorganic compound, it is poorly dispersed in organic solvents, and it is necessary to add a large amount of organic solvents to ensure the smooth progress of the reaction. The organic solvent needs to be distilled and recovered, which consumes a lot of energy and costs, which is not conducive to industrial production

Method used

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  • Phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant and preparation method thereof

Examples

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Effect test

Embodiment 1

[0022] Add 1,500 kg of montmorillonite to a ball mill connected with a nitrogen inlet pipe. The size of the ball mill is Ф900×1800, and the ball loading capacity is 1.5 tons. Under the condition of the drum speed of the ball mill at 38 rpm, add 150 kg of 3-ammonia Propyl trimethoxy silane and 175 kilograms of diphenoxy phosphorus oxychlorides were ground and reacted for 40 minutes under the condition of 0.5 cubic meters per minute of nitrogen flow rate to prepare phosphorus nitrogen silicon series compound loaded montmorillonite flame retardant, The yield was 97.9%.

Embodiment 2

[0024] The synthesis operation of the montmorillonite flame retardant supported by phosphorus nitrogen silicon compounds is the same as in Example 1, and the raw materials are: montmorillonite, N-aminoethyl-γ-aminopropyltrimethoxysilane, and dimethylphosphoryl chloride. The amount of montmorillonite added is 38,000 kg, and the mass ratio of montmorillonite to N-aminoethyl-γ-aminopropyltrimethoxysilane is 1.0:0.02, and N-aminoethyl-γ-aminopropyltrimethoxysilane The ratio of the feed material of oxysilane to dimethylphosphoryl chloride is 1.0:2.5, the size of the ball mill is Ф2200×7500, the ball loading capacity is 35 tons, the drum speed is 21.7 rpm, the grinding time is 20 minutes, and nitrogen is introduced The flow rate was 0.1 m3 / min and the yield was 99.1%.

Embodiment 3

[0026] The synthesis operation of phosphorus nitrogen silicon compound loaded montmorillonite flame retardant is the same as in Example 1, the raw materials are: montmorillonite, 3-(2-aminoethylamino)propyltriethoxysilane, diethylphosphoryl chloride . The addition of montmorillonite is 4500 kg, and the mass ratio of montmorillonite to 3-(2-aminoethylamino)propyltriethoxysilane is 1.0:0.38, 3-(2-aminoethylamino) The ratio of propyltriethoxysilane to diethylphosphoryl chloride is 1.0:2.2, the size of the ball mill is Ф1500×3000, the ball loading capacity is 7.5 tons, the drum speed is 29.7 rpm, and the grinding time is 150 minutes , the nitrogen flow rate was 20 cubic meters per minute, and the yield was 97.3%.

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Abstract

The invention relates to a flame retardant, in particular to a phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant and a preparation method thereof. The phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant is prepared through a solid-phase grafting reaction between a phosphorus-nitrogen-silicon compound and montmorillonite powder particles, wherein the phosphorus-nitrogen-silicon compound comprises an amido containing silane coupling agent and a phosphoryl chloride containing compound, and is grafted onto montmorillonite through chemical bonds. During preparation of the phosphorus-nitrogen-silicon compound loaded montmorillonite flame retardant, an amino in the silane coupling agent reacts with phosphorus oxychloride to generate a by-product, namely hydrogen chloride gas; one part of the hydrogen chloride gas is brought out of the reaction system through nitrogen gas, and the other part of the hydrogen chloride gas serves as a catalyst for a condensation reaction between the silane coupling agent and a hydroxy on the surface of montmorillonite, so that the silane coupling agent can be grafted into the surface of montmorillonite through the solid-phase grafting reaction, the rate of the solid-phase grafting reaction is improved, and the reaction time is shortened.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a phosphorus-nitrogen-silicon compound-loaded montmorillonite flame retardant and a preparation method thereof. Background technique [0002] As a flame retardant additive, montmorillonite has the advantages of high flame retardant efficiency, low addition amount, halogen-free, low toxicity, and environmental friendliness, and has broad application prospects in the field of polymer flame retardant modification. With the continuous deepening of composite material technology research, more and more polymer / montmorillonite composite materials, as high-performance and multi-functional flame-retardant materials, have more and more important roles in the electronics, aerospace, construction, automobile and other industries. more widely used. Halogen-free flame retardants - organophosphorus nitrogen compounds have the advantages of less smoke, low toxicity, hydrolysis resistance, and good stability...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/06C08K9/04C08K3/34C08L23/12
Inventor 黄国波
Owner 浙江超盛汽车零部件有限公司
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