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A kind of preparation method of phosphorus-nitrogen compound grafted hydrotalcite flame retardant

A technology of hydrotalcite and flame retardant is applied in the field of preparation of phosphorus-nitrogen compound grafted hydrotalcite flame retardant, which can solve the problems of poor dispersion, high energy consumption and high cost, achieve cost reduction, enhance flame retardant effect, Easy-to-use effects

Active Publication Date: 2018-05-22
福正集团股份有限公司
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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 compound-grafted hydrotalcite flame retardant, since hydrotalcite 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. After the reaction, it is necessary to Distillation and recovery of organic solvents consume a lot of energy and cost, which is not conducive to industrial production and application

Method used

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  • A kind of preparation method of phosphorus-nitrogen compound grafted hydrotalcite flame retardant

Examples

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Effect test

Embodiment 1

[0024] Add 100g of hydrotalcite to a stirring device connected with a nitrogen gas inlet pipe, and add 10.0g of 3-aminopropyltrimethyloxysilane and 13.0g of dichlorophosphate dropwise at a stirring rate of 2000 rpm. Phenyl ester was reacted at 100° C. for 2 hours under the condition of nitrogen flow rate of 100 cubic meters per hour to prepare a phosphorus-nitrogen compound grafted hydrotalcite flame retardant with a yield of 98.5%.

Embodiment 2

[0026] The synthesis operation of the phosphorus nitrogen compound grafted hydrotalcite flame retardant is the same as in Example 1. The mass ratio of hydrotalcite to 3-aminopropyltriethoxysilane is 1.0:0.03, and the mass ratio of 3-aminopropyltriethoxysilane to diphenyl chlorophosphate is 1.0:1.7, stirring The rate was 800 rpm, the reaction temperature was 50° C., the reaction time was 4 hours, the nitrogen flow rate was 15 cubic meters per hour, and the yield was 98.4%.

Embodiment 3

[0028] The synthesis operation of the phosphorus nitrogen compound grafted hydrotalcite flame retardant is the same as that of Example 1. In this example, 3-aminopropyltrimethoxysilane, hydrotalcite, and diphenyl chlorophosphate are used as raw materials. The mass ratio of hydrotalcite to 3-aminopropyltrimethoxysilane is 1.0:0.35, the mass ratio of 3-aminopropyltrimethoxysilane to diphenyl chlorophosphate is 1.0:1.0, and the stirring rate is 1200 rev / min, the reaction temperature is 80°C, the reaction time is 2.5 hours, the nitrogen flow rate is 40 cubic meters per hour, and the yield is 97.8%.

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Abstract

The invention relates to a preparation method of a flame retardant, in particular to a preparation method of a phosphorus-nitrogen compound grafted hydrotalcite flame retardant. The phosphorus-nitrogen compound grafted hydrotalcite flame retardant is prepared from an amino-containing silane coupling agent, diphenyl phosphoryl chloride and powdery hydrotalcite through solid-phase organic reaction. In the preparation process of the phosphorus-nitrogen compound grafted hydrotalcite flame retardant, the amino group of the silane coupling agent reacts with phosphoryl chloride to generate a by-product hydrogen chloride, and the hydrogen chloride serves as a catalyst for condensation reaction of the silane coupling agent and a hydrotalcite surface hydroxyl group, so that the silane coupling agent is grafted to the surface of the hydrotalcite through solid-phase reaction, and improvement of a phosphorus-nitrogen compound grafting rate on the surface of the hydrotalcite is facilitated.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of a phosphorus nitrogen compound grafted hydrotalcite flame retardant. Background technique [0002] Halogen-free flame retardants - organophosphorus nitrogen compounds have the advantages of less smoke, low toxicity, hydrolysis resistance, and good stability. Hydrotalcite / polymer composites are a "green" flame retardant material. Compared with other materials, it has the advantages of less dosage, low cost, high flame retardant efficiency, and less smoke generation. Combining the advantages of the two, an organophosphorus nitrogen compound that can realize the organicization of hydrotalcite is synthesized through molecular design. The compound reacts with hydrotalcite to obtain a new composite flame retardant—phosphorus nitrogen compound grafted water Talc flame retardant. Compared with the addition of hydrotalcite and conventional organic flam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/06C08K9/04C08K3/26C08L23/08
Inventor 黄国波
Owner 福正集团股份有限公司