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Chlorine-containing methyl silicate flame retardant and preparation method thereof

A technology of chloromethylsilicate and methylsilicate, which is applied in the field of methylsilicate triester compound and its preparation, can solve the problems of high price and limited application of organosilicon-based flame retardants, and achieve dual-element Synergistic effect of high flame retardant efficiency, simple preparation method, and good molecular symmetry

Inactive Publication Date: 2012-10-24
南通亮典彩印包装有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the application of silicone-based flame retardants is often limited due to their high price

Method used

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  • Chlorine-containing methyl silicate flame retardant and preparation method thereof
  • Chlorine-containing methyl silicate flame retardant and preparation method thereof
  • Chlorine-containing methyl silicate flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 In a 200ml four-necked flask equipped with a stirrer, a thermometer and a fractional distillation device, add 0.1mol (13.6g) of methyltrimethoxysilane and 0.3mol (38.7g) of dichloropropanol and 50ml of dioxane , make it warm up to 102°C and reflux, and continue to distill off the methanol produced by the reaction through the fractionation device (control the column top temperature not higher than 64°C), and the reflux time is about 14h, until the distilled methanol is close to the theoretical amount. Then distill off the solvent and excess dichloropropanol (for recycling), and cool to obtain a chloromethyl silicate flame retardant with a yield of 92%. Its flash point (open cup): 240±5°C, decomposition temperature: 270±5°C, density 1.371g / ml, refractive index n D 25 = 1.4906.

Embodiment 2

[0028] Example 2 In a 200ml four-neck flask equipped with a stirrer, a thermometer and a fractionation device, add 0.1mol (13.6g) methyltrimethoxysilane and 0.32mol (41.3g) dichloropropanol and 50ml toluene to make Raise the temperature to reflux at 104°C, and continuously distill the methanol generated by the reaction through the fractionation device (control the column top temperature not higher than 64°C). The methanol produced is close to the theoretical amount. Then distill off the solvent and excess dichloropropanol (recycled for use), and cool to obtain a chloromethyl silicate flame retardant with a yield of 94%. Its flash point (open cup): 240±5°C, decomposition temperature: 270±5°C, density 1.371g / ml, refractive index n D 25 = 1.4906.

Embodiment 3

[0029] Example 3 In a 200ml four-necked flask equipped with a stirrer, a thermometer and a fractional distillation device, add 0.1mol (13.6g) methyltrimethoxysilane and 0.34mol (43.9g) dichloropropanol and 50ml chlorobenzene to make It was heated to reflux at 104°C, and the methanol produced by the reaction was continuously distilled through the fractionation device (controlling the column top temperature not higher than 64°C). The distilled methanol is close to the theoretical amount. Then distill off the solvent and excess dichloropropanol (recycled for use), and cool to obtain a chloromethyl silicate flame retardant with a yield of 96%. Its flash point (open cup): 240±5°C, decomposition temperature: 270±5°C, density 1.371g / ml, refractive index n D 25 = 1.4906.

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Abstract

The invention relates to a chlorine-containing methyl silicate flame retardant, namely a tris(2,3-dichloropropyl) methyl silicate compound, and preparation method thereof. The structure of the compound is shown by a formula below. The preparation method comprises: reacting methyltrimethoxy silane and dichloropropanol in an organic solvent according to a certain molar ratio, distilling methanol generated by the reaction, and purifying to obtain the chlorine-containing methyl silicate flame retardant. The flame-retarding efficiency of the flame retardant is high, the synthesis process is simple, the cost is low, pollution is avoided, and thus, the flame retardant has a bright application prospect.

Description

technical field [0001] The invention relates to a chloromethyl silicate flame retardant and a preparation method thereof, in particular to a tris(2,3-dichloropropyl) methyl silicate compound and a preparation method thereof. Chloromethyl silicate is a synergistic flame retardant containing silicon and chlorine dual elements. It has high flame retardant performance and is suitable for flame retardant additives such as polyvinyl chloride, polyurethane, epoxy resin, and unsaturated resin. Background technique [0002] The wide application of organic synthetic polymer materials has promoted the research of flame retardant technology and the rapid development of flame retardant industry, and with the improvement of people's living standards, the requirements for flame retardants are getting higher and higher. The market always hopes to develop flame retardants with low toxicity, high efficiency and low price, that is, excellent cost performance. In order to achieve the above goa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5419C07F7/12C08L27/06C08L29/04C08L63/00C08L75/04
Inventor 王彦林韦春胜王伟
Owner 南通亮典彩印包装有限公司
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