Flame-retardant plasticizer of methyl silicate trichloroethyl ester compound and preparation method thereof

A technology of trichloroethyl methyl silicate, flame retardant plasticizer, applied in chemical instruments and methods, compounds of elements in Group 4/14 of the periodic table, organic chemistry, etc. It is related to the problems of high price of flame retardant plasticizers, and achieves the effect of no pollution, easy large-scale production and good flame retardancy.

Active Publication Date: 2012-10-17
江苏羚翎应急装备科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, phosphorus-based flame-retardant plasticizers have been used, and the development and application of silicon-based flame-retardant plasticizers has been limited due to their high price.

Method used

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  • Flame-retardant plasticizer of methyl silicate trichloroethyl ester compound and preparation method thereof
  • Flame-retardant plasticizer of methyl silicate trichloroethyl ester compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 In a 200ml four-neck flask equipped with a stirrer, a thermometer and a fractional distillation device, add 0.1mol (13.6g) methyltrimethoxysilane and 0.3mol (24.2g) chloroethanol and 40ml xylene to heat up 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 amount of methanol is close to the theoretical amount. Then distill off the solvent, excess chloroethanol (recovered for use) and low boilers, and cool to obtain trichloroethyl methylsilicate with a yield of 92%. Its decomposition temperature is 235±5°C, and its flash point (open cup) is 195±5°C. Density is 1.333 (20°C), refractive index n D 25 = 1.4558.

Embodiment 2

[0026] Example 2 In a 200ml four-neck flask equipped with a stirrer, a thermometer and a fractional distillation device, add 0.1mol (13.6g) methyltrimethoxysilane, 0.32mol (25.8g) chloroethanol and 40ml chlorobenzene to raise the temperature Reflux to 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 amount of methanol is close to the theoretical amount. Then distill off the solvent, excess chloroethanol (recovered for use) and low boilers, and cool to obtain trichloroethyl methylsilicate with a yield of 95%. Its decomposition temperature is 235±5°C, and its flash point (open cup) is 195±5°C. Density is 1.333 (20°C), refractive index n D 25 = 1.4558.

Embodiment 3

[0027] Example 3 In a 200ml four-neck flask equipped with a stirrer, a thermometer and a fractionation device, add 0.1mol (13.6g) methyltrimethoxysilane and 0.34mol (27.4g) chloroethanol and 40ml ethylene glycol diethyl ether, 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). As the reaction progresses, the reflux temperature gradually increases to 122°C, and the reflux time is about 10h. Until the distilled methanol is close to the theoretical amount. Then distill off the solvent, excess chloroethanol (recovered for use) and low boilers, and cool to obtain trichloroethyl methylsilicate with a yield of 96%. Its decomposition temperature is 235±5°C, and its flash point (open cup) is 195±5°C. Density is 1.333 (20°C), refractive index n D 25 = 1.4558.

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Abstract

The invention relates to a flame-retardant plasticizer of a methyl silicate trichloroethyl ester compound and a preparation method thereof, in particular to a methyl silicate tri(2-chloroethyl) ester compound and a preparation method thereof. The structure of the compound is shown as CH3Si(OCH2CH2Cl)3. The preparation method comprises the following steps of: mixing methyltrimethoxy silane and ethylene chlorohydrin in a certain molar ratio with an organic solvent by stirring; heating for refluxing; removing a fixed amount of methanol generated by a reaction by evaporating with a fractionating device; and purifying to obtain liquid methyl silicate trichloroethyl ester. The methyl silicate trichloroethyl ester obtained with the method has high flame retardance, high plasticity, a simple production process, small equipment investment and low cost, is environment-friendly and is easy for realizing industrial production.

Description

technical field [0001] The invention relates to a flame-retardant plasticizer trichloroethyl methyl silicate compound and a preparation method thereof. Specifically relates to a methyl silicate tris (2-chloroethyl) ester compound and a preparation method thereof. Trichloroethyl methyl silicate is a silicone flame retardant plasticizer, suitable for flame retardant plasticizing additives of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin, etc. Background technique [0002] Due to the extensive application of flammable polymer materials and plasticizers, flame retardants have been developed rapidly. At present, the amount of flame retardant is the second largest additive after the amount of plasticizer. From the perspective of ease of use, people always hope that the flame retardancy and plasticizing properties can be reflected in the same compound structure, that is, the synthesis of flame retardant plasticizers; from the application, it is found that some ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/5419C08L27/06C08L29/04C08L63/00C08L75/04
Inventor 王彦林王玉霞楼帅
Owner 江苏羚翎应急装备科技有限公司
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