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Retardant plasticizer methyl silicate ester compound and preparation method thereof

A technology of flame retardant plasticizer and methyl silicate tri-ester, which is applied in the field of methyl silicate triester compound and its preparation, can solve the problems of limited development and application, high price of silicon-based flame retardant plasticizer, etc., and achieve cost Low cost, easy large-scale production, cheap and easy-to-obtain raw materials

Inactive Publication Date: 2013-07-03
江门市鑫佰威塑胶制品有限公司
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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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  • Retardant plasticizer methyl silicate ester compound and preparation method thereof
  • Retardant plasticizer methyl silicate ester compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 In a 200ml four-neck flask equipped with a stirrer, a thermometer and a fractional distillation device, add 0.1mol (13.6g) of methyltrimethoxysilane and 0.3mol (28.4g) of monochloropropanol and 45ml of diethylene glycol Dimethyl ether, make it warm up to 104 ℃ and reflux, and continuously distill the methanol generated by the reaction through the fractionation device (control the column top temperature not higher than 64 ℃). As the reaction progresses, the reflux temperature gradually increases to 162 ℃, and the The time is about 6h, until the methanol evaporated is close to the theoretical amount. Then distill off the solvent, excess dichloropropanol (recovered for use) and low boilers, and cool to obtain tris(monochloropropyl)methylsilicate with a yield of 92%. Its flash point (open cup): 200±5°C, decomposition temperature: 250±5°C, density 1.273g / ml, refractive index n D 25 = 1.4486.

Embodiment 2

[0029] Example 2 In a 200ml four-necked flask equipped with a stirrer, a thermometer and a fractionation device, add 0.1mol (13.6g) methyltrimethoxysilane and 0.32mol (30.3g) monochloropropanol and 45ml xylene 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, excess dichloropropanol (recovered for use) and low boilers, and cool to obtain tris(monochloropropyl)methylsilicate with a yield of 94%. Its flash point (open cup): 200±5°C, decomposition temperature: 250±5°C, density 1.273g / ml, refractive index n D 25 = 1.4486.

Embodiment 3

[0030] 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 (32.2g) monochloropropanol and 45ml chlorobenzene to make It was heated to reflux at 104°C, and the methanol produced by the reaction was continuously distilled out 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, excess dichloropropanol (recovered for use) and low boilers, and cool to obtain tris(monochloropropyl)methylsilicate with a yield of 96%. Its flash point (open cup): 200±5°C, decomposition temperature: 250±5°C, density 1.273g / ml, refractive index n D 25 = 1.4486.

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Abstract

The invention relates to a retardant plasticizer methyl silicate ester compound and a preparation method thereof, in particular to methyl silicic acid tris(1-chloro-1-methylethyl)ester and a preparation method thereof. The compound has the structure shown as CH3Si(OC3H6Cl)3. The preparation method comprises the following steps of: mixing methyltrimethoxy silane and 1-chloro propanol in a certain molar ratio with an organic solvent, heating for refluxing, steaming out quantitative methanol generated in reaction by using a fractionating device, and performing passivation treatment to obtain colorless to light yellow liquid, namely the methyl silicate ester. The methyl silicate ester has good retardant plasticization; moreover, the production process is simple, equipment investment is low, cost is low, pollution is avoided and the invention is suitable for industrial production.

Description

technical field [0001] The invention relates to a flame-retardant plasticizer methyl silicate compound and a preparation method thereof. Specifically relates to a methyl silicate tris (monochloropropyl) ester compound and a preparation method thereof. Tris (monochloropropyl) 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] With the extensive application of synthetic organic polymer materials, the amount of plasticizer is huge. In order to solve the flammability problem of polymer materials, 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 s...

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 王彦林韦春胜王玉红
Owner 江门市鑫佰威塑胶制品有限公司
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