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Methyl silicic acid tri(2,3-dichloropropyl) ester compound and preparation method thereof

A technology of tri- and dichloropropyl methylsilicate, which is applied in the field of methylsilicate triester compounds and its preparation, can solve the problems of high price and restrictions, achieve low cost, solve the problem of comprehensive utilization, and high resistance The effect of fuel efficiency

Inactive Publication Date: 2013-01-23
枣阳市佳宝硅助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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

Method used

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  • Methyl silicic acid tri(2,3-dichloropropyl) ester compound and preparation method thereof
  • Methyl silicic acid tri(2,3-dichloropropyl) ester compound and preparation method thereof
  • Methyl silicic acid tri(2,3-dichloropropyl) ester compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 In a 200ml four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a hydrogen chloride absorption device, add 0.2mol (29.9g) of methyltrichlorosilane, and then start to drop 0.60mol (77.4 g) Dichloropropanol, and control the dropping temperature below 50°C. After the drop, maintain the reaction at 50°C for 20h under reflux. After the hydrogen chloride is released, the reaction ends. Add 1.0g of melamine, stir well, and remove by distillation under reduced pressure A small amount of low-boiling matter was filtered to obtain tris(2,3-dichloropropyl) methylsilicate as a light yellow oily liquid with a yield of 91%. 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

[0018] Example 2 In a 200ml four-neck flask equipped with a stirrer, a thermometer, a reflux condenser and a hydrogen chloride absorption device, add 0.2mol (29.9g) of methyltrichlorosilane, and then start to drop 0.64mol (82.56 g) Dichloropropanol, and control the dropping temperature below 50°C. After dropping, raise the temperature to 70°C and reflux for 16 hours. After the hydrogen chloride is released, the reaction ends. Add 1.0g of melamine, stir well, and distill under reduced pressure Excess dichloropropanol (for recycling) and a small amount of low-boiling matter were removed, and then filtered to obtain light yellow oily liquid tris(2,3-dichloropropyl)methylsilicate, 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

[0019] Example 3 In a 200ml four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a hydrogen chloride absorption device, add 0.2mol (29.9g) of methyltrichlorosilane, and then start to drop 0.68mol (87.72 g) dichloropropanol, and control the dropping temperature below 50°C. After dropping, raise the temperature to 100°C and reflux for 13 hours. After the hydrogen chloride is released, the reaction ends. Add 1.0g of melamine, stir well, and distill under reduced pressure Excess dichloropropanol (for recycling) and a small amount of low-boiling matter were removed, and then filtered to obtain light yellow oily liquid tris(2,3-dichloropropyl)methylsilicate 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 Si and Cl synergistic fire retardant methyl silicic acid tri(2,3-dichloropropyl) ester compound and a preparation method thereof. The structure of the compound is shown in the specification. The preparation method comprises the following steps: dropwise adding dichloropropanol with a certain molar ratio in methyl trichlorosilane at the temperature of 25 DEG C; heating to react for a period of time; after discharging hydrogen chloride, and purifying, so as to obtain the methyl silicic acid tri(2,3-dichloropropyl) ester. The methyl silicic acid tri(2,3-dichloropropyl)ester is high in inflaming retarding efficiency and is good in compatability with polymer materials, and has the advantages of simple process, less equipment investment and low cost. The preparation method is easy to achieve industrial production.

Description

technical field [0001] The invention relates to a tris(2,3-dichloropropyl) methyl silicate compound and a preparation method thereof. Tris(2,3-dichloropropyl) methylsilicate is a silicon-chloride dual-element synergistic flame retardant with high flame retardant performance, suitable for polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin, etc. fuel additives. Background technique [0002] The rapid development of synthetic polymer materials has brought civilization and progress to the society. Its flammability often causes fires and poses a serious threat to people's lives and property, which has also attracted people's attention. Thereby promoting the research of flame retardant technology and the rapid development of the flame retardant industry, and with the improvement of people's living standards, the requirements for flame retardants are getting higher and higher. It is always hoped that flame retardants with low toxicity, high efficiency and low price ...

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 王彦林韦春胜宋瑞峰
Owner 枣阳市佳宝硅助剂有限公司
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