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Methyl tri(2-chloroethoxy) silane compound and preparation method thereof

A technology of chloroethoxyl and methyl trisilane, which is applied in the field of methyltrisilane compound and its preparation, can solve the problems of expensive silicon-based flame-retardant plasticizers, development and application limitations, etc., and achieve easy scale production and low cost. Low, good flame retardancy effect

Active Publication Date: 2012-12-26
河南森远科技有限公司
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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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  • Methyl tri(2-chloroethoxy) silane compound and preparation method thereof
  • Methyl tri(2-chloroethoxy) silane 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 dropping funnel, a reflux condenser and a hydrogen chloride absorption device on the mouth of the condenser, add 0.2mol (29.9g) methyltrichlorosilane, Then add 0.6mol (48.3g) of chloroethanol dropwise under the condition of cooling in a water bath, and control the temperature at a rate of addition not to exceed 35°C. After the drop is completed, the temperature is raised to 100°C and the reaction is refluxed for 8 hours. After the melamine is stirred evenly, a small amount of low boiling point matter is removed by distillation under reduced pressure, cooled and filtered to obtain a colorless liquid methyl tris(2-chloroethoxy)silane, and the product yield is 91%. 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

[0018] Example 2 In a 200ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a reflux condenser and a hydrogen chloride absorption device at the mouth of the condenser, add 0.2mol (29.9g) methyltrichlorosilane, Then add 0.66mol (53.1g) of chloroethanol dropwise under the condition of water bath cooling, and control the temperature not to exceed 35°C with the rate of addition. Melamine, after stirring, remove excessive chlorohydrin (recycling) and a small amount of low boiling point by distillation under reduced pressure, cool and filter to obtain colorless liquid methyl tris (2-chloroethoxy) silane, product yield 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

[0019] Example 3 In a 200ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel, a reflux condenser and a hydrogen chloride absorption device connected to the mouth of the condenser, add 0.2mol (29.9g) methyltrichlorosilane, Then add 0.72mol (58g) of chloroethanol dropwise under the condition of cooling in a water bath, and control the temperature by the rate of addition to not exceed 35°C. After dropping, the temperature is raised to 70°C for reflux for 4 hours. After the hydrogen chloride is released, the reaction is completed, and 1.0g of melamine is added After stirring evenly, excessive chloroethanol (recycled) and a small amount of low boiling point were removed by distillation under reduced pressure, cooled and filtered to obtain a colorless liquid methyl tris (2-chloroethoxy) silane, and the product yield was 97%. 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...

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Abstract

The invention relates to a methyl tri(2-chloroethoxy) silane compound which is used as a silicon-halogen synergistic flame-retardant plasticizer and a preparation method thereof. The methyl tri(2-chloroethoxy) silane compound has the following structural formula: CH3Si(OCH2CH2Cl)3. The preparation method of the methyl tri(2-chloroethoxy) silane compound comprises the following steps: dropwise adding and stirring chloroethanol at a certain molar ratio to methyl trichlorosilane, carrying out a reaction on the chloroethanol and the methyl trichlorosilane for a certain time at a certain temperature, and purifying after finishing hydrogen chloride release and reaction to obtain methyl tri(2-chloroethoxy) silane. The methyl tri(2-chloroethoxy) silane can be used as the good flame-retardant plasticizer, and the process for producing the methyl tri(2-chloroethoxy) silane is simple, has low equipment investment and cost and is easy to realize industrial production.

Description

technical field [0001] The invention relates to a methyl tris(2-chloroethoxy)silane compound and a preparation method thereof. Methyltris(2-chloroethoxy)silane belongs to chlorine-containing organosilicon dual-element synergistic flame retardant and also has good plasticity, which is suitable as a flame retardant for polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin, etc. For burning plasticizers. Background technique [0002] At present, the amount of synthetic polymer materials and plasticizers used for processing is huge. Since most polymer materials are extremely flammable and often cause fires, flame retardants have been developed rapidly. Today, the amount of flame retardant is the second largest additive after the amount of plasticizer. From the perspective of ease of use and the idea of ​​improving the utilization rate of chemical atoms, people always hope that the flame retardancy and plasticizing properties can be reflected in the same compound str...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/5419
Inventor 王彦林周中凯龚菁
Owner 河南森远科技有限公司
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