Tri(chloroproply) methyl silicate compound and preparation method thereof

A technology of trichloropropyl methylsilicate, applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve development and application restrictions, silicon-based flame-retardant plasticization It solves the problem of comprehensive utilization, easy large-scale production, and low cost.

Active Publication Date: 2012-10-03
ENOVE PRECISION PLASTICS CATHETER
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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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  • Tri(chloroproply) methyl silicate compound and preparation method thereof
  • Tri(chloroproply) methyl silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 is equipped with agitator, thermometer, dropping funnel, reflux condenser and in the 200ml four-necked flask that is connected with hydrogen chloride absorption device on the condenser, adds 0.2mol (29.9g) methyltrichlorosilane, then Add 0.6mol (56.7g) of monochloropropanol dropwise under the cooling condition of water bath, and control the temperature not to exceed 40°C with the dropping rate, and maintain reflux at 40°C for 8 hours after the drop is completed. After the hydrogen chloride is released, the reaction is completed, and 1.0g is added 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 tris(monochloropropyl)methylsilicate, and the product yield is 90%. 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

[0019] Embodiment 2 Add 0.2mol (29.9g) methyltrichlorosilane in a 200ml four-necked flask equipped with agitator, thermometer, dropping funnel, reflux condenser and connected with a hydrogen chloride absorption device on the condenser, and then Add 0.64mol (60.48g) of monochloropropanol dropwise under the condition of cooling in a water bath, and control the temperature at a rate of addition not to exceed 40°C. g melamine, after stirring evenly, a small amount of low boiling point matter and excessive monochloropropanol (recycling) are removed by distillation under reduced pressure, cooling and filtering to obtain colorless liquid tris (monochloropropyl) methyl silicate, the product obtains The rate is 95%. 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

[0020] Example 3 In a 200ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel, a reflux condenser and a hydrogen chloride absorbing device at the mouth of the condenser, add 0.2mol (29.9g) of methyltrichlorosilane, and then Add 0.68mol (64.26g) of monochloropropanol dropwise under the condition of cooling in a water bath, and control the temperature at a rate of addition not to exceed 40°C. g melamine, after stirring evenly, a small amount of low boiling point matter and excessive monochloropropanol (recycling) are removed by distillation under reduced pressure, cooling and filtering to obtain colorless liquid tris (monochloropropyl) methyl silicate, the product obtains The rate is 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 tri(chloroproply) methyl silicate compound, which is a silicon-halogen combined flame-retarding plasticizer, and a preparation method thereof. The structure of the compound is represented by a formula below: CH3Si(OC3H6Cl). The preparation method comprises: dripping chloropropanol in a certain molar amount into methyl trichlorosilane with stirring; reacting for a certain time period at a certain temperature; and when chlorine hydride is completely released and the reaction is accomplished, obtaining tri(chloroproply) methyl silicate by purification. The flame-retarding and plasticizing performance of the tri(chloroproply) methyl silicate is high, the production process is simple, equipment investment is small, cost is low, and industrial production can be realized easily.

Description

technical field [0001] The invention relates to a tris(monochloropropyl) methyl silicate compound and a preparation method thereof. Tris(monochloropropyl)methylsilicate is a silicon-chlorine double-element synergistic flame-retardant plasticizer, which is suitable for flame-retardant plasticizing additives of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin, etc. Background technique [0002] With the rapid development and large-scale application of synthetic polymer materials, the amount of plasticizer is very large. Due to the flammability 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 synthesis of flame retardant plasticizers; from the application, it is found t...

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 王彦林王玉霞王乐然
Owner ENOVE PRECISION PLASTICS CATHETER
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