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Halogenated organic silicate ester flame-retardant plasticizer compound and preparation method thereof

A technology of flame retardant plasticizer and silicate, which is applied in the field of methyl silicate triester compound and its preparation, can solve the problems of high price and limitation of organosilicon products, and achieve high dual-element synergistic flame retardant efficiency, The effect of low cost and simple preparation method

Active Publication Date: 2013-02-27
ENOVE PRECISION PLASTICS CATHETER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, silicone products are expensive and restricted

Method used

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  • Halogenated organic silicate ester flame-retardant plasticizer compound and preparation method thereof
  • Halogenated organic silicate ester flame-retardant plasticizer compound and preparation method thereof
  • Halogenated organic silicate ester flame-retardant plasticizer compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and an extremely flexible and expandable soft seal at the top of the condenser, add 0.2mol (29.9g) of methyltrichlorosilane , Replace the air in the reaction system with nitrogen, and then pass 0.6mol (26.4g) of ethylene oxide under the liquid surface under the condition of cooling in an ice-water bath, and control the temperature at the rate of introduction to not exceed 70°C. Reaction 8h. After the reaction was finished, a small amount of low-boiling matter was distilled off under reduced pressure to obtain tris(2-chloroethyl) methyl silicate as a colorless liquid with a yield of 94%. 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 Add 0.2 mol (29.9 g) of methyltrichlorosilane to a 100 ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser, and an extremely flexible and expandable soft seal at the top of the condenser , replace the air in the reaction system with nitrogen, and then pass 0.65mol (28.6g) of ethylene oxide under the liquid surface under the condition of cooling in an ice-water bath, and control the temperature at a speed of not exceeding 60°C. After passing through, 60°C Reaction 6h. After the reaction, excess oxirane was distilled off under normal pressure (absorbed by water to produce ethylene glycol), and a small amount of low-boilers were distilled off under reduced pressure to obtain a colorless liquid tris(2-chloroethyl)methylsilicate , The product yield is 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.

Embodiment 3

[0019] Example 3 Add 0.2 mol (29.9 g) of methyltrichlorosilane to a 100 ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser tube and an extremely flexible and expandable soft seal at the top of the condenser tube , replace the air in the reaction system with nitrogen, and then pass 0.70mol (30.8g) of ethylene oxide under the liquid surface under the condition of cooling in an ice-water bath, and control the temperature at a speed of not exceeding 50°C, and 50°C after passing through Reaction 3h. After the reaction, excess oxirane was distilled off under normal pressure (absorbed by water to produce ethylene glycol), and a small amount of low-boilers were distilled off under reduced pressure to obtain a colorless liquid tris(2-chloroethyl)methylsilicate , The product yield is 98%. 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 halogenated organic silicate ester flame-retardant plasticizer, namely 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: introducing undersurface epoxy ethane with a certain molar ratio into methyl trichlorosilane under the cooling condition; reacting at the constant temperature for a certain period of time after the introduction; and removing excessive epoxy ethane and a small quantity of low-boiling-point substances by distilling to obtain colorless liquid methyl silicate tri(2-chloroethyl) ester. The methyl silicate tri(2-chloroethyl) ester 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 halogenated organosilicate flame retardant plasticizer compound and a preparation method thereof. Specifically relates to a methyl silicate tris (2-chloroethyl) ester compound and a preparation method thereof. Tris(2-chloroethyl)methylsilicate is a silicon-halogen-containing 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 wide application of polymer materials, because of its flammability, it often causes fires and poses a serious threat to people's lives and property, thus promoting the research of flame retardant technology and the rapid development of flame retardant plasticizer industry. Flame retardant plasticizer is a plastic processing aid with flame retardant function and plasticizing effect. It can overcome the problem of making polymer materials more f...

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 王彦林王玉霞杨海
Owner ENOVE PRECISION PLASTICS CATHETER
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