Tribromophenoxybromopropyl dimethylsilicate compound and preparation method thereof

Abstract

The invention relates to a tribromophenoxy bromopropyl dimethyl silicate compound and a preparation method thereof, in particular to bis(2,4,6-tribromophenoxy bromopropyl) dimethyl silicate compound and Its preparation method, the structure of the compound is shown in the following formula: in the formula, when m=1, n=0, and when n=1, m=0. The preparation method is: in a reactor equipped with a stirrer, a thermometer and a condenser tube, replace the air in the reactor with nitrogen, dissolve 2,4,6-tribromophenyl glycidyl ether in an organic solvent, Add 0.5 times mole of dimethyldibromosilane dropwise, react at 30°C-60°C for 5-11 hours after the drop, and obtain dimethylsilicate bis(2,4,6-tribromophenoxy bromopropyl) ester. The flame retardant of the present invention has high flame retardant efficiency and good compatibility with materials, is suitable for use as a flame retardant for polyvinyl chloride, polyester, epoxy resin, unsaturated resin, etc., and has simple production process, low cost and easy realization Industrial production.

Description

technical field

[0001] The invention relates to a silicon and bromine dual element synergistic flame retardant dimethyl silicate tribromophenoxybromopropyl ester compound and a preparation method thereof, in particular to bis(2,4,6-tribromodimethylsilicate) A phenoxybromopropyl) ester compound and a preparation method thereof, the compound is suitable for use as a flame retardant for polyvinyl chloride, polyester, epoxy resin, unsaturated resin and the like. Background technique

[0002] With the rapid development of science and technology in the world, the continuous improvement of people's living standards and the enhancement of safety and fire prevention awareness, the flame retardant industry has developed rapidly. Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogens when burned, the use of halogenated flame retardants has been restricted to a certain extent. However, due to the excellent comprehensive cost ...

Examples

Embodiment 1

[0027] Example 1 In a 250ml four-necked flask equipped with a stirrer, a thermometer and a condenser tube, replace the air in the bottle with nitrogen, and add 38.75g (0.1mol) of 2,4,6-tribromophenylepoxypropyl Ether and 100ml of benzene, add 10.9g (0.05mol) dimethyldibromosilane dropwise, and control the reaction temperature not higher than 30°C at the rate of addition, after the drop is completed, raise the temperature to 30°C, keep the temperature for 11 hours, and distill off the solvent under reduced pressure and a small amount of low boiling point substances to obtain bis(2,4,6-tribromophenoxybromopropyl) dimethyl silicate, the yield: 94.8%.

Embodiment 2

[0028] Example 2 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a condenser tube, replace the air in the bottle with nitrogen, and add 38.75g (0.1mol) of 2,4,6-tribromophenylepoxypropyl Ether and 130ml xylene, add 10.9g (0.05mol) dimethyldibromosilane dropwise, and control the reaction temperature not higher than 30°C with the rate of addition. Solvent and a small amount of low-boiling point substances, to obtain bis(2,4,6-tribromophenoxybromopropyl) dimethyl silicate, the yield: 98.3%.

Embodiment 3

[0029] Example 3 In a 250ml four-necked flask equipped with a stirrer, a thermometer and a condenser, replace the air in the bottle with nitrogen, and add 38.75g (0.1mol) of 2,4,6-tribromophenylepoxypropyl Ether and 120ml xylene, add 10.9g (0.05mol) dimethyldibromosilane dropwise, and control the reaction temperature not higher than 30°C with the rate of addition. Solvent and a small amount of low-boiling point substances, to obtain bis(2,4,6-tribromophenoxybromopropyl) dimethyl silicate, yield: 97.5%.

technical field

[0001] The invention relates to a silicon and bromine dual element synergistic flame retardant dimethyl silicate tribromophenoxybromopropyl ester compound and a preparation method thereof, in particular to bis(2,4,6-tribromodimethylsilicate) A phenoxybromopropyl) ester compound and a preparation method thereof, the compound is suitable for use as a flame retardant for polyvinyl chloride, polyester, epoxy resin, unsaturated resin and the like. Background technique

[0002] With the rapid development of science and technology in the world, the continuous improvement of people's living standards and the enhancement of safety and fire prevention awareness, the flame retardant industry has developed rapidly. Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogens when burned, the use of halogenated flame retardants has been restricted to a certain extent. However, due to the excellent comprehensive cost ...

Examples

Embodiment 1

[0027] Example 1 In a 250ml four-necked flask equipped with a stirrer, a thermometer and a condenser tube, replace the air in the bottle with nitrogen, and add 38.75g (0.1mol) of 2,4,6-tribromophenylepoxypropyl Ether and 100ml of benzene, add 10.9g (0.05mol) dimethyldibromosilane dropwise, and control the reaction temperature not higher than 30°C at the rate of addition, after the drop is completed, raise the temperature to 30°C, keep the temperature for 11 hours, and distill off the solvent under reduced pressure and a small amount of low boiling point substances to obtain bis(2,4,6-tribromophenoxybromopropyl) dimethyl silicate, the yield: 94.8%.

Embodiment 2

[0028] Example 2 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a condenser tube, replace the air in the bottle with nitrogen, and add 38.75g (0.1mol) of 2,4,6-tribromophenylepoxypropyl Ether and 130ml xylene, add 10.9g (0.05mol) dimethyldibromosilane dropwise, and control the reaction temperature not higher than 30°C with the rate of addition. Solvent and a small amount of low-boiling point substances, to obtain bis(2,4,6-tribromophenoxybromopropyl) dimethyl silicate, the yield: 98.3%.

Embodiment 3

[0029] Example 3 In a 250ml four-necked flask equipped with a stirrer, a thermometer and a condenser, replace the air in the bottle with nitrogen, and add 38.75g (0.1mol) of 2,4,6-tribromophenylepoxypropyl Ether and 120ml xylene, add 10.9g (0.05mol) dimethyldibromosilane dropwise, and control the reaction temperature not higher than 30°C with the rate of addition. Solvent and a small amount of low-boiling point substances, to obtain bis(2,4,6-tribromophenoxybromopropyl) dimethyl silicate, yield: 97.5%.

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