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Fire retardant silicic acid di(tribromophenyl)dichloroethyl ester compound and its preparation method

A technology of tribromophenyl and dichloroethyl ester, which is applied in the direction of silicon organic compounds, can solve the problems that the process of non-halogenation will not be too fast, and the non-halogenation of flame retardants will take a long time, so as to achieve excellent cost performance and high flame retardant performance , to overcome the effect of low activity

Active Publication Date: 2015-07-08
张家港市乐余科创园投资发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the general development trend is that although the call for non-halogenation is high, the process of non-halogenation will not be too fast, that is, the non-halogenation of flame retardants will be a relatively long process

Method used

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  • Fire retardant silicic acid di(tribromophenyl)dichloroethyl ester compound and its preparation method
  • Fire retardant silicic acid di(tribromophenyl)dichloroethyl ester compound and its preparation method
  • Fire retardant silicic acid di(tribromophenyl)dichloroethyl ester compound and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 In a 150ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel and a reflux condenser and an extremely stretchable and expandable soft seal at the top of the condenser, replace the air in the bottle with nitrogen Finally, add 70ml of dioxane and 8.50g (0.05mol) of silicon tetrachloride, start stirring, and under cooling in an ice-water bath, 2.20g (0.05mol) of ethylene oxide is introduced under the liquid surface, controlled by the rate of introduction. The temperature is below 20°C. After passing through, refit the hydrogen chloride absorption device at the top of the condenser, add 33.08g (0.1mol) of tribromophenol, raise the temperature to 80°C, and keep it warm for 4 hours. After the hydrogen chloride is released, cool down to 30°C Next, restore the soft sealing sleeve device at the upper port of the condenser tube, and then inject 4.41g (0.1mol) of ethylene oxide under the liquid surface, and control the temperature at the rate of int...

Embodiment 2

[0030]Example 2 In a 150ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel and a reflux condenser and an extremely stretchable and expandable soft seal at the top of the condenser, replace the air in the bottle with nitrogen Finally, add 70ml of toluene and 8.50g (0.05mol) of silicon tetrachloride, start stirring, under the cooling of ice-water bath, feed 2.20g (0.05mol) of ethylene oxide under the liquid surface, and control the temperature at 20 Below ℃, after passing through, refit the hydrogen chloride absorption device at the upper port of the condenser, add 33.08g (0.1mol) tribromophenol, raise the temperature to 85 ℃, keep the temperature for 3.5h, after the hydrogen chloride is released, cool down to below 30 ℃, Restore the soft sealing sleeve device at the upper opening of the condenser tube, and then inject 3.08g (0.07mol) of ethylene oxide under the liquid surface, and control the temperature at the rate of introduction to not exceed 35°C. ...

Embodiment 3

[0031] Example 3 In a 150ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a reflux condenser and an extremely stretchable and expandable soft seal at the top of the condenser, replace the air in the bottle with nitrogen Finally, add 70ml of carbon tetrachloride and 8.50g (0.05mol) of silicon tetrachloride, start stirring, and under cooling in an ice-water bath, feed 2.20g (0.05mol) of ethylene oxide under the liquid surface to control the feed rate. The temperature is below 20°C. After passing through, refit the hydrogen chloride absorption device at the upper port of the condenser, add 33.08g (0.1mol) tribromophenol, raise the temperature to 65°C, and keep the temperature for 6 hours. After the hydrogen chloride is released, cool down to 30°C Next, restore the soft sealing sleeve device at the upper port of the condenser tube, and then inject 2.20g (0.05mol) of ethylene oxide under the liquid surface, and control the temperature at the rate of...

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Abstract

The invention relates to a fire retardant silicic acid di(tribromophenyl)dichloroethyl ester compound and its preparation method. The structure of the compound is as shown in the specification. The preparation method comprises the following steps: controlling the temperature to below 20 DEG C, letting equimolar oxirane be blown below the liquid level of a silicon tetrachloride organic solution, adding tribromophenol which accounts for two times larger than equimolar oxirane, keeping the temperature at 65-90 DEG C and reacting for 3-6h, letting a certain mol ration of oxirane be blown below the liquid level, keeping the temperature at 40-60 DEG C and reacting for 2-4h, and carrying out underpressure distillation to remove a solvent so as to obtain a product silicic acid di(tribromophenyl)dichloroethyl ester. The silicic acid di(tribromophenyl)dichloroethyl ester provided by the invention is an excellent flame retardation plasticizer, has charcoal-forming and antidrip effects, has good compatibility with a high-molecular material, and can be used as a fire retardant of materials such as polyvinyl chloride, nonsaturated polyester, polyurethane and epoxy resin, etc. Raw materials of the fire retardant provided by the invention are cheap and easily available. Production costs are low. Equipment investment is little. The production technology is simple. The preparation method is easy for large-scale production.

Description

technical field [0001] The invention relates to a flame retardant bis(tribromophenyl) dichloroethyl silicate compound and a preparation method thereof. The compound can be used as a flame retardant for materials such as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin. Fuel. Background technique [0002] With the increasingly stringent flame retardant legislation, the successive introduction of industry directives and the enhancement of environmental protection awareness, the global consumption of flame retardants is growing rapidly, especially the more urgent demand for new, efficient and environmentally friendly flame retardants. [0003] At present, halogen-based flame retardants are the most widely used organic flame retardants with the highest comprehensive cost performance, but generally halogen-containing flame retardant materials will release a large amount of harmful gases such as smoke and dioxin when a fire occurs, especially the European Un...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/06C08K5/5415C08L27/06C08L67/06C08L75/04C08L63/00
Inventor 王彦林孟凡一
Owner 张家港市乐余科创园投资发展有限公司
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