Flame retardant ethylenedioxyethylene disilicate dichloropropyl ester compound and preparation method thereof

A flame retardant and dichloropropoxy technology, applied in the field of flame retardant bis[trisilyloxy]ethane compound and its preparation, can solve the problem that the non-halogenation process will not be too fast, and can overcome the reaction Volatile, good compatibility, high synergistic flame retardant effect

Active Publication Date: 2016-04-27
山东产研中科高端化工产业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced harmful substances when they burned, the use of halogenated flame retardants has been restricted. However, due to the excellent overall cost performance of halogenated flame retardants, it is still difficult to find ideal alternatives. Therefore, the non-halogenation process will not be too fast, but research and development of high-efficiency halogenated flame retardants to reduce the amount of flame retardants added, thereby reducing the toxicity during combustion, has become an important research direction for flame retardants

Method used

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  • Flame retardant ethylenedioxyethylene disilicate dichloropropyl ester compound and preparation method thereof
  • Flame retardant ethylenedioxyethylene disilicate dichloropropyl ester compound and preparation method thereof
  • Flame retardant ethylenedioxyethylene disilicate dichloropropyl ester compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and an extremely expandable sealing sleeve is installed on the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 60ml of dioxane ring and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, the temperature of the reaction system was reduced to below 30°C, and 18.504g (15.68ml, 0.2mol) of epichlorohydrin was added dropwise, During the dropwise addition process, the reaction temperature should not be higher than 40°C. After the dropwise addition, the temperature was raised to 50°C, and the temperature was kept for 2 hours; then, the upper port of the reflux condenser tube was replaced with a drying tube, and 3.1g (2.78ml, 0.05mol) of ethylene di Drop the alcohol into the four-necked flask, control the reaction temperature not higher than 55°C with the dropping speed, raise the tempera...

Embodiment 2

[0030]Example 2 In a 250ml four-neck flask equipped with an agitator, a thermometer and a high-efficiency reflux condenser, and an extremely expandable sealing sleeve at the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 60ml tetrachloride Carbon and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, the temperature of the reaction system was reduced to below 30°C, and 18.504g (15.68ml, 0.2mol) of epichlorohydrin was added dropwise, During the dropwise addition process, the reaction temperature should not be higher than 40°C. After the dropwise addition, the temperature was raised to 50°C, and the temperature was kept for 2 hours; then, the upper port of the reflux condenser tube was replaced with a drying tube, and 3.1g (2.78ml, 0.05mol) of ethylene di Drop the alcohol into the four-necked flask, control the reaction temperature not higher than 55°C with the dropping speed, raise the temperature to...

Embodiment 3

[0031] Example 3 In a 250ml four-necked flask equipped with an agitator, a thermometer and a high-efficiency reflux condenser, and an extremely expandable seal at the top of the condenser, replace the air in the bottle with nitrogen, and add 60ml of ethylene glycol Dimethyl ether and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, the temperature of the reaction system was reduced to below 30°C, and 18.504g (15.68ml, 0.2mol) of epoxy chloride was added dropwise Propane, the dropwise addition process controls the reaction temperature not to be higher than 40°C. After the drop, the temperature is raised to 50°C, and the heat preservation reaction is carried out for 2 hours; then the upper port of the reflux condenser is replaced with a drying tube, and 3.1g (2.78ml, 0.05mol) Ethylene glycol was dropped into the four-necked flask, and the reaction temperature was controlled by the dropping speed to not be higher than 60°C. After the d...

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Abstract

The invention relates to a fire retardant ethylenedioxy bisilicate dichloropropyl compound and a preparation method thereof. A structure of the compound is represented by a formula as shown in the specification. The preparation method comprises the following steps of dropwise adding epoxy chloropropane which is 2 times of the mole of silicon tetrachloride in an organic solution of the silicon tetrachloride at a temperature below 30 DEG C, and reacting for 2 hours at 50 DEG C; dropwise adding ethanediol which is 0.5 time of the mole of the silicon tetrachloride, and then reacting for 7-10 hours at 65-80 DEG C; cooling to less than 50 DEG C, dropwise adding the epoxy chloropropane which is 1-1.5 times of the mole of the silicon tetrachloride, and reacting for 5-8 hours at 70-85 DEG C; and purifying to obtain the fire retardant ethylenedioxy bisilicate dichloropropyl compound. The compound provided by the invention comprises silicon and chlorine which are flame retardant elements and is high in flame retardant synergism; the compound can be used as a fire retardant of materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin; the preparation process is simple, low in cost and easy for industrial production.

Description

technical field [0001] The invention relates to a flame retardant ethylenedioxyethylene bisilicate dichloropropyl ester compound and a preparation method thereof, in particular to a flame retardant bis[tri(dichloropropoxy)silyloxy]ethane compound According to the preparation method thereof, the compound has high synergistic flame retardant effect of silicon and chlorine dual elements, and is suitable for being used as a flame retardant for materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin. Background technique [0002] Due to the rapid development of science, technology and economy, people's safety awareness has been continuously enhanced, which has promoted the rapid development of the flame retardant industry. Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced harmful substances when they burned, the use of halogenated flame retardants has been restricted. However, due to the excellent...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07F7/04C08K5/5415C08K13/02C08L27/06
Inventor王彦林董信
Owner山东产研中科高端化工产业技术研究院有限公司