Flame retardant Cyke dichloropropyl trisilicate compound and preparation method thereof

A flame retardant and dichloropropoxy technology, which is applied in the field of flame retardant Seike dichloropropyl trisilicate compound and its preparation, can solve the problem that the non-halogenation process will not be too fast, and improve the difficulty of dispersion. Low activity, good application and development prospects, good compatibility

Active Publication Date: 2015-12-09
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 the research and development of high-efficiency halogenated flame retardants to reduce the amount of flame retardants added to reduce the toxicity during combustion has become an important research direction for flame retardants

Method used

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  • Flame retardant Cyke dichloropropyl trisilicate compound and preparation method thereof
  • Flame retardant Cyke dichloropropyl trisilicate compound and preparation method thereof
  • Flame retardant Cyke dichloropropyl trisilicate compound and preparation method thereof

Examples

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Effect test

Embodiment 1

[0030] 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 20ml of dioxane ring and 8.5g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, the temperature of the reaction system was reduced to below 30°C, and 9.25g (7.80ml, 0.1mol) of epichlorohydrin was added dropwise , the dropwise addition process controls the reaction temperature not to be higher than 40°C. After the drop, raise the temperature to 50°C and keep it warm for 2 hours; 50ml of dioxane solution was dropped into a four-necked flask, and the reaction temperature was controlled by the dropping rate to not be higher than 65°C. After the drop was completed, the temperature was raised to 95°C, and the reaction was carried out for 9 hours. After the HCl gas was released, t...

Embodiment 2

[0031] Example 2 In a 250ml four-necked flask equipped with an agitator, a thermometer and a high-efficiency reflux condenser, and an extremely expandable sealing sleeve on the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 20ml of dichloroethylene Alkane and 8.5g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, the temperature of the reaction system was reduced to below 30°C, and 9.25g (7.80ml, 0.1mol) of epichlorohydrin was added dropwise , the dropwise addition process controls the reaction temperature not to be higher than 40°C. After the drop, raise the temperature to 50°C and keep it warm for 2 hours; 50ml of dichloroethane solution was dropped into a four-necked flask, and the reaction temperature was controlled by the dropping rate not higher than 65°C. After dropping, the temperature was raised to 80°C and reacted for 13 hours. After the HCl gas was released, the system was cooled down to Be...

Embodiment 3

[0032] Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and an extremely expandable sealing sleeve on the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 20ml of diethylene glycol Alcohol dimethyl ether and 8.5g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, so that the temperature of the reaction system was reduced to below 30 ° C, and 9.25g (7.80ml, 0.1mol) of ring Oxychloropropane, the dropwise addition process controls the reaction temperature not to be higher than 40°C. After the drop is completed, the temperature is raised to 50°C, and the heat preservation reaction is carried out for 2 hours; Drop the solution dissolved in 50ml of diethylene glycol dimethyl ether into a four-necked flask, control the reaction temperature not higher than 65°C with the dropping speed, raise the temperature to 90°C after the drop, react for 10h, a...

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Abstract

The invention relates to a flame retardant tris(hydroxyethyl) isocyanurate trisilicate dichlorohydrin compound and a preparation method thereof. The compound has a structure shown in the specification, wherein m is an integer from 0 to 3. The preparation method comprises the following steps: dropwise adding epoxy chloropropane into an organic solution of silicon tetrachloride at a temperature being below 30 DEG C and reacting for 2 hours at 50 DEG C, wherein the molar mass of the epoxy chloropropane is 2 times that of the silicon tetrachloride; dropwise adding an organic solution of tris(hydroxyethyl) isocyanurate and reacting for 9-13 hours at 80-95 DEG C, wherein the molar mass of the organic solution of the tris(hydroxyethyl) isocyanurate is 1 / 3 that of the silicon tetrachloride; dropwise adding the epoxy chloropropane and reacting for 4-7 hours at 70-90 DEG C, wherein the molar mass of the epoxy chloropropane is 1-1.5 times that of the silicon tetrachloride; performing purification treatment to obtain the tris(hydroxyethyl) isocyanurate trisilicate dichlorohydrin. The flame retardant contains three flame retardant elements including silicon, nitrogen and chlorine, is suitable to be used as flame retardants of the materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin, is high in synergistic flame retardant performance, simple in preparation process and low in cost, and can be easily put into industrial production.

Description

technical field [0001] The present invention relates to a kind of flame retardant Sike dichloropropyl trisilicate compound and its preparation method, in particular to a kind of flame retardant tris[2-tris(dichloropropoxy)silyloxyethyl]iso The invention relates to a cyanurate compound and a preparation method thereof. The three elements of the compound silicon, nitrogen and chlorine have high synergistic flame retardant performance, and are suitable for use 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 be...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07F7/04C08K5/5455C08L27/06
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