Flame retardant ethylenedioxyethylene disilicate chloroethyl ester compound and preparation method thereof

A flame retardant and compound technology, which is applied in the field of flame retardant bis[trisilyloxy]ethane compound and its preparation, can solve problems such as fire, threats to people's life and property safety, etc., and achieves low equipment investment and good application and development prospects, overcoming the volatile effect of the reaction

Active Publication Date: 2015-12-02
山东产研中科高端化工产业技术研究院有限公司
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Due to the rapid development of science and technology, the consumption of organic polymer synthetic materials has become an important indicator to measure the degree of development of a country or region, but most polymer materials are flammable and often cause fires, causing serious damage to people's lives and property. Serious threat, thus promoting the development of flame retardant materials and flame retardant technology

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Flame retardant ethylenedioxyethylene disilicate chloroethyl ester compound and preparation method thereof
  • Flame retardant ethylenedioxyethylene disilicate chloroethyl ester compound and preparation method thereof
  • Flame retardant ethylenedioxyethylene disilicate chloroethyl ester compound and preparation method thereof

Examples

Experimental program
Comparison scheme
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 an ice-water bath, the temperature of the reaction system was reduced to 0°C, and 8.8g (10.10ml, 0.2mol) of ethylene oxide was introduced under the liquid surface Alkanes, feed the process to control the reaction temperature not higher than 15°C. After the addition, raise the temperature to 25°C, and keep the temperature for 1h; Ethylene glycol was dropped into the four-necked flask, and the reaction temperature was controlled by the dropping rate to not be higher than 35°C. After the drop, the temperature was raised to 55°C, and the reaction was carried out for 5 hours; after the HCl gas was released, the temperat...

Embodiment 2

[0030]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 60ml of dichloroethylene Alkane and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with an ice-water bath, the temperature of the reaction system was reduced to 0°C, and 8.8g (10.10ml, 0.2mol) of ethylene oxide was introduced under the liquid surface Alkanes, feed the process to control the reaction temperature not higher than 15°C. After the addition, raise the temperature to 25°C, and keep the temperature for 1h; Ethylene glycol was dropped into the four-necked flask, and the reaction temperature was controlled by the dropping speed to not be higher than 35°C. After the drop, the temperature was raised to 50°C, and the reaction was carried out for 7 hours; after the HCl gas was released, the temper...

Embodiment 3

[0031] Example 3 In a 250ml four-neck 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 acetonitrile and 17g (11.47ml, 0.1mol) silicon tetrachloride, under stirring, cool with ice-water bath, make reaction system temperature drop to 0 ℃, pass into 8.8g (10.10ml, 0.2mol) ethylene oxide under the liquid level, pass During the feeding process, the reaction temperature is controlled to be no higher than 15°C. After the addition, the temperature is raised to 25°C, and the heat preservation reaction is carried out for 1 hour; then the upper port of the reflux condenser tube is replaced with a drying tube, and 3.1g (2.78ml, 0.05mol) of ethylene glycol Drop it into a four-necked flask, and control the reaction temperature at a rate not higher than 35°C. After the drop, raise the temperature to 60°C, and react for 5 hours; after ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
flash pointaaaaaaaaaa
densityaaaaaaaaaa
refractive indexaaaaaaaaaa
Login to View More

Abstract

The invention relates to a flame retardant ethylenedioxy dual-silicate ethyl chloride compound and a preparation method thereof. The compound has the structure shown as the formula specified in the specification. The preparation method comprises the following steps: introducing ethylene oxide into an organic solution of the silicon tetrachloride at a temperature being below 0 DEG C and reacting for 1 hour at 25 DEG C, wherein the molar mass of the ethylene oxide is 2 times that of the silicon tetrachloride; dropwise adding an organic solution of ethylene glycol and reacting for 4-7 hours at 50-65 DEG C, wherein the molar mass of the organic solution of the ethylene glycol is 0.5 time that of the silicon tetrachloride; cooling to the temperature being below 20 DEG C, introducing the ethylene oxide, and reacting for 3-6 hours at 35-50 DEG C, wherein the molar mass of the ethylene oxide is 1-1.5 times that of the silicon tetrachloride; and performing purification to obtain the flame retardant ethylenedioxy dual-silicate ethyl chloride. The compound disclosed by the invention has high synergistic flame retardant performance of the double elements of silicon and chloride, is suitable to be used as flame retardants of the materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin, is simple in preparation process and low in cost, and can be put into industrial production easily.

Description

technical field [0001] The invention relates to a flame retardant ethylenedioxyethylene disilicate chloroethyl ester compound and a preparation method thereof, in particular to a flame retardant bis[tri(chloroethoxy)silyloxy]ethane compound and its preparation method. The preparation method, the compound can be used as a flame retardant for materials such as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin. Background technique [0002] Due to the rapid development of science and technology, the consumption of organic polymer synthetic materials has become an important indicator to measure the degree of development of a country or region, but most polymer materials are flammable and often cause fires, causing serious damage to people's lives and property. Therefore, it promotes the development of flame retardant materials and flame retardant technology. With the continuous enhancement of people's awareness of environmental protection, more stringent r...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & AuthorityPatents(China)
IPC IPC(8): C07F7/04C08K5/5415C08L27/06C08L67/06C08L75/04C08L63/00
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