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Flame retardant ethylenedioxyethylene disilicate chloropropyl compound and preparation method thereof

A flame retardant and compound technology, applied in the field of flame retardant bis[trisilyloxy]ethane compound and its preparation, can solve the problems that the by-product silicon tetrachloride cannot be processed, comprehensive utilization restricts the development of photovoltaic industry, etc. , achieve good application and development prospects, overcome the effect of volatile reaction and 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

[0004] The shortage of energy has promoted the development of the photovoltaic industry. At the same time, the polysilicon industry produces a large amount of by-product silicon tetrachloride that cannot be processed. Therefore, the comprehensive utilization of silicon tetrachloride has become a bottleneck restricting the development of my country's photovoltaic industry.

Method used

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  • Flame retardant ethylenedioxyethylene disilicate chloropropyl compound and preparation method thereof
  • Flame retardant ethylenedioxyethylene disilicate chloropropyl compound and preparation method thereof
  • Flame retardant ethylenedioxyethylene disilicate chloropropyl compound and preparation method thereof

Examples

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Embodiment 1

[0032]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 11.6g (13.98ml, 0.2mol) of propylene oxide was added dropwise under the liquid surface , the dropwise addition process controls the reaction temperature not to be higher than 25°C. After the drop is completed, the temperature is raised to 40°C, and the heat preservation reaction is carried out for 1h; Diol was dropped into the four-necked flask, and the reaction temperature was controlled by the dropping rate not to be higher than 50°C. After the drop, the temperature was raised to 65°C, and the reaction was carried out for 7 hours; af...

Embodiment 2

[0033] 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 Alkanes and 17g (11.47ml, 0.1mol) silicon tetrachloride, under stirring, cool with ice-water bath, make reaction system temperature drop to 0 ℃, add dropwise 11.6g (13.98ml, 0.2mol) propylene oxide , the dropwise addition process controls the reaction temperature not to be higher than 25°C. After the drop is completed, the temperature is raised to 40°C, and the heat preservation reaction is carried out for 1h; Diol was dropped into the four-necked flask, and the reaction temperature was controlled by the dropping rate not to be higher than 50°C. After the drop, the temperature was raised to 60°C and reacted for 8 hours; after the HCl gas was released, the system was cooled to below 30°C, and the R...

Embodiment 3

[0034] 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 Diphenyl ether and 17g (11.47ml, 0.1mol) of silicon tetrachloride were cooled with an ice-water bath under stirring, so that the temperature of the reaction system was lowered to 0°C, and 11.6g (13.98ml, 0.2mol) of tetrachloride was added dropwise under the liquid surface. Oxygen propylene, the dropwise addition process controls the reaction temperature not to be higher than 25°C. After the drop is completed, the temperature is raised to 40°C, and the temperature is kept for 1 hour; then the upper port of the reflux condenser is replaced with a drying tube, and 3.1g (2.78ml, 0.05mol ) Ethylene glycol is dropped into the four-necked flask, and the reaction temperature is controlled by the dropping rate not to be highe...

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Abstract

The invention relates to a flame retardant ethylenedioxy dual-silicate propyl chloride 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 propylene epoxide into an organic solution of the silicon tetrachloride at a temperature being below 0 DEG C and reacting for 1 hour at 40 DEG C, wherein the molar mass of the propylene epoxide is 2 times that of the silicon tetrachloride; dropwise adding ethylene glycol and reacting for 6-9 hours at 55-75 DEG C, wherein the molar mass of the ethylene glycol is 0.5 time that of the silicon tetrachloride; cooling to the temperature being below 30 DEG C, dropwise adding the propylene epoxide and reacting for 4-7 hours at 60-80 DEG C, wherein the molar mass of the propylene epoxide is 1-1.5 times that of the silicon tetrachloride; performing purification treatment to obtain the flame retardant ethylenedioxy dual-silicate propyl chloride. The compound disclosed by the invention has high synergistic flame retardant performance of 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 chloropropyl ester compound and a preparation method thereof, in particular to a flame retardant bis[tri(chloropropoxy)silyloxy]ethane compound and its preparation method. The preparation method is that the compound, silicon and chlorine, has high synergistic flame retardant performance, and is suitable for use as a flame retardant for materials such as polyvinyl chloride, polyurethane, epoxy resin, and unsaturated resin. Background technique [0002] With the successive promulgation of increasingly stringent flame retardant legislation, fire safety standards and industry directives around the world, the demand for flame retardant polymer materials is getting higher and higher, and the global market demand for flame retardants has shown a rapid growth trend in the past two decades. , especially the more urgent demand for new, efficient and environmentally friendly flame retarda...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/04C08L27/06C08K5/5415
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
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