Preparation method of flame retardant bis[tri(chloroethoxy)silyloxy]ethane

A technology of chloroethoxy and silyloxy, which is applied in the direction of silicon organic compounds, can solve problems such as fire, threats to people's life and property safety, and achieve low production costs, overcoming volatile reactions, and good plasticity

Active Publication Date: 2016-06-29
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The advancement of science and technology has promoted the rapid development of polymer synthetic materials. The current consumption of organic polymer synthetic materials has become one of the important indicators to measure whether a country or region is developed; however, most polymer materials are flammable and often cause Fire poses a serious threat to people's life and property safety, thus promoting the development of flame retardant materials and flame retardant technology

Method used

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  • Preparation method of flame retardant bis[tri(chloroethoxy)silyloxy]ethane
  • Preparation method of flame retardant bis[tri(chloroethoxy)silyloxy]ethane
  • Preparation method of flame retardant bis[tri(chloroethoxy)silyloxy]ethane

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 a drying tube on the condenser, replace the air in the bottle with nitrogen, add 60ml of dichloroethane and 17g (11.47ml, 0.1mol) silicon tetrachloride, under stirring, cool with a cold water bath, reduce the temperature of the reaction system to below 20°C, add 8.051g (6.71ml, 0.1mol) chloroethanol dropwise, and control the reaction during the dropwise addition The temperature is not higher than 30°C. After the drop, the temperature is raised to 35°C, and the temperature is kept for 1 hour; after the HCl gas is released, 3.1g (2.78ml, 0.05mol) of ethylene glycol is dropped into the four-necked flask, and the drop rate is Control the reaction temperature not higher than 45°C, raise the temperature to 50°C after dripping, and react for 8 hours; after the HCl gas is released, cool the system down to below 40°C, add 16.50g (13.74ml, 0.205mol) of chloroetha...

Embodiment 2

[0030]Example 2 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the upper mouth of the condenser, replace the air in the bottle with nitrogen, add 60ml of dioxane and 17g (11.47ml, 0.1mol) silicon tetrachloride, under stirring, cool with a cold water bath, reduce the temperature of the reaction system to below 20°C, add 8.051g (6.71ml, 0.1mol) chloroethanol dropwise, and control the reaction during the dropwise addition The temperature is not higher than 30°C. After dropping, raise the temperature to 35°C and keep it warm for 1 hour; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask to Acceleration controls the reaction temperature not to be higher than 45°C. After the drop is completed, the temperature is raised to 65°C and reacted for 5 hours; after the HCl gas is released, the temperature of the system is lowered to below 40°C, and 16.905g (14...

Embodiment 3

[0031] Embodiment 3 In the 250ml four-necked flask that stirrer, thermometer and high-efficiency reflux condenser are equipped with, and drying tube is housed on the condenser upper mouth, replace the air in the bottle with nitrogen, add 60ml acetonitrile and 17g (11.47ml , 0.1mol) silicon tetrachloride, under stirring, cool with a cold water bath to reduce the temperature of the reaction system to below 20°C, add 8.051g (6.71ml, 0.1mol) chloroethanol dropwise, and control the reaction temperature during the dropwise addition. At 30°C, after dropping, raise the temperature to 35°C, and keep it warm for 1 hour; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask, and control the reaction with the dropping rate The temperature is not higher than 45°C. After the dripping, the temperature is raised to 60°C, and the reaction is 6h; after the HCl gas is released, the temperature of the system is lowered to below 40°C, and 17.71g (1...

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Abstract

The invention relates to a method for preparing a flame retardant bis[tri(chloroethoxy)silicon-acyloxy]ethane. The structure of the compound is represented by a formula shown in a drawing. The preparation method comprises the steps of reacting silicon tetrachloride with chloroethanol of a mole which is equal to that of silicon tetrachloride in an organic solvent at the temperature below 20 DEG C, then, dropwise adding glycol of a mole which is 0.5 times that of silicon tetrachloride, heating to the temperature of 50-70 DEG C after completing dripping, and reacting for 5-8 hours; then, dropwise adding chloroethanol of a mole which is 2-3 times that of silicon tetrachloride, and carrying out heat-preservation reaction for 6-9 hours at the temperature of 60-75 DEG C; adding an acid binding agent, and carrying out heat preservation for 1 hour while stirring; purifying, thereby obtaining the flame retardant bis[tri(chloroethoxy)silicon-acyloxy]ethane. The compound disclosed by the invention has high flame retarding efficacy due to the synergism of silicon and chlorine and is suitable for serving as a flame retardant for materials, such as polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like, and the preparation method is simple and is low in cost, so that the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a method for preparing a flame retardant bis[tri(chloroethoxy)silyloxy]ethane. 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] The advancement of science and technology has promoted the rapid development of polymer synthetic materials. The current consumption of organic polymer synthetic materials has become one of the important indicators to measure whether a country or region is developed; however, most polymer materials are flammable and often cause Fire poses a serious threat to people's life and property safety, thus promoting the development of flame retardant materials and flame retardant technology. With the continuous enhancement of people's awareness of environmental protection, more stringent requirements have been put forward for halogenated flame retardants in recent years, that is, they...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/04C08K5/5415C08L27/06
Inventor 王彦林董信
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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