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Flame retardant tri(dibromopropyl)tribromophenyl silicate esterification compound and preparation method thereof

A technology of dibromopropyl and tribromophenyl esters, which is applied in the direction of silicon organic compounds, can solve the problem that the by-product silicon tetrachloride cannot be processed, and achieve good application and development prospects, low production costs, and stable physical and chemical properties. Effect

Active Publication Date: 2013-10-09
张家港市乐余科创园投资发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, 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 technology restricting my country's photovoltaic industry.

Method used

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  • Flame retardant tri(dibromopropyl)tribromophenyl silicate esterification compound and preparation method thereof
  • Flame retardant tri(dibromopropyl)tribromophenyl silicate esterification compound and preparation method thereof
  • Flame retardant tri(dibromopropyl)tribromophenyl silicate esterification compound and preparation method thereof

Examples

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Effect test

Embodiment 1

[0031]Example 1 In the 500ml four-necked flask equipped with agitator, thermometer, dropping funnel and high-efficiency reflux condenser and a hydrogen chloride absorbing device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 100ml of dioxane and 16.99g (0.1mol) of silicon tetrachloride, under stirring, cool with an ice-water bath, reduce the temperature of the reaction system to 0°C, and drop 21.79g of silicon tetrachloride into the organic solution (0.1mol) 2,3-dibromo-1-propanol, the temperature of the dropwise addition process is controlled below 8°C, after the drop is completed, the temperature is raised to 35°C in 1h, and the heat preservation reaction is carried out for 1h. After the hydrogen chloride is released, add 33.08g ( 0.1mol) of tribromophenol, raised the temperature to 80°C, and kept the temperature for 2 hours. Acceleration control temperature does not exceed 50°C. After dripping, raise the...

Embodiment 2

[0032] Example 2 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and a hydrogen chloride absorbing device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 100ml of ethylene glycol dimethyl ether and 16.99g (0.1mol) of silicon tetrachloride, under stirring, cool with an ice-water bath, reduce the temperature of the reaction system to 0°C, and add dropwise to the organic solution of silicon tetrachloride 21.79g (0.1mol) 2,3-dibromo-1-propanol, the dropwise addition process controls the temperature below 8°C, after the drop is completed, the temperature is raised to 35°C for 1h, and the temperature is kept for 1h. After the hydrogen chloride is released, add 33.08 g (0.1mol) tribromophenol, heat up to 60°C, keep warm for 4 hours, after the hydrogen chloride is released, cool down to below 40°C, then add 43.58g (0.2mol) 2,3-dibromo-1-pro...

Embodiment 3

[0033] Example 3 In a 500ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and a hydrogen chloride absorbing device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 100ml acetonitrile and 16.99g (0.1mol) silicon tetrachloride, under stirring, cool with ice-water bath, make reaction system temperature drop to 0 ℃, dropwise add 21.79g (0.1mol) in the organic solution of silicon tetrachloride ) 2,3-dibromo-1-propanol, the dropwise addition process controls the temperature below 8°C, after the drop is completed, the temperature is raised to 35°C for 1h, and the temperature is kept for 1h, after the hydrogen chloride is released, add 33.08g (0.1mol) Tribromophenol, heat up to 70°C, keep warm for 3 hours, after the hydrogen chloride is released, cool down to below 40°C, then add 43.58g (0.2mol) 2,3-dibromo-1-propanol dropwise, and control the temperat...

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Abstract

The invention relates to a flame retardant tri(dibromopropyl)tribromophenyl silicate esterification compound and a preparation method thereof. The structure of the compound is shown in the specification, wherein R2=CH2Br if R1=H; and R2=H if R1=CH2Br. The preparation method comprises the following steps of: dropwise adding equimolar dibromopropyl alcohol into an organic solvent of silicon tetrachloride at a temperature below 8 DEG C, and reacting for 1 hour at 35 DEG C; adding equimolar tribromophenol, and reacting for 2-4 hours at 50-80 DEG C; dropwise adding dibromopropyl alcohol of twice molar weight, and reacting for 3-5 hours at 50-70 DEG C; and performing reduced-pressure distillation to remove the solvent to obtain the product tri(dibromopropyl)tribromophenyl silicate. The product is an excellent flame-retardant plasticizer with a charring anti-drop effect and can be used as a flame retardant for the materials such as polyvinyl chloride, unsaturated polyester, polyurethane, epoxy resin and the like; and moreover, the flame retardant has the advantages of cheap and easily-available raw materials, low production cost, low equipment investment and simple production technology, and is easy to produce in a large scale.

Description

technical field [0001] The invention relates to a flame retardant tris(dibromopropyl)tribromophenyl silicate compound and a preparation method thereof. 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] With the rapid development of the polymer material industry, its polymer materials have been more and more widely used in daily life, manufacturing and engineering construction. These polymer materials are easy to be ignited and cause fires, which seriously endanger people's lives and property security. Therefore, the research and wide application of flame retardants are promoted. Among them, silicon-based flame retardants have become one of the new technologies for the development of low-smoke, low-toxicity flame-retardant materials due to their excellent thermal stability, effective anti-melt dripping and flame-retardant and smoke-suppressing prope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/06C08K5/5415C08L27/06C08L67/06C08L75/04C08L63/00
Inventor 王彦林孟凡一贺婧施雯刘芳
Owner 张家港市乐余科创园投资发展有限公司
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