Flame retardant trichloroethyltribromophenoxychloropropylsilicate ester compound and preparation method thereof

A technology of tribromophenoxy and chloroethyl, which is applied in the direction of silicon organic compounds, etc., to achieve the effect of low cost, cheap and easy-to-obtain raw materials, and good structural plasticity

Active Publication Date: 2012-10-17
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

AI Technical Summary

Problems solved by technology

Due to the development of the global economy and the continuous improvement of people's living standards, the awareness of environmental protection has been continuously enhanced, and the environmental protection requirements for flame retardants have also been continuously improved. Although the flame retardant industry is developing rapidly, it is far from meeting the needs of material development. People always It is hoped that new high-efficiency, low-toxicity and low-cost flame retardants or flame-retardant plasticizers will appear on the market

Method used

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  • Flame retardant trichloroethyltribromophenoxychloropropylsilicate ester compound and preparation method thereof
  • Flame retardant trichloroethyltribromophenoxychloropropylsilicate ester compound and preparation method thereof
  • Flame retardant trichloroethyltribromophenoxychloropropylsilicate ester compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of tetrahydrofuran, 5.1g (0.03mol, 3.4ml) of silicon tetrachloride, and add 50ml of it dropwise within 60min at 20°C. A solution of 11.6g (0.03mol) tribromophenyl glycidyl ether dissolved in tetrahydrofuran, the dropwise addition process controls the temperature not to exceed 35°C, after the drop is completed, the temperature is raised to 60°C within 1 hour, kept for 6 hours, and then cooled to 35°C , under cooling, add 7.25g (0.09mol) of chloroethanol dropwise, control the temperature during the dropping process to not exceed 40°C, then raise the temperature to 50°C within 1h and keep it warm for 6h, cool down to 35°C, and add about 0.5g of triethylamine acid-binding agent , adjusted to pH=5-6, stirred for 1 h, filtered, the filtrate was distilled to remove the organic solvent (recycled), and then evaporated a small amount of low-boiling matter u...

Embodiment 2

[0027] Example 2 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of chloroform, 5.1g (0.03mol, 3.4ml) of silicon tetrachloride, and add 50ml of it dropwise within 60min at 20°C. A solution of 11.6g (0.03mol) tribromophenylglycidyl ether dissolved in chloroform, the dropwise addition process controls the temperature not to exceed 35°C, after the drop is completed, the temperature is raised to 60°C within 1 hour, kept for 5 hours, and then cooled to 35°C , under cooling, add 7.97g (0.099mol) of chloroethanol dropwise, and control the temperature during the dropping process to not exceed 40°C, then raise the temperature to 55°C within 1h and keep it for 5h, cool down to 35°C, and add about 0.5g N,N-dimethyl Aniline acid-binding agent, adjusted to pH = 5-6, stirred for 1 h, filtered, the filtrate was distilled to remove the organic solvent (for recycling), and then distilled off excess chloroethanol (for recycling)...

Embodiment 3

[0028]Example 3 In a 100ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of acetonitrile, 5.1g (0.03mol, 3.4ml) of silicon tetrachloride, and add 50ml of it dropwise within 60min at 20°C. A solution of 11.6g (0.03mol) tribromophenylglycidyl ether dissolved in acetonitrile, the dropwise addition process controls the temperature not to exceed 35°C, after the drop is completed, the temperature is raised to 70°C within 1 hour, kept for 4 hours, and then cooled to 35°C , under cooling, add 8.70g (0.108mol) of chloroethanol dropwise, and control the temperature during the dropping process to not exceed 40°C, then raise the temperature to 60°C within 1h and keep it warm for 4h, cool down to 35°C, add about 0.5g of melamine acid-binding agent, adjust to pH = 5-6, stirred for 1 hour, filtered, the filtrate was distilled to remove the organic solvent (for recycling), and then distilled off excess chloroethanol (for recycling) a...

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Abstract

The invention relates to a silicon-halogen synergic flame retardant compound and a preparation method thereof. The compound has the structural formula shown in the specification. The preparation method comprises the following steps of: at 20 DEG C, dropwise adding equimolar organic solvent solution of tribromophenylepoxypropyl ester into silicon tetrachloride; after the solution is completely added dropwise, keeping temperature at 60-80 DEG C, and reacting for 4-6 hours; dropwise adding chloroethanol of a certain molar ratio at 35 DEG C; keeping temperature at 50-70 DEG C and reacting for 3-6 hours; and purifying to obtain a light yellow liquid product tri(2-chloroethyl)-2-chloro-3-(2,4,6-tribromophenoxy)propyl silicate. The compound is an efficient flame retardant and is suitable to be used as a flame-retardant plasticizer of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like; and the production technology is simple, the equipment investment is low, and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant trichloroethyl tribromophenoxy chloropropyl silicate compound and a preparation method thereof, in particular to a silicic acid tris(2-chloroethyl)-2-chloro-3- (2,4,6-Tribromophenoxy)propyl ester compound and its preparation method. The compound is a silicon-halogen synergistic flame retardant, and is suitable for use as a flame-retardant plasticizer for materials such as polyvinyl chloride, polyurethane, epoxy resin, and unsaturated resin. Background technique [0002] At present, due to the development of synthetic polymer material science and its more and more wide application, its flammability often causes fires, which poses a serious threat to people's lives and property, thus promoting the research of flame retardant science and technology and the flame retardant industry. rapid development. Due to the development of the global economy and the continuous improvement of people's living standards, the aw...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/04C08K5/5415C08L27/06
Inventor 王彦林徐玫俞春雷
Owner 张家港市乐余科创园投资发展有限公司
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