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Chloro- and bromo-containing silicate flame retardant compound and preparation method thereof

A technology of compound and flame retardant plasticizer, which is applied in the field of tri-2-chloro-3-propyl silicate compound and its preparation, to achieve the effects of cheap and easy-to-obtain raw materials, easy large-scale production, and good environmental benefits

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

At present, there are many studies on flame retardant plasticizers of phosphate esters, but they are far from meeting the needs of material development. People always hope that there will be new flame retardant plasticizers with high efficiency, low toxicity and low price in the market.

Method used

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  • Chloro- and bromo-containing silicate flame retardant compound and preparation method thereof
  • Chloro- and bromo-containing silicate flame retardant compound and preparation method thereof
  • Chloro- and bromo-containing silicate flame retardant compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 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) tribromophenylglycidyl 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 40°C , and an extremely flexible expansion soft sealing sleeve is installed on the upper mouth of the condenser tube, 4.0g (0.09mol) of ethylene oxide is introduced, and the temperature of the feeding process is controlled not to exceed 45°C, and then kept at 50°C for 5h, the pH of the reaction system When the value reaches 5-6, the reaction is over, and the tetrahydrofuran (recycled) is distilled off under reduced pressure to obtain a light yellow liquid si...

Embodiment 2

[0026] 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 1h, kept for 5h, and then cooled to 40°C , and an extremely flexible expansion soft sealing sleeve is installed on the upper opening of the condenser tube, 4.4g (0.099mol) of ethylene oxide is introduced, and the temperature is controlled not to exceed 45 °C during the introduction process, and then kept at 50 °C for 4 hours, the pH of the reaction system When the value reaches 5-6, the reaction is over, and the chloroform (recycled) is removed by distillation under reduced pressure to obtain a light yellow liqu...

Embodiment 3

[0027] 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 40°C , and an extremely flexible expansion soft sealing sleeve is installed on the upper mouth of the condenser tube, and 4.8g (0.108mol) of ethylene oxide is introduced into the process. When the value reaches 5-6, the reaction is over, and the acetonitrile (recycled) is distilled off under reduced pressure to obtain a light yellow liquid tris(2-chloroethyl)-2-chloro-3-(2,4,6-tribromobenzene) Oxygen) propyl ester, product yield 97.3%. Its flash point (open cu...

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Abstract

The invention relates to a silicon-halogen synergistic flame retardant plasticizer tri(2-chloroethyl)-2-chloro-3-(2, 4, 6-tribromophenoxy)propyl silicate compound and a preparation method of the compound. The compound is characterized in that the structure is shown as follows in the specification. The method comprises the steps of adding tetrachlorosilane into a reactor, dripping equivalent molartribromophenylglycidyl ether organic solvent solution, performing a heat preservation process for a reaction at 60 DEG C-80 DEG C for 4-6 hours after the organic solvent solution is dripped, pumping ethylene oxide into the 40 DEG C solution at a certain molar ratio and below the liquid surface, performing another heat preservation process for another reaction at 50 DEG C-60 DEG C for 3-5 hours, and purifying to obtain a yellow liquid of tri(2-chloroethyl)-2-chloro-3-(2, 4, 6-tribromophenoxy) propyl silicate. The compound is a highly effective flame retardant and used as the flame retardant for poly(vinyl chloride), polyurethane, epoxy resin, unsaturated resin and the like. The method is simple in manufacturing technique, low in investment, and easily realizes the industrial production.

Description

technical field [0001] The invention relates to a chlorine-containing, bromosilicate flame retardant compound and a preparation method thereof, in particular to a tris(2-chloroethyl)-2-chloro-3-(2,4,6-trisilicate) Bromophenoxy) propyl ester compound and preparation method thereof. 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] Today's polymer materials are more and more widely used, but because of their flammable characteristics, they often cause fires and pose a serious threat to people's lives and property, thus promoting the research of flame retardant technology and the rapid development of flame retardant plasticizer industry. develop. Flame retardant plasticizer is a plastic processing aid with both flame retardant function and plasticizing effect. It can overcome the problem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5415C07F7/04C08L27/06C08L75/04C08L63/00C08L101/00
Inventor 王彦林俞春雷刘颖棋范腊梅
Owner 张家港市乐余科创园投资发展有限公司
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