Tris(dichloropropyl) tribromophenoxy chloropropyl silicate compound and preparation method thereof

A kind of technology of tribromophenoxy chloropropyl ester and tribromophenyl glycidyl ether, which is applied in the field of tribromophenoxy chloropropyl silicate compound and preparation thereof, and can solve the problem of high price and use. narrow range and other problems, to achieve the effects of low cost, good structural plasticity and simple preparation method

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

However, silicone-based products are expensive and limited in scope of use.

Method used

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  • Tris(dichloropropyl) tribromophenoxy chloropropyl silicate compound and preparation method thereof
  • Tris(dichloropropyl) tribromophenoxy chloropropyl silicate compound and preparation method thereof
  • Tris(dichloropropyl) tribromophenoxy chloropropyl silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 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) of 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 1h, kept for 6h, and then cooled under cooling conditions 11.61 g (0.09 mol) of 2,3-dichloropropanol was added dropwise within 1 hour. After the drop was completed, the temperature was kept at 50°C for 8 hours. to pH = 5-6, stirred for 1 hour, filtered, the filtrate was distilled to remove the organic solvent (recycled), and then evaporated a small amount of low boiling point substances under reduced pressure to obtain a pale yellow liquid tris(2,3-dichloropropyl) trisilicate Bromophenoxychloroprop...

Embodiment 2

[0031]Example 2 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 drop 50ml of it 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 60°C within 1h, kept for 5h, and then cooled under cooling conditions 12.77g (0.099mol) of 2,3-dichloropropanol was added dropwise within 1 hour. After the drop, the temperature was kept at 70°C for 7 hours. After the reaction was completed, the temperature was lowered to 40°C, and about 0.5g of N,N-dimethylaniline was added. Acid-binding agent, adjust to pH=5-6, stir for 1h, filter, distill off the organic solvent (for recycling) from the filtrate, then distill off excess dichloropropanol (for recycling) and a small amount of...

Embodiment 3

[0032] Example 3 In a 100ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of dichloroethane, 5.1g (0.03mol, 3.4ml) of silicon tetrachloride, and drop it in 60min at 20°C Add a solution of 11.6g (0.03mol) tribromophenylglycidyl ether dissolved in 50ml of dichloroethane, and control the temperature during the dropwise addition to not exceed 35°C. After the dropwise addition, the temperature will be raised to 70°C within 1h and kept for 4h , and then under cooling conditions, 13.93g (0.108mol) of 1,3-dichloropropanol was added dropwise within 1 hour. After the drop, the temperature was kept at 80°C for 6 hours. Acid agent, adjust to pH=5-6, stir for 1h, filter, distill off the organic solvent (for recycling) from the filtrate, then distill off excess dichloropropanol (for recycling) and a small amount of low boiling point substances under reduced pressure to obtain light yellow Liquid tris(1,3-dichloropropyl)tribromophe...

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Abstract

The invention relates to a tris(dichloropropyl) tribromophenoxy chloropropyl silicate compound which is a silicon-halogen synergistic fire retardant, and a preparation method of the compound. The compound has a structure shown in a formula described in the specification; and in the formula, OC3H5Cl2 is OCH2CHClCH2Cl or OCH (CH2Cl) 2. The preparation method of the compound comprises the following steps: reacting tribromophenyl glycidyl ether and silicon tetrachloride according to the same molar ratio in an organic solvent for 4-6h at 60-80 DEG C; then dropwise adding dichloropropanol according to a certain molar ratio, reacting for 4-8h at 50-100 DEG C; and finally purifying to obtain faint yellow liquid which is the tris(dichloropropyl) tribromophenoxy chloropropyl silicate. The compound is applicable to fire retardants for polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and other materials; and the production process is simple, low in equipment investment and cost, and suitable for industrial production.

Description

technical field [0001] The invention relates to a tri(dichloropropyl)tribromophenoxychloropropyl silicate compound and a preparation method thereof. Tris(dichloropropyl)tribromophenoxychloropropyl silicate is a silicon-halogen synergistic flame retardant, which is suitable for flame retardants or enhancers of materials such as polyvinyl chloride, polyurethane, epoxy resin, and unsaturated resin. plasticizer. Background technique [0002] Polymer materials are used more and more widely, but because of their flammable characteristics, they often cause fires, thus promoting the rapid development of flame retardant science and technology. Flame retardant plasticizer is a polymer material processing aid with both flame retardant function and plasticizing effect. It can overcome the problem of making polymer materials more flammable due to the addition of plasticizers. At present, there are few excellent flame-retardant plasticizers, and people always expect to develop new flame...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/06C08K5/5415C08K13/02C08L27/06
Inventor 王彦林董淑玲袁文常俞春雷
Owner 张家港市乐余科创园投资发展有限公司
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