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Flame retardant bis[tris(3-bromopropoxy)silyloxy]ethane compound and preparation method thereof

A technology of bromopropoxy and silyloxy, which is applied in the field of flame retardant bis[trisilyloxy]ethane compound and its preparation, can solve the problem of low influence on material mechanical processing performance, high flame retardant efficiency, difficult Find substitutes and other issues to achieve synergistic effects of high flame retardant performance, good plasticity, and large molecular weight

Active Publication Date: 2016-02-24
山东产研中科高端化工产业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogen dioxins when burned, the use of halogenated flame retardants has been restricted, but due to the excellent comprehensive cost performance of halogenated flame retardants and high flame retardant performance It has little effect on the mechanical processing performance of materials, and it is difficult to find ideal substitutes. Although the calls for halogen-free environmentally friendly flame retardants are high, halogen-free is still a long process, so it is necessary to develop high-efficiency halogen-based flame retardants to reduce flame retardancy. It has become an important research direction of halogenated flame retardants to reduce its toxicity by reducing the dosage of the agent.

Method used

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  • Flame retardant bis[tris(3-bromopropoxy)silyloxy]ethane compound and preparation method thereof
  • Flame retardant bis[tris(3-bromopropoxy)silyloxy]ethane compound and preparation method thereof
  • Flame retardant bis[tris(3-bromopropoxy)silyloxy]ethane compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 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) of silicon tetrachloride, under stirring, cooled with a cold water bath, so that the temperature of the reaction system was lowered below 25°C, 13.9g (8.88ml, 0.1mol) of 3-bromopropanol was added dropwise, and The process controls the reaction temperature not to be higher than 30°C. After dripping, raise the temperature to 45°C and keep it warm for 2 hours; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask , control the reaction temperature not higher than 50°C with the dropping speed, raise the temperature to 55°C after dropping, and react for 10h; ) 3-bromopropanol, the reaction temperature is controlled by the dropping rate not higher than 55°C, after the drop, the te...

Embodiment 2

[0026] 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 condenser, replace the air in the bottle with nitrogen, add 60ml carbon tetrachloride and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to lower the temperature of the reaction system below 25 ° C, dropwise added 13.9g (8.88ml, 0.1mol) 3-bromopropanol, dropwise added The process controls the reaction temperature not to be higher than 30°C. After dripping, raise the temperature to 45°C and keep it warm for 2 hours; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask , control the reaction temperature not higher than 50°C with the dropping speed, raise the temperature to 65°C after dropping, and react for 8h; ) 3-bromopropanol, the reaction temperature is controlled by the dropping rate not higher than 55°C, after the drop, the temper...

Embodiment 3

[0027]Example 3 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) of silicon tetrachloride, under stirring, cooled with a cold water bath, so that the temperature of the reaction system was lowered below 25°C, 13.9g (8.88ml, 0.1mol) of 3-bromopropanol was added dropwise, and The process controls the reaction temperature not to be higher than 30°C. After dripping, raise the temperature to 45°C and keep it warm for 2 hours; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask , control the reaction temperature not higher than 50°C with the dropping speed, raise the temperature to 70°C after dropping, and react for 7h; ) 3-bromopropanol, the reaction temperature is controlled by the dropping rate not higher than 55°C, after the dr...

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Abstract

The invention relates to a fire retardant 2[3(3-bromine propoxy) silicon acyloxy] ethane compound and a preparation method thereof. The structure of the compound is shown as the following formula. The preparation method comprises the following steps: reacting silicon tetrachloride with 3-trimethylene bromohydrin of the same mole of the silicon tetrachloride in organic solvent at below 25 DEG C, then dropwise adding ethanediol 0.5 mole of silicon tetrachloride, rising temperature up to 55-75 DEG C, reacting for 6-10 hours; then dripping 3-trimethylene bromohydrin 2-3 mole of silicon tetrachloride, thermal reacting for 7-10 hours at 65-85 DEG C; then adding acid-binding agent, stirring and performing heat preservation for 1 hour; purifying so as to obtain the fire retardant 2[3(3-bromine propoxy) silicon acyloxy] ethane. The compound has high antiflaming efficiency, is applicable to fire retardants made of materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin, is simple to prepare, has low cost, and is easy to realize industrial production.

Description

technical field [0001] The invention relates to a flame retardant bis[tris(3-bromopropoxy)silyloxy]ethane compound and a preparation method thereof. The compound can be used as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy Flame retardant for materials such as resins. Background technique [0002] With the continuous improvement of people's living standards, the awareness of safety and fire prevention has been continuously enhanced, which has promoted the rapid development of the flame retardant industry. Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogen dioxins when they were burned, the use of halogenated flame retardants was restricted. It has little effect on the mechanical processing performance of materials, and it is difficult to find ideal substitutes. Although the calls for halogen-free environmentally friendly flame retardants are high, halogen-free is still a long process, so it ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/04C08K5/5415C08L27/06
Inventor 王彦林杨海军董信
Owner 山东产研中科高端化工产业技术研究院有限公司
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