Preparation method of dimethyl dibromo neopentyl dioxy cyclosilane compound as fire retardant

A technology of dimethyldibromoneopentyldioxycyclosilane and dibromoneopentyl glycol, which is applied in the field of preparation of flame retardant dimethyldibromoneopentyldioxycyclosilane compounds, and can solve the problem of halogenated The development of flame retardants is restricted and other issues, and the effect of cheap raw materials, low cost and good compatibility is achieved

Inactive Publication Date: 2015-06-17
苏州阳桥新型材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the development of halogenated flame retardants is limited due to the fact that it will decompose and produce harmful gases such as hydrogen halide during combustion.

Method used

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  • Preparation method of dimethyl dibromo neopentyl dioxy cyclosilane compound as fire retardant
  • Preparation method of dimethyl dibromo neopentyl dioxy cyclosilane compound as fire retardant
  • Preparation method of dimethyl dibromo neopentyl dioxy cyclosilane compound as fire retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 In a 100ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, 13.1g (0.05mol) of dibromoneopentyl glycol, 6.01g (0.05mol) of dimethyldimethoxysilane and 40ml of toluene, heated up to 80°C to start the boiling fractionation reaction, controlled the top temperature of the fractionation column not higher than 65°C, and continuously separated the generated methanol. As the reaction progressed, the free dimethyldimethoxysilane decreased, and the reaction system Gradually raise the temperature, and keep it warm at 110°C for about 7 hours. When the fractionated methanol reaches the theoretical amount, stop the reaction, distill off the organic solvent (recycled for use) and a small amount of low boiling point substances, and add the product mass in grams twice the volume in milliliters of water, stirred for 30 min, filtered with suction, rinsed with water of 0.5 times the volume in milliliters of the product mass in g...

Embodiment 2

[0024] Example 2 In a 100ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, 13.1g (0.05mol) of dibromoneopentyl glycol, 6.01g (0.05mol) of dimethyldimethoxysilane and 50ml of xylene, heated up to 80°C to start the boiling fractionation reaction, controlled the top temperature of the fractionation column not higher than 65°C, continuously separated the generated methanol, and the free dimethyldimethoxysilane decreased as the reaction progressed, and the reaction system Gradually raise the temperature, and keep it warm at 140°C for about 6 hours. When the fractionated methanol reaches the theoretical amount, stop the reaction, distill off the organic solvent (recovered for use) and a small amount of low boiling point substances, and add 2 times the volume of the product in milliliters several times of water, stirred for 30min, suction filtered, then rinsed with water of 0.5 times the volume in milliliters of the product mass i...

Embodiment 3

[0025] Example 3 In a 100ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, 13.1g (0.05mol) of dibromoneopentyl glycol, 6.01g (0.05mol) of dimethyldimethoxysilane and 50ml tetrachloroethane, heat up to 80°C to start the boiling fractionation reaction, control the fractionation column top temperature not higher than 65°C, continuously separate the generated methanol, and the free dimethyldimethoxysilane will decrease as the reaction progresses, The temperature of the reaction system is gradually raised, and the reaction is carried out at 130°C for about 7 hours. When the fractionated methanol reaches the theoretical amount, the reaction is stopped, and the organic solvent (recycled) and a small amount of low boiling point substances are distilled off. Water in milliliters by volume, stirred for 30 minutes, filtered with suction, then rinsed with water of 0.5 times the mass of the product in milliliters by volume, drained, and...

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Abstract

The invention relates to a preparation method of a dimethyl dibromo neopentyl dioxy cyclosilane compound as a fire retardant. The structural formula of the compound is shown in the description. The preparation method comprises the following steps: in a reactor provided with an efficient fractionating device, mixing dibromoneopentyl glycol and equimolar dimethyl dimethoxy silicane with an organic solvent; heating to 80 DEG C until boiling; starting a fractionation reaction; controlling the temperature of the top of a fractionating column to be no higher than 65 DEG C, and continuously separating generated methanol; when the temperature of the reacting system is gradually increased with the progress of the reaction, performing a heat preservation reaction at the temperature of 80-160 DEG C for 5-12 hours; when the fractionated methanol reaches a theoretical amount, stopping the reaction; distilling off the organic solvent, and performing purification so as to obtain a white solid dimethyl dibromo neopentyl dioxy cyclosilane. The fire retardant provided by the invention is high in flame retardant efficacy because of synergistic flame retardant of silicon-bromine bielement, and suitable for being used as the fire retardant of polyolefine, polyurethane, an epoxy resin, an unsaturated resin and the like. The production technology is simple, the investment in equipment is small, the raw materials are easy to obtain, and the cost is low.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant dimethyl dibromoneopentadioxycyclosilane compound. Dimethyldibromoneopentyldioxycyclosilane is a bromine-containing silicone flame retardant, suitable for use as a flame retardant for materials such as polyolefins, polyurethanes, epoxy resins, and unsaturated resins. Background technique [0002] Because synthetic polymer materials have excellent mechanical processing and special application properties, they are more and more widely used in various fields of society. But most of them are flammable, so they promote the rapid development of flame retardant science and technology. Among them, halogenated flame retardants have the advantages of good flame retardant effect and low price, so halogenated flame retardants are the most produced and used organic flame retardants. However, the development of halogen-based flame retardants is limited because it decomposes to produce harmful gases...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08K5/549C08L27/06
Inventor 韩虹王彦林王世杰王景
Owner 苏州阳桥新型材料有限公司
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