Flame retardant dimethyl dibromo neopentyl glycol silicate compound and preparation method thereof

A technology of dibromoneopentyl glycol dimethyl silicate and dibromoneopentyl glycol, which is applied in the field of flame retardant dibromoneopentyl glycol dimethyl silicate, and can solve the problem of halogen-based flame retardancy In order to achieve the effects of high flame retardant efficiency, good processing performance and stable physical and chemical properties of silicon and bromine synergistically

Active Publication Date: 2015-07-01
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when it is burned, it will decompose and produce harmful gases such as hydrogen halide, which limits the development of halogenated flame retardants.

Method used

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  • Flame retardant dimethyl dibromo neopentyl glycol silicate compound and preparation method thereof
  • Flame retardant dimethyl dibromo neopentyl glycol silicate compound and preparation method thereof
  • Flame retardant dimethyl dibromo neopentyl glycol silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 Add 30ml ethylene glycol dimethyl ether and 13.1g (0.05mol ) dibromoneopentyl glycol, at 20°C, add 6.45g (0.05mol) of dimethyldichlorosilane dropwise, and control the temperature during the dropwise addition to not exceed 40°C. , add about 0.55g triethylamine acid-binding agent, adjust to pH = 5-6, stir for 1h, suction filter while hot, distill the filtrate to remove solvent and a small amount of low boiling point, add product mass 2 times the volume of water in milliliters , stirred for 30 minutes, filtered with suction, rinsed with water of 0.5 times the volume of the product in milliliters, drained, and the filter cake was dried to obtain a white solid, dibromoneopentyl glycol dimethyl silicate, with a product yield of 95.2 %.

Embodiment 2

[0031] Example 2 Add 40ml of acetonitrile and 13.1g (0.05mol) of dibromoneopentyl to a 100ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a drying tube and a hydrogen chloride absorption device at the upper mouth of the condenser Diol, at 20°C, add 6.45g (0.05mol) dimethyldichlorosilane dropwise, the dropwise addition process controls the temperature not to exceed 40°C, after the drop is over, heat up to 80°C in 1 hour, keep warm for 6 hours, add about 0.45g N,N-Dimethylaniline acid-binding agent, adjusted to pH = 5-6, stirred for 1 hour, suction filtered while hot, the filtrate was distilled to remove solvent and a small amount of low boiling point, and added water in milliliters twice the volume of the product in grams , stirred for 30 minutes, filtered with suction, rinsed with water of 0.5 times the volume of the product in milliliters, drained, and the filter cake was dried to obtain a white solid dibromoneopentyl glycol di...

Embodiment 3

[0032] Example 3 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a drying tube and a hydrogen chloride absorption device at the upper mouth of the condenser, add 50ml of dichloroethane and 13.1g (0.05mol) of dichloroethane. Bromoneopentyl glycol, at 20°C, add 6.45g (0.05mol) of dimethyldichlorosilane dropwise, the dropwise addition process controls the temperature not to exceed 40°C, after the drop, heat up to 82°C in 1h, keep the temperature for 6h, add About 0.4g of pyridine acid-binding agent, adjusted to pH=5-6, stirred for 1h, suction filtered while hot, the filtrate was distilled to remove solvent and a small amount of low boiling point substances, added water in milliliters with the mass of the product twice the volume, stirred for 30min, Suction filtration, then rinsing with 0.5 times the volume of the product in milliliters, draining, and drying the filter cake to obtain dibromoneopentyl glycol dimethyl silica...

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Abstract

The invention relates to a flame retardant dimethyl dibromo neopentyl glycol silicate compound and a preparation method thereof. The structure of the dimethyl dibromo neopentyl glycol silicate compound can be shown in the formula (described in the specification). The preparation method of the dimethyl dibromo neopentyl glycol silicate compound comprises the following steps: at the temperature of 20 DEG C, dropwise adding dimethyl dichlorosilane, or dimethyl dibromosilane into an organic solvent solution dissolved with equimolar of dibromo neopentyl glycol, wherein during the dropwise adding, the temperature is controlled to be not higher than 50 DEG C, then heating to 70-130 DEG C within 1-2 hours, carrying out heat preservation and reaction for 4-8 hours, and purifying, so that white solid dimethyl dibromo neopentyl glycol silicate is obtained. The dimethyl dibromo neopentyl glycol silicate has the advantages that silicon and bromine elements are synergistic, flame-retardant efficiency is high, char forming characteristic is good, and material compatibility is good, so that the dimethyl dibromo neopentyl glycol silicate is applicable to serving as flame retardant of materials such as polyolefin, polyurethane, epoxy resin and unsaturated resin; meanwhile, a production process is simple, equipment investment is low, raw materials are available, cost is low, and industrial production can be easily realized.

Description

technical field [0001] The invention relates to a flame retardant dibromoneopentyl glycol dimethyl silicate compound and a preparation method thereof. Dibromoneopentyl glycol dimethyl silicate is a silicon-halogen synergistic flame retardant, suitable for use as a flame retardant for materials such as polyolefins, polyurethanes, epoxy resins, and unsaturated resins. Background technique [0002] Synthetic organic polymer materials have excellent application properties and are easy to process and shape, and are more and more widely used in various fields such as transportation, building materials, electronic appliances, daily furniture, and interior decoration. However, polymer materials are flammable, which promotes the rapid development of flame retardant science and technology. Among them, halogenated flame retardants have the advantages of low price, less addition amount, and good flame retardant effect, and are the organic flame retardants with the largest production an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08K5/549C08L27/06
Inventor 冯芳王世杰王彦林
Owner SUZHOU UNIV OF SCI & TECH
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