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Flame retardant 1,2-ortho-diol dimethyl silicate compound and preparation method thereof

A technology of dimethyl silicic acid and o-diol ester, which is applied in the field of flame retardant dimethyl silicic acid-1, can solve problems such as a large amount of hydrogen halide gas, secondary hazards, etc., and achieves good application development prospects and low cost. , the preparation method is simple

Inactive Publication Date: 2015-06-10
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has been found in practice that in the event of a fire, halogenated flame retardants will produce a large amount of smoke and toxic corrosive hydrogen halide gas during the flame retardant process, causing secondary hazards.

Method used

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  • Flame retardant 1,2-ortho-diol dimethyl silicate compound and preparation method thereof
  • Flame retardant 1,2-ortho-diol dimethyl silicate compound and preparation method thereof
  • Flame retardant 1,2-ortho-diol dimethyl silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 In 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, add 30ml of ethylene glycol dimethyl ether and 7.6g (0.1mol ) 1,2-propanediol, at 20°C, add 12.9g (0.1mol) dimethyldichlorosilane dropwise, the dropwise addition process controls the temperature not to exceed 40°C, after the drop is completed, heat up to 70°C for 1h, and keep the temperature for 8h, Add about 0.4g of triethylamine acid-binding agent, adjust to pH=5-6, stir for 1 hour, filter while hot, distill off the solvent and a small amount of low boiling point from the filtrate to obtain colorless and transparent liquid dimethyl silicic acid-1,2 -Propylene glycol ester, product yield 94.5%, refractive index n D 25 =1.4344, density (25°C) 1.146±0.005g / cm 3 , boiling point 198°C.

Embodiment 2

[0039] Example 2 In the 100ml four-neck flask equipped with agitator, thermometer, high-efficiency reflux condenser and drying tube and hydrogen chloride absorption device at the upper mouth of the condenser, add 50ml dichloroethane and 7.6g (0.1mol) 1 , 2-propanediol, at 20°C, add 12.9g (0.1mol) dimethyldichlorosilane dropwise, and the temperature during the dropwise addition should not exceed 40°C. 0.3g of pyridine acid-binding agent, adjusted to pH = 5-6, stirred for 1 hour, filtered while hot, distilled off the solvent and a small amount of low boiling point from the filtrate to obtain 1,2-propylene glycol dimethyl silicate as a colorless and transparent liquid, Product yield 96.5%, refractive index n D 25 =1.4344, density (25°C) 1.146±0.005g / cm 3 , boiling point 198°C.

Embodiment 3

[0040]Embodiment 3 In the 100ml four-necked flask that stirrer, thermometer, high-efficiency reflux condensation tube are equipped with and drying tube and hydrogen chloride absorption device are equipped with at the top of condensation tube, add 30ml1, 4-dioxane and 7.6g (0.1 mol) 1,2-propanediol, at 20°C, add 12.9g (0.1mol) dimethyldichlorosilane dropwise, the dropwise addition process controls the temperature not to exceed 40°C, after the drop is completed, heat up to 100°C for 2h, and keep the temperature for 5h , add about 0.4g melamine acid-binding agent, adjust to pH = 5-6, stir for 1h, filter while hot, and distill off the solvent and a small amount of low boiling point from the filtrate to obtain colorless and transparent liquid dimethyl silicate-1,2- Propylene glycol ester, product yield 97.2%, refractive index n D 25 =1.4344, density (25°C) 1.146±0.005g / cm 3 , boiling point 198°C.

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Abstract

The invention relates to a flame retardant 1,2-ortho-diol dimethyl silicate compound and a preparation method thereof. The structure of the compound is disclosed in the specification, wherein R is methyl, ethyl, propyl or butyl group. The preparation method comprises the following steps: dropwisely adding dimethyl dichlorosilane or dimethyl dibromosilane into an organic solvent solution dissolved with equal mole of 1,2-ortho-diol at 20 DEG C, wherein the temperature in the dropwise addition does not exceed 50 DEG C; after finishing the dropwise addition, heating to 70-130 DEG C within 1-2 hours, keeping the temperature to react for 4-8 hours, and purifying to obtain the colorless transparent liquid 1,2-ortho-diol dimethyl silicate. The 1,2-ortho-diol dimethyl silicate has the advantages of high flame-retardant efficiency, favorable carbonization property and favorable plasticity, and is suitable to be used as a flame retardant for polyvinyl chloride, polyurethane, epoxy resins, unsaturated resins and other materials. The preparation method has the advantages of simple production technique, low equipment investment and low cost, and can easily implement industrial production.

Description

technical field [0001] The invention relates to a flame retardant dimethyl silicate-1,2-o-diol ester compound and a preparation method thereof. Dimethyl silicate-1,2-o-diol ester is a halogen-free silicone flame retardant, suitable for use as a flame retardant for materials such as polyvinyl chloride, polyurethane, epoxy resin, and unsaturated resin. Background technique [0002] In recent years, organic synthetic polymer materials have been developed very rapidly and are widely used in various fields. However, due to the flammability of polymer materials, fires often occur, thus promoting the development of flame retardants. Among them, halogenated flame retardants have a long history of development, mature application technology, high comprehensive cost performance, and are the most widely used. However, it has been found in practice that in the event of a fire, halogenated flame retardants will produce a large amount of smoke and toxic corrosive hydrogen halide gas duri...

Claims

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Application Information

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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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