Tetrabromobisphenol-A polydimethylsilicate polymer and preparation method thereof

A technology of polydimethylsilicic acid tetrabromobisphenol and dimethylsilicic acid tetrabromobisphenol is applied in the field of polydimethylsilicic acid tetrabromobisphenol A polymer and preparation thereof, and can solve fire, People's lives and property safety threats and other issues, to prevent secondary combustion, simplify the post-processing process, and achieve the effect of low volatility

Active Publication Date: 2017-12-22
HUZHOU RUIGAO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these polymer materials are flammable and often cause fires, posing a serious threat to people's lives and property.

Method used

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  • Tetrabromobisphenol-A polydimethylsilicate polymer and preparation method thereof
  • Tetrabromobisphenol-A polydimethylsilicate polymer and preparation method thereof
  • Tetrabromobisphenol-A polydimethylsilicate polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube on the top of the condenser tube, replace the air in the bottle with nitrogen, and add 27.19g (0.05mol) tetrabromobis Phenol A, 140ml toluene and 10.1g (0.1mol) triethylamine, add 6.45g (0.05mol) dimethyldichlorosilane dropwise, control the reaction temperature not higher than 40°C at the rate of addition, and raise the temperature to 70°C after dropping , heat preservation reaction for 8 hours, then add 0.15g of methanol dropwise as an end-capping agent, heat preservation reaction for 0.5h; lower the temperature to below 30°C, then add 30ml of distilled water to wash twice, separate the layers, and use 10g of anhydrous sodium sulfate for the obtained toluene layer. Dry, filter with suction, and distill the filtrate to remove toluene under reduced pressure to obtain tetrabromobisphenol A polydimethylsilicate, with a yield of 93.8%.

Embodiment 2

[0039]Example 2 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube on the top of the condenser tube, replace the air in the bottle with nitrogen, and add 27.19g (0.05mol) tetrabromobis Phenol A, 75ml dichloroethane and 12.63g (0.125mol) triethylamine, add dropwise 6.45g (0.05mol) dimethyldichlorosilane, control the reaction temperature with the dropping rate not higher than 40°C, and raise the temperature after dropping to 55°C, heat-retain for 10 hours, then add dropwise 0.1g of methanol as an end-capping agent, heat-retain for 0.5h; lower the temperature to below 30°C, then add 60ml of distilled water to wash twice, separate the liquid, and use the obtained dichloroethane layer with 5g of anhydrous sodium sulfate was dried, filtered with suction, and the filtrate was distilled off under reduced pressure to remove dichloroethane to obtain tetrabromobisphenol A polydimethylsilicate, with a yield of 90.8%.

Embodiment 3

[0040] Example 3 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser, and a drying tube at the top of the condenser, replace the air in the bottle with nitrogen, and add 27.19g (0.05mol) tetrabromobis Phenol A, 110ml xylene and 12.63g (0.125mol) triethylamine, add dropwise 6.45g (0.05mol) dimethyl dichlorosilane, control the reaction temperature with the dropping rate not higher than 40°C, and raise the temperature to 70°C after dropping. ℃, heat preservation reaction for 7 hours, then dropwise add 0.15g of methanol as an end-capping agent, heat preservation reaction for 0.5h; lower the temperature to below 30°C, then add 30ml of distilled water to wash twice, separate the liquid, and wash the obtained xylene layer with 8g of anhydrous sulfuric acid Magnesium was dried, suction filtered, and the filtrate was distilled off under reduced pressure to remove xylene to obtain tetrabromobisphenol A polydimethylsilicate. Yield: 93.1%, weight average m...

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Abstract

The invention relates to a tetrabromobisphenol A polydimethylsilicate polymer and a preparation method thereof. The structure of the polymer is as follows: n=10-60. The preparation method is: in the presence of triethylamine, react tetrabromobisphenol A with equimolar dimethyldihalosilane in an organic solvent; or tetrabromobisphenol A sodium and equimolar dimethyldihalosilane Reaction; After purification, tetrabromobisphenol A polydimethylsilicate was obtained. The polydimethylsilicate tetrabromobisphenol A ester of the present invention has large molecular weight, good compatibility with materials, low mobility and high flame retardant efficiency, and is suitable for polyolefin, polyester, polyurethane, polyamide and epoxy resin , unsaturated resin, etc., and the production process is simple, the cost is low, and it is easy to realize industrial production.

Description

technical field [0001] The present invention relates to a kind of synergistic flame retardant polydimethyl bromobisphenol A ester polymer of silicon and bromine double element and its preparation method, and this polymer is suitable for polyolefin, polyester, polyurethane, polyamide, Flame retardant for epoxy resin, unsaturated resin, etc. Background technique [0002] With the advancement of science and technology, synthetic fibers, plastics, rubber and other polymer materials are more and more widely used in various fields. Most of these polymer materials are flammable, often cause fires, and pose a serious threat to people's lives and property. In order to solve the problems of flammability and dripping when burning synthetic materials, the most effective method is to add flame retardants. At present, halogenated flame retardants are the organic flame retardants with the largest output and usage. However, with the continuous improvement of people's awareness of environ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/24C08G77/06C08G77/08C08L83/08
Inventor 王彦林杨海军
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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