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Polydimethyl silicate terephthalic diester polymer as flame-retardant charring agent and preparation method thereof

A technology of dimethyl silicic acid and phenylene diester, which is applied in the field of silicon-based flame-retardant char-forming agent polydimethylsilicate terephthalate polymer and its preparation, can solve the problems of poor processing performance, low decomposition temperature, Polarity and other issues, to achieve excellent flame retardant effect, high decomposition temperature, large molecular weight effect

Active Publication Date: 2015-06-17
HUZHOU RUIGAO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

People such as pentaerythritol have been found to have a certain char-forming effect, and are also used in some materials, but most of the char-forming agents currently have the disadvantages of high polarity, easy water absorption, low decomposition temperature and poor processing performance.

Method used

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  • Polydimethyl silicate terephthalic diester polymer as flame-retardant charring agent and preparation method thereof
  • Polydimethyl silicate terephthalic diester polymer as flame-retardant charring agent and preparation method thereof
  • Polydimethyl silicate terephthalic diester polymer as flame-retardant charring agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 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 5.50g (0.05mol) of terephthalate Phenol, 80ml dichloroethane and 10.1g (0.1mol) triethylamine, dropwise add 6.45g (0.05mol) dimethyl dichlorosilane, control the reaction temperature with the rate of addition not higher than 40 ℃, be warmed up to 65°C, keep warm for 9 hours; then add 0.08g of methanol dropwise as an end-capping agent, keep warm for 0.5h; cool down to below 30°C, then add 30ml of distilled water to wash twice, separate the liquids, and wash the obtained dichloroethane layer with 4g Dry it with anhydrous sodium sulfate, filter it with suction, and distill off the filtrate under reduced pressure to remove dichloroethane to obtain polydimethylsilicate terephthalate with a yield of 92.7%.

Embodiment 2

[0041]Example 2 In a 250ml four-neck 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 5.50 g (0.05 mol) of terephthalic acid Phenol, 110ml toluene and 12.63g (0.125mol) triethylamine, add dropwise 6.45g (0.05mol) dimethyl dichlorosilane, control the reaction temperature with the rate of addition not higher than 40°C, and raise the temperature to 70°C after dropping, Heat preservation reaction for 7 hours; then add 0.08g 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 liquid, and dry the obtained toluene layer with 6g of anhydrous magnesium sulfate , suction filtration, and the filtrate was distilled under reduced pressure to remove toluene to obtain polydimethylsilicate terephthalate, yield: 93.5%, weight average molecular we...

Embodiment 3

[0042] Example 3 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 5.50 g (0.05 mol) of terephthalic acid Phenol, 80ml xylene and 11.11g (0.11mol) 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 to 50°C after dropping , heat preservation reaction for 12 hours; then add 0.08g of methanol dropwise as an end-capping agent, heat preservation reaction for 0.5h; lower the temperature to below 30°C, then add 50ml of distilled water to wash twice, separate the liquid, and wash the obtained xylene layer with 8g of anhydrous sodium sulfate After drying and suction filtration, the filtrate was distilled off under reduced pressure to remove xylene to obtain polydimethylsilicate terephthalate with a yield of 91.6%.

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Abstract

The invention relates to a polydimethyl silicate terephthalic diester polymer as a flame-retardant charring agent and a preparation method thereof. The structural formula of the polymer is shown in the description, and in the structural formula, n is equal to 20-50. The preparation method comprises the following steps: in the presence of triethylamine, enabling hydroquinone to react with equimolar dimethyl dihalide silane in an organic solvent, or enabling hydroquinone sodium to react with equimolar dimethyl dihalide silane in an organic solvent, and performing purification so as to obtain polydimethyl silicon acid terephthalic diester. The polydimethyl silicate terephthalic diester disclosed by the invention is high in molecular weight, is good in material compatibility, is not easy to separate out, is good in charring performance, and is suitable for being used as a flame-retardant charring agent of polyolefine, polyester, polyamide, an epoxy resin, an unsaturated resin and the like. The production technology is simple, the cost is low, and the industrialized production is easy to realize.

Description

technical field [0001] The invention relates to a silicon-based flame-retardant char-forming agent polydimethylsilicate terephthalate polymer and a preparation method thereof. The polymer is suitable for use in polyolefins, polyesters, polyamides, epoxy resins, unsaturated Flame retardant char forming agent for resin etc. Background technique [0002] The most effective way to solve the flammability problem of synthetic polymer materials is to add flame retardants to the materials, but flame retardants can generally prevent and slow down the burning of materials or make materials more flammable, and cannot change the melting phase of materials when heated. The characteristic of change, that is, when the material is burned at high temperature, it will become a liquid flow or drip, which will move with the flame and cause secondary combustion. In order to solve the flammability and dripping problems of synthetic materials, the most effective method is to add a char-forming ag...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/18C08G77/08C08G77/06C08L83/06
Inventor 王彦林赖超杨海军
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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