A kind of polymerized organosilicon flame retardant charcoal agent polymer and preparation method thereof

A technology of organosilicon and char-forming agent, which is applied to silicon-based flame retardant char-forming agent poly(resorcinol dimethyl silicate) polymer and its preparation, polymeric organosilicon flame retardant char-forming agent polymer and its preparation In the field of preparation, it can solve the problems of low decomposition temperature, poor processing performance, easy water absorption, etc., and achieve the effects of low volatility, excellent flame retardant effect and large molecular weight.

Active Publication Date: 2018-04-27
HUZHOU RUIGAO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pentaerythritol and pentaerythritol phosphate are carbon-forming agents that have been used and tried by people, but most of the above-mentioned char-forming agents have the disadvantages of high polarity, easy water absorption, low decomposition temperature and poor processability.

Method used

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  • A kind of polymerized organosilicon flame retardant charcoal agent polymer and preparation method thereof
  • A kind of polymerized organosilicon flame retardant charcoal agent polymer and preparation method thereof
  • A kind of polymerized organosilicon flame retardant charcoal agent polymer 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 condensing tube, and a drying tube at the top of the condensing tube, replace the air in the bottle with nitrogen, and add 5.50 g (0.05 mol) of resorcinol Phenol, 110ml dichloroethane and 10.1g (0.1mol) triethylamine, dropwise add 6.45g (0.05mol) dimethyldichlorosilane, control the reaction temperature with the rate of addition not higher than 30 ℃, be warmed up to 65°C, heat preservation reaction for 10 hours, then dropwise add 0.04g 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 dichloroethane layer with 6g Dry over anhydrous sodium sulfate, filter, and distill off the filtrate under reduced pressure to remove dichloroethane to obtain resorcinol polydimethylsilicate with a yield of 92.8%.

Embodiment 2

[0041] 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, the air in the bottle was replaced with nitrogen, and 5.50g (0.05mol) of benzenediol was added. Phenol, 80ml toluene and 11.11g (0.11mol) triethylamine, add dropwise 6.45g (0.05mol) dimethyldichlorosilane, control the reaction temperature with the rate of addition not higher than 30°C, and raise the temperature to 70°C after dropping, Insulate and react for 7 hours, then add 0.05g of methanol dropwise as an end-capping agent, and insulate for 0.5h; lower the temperature to below 30°C, then add 30ml of distilled water to wash twice, separate the layers, and dry the obtained toluene layer with 7g of anhydrous magnesium sulfate , filtered, and the filtrate was distilled off toluene under reduced pressure to obtain resorcinol polydimethylsilicate. Yield: 93.9%, weight average molecular weight: 8314, number average molecular...

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 m-phthalide Phenol, 90ml 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 30°C, and raise the temperature to 50°C after dropping , heat preservation reaction for 12 hours, then add 0.04g of methanol dropwise as an end-capping agent, heat preservation reaction for 0.5h; lower the temperature to below 30°C, then add 40ml of distilled water to wash twice, separate the liquid, and wash the obtained xylene layer with 9g of anhydrous sodium sulfate After drying and filtering, the filtrate was distilled off under reduced pressure to remove xylene to obtain resorcinol polydimethylsilicate with a yield of 92.6%.

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Abstract

The present invention relates to a polymerized organic silicon flame-retardant char-forming agent polymer and a preparation method thereof, in particular to a flame-retardant char-forming agent polydimethylsilicate resorcinol ester polymer and a preparation method thereof. The structure of the object is shown in the following formula: n=30~80 in the formula. The preparation method is: in an organic solvent, in the presence of triethylamine, react resorcinol with equimolar dimethyldihalosilane; or react sodium resorcinol with equimolar dimethyldihalosilane, After purification, resorcinol polydimethylsilicate is obtained. The polydimethylsilicate resorcinol ester of the present invention has large molecular weight, high decomposition temperature, good compatibility with materials, no migration, good char formation, and is suitable for use as polyolefin, polyester, polyamide, 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 invention relates to a polymerized organic silicon flame-retardant char-forming agent polymer and a preparation method thereof, in particular to a silicon-based flame-retardant char-forming agent polydimethylsilicate resorcinol ester polymer and a preparation method thereof. The polymer is suitable for use as a flame-retardant char-forming agent for polyolefins, polyesters, polyamides, epoxy resins, unsaturated resins, etc. Background technique [0002] Adding flame retardants to materials is an effective way to overcome the problem of flammability of synthetic polymer materials. However, because polymer materials generally have the property of three states, that is, when the material is burned at a high temperature, it will flow or drip into a liquid, which will move with the flame and cause secondary combustion. In order to solve the dripping problem of synthetic materials, the most effective method is to add a char-forming agent. The carbon fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/52C08G77/06C08L83/14C08L67/02C08L23/12
Inventor 翟忠杰董信杨海军王彦林
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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