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Flame retardant dilphosphonic heterocyclic polysilicate compound and preparation method thereof

A technology of bisphosphonyl and flame retardant, which is applied in the field of flame retardant bisphosphonyl heterocyclic polysilicate compound and its preparation, can solve problems such as threats to life and property safety, fire, etc., and achieves improved flame retardant carbonization Efficacy, improved compatibility, novel structure

Active Publication Date: 2019-06-14
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most polymer materials are flammable and often cause fires, posing a serious threat to people's life and property safety. If it is not a new standard, it greatly promotes the progress of flame retardant materials and flame retardant technology

Method used

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  • Flame retardant dilphosphonic heterocyclic polysilicate compound and preparation method thereof
  • Flame retardant dilphosphonic heterocyclic polysilicate compound and preparation method thereof
  • Flame retardant dilphosphonic heterocyclic polysilicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 19.6g (0.10mol) di Trihydroxymethylphosphine oxide cyclic ester of methyl silicate and 90ml of ethylene glycol diethyl ether, then add 6.45g (0.05mol) of dimethyldichlorosilane dropwise, and control the temperature of the dropping process not to be higher than 50°C. Afterwards, the temperature was raised to 70°C, and the temperature was kept for 3 hours, and then the temperature was raised to 120°C under reflux, and the temperature was kept for 9 hours. into 60ml of ice water, stirred rapidly for 30min, filtered with suction, and the filter cake was vacuum-dried to obtain the flame retardant bisphosphonoheterocyclic polysilicate product. The yield is 92.2%, the melting point is 190±2°C, and the decomposition temperature is 376±5°C.

Embodiment 2

[0026] Example 2 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 20.58g (0.105mol) di Trihydroxymethylphosphine oxide cyclic ester of methyl silicate and 100ml of diethylene glycol dimethyl ether, then add 6.45g (0.05mol) of dimethyldichlorosilane dropwise, and control the temperature of the dropping process to not be higher than 50°C. After dripping, raise the temperature to 70°C, keep the temperature for 3 hours, then reflux and raise the temperature to 140°C, keep the temperature for 7 hours, let the hydrogen chloride be released, stop the reaction, cool to room temperature, and distill the solvent under reduced pressure to obtain a turbid viscous liquid; The product was poured into 60ml of ice water, stirred rapidly for 30 minutes, filtered with suction, and the filter cake was vacuum-dried to obtain the produc...

Embodiment 3

[0027] Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 21.56g (0.11mol) of di Trihydroxymethylphosphine oxide cyclic ester of methyl silicate and 110ml of tetrachloroethane, then add 6.45g (0.05mol) of dimethyldichlorosilane dropwise, and control the temperature of the dropping process not to be higher than 50°C. Raise the temperature to 70°C, keep the temperature for 3 hours, then reflux and raise the temperature to 130°C, keep the temperature for 7 hours, let the hydrogen chloride be released, stop the reaction, cool to room temperature, and distill the solvent under reduced pressure to obtain a cloudy viscous liquid; then pour the crude product into 60ml of ice water, stirred rapidly for 30 minutes, suction filtered, and the filter cake was vacuum-dried to obtain the product flame retardant bisphosphon...

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Abstract

The invention relates to a flame retardant dilphosphonic heterocyclic polysilicate compound and a preparation method thereof. The structure of the compound is shown as a formula in the description. The preparation method comprises the following steps of adding dimethyldichlorosilance and 2 to 2.4 mol of phosphocycloxy dimethylsilicate into an organic solvent; performing heat insulation reaction for 6 to 9h at 120 to 160 DEG C for completely exhausting hydrogen chloride; performing purification treatment; obtaining a product of the flame retardant dilphosphonic heterocyclic polysilicate. The compound provided by the invention belongs to an excellent silicon phosphorus cooperated flame retardant char forming agent which can be used as the flame retardant char forming agent of polyamide, polyester, polyurethane, polyolefin, epoxy resin, unsaturated resin and the like; the process is simple; the equipment investment is low; the industrialized production can be easily realized.

Description

technical field [0001] The invention relates to a flame retardant bisphosphono heterocyclic polysilicate compound and a preparation method thereof, in particular to a flame retardant dimethyl silicate bis[1,1-dimethyl-1-silica -2,6-dioxa-4-oxyl-4-phosphine hetero-(4)-methylene] ester compound and its preparation method, the compound contains phosphorus and silicon dual flame retardant elements, and can be used as polyamide , polyester, polyurethane, polyolefin, epoxy resin and unsaturated resin flame retardant charcoal agent. Background technique [0002] The advancement of science and technology has promoted the rapid development of the polymer material industry, and the consumption of organic synthetic polymer materials has become one of the important indicators to measure the development of a country or region. However, most polymer materials are flammable and often cause fires, posing a serious threat to people's lives and property. If not, the new standard has greatly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/549C08L63/00C07F9/6596
Inventor 王彦林王世杰文震
Owner SUZHOU UNIV OF SCI & TECH
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