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Flame retardant namely phenyl thiophosphonic acid bis(silicic acid phosphonyl heterocycle methylene)ester compound and preparation method thereof

A technology of phosphonyl heterocyclic methylene silicate and hindered phenyl thiophosphonic acid, which is applied in the field of phosphorus and sulfur tri-element synergistic flame retardant phenyl and organic silicon, and can solve the problem that flame retardants are difficult to meet actual needs and other problems, to achieve the effect of easy large-scale transformation and production, stable structure and convenient operation

Inactive Publication Date: 2019-05-31
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The application of flame retardants has been very common in various fields of society, and today, people pay more attention to ecological protection, and people put forward higher requirements for flame retardants. It is increasingly difficult for flame retardants containing only a single flame retardant element to meet the actual requirements. need

Method used

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  • Flame retardant namely phenyl thiophosphonic acid bis(silicic acid phosphonyl heterocycle methylene)ester compound and preparation method thereof
  • Flame retardant namely phenyl thiophosphonic acid bis(silicic acid phosphonyl heterocycle methylene)ester compound and preparation method thereof
  • Flame retardant namely phenyl thiophosphonic acid bis(silicic acid phosphonyl heterocycle methylene)ester compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1 In a 250ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected to the upper mouth of the condenser, the air in the bottle was driven out with nitrogen, and 100ml of diethylene glycol dimethyl was added. Ether, 21.56g (0.11mol) trimethylolphosphine oxide cyclic ester of dimethyl silicate, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is completely dissolved, 9.7g ( 0.05mol) of phenylphosphonothioate dichloride, the dropwise addition process controls the temperature not to exceed 80°C, raises the temperature to 145°C after dripping, and keeps the temperature for 11 hours. After the hydrogen chloride is released, adjust the pH of the reaction system to 6 with a pyridine acid-binding agent -7, diethylene glycol dimethyl ether (recycled) was removed by distillation under reduced pressure, 90ml of ethanol was added to the crude product for heating an...

Embodiment 2

[0026] Example 2 In a 250ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorbing device connected to the upper mouth of the condenser, use nitrogen to exhaust the air in the bottle, and add 115ml of cyclohexanone, 22.54g (0.115mol) trimethylolphosphine oxide cyclic ester of dimethyl silicate, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is completely dissolved, 9.7g (0.05mol) of benzene is added dropwise at 30°C Phosphonothioyl dichloride, control the temperature during the dropping process to not exceed 80°C, raise the temperature to 140°C after dropping, keep the temperature for 10 hours, wait until the hydrogen chloride is released, adjust the pH of the reaction system to 6-7 with triethylamine acid-binding agent , cyclohexanone (recycling) was removed by distillation under reduced pressure, 90ml of ethanol was added to the crude product for heating and dissolving, cooling, c...

Embodiment 3

[0027] Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected to the upper mouth of the condenser, the air in the bottle was exhausted with nitrogen, and 95ml anisole, 20.58g (0.105mol) trihydroxymethylphosphine oxide dimethylsilicate cyclic ester, after the trihydroxymethylphosphine oxide dimethylsilicate cyclic ester is completely dissolved, add 9.7g (0.05mol) benzene Phosphonothioyl dichloride, during the dropping process, the temperature should not exceed 80°C. After the dropping, the temperature was raised to 140°C, and the temperature was kept for 10 hours. After the hydrogen chloride was released, the pH of the reaction system was adjusted to 6-7 with pyridine Cyclohexanone (recovered and used) was removed by distillation under pressure, and 90ml of ethanol was added to the crude product for heating and dissolving, cooling, crystallization, filtration, and vacuum ...

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Abstract

The invention relates to a flame retardant namely a phenyl thiophosphonic acid bis(silicic acid phosphonyl heterocycle methylene)ester compound and a preparation method thereof. The structure of the compound is represented in the description. The preparation method comprises following steps: adding phenylthiophosphonic dichloride and dimethyl silicic acid trihydroxymethyl phosphine oxide cyclic ester into an organic solvent, controlling the mole ratio of phenylthiophosphonic dichloride to dimethyl silicic acid trihydroxymethyl phosphine oxide cyclic ester to be 1:2 to 1:2.4; dropwise adding phenylthiophosphonic dichloride at a temperature of 30 DEG C, during the addition process, controlling the temperature to be lower than 80 DEG C, after addition, raising the temperature to 130-150 DEG C, maintaining the temperature to carry out reactions for 9 to 12 hours, and after hydrogen chloride is completely released, purifying the reaction product to obtain a white solid namely phenyl thiophosphonic acid bis(silicic acid phosphonyl heterocycle methylene)ester. The compound is an excellent silicon-phosphor-sulfur synergetic flame retardant, which can be applied to epoxy resin, polyester, polyurethane, unsaturated resin, polyolefin, and the like. The technology is simple, the equipment investment is little, and industrial production is easy to realize.

Description

technical field [0001] The present invention relates to an organosilicon, phosphine and sulfur flame retardant phenylthiophosphonic acid bis(phosphonoheterocyclic methylene silicate) compound and a preparation method thereof, in particular to an organosilicon, phosphorus, sulfur three Elemental synergistic flame retardant phenylthiophosphonic acid bis(1,1-dimethyl-1-sila-2,6-dioxa-4-oxyl-4-phosphano-<4>-methylene Base) ester compound and preparation method thereof, the compound is a flame retardant containing three flame retardant elements silicon, phosphorus, and sulfur, and can be used as a flame retardant for materials such as epoxy resin, polyester, and unsaturated resin. Background technique [0002] The application of flame retardants has been very common in various fields of society, and today, people have put forward higher requirements for flame retardants, and it is increasingly difficult for flame retardants containing only a single flame retardant element t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6596C08K5/549C08L63/00C08L67/02
Inventor 王彦林王世杰陆嘉俊
Owner SUZHOU UNIV OF SCI & TECH