Flame retardant phosphate tri(dimethyl siliconyl heterocyclic methylene) ester compound and preparation method thereof

A technology of dimethylsilylphosphonoheterocyclic methylene and trimethylol dimethylsilicate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., capable of Solve the secondary hazards of life safety and other issues, and achieve the effect of high synergistic flame retardant efficiency, low cost, and moderate polarity

Inactive 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

Although halogenated flame retardants have good flame retardant properties, the toxic gases such as dioxins produced during combustion will cause secondary harm to people's life safety.

Method used

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  • Flame retardant phosphate tri(dimethyl siliconyl heterocyclic methylene) ester compound and preparation method thereof
  • Flame retardant phosphate tri(dimethyl siliconyl heterocyclic methylene) ester compound and preparation method thereof
  • Flame retardant phosphate tri(dimethyl siliconyl heterocyclic methylene) ester 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, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected to the upper mouth of the condenser, use nitrogen to exhaust the air in the bottle, and at 20°C, add 29.4g ( 0.15mol) trimethylol phosphine oxide cyclic ester of dimethyl silicate and 90ml of diethylene glycol dimethyl ether, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is completely dissolved and dispersed, add dropwise 7.675g (0.05mol) phosphorus oxychloride, control the dripping process not to exceed 60°C, after the dropwise addition, the temperature is raised to 100°C, and the temperature is kept for 10 hours to make the hydrogen chloride completely released, and the solvent is distilled off under reduced pressure to obtain a turbid viscous liquid; The crude product was poured into 100 ml of ice water and stirred rapidly for 30 min, filtered with suction, rinsed with 50 ml of wat...

Embodiment 2

[0026] Example 2 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, use nitrogen to exhaust the air in the bottle, and at 20°C, add 30.38g ( 0.155mol) trimethylol phosphine oxide cyclic ester of dimethyl silicate and 120ml anisole, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is completely dissolved and dispersed, add 7.675g (0.05 mol) phosphorus oxychloride, control the dropping process not to exceed 60°C, raise the temperature to 130°C after dropping, keep the temperature for 9 hours, let the hydrogen chloride be released, and distill off the solvent under reduced pressure to obtain a turbid viscous liquid; then pour the crude product into Stir rapidly in 100 ml of ice water for 30 min, filter with suction, rinse with 50 ml of water, and vacuum-dry the filter cake to obtain the product tris(dimethylsilylphosphon...

Embodiment 3

[0027] Example 3 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 exhausted with nitrogen, and at 20°C, 31.36g ( 0.16mol) trihydroxymethylphosphine oxide dimethylsilicate cyclic ester and 140ml xylene, after the trimethylolphosphine oxide cyclic ester dimethylsilicate is completely dissolved and dispersed, add 7.675g (0.05mol ) phosphorus oxychloride, control the dropping process not to exceed 60°C, raise the temperature to 120°C after dropping, keep the temperature for 9 hours, let the hydrogen chloride be released, and distill off the solvent under reduced pressure to obtain a turbid viscous liquid; then pour the crude product into 100ml Stir rapidly in ice water for 30 min, filter with suction, rinse with 50 ml of water, and dry the filter cake in vacuum to obtain the product tris(dimethylsilylphosphonoheter...

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Abstract

The invention relates to a flame retardant phosphate tri(dimethyl siliconyl heterocyclic methylene) ester compound and a preparation method thereof. The structure of the compound is shown as a formulain the description. The preparation method comprises the following steps of dissolving dimethyl silicate trimethylol phosphine oxide cyclic ester into organic solvents at 20 DEG C under the nitrogengas protection; then, dripping phosphorus oxychloride; controlling the mol ratio of the phosphorus oxychloride to the dimethyl silicate trimethylol phosphine oxide cyclic ester to be 1:3-1:3.6; controlling the temperature not to exceed 60 DEG C in the dripping process; after the dripping completion, raising the temperature to 80 to 130 DEG C; performing heat insulation reaction for 8 to 10h for completely exhausting hydrogen chloride; performing purification treatment to obtain phosphate tri(dimethyl siliconyl heterocyclic methylene) ester. The compound has the advantages that double elementsof phosphorus and silicon are cooperated for flame retardance; the flame retardant efficiency is high; the compound is suitable for being used as the flame retardant for polyamide, polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin and the like; the preparation method uses one-step reaction; the process is simple; the equipment investment is low; the industrialized production canbe easily realized.

Description

technical field [0001] The invention relates to a flame retardant tris(dimethylsilylphosphonoheterocyclic methylene) phosphate compound and a preparation method thereof, in particular to a phosphoric acid tris[1,1-dimethyl-1-sila- 2,6-dioxa-4-oxygen-4-phosphine hetero-(4)-methylene] ester compound and its preparation method, the compound is suitable for polyamide, polyester, polyurethane, epoxy resin, Flame retardant for unsaturated resin, polyolefin and other materials. Background technique [0002] With the rapid development of polymer materials, the application of flame retardant materials is becoming more and more common, and due to the enhancement of people's awareness of environmental protection, there are higher requirements for flame retardants. At the same time, more attention is paid to its friendliness to the environment, so it promotes the rapid development of non-halogenated flame retardants, thereby promoting the development of green and environmentally friend...

Claims

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Application Information

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