The preparation method of methyl phenyl silicate bis(phosphine heterocyclic methyl) ester compound

A technology of methylphenyldimethoxysilane and methylphenyl, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve material dripping, secondary Combustion and other problems, to achieve the effect of preventing molten dripping, increasing compatibility, and high flame retardant performance

Active Publication Date: 2017-12-01
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, the addition of flame retardants to polymer materials can prevent the material from burning, but at high temperatures, the material often melts and drips when heated, resulting in secondary combustion

Method used

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  • The preparation method of methyl phenyl silicate bis(phosphine heterocyclic methyl) ester compound
  • The preparation method of methyl phenyl silicate bis(phosphine heterocyclic methyl) ester compound
  • The preparation method of methyl phenyl silicate bis(phosphine heterocyclic methyl) ester compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 In a 150ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, replace the air in the bottle with nitrogen, and add 22.31g (0.115mol) of 4-hydroxymethyl-4-ethyl-cycloformazol base phosphonate, 9.11g (0.05mol) methylphenyldimethoxysilane, 50ml diethylene glycol dimethyl ether and 0.40g sodium methoxide, the temperature is raised to 160°C, and the temperature at the top of the fractionation column is controlled not to be higher than 65°C , Fractional distillation of the generated methanol, reaction for 12h, after fractional distillation of the theoretical amount of methanol, change to a vacuum distillation device, vacuum distillation to remove diethylene glycol dimethyl ether (recycling), then add 30ml of distilled water, stir to make the solid Disperse in water, filter with suction, and dry to obtain bis(phosphine heterocyclic methyl) methylphenylsilicate as a white solid, with a product yield of 90.0%.

Embodiment 2

[0026] Example 2 In a 150ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, replace the air in the bottle with nitrogen, and add 23.28g (0.12mol) of 4-hydroxymethyl-4-ethyl-cycloformazol base phosphonate, 9.11g (0.05mol) methylphenyldimethoxysilane, 40ml xylene and 0.55g sodium methoxide, heat up to 140°C, control the temperature at the top of the fractionation column to not be higher than 65°C, and fractionate the generated Methanol, reacted 10h, after the theoretical amount of methanol was distilled off, it was changed to a vacuum distillation device, and xylene was removed by vacuum distillation (recycling), and then 50ml of distilled water was added, stirred to make the solid dispersed in water, suction filtered, dried, The white solid methylphenylsilicate bis(phosphine heterocyclic methyl) ester was obtained, and the product yield was 91.2%.

Embodiment 3

[0027] Example 3 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, replace the air in the bottle with nitrogen, and add 19.40g (0.10mol) of 4-hydroxymethyl-4-ethyl-cycloformazol Base phosphonate, 9.11g (0.05mol) methylphenyldimethoxysilane, 30ml DMF and 0.65g sodium methoxide, raise the temperature to 130°C, control the temperature at the top of the fractionation column to not be higher than 65°C, and fractionate the generated methanol , fractionation reaction 9h, after the theoretical amount of methanol is fractionated, it is changed to a vacuum distillation device, and the DMF (recycled) is removed by vacuum distillation, and then 40ml of distilled water is added, stirred to make the solid dispersed in water, suction filtered, and dried to obtain Bis(phosphine heterocyclic methyl) methyl phenyl silicate as a white solid with a yield of 80.7%.

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Abstract

The invention relates to a method for preparing the flame-retardant agent of a methylphenyl silicic acid bis(phosphorous heterocyclic methyl) ester compound. The structure of the compound is as shown in the description. The preparation method includes the steps that nitrogen gas is used for replacing air in a reactor provided with an efficient fractionation device, the molar ratio of dimethoxymethylphenylsilane to 1-oxo-1-methyl-4-ethyl-4-methylol-2,6-dioxa-1- phosphorinane is controlled to be 1:2-1:2.6, the temperature is raised to 100-160 DEG C, the temperature of the top of a dephlegmator is controlled to be not higher than 65 DEG C, generated methyl alcohol is fractionated, a fractionation reaction is carried out for 9-17 hours, the reaction does not stop till the fractionated methyl alcohol reaches a theoretical amount, and methylphenyl silicic acid bis(phosphorous heterocyclic methyl) ester is obtained after purification. The flame-retardant agent is stable in structure performance, high in decomposition temperature and suitable for being used as flame retardancy of polyester PBT, PET, nylon, PC and other materials. The preparation technology is simple, equipment investment is little, large-scale production is easy, and application and development prospects are good.

Description

technical field [0001] The invention relates to a method for preparing a flame retardant methylphenylsilicate bis(phosphine heterocyclic methyl) ester compound, in particular to a flame retardant methylphenyl bis(1-oxo-1-methyl- The preparation method of 4-ethyl-1-phospha-2,6-dioxa-cyclohexyl-<4>-methoxy)silane compound, the compound contains phosphorus and silicon double flame retardant elements, phosphorus silicon Synergy has high flame retardant performance and is suitable for use as a flame retardant for polyester PBT, PET, nylon, PC, polyurethane, unsaturated resin, epoxy resin and other materials. Background technique [0002] With the rapid development of global science, technology and economy, flame retardant materials are developing rapidly. At the same time, due to the enhancement of environmental safety awareness, higher requirements are put forward for flame retardants. Flame retardant materials are required to be friendly to the environment, so the non-ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574
Inventor 王彦林李果
Owner SUZHOU UNIV OF SCI & TECH
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