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Reactive flame-retardant organic phosphonate compound and preparation method thereof

A reactive flame retardant and phosphonate technology, applied in organic chemistry, chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, etc., can solve problems such as incompatibility and affecting material properties, Achieve the effects of good stability, good flame retardancy and good plasticity

Active Publication Date: 2016-01-06
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the more or less incompatibility between the additive flame retardant and the polymer matrix, it will be accompanied by escape and decomposition during processing, which will affect the performance of the material

Method used

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  • Reactive flame-retardant organic phosphonate compound and preparation method thereof
  • Reactive flame-retardant organic phosphonate compound and preparation method thereof
  • Reactive flame-retardant organic phosphonate compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 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, add 40ml ethylene glycol dimethyl ether, 13.42g (0.10mol) trimethylolpropane, 12.41g (0.10mol) dimethyl methylphosphonate, 0.12g sodium methoxide, then raise the temperature to 80°C, control the temperature at the top of the fractionation column to not be higher than 65°C, fractionate the generated methanol, react for 10h, and wait until no methanol is produced , changed to a vacuum distillation device, vacuum distillation to remove ethylene glycol dimethyl ether (recycled), then add 20ml of ice water to wash, stir, stand at 0°C for stratification, separate the lower layer of material liquid, and vacuum distillation Remove a small amount of water and a small amount of low-boiling matter to obtain a reactive flame retardant organic phosphonate. The product yield is 92.5%. Its flash point (open cup): 198±5°C, ...

Embodiment 2

[0028] 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, add 50ml xylene, 13.42g (0.10mol) trimethylolpropane, 16.13g (0.13 mol) dimethyl methylphosphonate, 0.2g sodium methoxide, and then raise the temperature to 140°C, control the temperature at the top of the fractionation column to not be higher than 65°C, fractionate the generated methanol, and react for 5 hours. After no methanol is produced, change to reduce Distillation device, vacuum distillation to remove xylene (recycling), then add 25ml of ice water to wash, stir, stand at 0°C for stratification, separate the lower layer of material liquid, vacuum distillation to remove a small amount of water and a small amount of low boiling point The reaction type flame retardant organic phosphonate was obtained, the product yield was 95.8%, its flash point (open cup): 198±5°C, decomposition temperature: 230±5°C, de...

Embodiment 3

[0029] Example 3 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, add 50mlDMF, 13.42g (0.10mol) trimethylolpropane, 14.89g (0.12mol) Dimethyl methylphosphonate, 0.24g of sodium methoxide, then heat up to 120°C, control the temperature at the top of the fractionation column to not be higher than 65°C, fractionate the generated methanol, react for 8 hours, and change to vacuum distillation after no methanol is produced device, remove DMF by distillation under reduced pressure (recycling), then add 35ml of ice water to wash, stir, stand at 0°C for stratification, separate the lower layer material liquid, and remove a small amount of water and a small amount of low boiling point matter by distillation under reduced pressure to obtain Reactive flame retardant organic phosphonate, product yield 96.2%, flash point (open cup): 198±5°C, decomposition temperature: 230±5°C, density (...

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Abstract

The invention relates to a reactive flame-retardant organic phosphonate compound and a preparation method thereof. Please see the formula of the structure of the compound in the specification. The preparation method includes the steps that air in a reactor with a fractional device is replaced with nitrogen, the molecular ratio of tri-methylol propane to dimethyl methylphosphonate is controlled to be 1:1-1:1.3, then organic solvents and catalysts are added, temperature is raised to 80-140 DEG C, the temperature of the top of a fractional column is controlled to be not higher than 65 DEG C, generated methyl alcohol is fractionated, a fractional reaction is carried out for 5-10 h until no methyl alcohol is generated, and reactive flame retardant organic phosphonate is obtained through purification. The reactive flame-retardant organic phosphonate compound has good plasticity, good in macro-molecular compatibility, suitable for flame retardants of polyester PBT, polyurethane, epoxy resin, unsaturated resin and other materials, low in production cost, small in equipment investment and very good in application and development prospect, raw materials are easy to obtain, and large-scale production is easy.

Description

technical field [0001] The invention relates to a reactive flame retardant organic phosphonate compound and a preparation method thereof, in particular to a flame retardant 1-oxygen-1-methyl-4-ethyl-4-hydroxymethyl-2,6 - a dioxa-1-phosphorinane compound and a preparation method thereof, the compound can be used as a flame retardant for epoxy resin, unsaturated resin, polyurethane and other materials, and can also be used as a synthetic intermediate of organic phosphine. Background technique [0002] After entering the 21st century, polymer materials have been widely used in construction, electronic appliances, transportation and other fields, but their flammability poses a serious threat to people's lives and properties. According to the results of fire investigations in recent years, it is found that combustible polymer materials are one of the main sources of ignition for urban fires and building fires. People are always eager to use flame-retardant polymer materials to pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5357C07F9/6574C08L63/00
Inventor 王彦林李果
Owner SUZHOU UNIV OF SCI & TECH
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