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The preparation method of 2-ethyl methacrylate base benzyl phosphate

A technology of ethyl methacrylate-based benzyl phosphate and ethyl methacrylate-based dichlorophosphate, which is applied in the field of flame retardants, can solve the problems of high toxicity and low yield, and achieve improved purity and reduced Effects of production cost and shortened production time

Active Publication Date: 2015-09-02
ZHANGJIAGANG DONGDA IND TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is: to overcome the shortcomings of low yield and high toxicity of the existing technology, and to provide a preparation method for 2-ethyl methacrylate benzyl phosphate

Method used

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  • The preparation method of 2-ethyl methacrylate base benzyl phosphate
  • The preparation method of 2-ethyl methacrylate base benzyl phosphate
  • The preparation method of 2-ethyl methacrylate base benzyl phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Dissolve 118g of hydroxyethyl methacrylate, 142g of phosphorus oxychloride, and 154g of DIEA in a three-necked flask added with 378g of acetone, and stir the reaction at 0-10°C for 2h; add 284g of benzyl alcohol and 286g of DIEA dropwise, The reaction was vigorously stirred for 2.5 h; left to stand overnight, filtered with suction, and the filtrate (clear) was rotary evaporated to remove the solvent to obtain a crude product. The yield of the product was 92% as measured by liquid phase mass spectrometry.

Embodiment 2

[0023] Dissolve 177g of hydroxyethyl methacrylate, 230g of phosphorus oxychloride, and 248g of DIEA in a three-necked flask with 585g of acetone, and stir for 2 hours at 0-10°C; add 461g of benzyl alcohol and 548g of DIEA dropwise, The reaction was vigorously stirred for 2.5 h; left to stand overnight, filtered with suction, and the filtrate (clear) was rotary evaporated to remove the solvent to obtain a crude product. The yield of the product was 93.1% as determined by liquid phase mass spectrometry.

Embodiment 3

[0025] Dissolve 270g of hydroxyethyl methacrylate, 378g of phosphorus oxychloride, and 386g of DIEA in a three-necked flask added with 950g of acetone, and stir at 0-10°C for 2 hours; add 648g of benzyl alcohol and 681g of DIEA dropwise, The reaction was vigorously stirred for 2.5 h; left to stand overnight, suction filtered, and the filtrate (clear) was rotovapped to remove the solvent to obtain a crude product. The yield of the product was 93.4% as determined by liquid phase mass spectrometry.

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Abstract

The invention discloses a preparation method of 2-ethyl methacrylate benzyl phosphate. The method includes taking hydroxyethyl methylacrylate (HEMA) and phosphorus oxychloride as raw materials, taking N,N-diisopropylethylamine (DIEA) as a deacid reagent and acetone as a solvent to perform an ester condensation reaction to obtain 2-ethyl methacrylate dichlorophosphate; and subjecting the 2-ethyl methacrylate dichlorophosphate and benzyl alcohol to alcoholysis under actions of DIEA and acetone to obtain the 2-ethyl methacrylate benzyl phosphate. According to the method, the N,N-diisopropylethylamine (DIEA) serves as the deacid reagent, the nucleophilicity is lower than that of triethylamine, side reactions are few, impurities in a product are few, the purity reaches above 98%, and a following purification step is reduced.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a preparation method of 2-ethyl methacrylate benzyl phosphate. Background technique [0002] According to statistics, about half of all fires are caused by textiles. For this reason, developed countries have formulated flame-retardant standards and fire regulations for various textiles as early as the 1960s, clearly stipulating that in some specific places, children's clothing Textiles used in toys, toys, etc. must be treated with flame retardant. In 1995, the Ministry of Construction and the Fire Department of the Ministry of Public Security issued a series of regulations such as the "Code for Fire Protection Design of Building Interior Decoration" in 1995. Railways, aviation, automobiles, ships, etc. have all formulated detailed flame-retardant requirements for flame-retardant materials and decorative fabrics. [0003] At present, the three commonly used flame retard...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/08
Inventor 顾丰平
Owner ZHANGJIAGANG DONGDA IND TECH RES INST
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