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Preparation method of alkyl phosphonic acid diaryl ester

A technology of diaryl alkyl phosphonate and dialkyl alkyl phosphonate, which is applied in the field of preparation of diaryl alkyl phosphonate, can solve problems such as difficult industrial preparation and influence on product color, and achieve The effect of complete reaction, strong catalytic activity, and avoiding waste of raw materials

Pending Publication Date: 2022-02-11
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method also uses methyl iodide as a catalyst, and requires a rectification column to purify the product. Diphenyl methylphosphonate is easy to decompose during the rectification process, and it is difficult to carry out industrial preparation.
[0005] Chinese patent CN101031578A uses sodium iodide as a catalyst, triphenyl phosphite and dimethyl methyl phosphonate undergo an isomerization reaction after transesterification, and nuclear magnetic analysis during the reaction shows that it contains 88% diphenyl methyl phosphonate At the same time, about 6% of phenol by-products and about 3% of triphenyl phosphate by-products will be produced; and after the reaction, sodium iodide is dissolved in the product, and the color of the final product is slightly red, and the color number is greater than 100. This may be because sodium iodide generates transition state substances during the reaction process, and redox reactions occur, thereby affecting the color of the product

Method used

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  • Preparation method of alkyl phosphonic acid diaryl ester
  • Preparation method of alkyl phosphonic acid diaryl ester
  • Preparation method of alkyl phosphonic acid diaryl ester

Examples

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preparation example Construction

[0022] The present invention provides a method of preparing an alkylphosphonic acid diaryl ester, comprising the steps of:

[0023] In the protective atmosphere, the phosphite triaryl ester is mixed with the alkylphosphonic acid dialkyl ester to obtain an isomerization reaction product system by mixing the phosphite.

[0024] The isomerization reaction product system was first reduced pressure distillation, and the residual system was mixed with an inert orprotic solvent, and the resulting liquid material was sequentially washed, water washing and second pressure reduction distillation to obtain an alkane Narphonic acid diaryl ester.

[0025] In the protective atmosphere, the phosphite triaryl ester is mixed with the alkylphosphonic acid dialkyl ester in the protective atmosphere to obtain an isomerization reaction product system. The present invention is not particularly limited to providing the protective gas of the protective atmosphere, and is specifically, such as nitrogen. I...

Embodiment 1

[0040] Diphenyl methylphosphonic acid, including the steps of:

[0041] (1) Tutinyl phosphite (620 kg, 2 kmol) and the catalyst absorbed until the nickel (1.29% of the mass of triphenyl ester of phosphite) were added to the reactor, and the nitrogen protection was raised to 180 ~ 200 ° C, then Methyl phosphomethane (273 kg, 2.2 kmol) of methylphosphonic acid (273 kg, 2.2 kmol) was slowly added dropwise, and the dropwise addition was 2 h. After the dropwise addition was completed, the liquid chromatographic monitor reaction progression, the phosphite triphenyl reaction was completely The reaction was stopped to obtain a product system; data using liquid chromatography during the reaction as shown in Table 1, the content of each substance in Table 1 is a mass content:

[0042] Table 1 Monitoring data using liquid chromatography

[0043]

[0044] (2) The product system is lowered to 70 to 80 ° C, and the first decompression distillation is carried out under a vacuum degree of 3 to ...

Embodiment 2

[0051] As in Example 1, the difference is only that the reaction temperature is 200 to 210 ° C; the final prepared target product was 95%, the phenol content was 180 ppm, the acid value was 0.16 mg KOH / g.

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Abstract

The invention provides a preparation method of alkyl phosphonic acid diaryl ester, and belongs to the technical field of organic synthesis. The preparation method of alkyl diaryl phosphonate provided by the invention comprises the following steps: in a protective atmosphere, taking Raney nickel as a catalyst, mixing phosphorous acid triaryl ester and alkyl dialkyl phosphonate, and carrying out isomerization reaction to obtain an isomerization reaction product system; and carrying out first reduced pressure distillation on the isomerization reaction product system, mixing the residual system with an inert aprotic solvent, carrying out solid-liquid separation, and sequentially carrying out alkali washing, water washing and second reduced pressure distillation on the obtained liquid material to obtain alkyl diaryl phosphonate. According to the invention, raney nickel is used as a catalyst, and meanwhile, a target product with high yield and high purity can be obtained through a proper post-treatment method; and the method provided by the invention is good in stability and suitable for industrial production.

Description

Technical field [0001] The present invention relates to the field of organic synthesis, and more particularly to a method of preparing an alkylphosphonic acid dirylates. Background technique [0002] The alkylphosphonic acid diaryl ester and its derivative are widely used as a flame retardant in an epoxy resin electrical circuit board, and there are many preparation processes of the alkylphosphonic acid dirylates, but there is generally existed during industrial application. some problems. [0003] As disclosed in U.S. Patent No. 4,377,537, the methylphosphinate diphenyl ester is prepared by reaction of phosphite and methanol in the presence of a catalytic amount of iodide, and the phenol by-product is easily generated during the reaction. % Or so, while also generating very unstable diphenyl hydrophane phosphrates, it is necessary to remove the two by more complex post-treatment methods; and iodide is a volatile substance having high toxicity, endanger human Good health, polluti...

Claims

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Application Information

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IPC IPC(8): C07F9/40
CPCC07F9/4084
Inventor 王秋伟方剑金译艇冯舜黄江
Owner ZHEJIANG WANSHENG
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