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Method for purifying 2'-hydroxy biphenyl-2-phosphinic acid

A technology of hydroxybiphenyl and purification method, which is applied in the purification field of increasing the main content of 2'-hydroxybiphenyl-2-phosphinic acid, and achieves the effects of safe and simple operation, increased main content and stable product quality

Inactive Publication Date: 2011-05-04
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the existing preparation technology, due to the influence of materials and water quality, the main content of 2'-hydroxybiphenyl-2-phosphinic acid products is only about 92%. If the content of 2'-hydroxybiphenyl-2 - The content of DOPO metal ions prepared by phosphinic acid as an intermediate cannot meet the needs of current applications

Method used

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  • Method for purifying 2'-hydroxy biphenyl-2-phosphinic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In the reactor with heater, stirrer, thermometer, add 300g 15wt% 2'-hydroxybiphenyl-2-phosphinic acid aqueous solution, drip 55ml 15wt% sodium hydroxide solution under stirring at 20-25 ℃, Stir for 15 minutes, use the Lei Magnetic pHS-3C precision pH meter to control the pH value of the final solution to 9.5-10.0, add 2g of activated carbon (200 mesh), and control the temperature at 25-30°C for 2 hours, and filter while it is hot to obtain 43.5 g of purified product, yield 96.67%.

[0020] 2'-Hydroxybiphenyl-2-phosphinic acid HPLC analysis results:

[0021] The purity of 2'-hydroxybiphenyl-2-phosphinic acid before purification is 92.15%, and the content of the starting materials and other impurities for the synthesis of 2'-hydroxybiphenyl-2-phosphinic acid accounted for 3.53% of the total mass respectively % and 4.02%;

[0022] The purity of 2'-hydroxybiphenyl-2-phosphinic acid after purification is 97.50%, and the content of the starting materials and other impuritie...

Embodiment 2

[0025] Add 300g of 15wt% 2'-hydroxybiphenyl-2-phosphinic acid aqueous solution into the reactor with heater, stirrer and thermometer, and after stirring for 1 hour at 20-25°C, add 56ml of 32wt% hydrogen Sodium oxide solution, stirred for 25 minutes, controlled the pH value of the final solution to 10.0-10.5 with a Lei Magnetic pHS-3C precision pH meter, added 2.5g of activated carbon (specification 150 mesh), controlled the temperature at 25-30°C and stirred for 2.5 hours, Filtration while hot gave 43.0 g of purified product with a yield of 95.56%.

[0026] 2'-Hydroxybiphenyl-2-phosphinic acid HPLC analysis results:

[0027] The purity of 2'-hydroxybiphenyl-2-phosphinic acid before purification is 92.44%, and the content of starting materials and other impurities for the synthesis of 2'-hydroxybiphenyl-2-phosphinic acid account for 3.07% of the total mass respectively and 4.37%;

[0028] After purification, the purity of 2'-hydroxybiphenyl-2-phosphinic acid is 97.85%, and th...

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Abstract

The present invention discloses a purification method for 2'-dihydroxybiphenyl-2-phosphine, in which the water solution of 2'-dihydroxybiphenyl-2-phosphine is adopted as the raw material, which undergoes the reaction under the presence of an alkali solution, then decoloration is performed with active carbon, and then the purified 2'-dihydroxybiphenyl-2-phosphine is obtained, with the yield rate of 95 to 97 percent and the content of the intended final product more than 97.5 percent. Compared with the technique in the prior art, the present invention efficiently raises the content of 2'-dihydroxybiphenyl-2-phosphine as the intended products and has simple and safe operation with stable quality of the products, thereby being suitable for industrialized production. 2'-dihydroxybiphenyl-2-phosphine produced by the present invention can be adopted as raw material, which may undergo acidification and cyclation to prepare the flame retardant of 9.10-bihydro-9-oxo-10- phosphaphenantbrene (DOPO) with the purification degree (HPLC) above 99.5 percent and the content of individual metal ions below 10 ppm.

Description

technical field [0001] The invention relates to a purification method of 2'-hydroxybiphenyl-2-phosphinic acid, in particular to a purification method for increasing the main content of 2'-hydroxybiphenyl-2-phosphinic acid. Background technique [0002] 2'-Hydroxybiphenyl-2-phosphinic acid is an important intermediate in organic synthesis. It can be used as an intermediate of plastics for electronic equipment, circuit boards, semiconductor packaging materials, photosensitive materials and luminescent materials, etc., and can be used in the preparation of polymer materials such as polyester, polyphenylene ether, ABS, PS and phenolic resin. have a wide range of applications, [0003] Its structural formula is as follows: [0004] [0005] In the prior art, o-phenylphenol and phosphorus trichloride are used as raw materials, and Lewis acid is used as a catalyst to obtain 9,10-dihydro-9-chloro-10-phosphaphenanthrene through esterification and Friedel-Crafts acylation. After...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/32
Inventor 顾小焱蒋旭亮
Owner SHANGHAI CHEM REAGENT RES INST