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Prepn process of cyclic phosphonate compound

A technology for cyclic phosphonates and compounds, which is applied in the field of preparation of cyclic phosphonate compounds, can solve the problems of oxide organic phosphoric acid impurities, increase production costs, uneven heating of materials, etc., achieves fast reaction speed and simplifies processes Difficulty, good product quality

Inactive Publication Date: 2007-12-19
SHENYANG RES INST OF CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the preparation method reported in the above patent, the wet product of HPPA is directly heated at high temperature to dehydrate and close the loop to form HCA. This method has low thermal efficiency, uneven local heating of the material, and easy formation of oxide organic phosphate impurities, so that HCA can be used in semiconductor sealing materials and other applications. many problems
In response to this problem, in 2002, Sanko Corporation of Japan proposed an improved method for the synthesis of high-purity and high-quality organic cyclic phosphonic acid by intramolecular dehydration and ring closure in JP2002167393, but it still requires direct heating of HPPA for dehydration and closure of the ring, requiring the use of electrical The special equipment of the furnace dryer and the dehydration time is too long, which increases the production cost of the product

Method used

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  • Prepn process of cyclic phosphonate compound
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  • Prepn process of cyclic phosphonate compound

Examples

Experimental program
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Effect test

example 1

[0015] Example 1 Methanol is used as solvent intramolecular dehydration ring-closing to synthesize HCA

[0016]

[0017] (1). Preparation of HPPA

[0018] Add 1400 kg of OPP, 1200 kg of phosphorus trichloride, and 25 kg of zinc chloride into a 5000-liter reactor, slowly raise the temperature to 70°C for reflux, then gradually raise the temperature to 120-165°C, and maintain the reaction for 10-30 hours. Colorless to orange is the end of the reaction. After the reaction, the temperature was lowered to 60-100° C., and 1600 kg of toluene was added to dissolve the generated DOP-Cl. The insoluble matter was removed by filtration. Add 400 kg of water dropwise to the filtrate for hydrolysis, the hydrolysis reaction is carried out between 30-80°C, and it takes about 2 hours to complete. After the reaction, the material was down to 25° C., crystallized, and centrifuged to obtain 1967 kg of HPPA wet product with a solid content of 85%. The HPLC (normalization method) analysis prod...

example 2

[0024] Example 2 ethanol as solvent intramolecular dehydration ring-closure synthesis of HCA

[0025] Feeding and operating steps are the same as example 1, and the solvent is replaced with 150 kilograms of ethanol. Obtain 254 kg of white flake product, purity: 99.1%, yield 93.6%. Melting point: 118-119°C, OPP content 0.03%, chloride ion content 30ppm.

example 3

[0026] Example 3 water as solvent intramolecular dehydration ring-closing synthesis of HCA

[0027] Feeding and operation steps are the same as example 1, and solvent is replaced with 150 kilograms of water. 255 kg of white flakes were obtained with a purity of 99.2% and a yield of 94.0%. Melting point: 118-119°C, OPP content 0.01%, chloride ion content 30ppm.

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Abstract

The present invention discloses preparation process of cyclic phosphonate compound. The preparation process includes intramolecular dewatering and ring closing reaction of substituted or un-substituted 2-hydroxybiphenyl-2-hypophosphorous acid in polar protic solvent. The preparation process of the present invention has fast reaction, short production period, simplified reaction, high product quality and other advantages.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of cyclic phosphonate compounds. Background technique [0002] There have been many reports on the preparation methods of cyclic phosphonate compounds. Such compounds such as 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (HCA for short) are widely used in polymer products as an excellent flame retardant. Among them, US3702878 first reported the synthesis of HCA series novel cyclic phosphonate compounds. Reported in JP10001490 by the intramolecular dehydration ring-closing method of phosphonic acid compound: The hydrolysis reaction is carried out in solvents such as toluene or chlorobenzene to obtain the compound 2-hydroxybiphenyl-2-phosphinic acid (HPPA for short), and the wet product of HPPA is directly heated and dehydrated to form HCA. US6,291,626 also adopts the method of directly heating HPPA and dehydrating under reduced pressure, wh...

Claims

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Application Information

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IPC IPC(8): C07F9/6571C09K21/12
Inventor 张彦英何虹祥徐龙鹤
Owner SHENYANG RES INST OF CHEM IND
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