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 Co

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0015] Example 1: Intramolecular dehydration and ring closure of methanol as solvent to synthesize HCA

[0016]

[0017] (1). Preparation of HPPA

[0018] 1400 kilograms of OPP, 1200 kilograms of phosphorus trichloride, 25 kilograms of zinc chloride are added in 5000 liters of reaction kettles, slowly be warming up to 70 ℃ of refluxes, then gradually be warming up to 120-165 ℃, maintain reaction 10-30 hours, the reaction solution by Colorless to orange is the end point of the reaction. After the reaction was completed, the temperature was lowered to 60-100° C., and 1600 kg of toluene was added to dissolve the generated DOP-Cl. The insolubles were removed by filtration. 400 kg of water was added dropwise to the filtrate for hydrolysis, and the hydrolysis reaction was carried out at 30-80° C. and completed in about 2 hours. After the reaction was completed, the material was lowered to 25° C., crystallization was precipitated, and centrifugation was performed to obtain 1967...

Example Embodiment

[0024] Example 2 Ethanol is used as solvent to synthesize HCA by intramolecular dehydration and ring closure

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

Example Embodiment

[0026] Example 3 Intramolecular dehydration and ring closure of water as solvent to synthesize HCA

[0027] Feeding and operation steps are the same as Example 1, and the solvent is replaced with 150 kg of water. 255 kg of white flakes were obtained, purity: 99.2%, yield 94.0%. Melting point: 118-119℃, 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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