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
4 Cites 10 Cited by

AI-Extracted Technical Summary

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...
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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.

Application Domain

Technology Topic

Protic solventHypophosphorous acid +4

Image

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

Examples

  • Experimental program(7)

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 kg of HPPA wet product with a solid content of 85%. The HPLC (normalization method) analysis product purity was 99.2%, and the OPP content was 0.2-1.5%.
[0019] (2). Preparation of HCA
[0020] 300 kilograms of above-mentioned HPPA wet products, 150 kilograms of methanol and 1.5 kilograms of BHT are dropped into the reactor, stirred and heated to 70-100 ℃, carry out atmospheric distillation for 1-2 hours, then be warming up to between 110-130 ℃ and carry out underpressure distillation (The pressure is kept below -0.095Mpa), and it is steamed until there is no fraction (about 0.5 hours). Introduce nitrogen to normal pressure, between 100-130 ℃, discharge to drier, solidify to obtain 255 kg of white flakes, HPLC (normalization method) analysis (the same below) product purity: 99.0%, yield 94.0 %% (calculated in OPP). Melting point: 118-119℃, OPP content 0.02%, chloride ion content 35ppm.
[0021] The product structure has been confirmed as HCA by NMR verification, and the NMR data are as follows:
[0022] 1 H NMR (CDCl 3 , 300MHz)δ9.050, 7.074(s, P-H), 7.29(d, J=8.4Hz, 1H), 7.29(t, J=8.4Hz, 1H), 7.41(td, J=8.4Hz, 0.9Hz, 1H), 7.55(td, J=7.8Hz, 3.0Hz, 1H), 7.75(t, J=7.8Hz, 1H), 7.92(ddd, J=13.2Hz, 7.8Hz, 0.9Hz, 1H), 7.96( d, J=8.4Hz, 1H), 7.98 (d, J=8.4Hz, 1H).
[0023] The melting point of HCA was determined with a Pekin-Elmer DSC-7 thermal analyzer, the heating rate was 20°C/min, and the DSC curve had only one absorption peak at 119°C.

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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PUM

PropertyMeasurementUnit
Melting point118.0 ~ 119.0°C
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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