Method for preparing diisopropyl phosphite

A technology of diisopropyl phosphite and isopropanol, which is applied in the field of phosphite preparation, can solve the problems of weakening the decomposition effect of hydrogen chloride on phosphate ester, high equipment cost, and cumbersome operation, so as to reduce the amount of dissolution and production cost Low, reduce the effect of side effects

Active Publication Date: 2008-08-27
太仓市茜泾化工有限公司
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Problems solved by technology

[0004] The Chinese invention patent with the patent number "02146607.6" discloses a method for preparing phosphite, which uses a mixed solution composed of a weak acid salt of ammonium and phosphite to react the reaction system during the esterification reaction. Cooling is carried out to weaken the decomposition of hydrogen chloride to phosphate, and ammonia gas deacidification is used to ensure the yield of phosphite, and diisopropyl phosphite is prepared by this method, using weak acid salt of ammonium and phosphite The premise of cooling the reaction system by the mixed liquid formed is first to obtain phosphite by other methods, which undoubtedly brings about cost increase and complicated operation. In addition, the use of ammonia gas for deacidification, although the yield can be guaranteed to a certain extent, But the equipment cost is higher

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Embodiment Construction

[0020] The specific embodiment of the present invention is described below:

[0021] According to the preparation method of the diisopropyl phosphite of the present embodiment comprises the steps successively:

[0022] (1), 360kg of benzene is put into a 1000L batching kettle, the jacket is turned on to freeze, and 200kg of phosphorus trichloride is slowly drawn in at a controlled temperature of 7-9°C to form the first mixed solution, which is drawn into a high position for use.

[0023] (2) Put 360kg of benzene, 240kg of isopropanol and 404kg of triethylamine into a 2000L reactor to form a second mixed liquid, cool the second mixed liquid to 7-10°C, and slowly mix the first mixed liquid at this temperature The solution was added, and the dripping was completed in three hours. After dripping, keep the reaction system at this temperature for 1 hour; then slowly raise the temperature to 20-30°C for 2 hours, (the temperature rise must be slow, the temperature rises in proportion...

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Abstract

The invention relates to a method for preparing diisopropyl phosphate via the esterification of phosphorus trichloride and isopropanol, which comprises adding phosphorus trichloride into benzene solvent to form a first mixture, adding benzene, isopropanol and weak alkaline organic catalyst into a reactor to form a second mixture, slowly adding the first mixture into the second mixture to form a reaction system, increasing and controlling temperature, reacting for 4.5-9h to obtain the mixture containing diisopropyl phosphate, deacidifying the mixture via pure alkali, filtering, distilling, depressurizing and distilling to obtain final diisopropyl phosphate product. The preparation method has low cost and high yield.

Description

technical field [0001] The invention relates to a preparation method of phosphite. Background technique [0002] Both phosphite and phosphate are intermediates for the preparation of organophosphorus pesticides. At present, when preparing (phosphite) esters, phosphorus trichloride, phosphorus oxychloride or phosphorus thionium chloride are generally used for esterification reaction with alcohols (such as methanol, ethanol) or phenols (such as phenol), and the reaction releases hydrogen chloride. And other chlorides; the mixture containing liquid hydrogen chloride and crude ester generated by the reaction is deacidified (that is, the mixture flows into the deacidification tank after being cooled by the condenser, and is heated and deacidified) to obtain the crude (phosphite) ester . The crude product is subjected to fractional distillation under reduced pressure to obtain the corresponding pure (phosphite) ester. In this preparation method, because the esterification react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/142
Inventor 秦正浩
Owner 太仓市茜泾化工有限公司
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