Production technology of dimethyl phosphite

A dimethyl phosphite and production process technology, which is applied in the field of dimethyl phosphite production process, can solve the problems of limited production capacity, long production cycle, low utilization rate of equipment, etc., and achieve the improvement of purity and the reduction of temperature and time Effect

Inactive Publication Date: 2016-06-29
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of dimethyl phosphite is obtained by the direct reaction of methanol and phosphorus trichloride. The specific methods include: solvent reaction and solvent-free reaction. The specific methods include vapor-liquid reaction, vapor-vapor reaction, discontinuous method, continuous met...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] First, methanol and phosphorus trichloride are sprayed into the esterification reaction kettle slowly and oppositely in a mist form at the same time, and the molar ratio of the spraying amount is methanol: phosphorus trichloride=3:1, and at the same time, the upper half of the reaction kettle is filled Nitrogen, the reaction is exothermic, the condenser is used to condense, and the reaction temperature is controlled between 42°C by controlling the amount of methanol injected, and the solid in the esterification reactor after the reaction is completed is the crude dimethyl phosphite;

[0019] Secondly, the crude dimethyl phosphite in the neutralization tank is slowly sprayed into the mist of ammonia to neutralize, and the pH of the material in the neutralization tank is adjusted to 6.5, and the material in the neutralization tank is dimethyl phosphite and A mixture of ammonium chloride;

[0020] Thirdly, the materials in the neutralization tank are sent to the rectification t...

Embodiment 2

[0024] First, methanol and phosphorus trichloride are sprayed into the esterification reaction kettle slowly and oppositely in a mist form at the same time, and the molar ratio of the spraying amount is methanol: phosphorus trichloride=3:1, and at the same time, the upper half of the reaction kettle is filled Nitrogen, the reaction is exothermic, the condenser is used for condensation, and the reaction temperature is controlled to be between 43°C by controlling the amount of methanol injected, and the solid in the esterification reactor after the reaction is complete is the crude dimethyl phosphite;

[0025] Secondly, the crude dimethyl phosphite in the neutralization tank is slowly sprayed into the mist of ammonia for neutralization, and the pH of the material in the neutralization tank is adjusted to stop when the pH value is 7.0. The material in the neutralization tank is dimethyl phosphite and A mixture of ammonium chloride;

[0026] Thirdly, the materials in the neutralization...

Embodiment 3

[0030] First, methanol and phosphorus trichloride are sprayed into the esterification reaction kettle slowly and oppositely in a mist form at the same time, and the molar ratio of the spraying amount is methanol: phosphorus trichloride=3:1, and at the same time, the upper half of the reaction kettle is filled Nitrogen, the reaction is exothermic, the condenser is used for condensation, and the reaction temperature is controlled between 44°C by controlling the amount of methanol injected, and the solid in the esterification reactor after the reaction is complete is the crude dimethyl phosphite;

[0031] Secondly, the crude dimethyl phosphite in the neutralization tank is slowly sprayed into the mist of ammonia for neutralization, and the pH of the material in the neutralization tank is adjusted to stop when the pH value is 7.0. The material in the neutralization tank is dimethyl phosphite and A mixture of ammonium chloride;

[0032] Thirdly, the materials in the neutralization tank ...

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PUM

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Abstract

The invention provides a production process of dimethyl phosphite, and its preparation process is as follows: first, methanol and phosphorus trichloride are sprayed into the esterification reaction kettle slowly and relatively in the form of mist, and at the same time, the upper half of the reaction kettle is filled with Nitrogen, the reaction is exothermic, and the condenser is used to condense. After the reaction is completed, the solid in the esterification reactor is crude dimethyl phosphite; secondly, slowly spray the crude dimethyl phosphite in the neutralization tank into atomized ammonia For neutralization, the material in the neutralization tank is a mixture of dimethyl phosphite and ammonium chloride; the material in the neutralization tank is sent to the rectification tower for rectification, all of which are distilled out, and the remaining rectification residue of dimethyl phosphite liquid; finally, the rectification raffinate is filtered through molecular sieves, and then the rectification raffinate is rectified. The invention can improve the purity of dimethyl phosphite, so that the purity of dimethyl phosphite is 95.6%.

Description

Technical field [0001] The invention relates to the field of fine chemical production, in particular to a production process of dimethyl phosphite. Background technique [0002] Dimethyl phosphite, molecular formula is C2H7O3P, molecular weight is 110.05, appearance is colorless transparent liquid, slightly scented, boiling point is 170℃, relative density is 1.20, soluble in water, soluble in most organic solvents such as alcohol and ether. The preparation method of dimethyl phosphite is prepared by the direct reaction of methanol and phosphorus trichloride. The specific methods are: solvent reaction and solvent-free reaction. Specific methods include vapor-liquid reaction, vapor-vapor reaction, discontinuous method, continuous method, etc. Because the reaction is a violent exothermic reaction, the reaction speed is fast, it is completed in an instant, the discontinuous operation is frequent, the labor intensity is high, and the production cycle is long, the equipment utilization...

Claims

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Application Information

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IPC IPC(8): C07F9/142
CPCC07F9/142
Inventor 黄中桂徐占友段利滢余玉好
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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