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Preparation method of 0-ethyl sodium phosphate

A technology of sodium ethyl phosphate and hypophosphorous acid, which is applied in the direction of phosphorus organic compounds, can solve the problems of insufficient stability of sodium 0-ethyl phosphate, excessive impurities, difficulty in meeting international market demand, etc., and is suitable for large-scale promotion, The effect of fast reaction speed and high product yield

Inactive Publication Date: 2017-11-24
ZHEJIANG JIAHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above is a relatively mature preparation process, but the content of the prepared sodium 0-ethylphosphate is not stable enough, and the impurities contained exceed the standard, which is difficult to meet the needs of the international market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In the embodiment of the present invention, a preparation method of sodium O-ethylphosphate comprises the following steps:

[0029] 1) Mix hypophosphorous acid and sodium hydroxide solution, wherein the concentration of sodium hydroxide solution is 2mol / L, the molar ratio of hypophosphorous acid and sodium hydroxide is 1.1:1, then heat and stir at 42°C for 35min, the stirring speed Be 250r / min, make mixture A;

[0030] 2) Ethanol and dimethyl sulfone were mixed and stirred evenly at a stirring speed of 150 r / min to prepare mixture B; the mass ratio of ethanol to dimethyl sulfone was 45:1, and the molar ratio of ethanol to hypophosphorous acid was 4:1. Under the condition of decompression to 200Pa, the steam generated by heating the mixture B and the steam generated by the mixture A were mixed and reacted for 35 minutes, and the collected product was vacuum treated at 50°C for 40 minutes to obtain 0-ethyl sodium phosphate.

[0031] After testing, the content of sodium O...

Embodiment 2

[0033] In the embodiment of the present invention, a preparation method of sodium O-ethylphosphate comprises the following steps:

[0034] 1) Mix hypophosphorous acid and sodium hydroxide solution, wherein the concentration of sodium hydroxide solution is 4mol / L, the molar ratio of hypophosphorous acid and sodium hydroxide is 1.2:1, then heat and stir at 45°C for 40min, the stirring speed Be 300r / min, make mixture A;

[0035] 2) Ethanol and dimethyl sulfone were mixed and stirred evenly at a stirring speed of 200 r / min to prepare mixture B; the mass ratio of ethanol to dimethyl sulfone was 50:1, and the molar ratio of ethanol to hypophosphorous acid was 6:1. Under the condition of decompression to 300Pa, the steam generated by heating the mixture B and the steam generated by the mixture A were mixed and reacted for 50 minutes, and the collected product was vacuum treated at 55°C for 60 minutes to obtain 0-ethyl sodium phosphate.

[0036] After testing, the content of sodium O...

Embodiment 3

[0038] In the embodiment of the present invention, a preparation method of sodium O-ethylphosphate comprises the following steps:

[0039] 1) Mix hypophosphorous acid and sodium hydroxide solution, wherein the concentration of sodium hydroxide solution is 3mol / L, the molar ratio of hypophosphorous acid and sodium hydroxide is 1.1:1, then heat and stir at 44°C for 38min, the stirring speed Be 280r / min, make mixture A;

[0040] 2) Ethanol and dimethyl sulfone were mixed and stirred evenly at a stirring speed of 180 r / min to prepare mixture B; the mass ratio of ethanol to dimethyl sulfone was 48:1, and the molar ratio of ethanol to hypophosphorous acid was 5:1. Under the condition of decompression to 200Pa, the steam generated by heating the mixture B and the steam generated by the mixture A were mixed and reacted for 40 minutes, and the collected product was vacuum treated at a temperature of 52°C for 50 minutes to obtain 0-ethyl sodium phosphate.

[0041] After testing, the co...

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Abstract

The invention discloses a preparation method of 0-ethyl sodium phosphate. The preparation method comprises the following steps: mixing hypophosphorous acid with a sodium hydroxide solution with the concentration of 2-4 mol / L, and then performing heating and stirring for 35-40 min at the temperature of 42-45 DEG C to obtain a mixture A, wherein the molar ratio of hypophosphorous acid to a sodium hydroxide solution is (1.1-1.2):1; mixing ethyl alcohol with dimethyl sulfone, and performing uniform stirring to prepare a mixture B; and under the reduced-pressure condition, enabling a mixing reaction between steam generated by heating the mixture B and the mixture A to obtain 0-ethyl sodium phosphate. Hypophosphorous acid reacts with the sodium hydroxide solution; in the situation that a bit of hypophosphorous acid is remained, a gas-phase reaction is performed between hypophosphorous acid and the mixture of ethyl alcohol and dimethyl sulfone to realize synthesis of 0-ethyl sodium phosphate; dimethyl sulfone serves as a catalyst; the reaction speed and the product yield are high; the content of 0-ethyl sodium phosphate is 92% or above in the refining process; and the preparation method is simple, easy to operate, short in time and suitable for large-scale popularization.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of sodium O-ethylphosphate. Background technique [0002] 0-Sodium ethyl phosphate product structure The main use of 0-ethyl sodium phosphate is to produce agricultural fungicides. [0003] Existing O-ethyl sodium phosphate is mainly obtained through the esterification reaction of phosphorus trichloride and ethanol, the saponification reaction of diethyl phosphite and sodium hydroxide, and concentrated crystallization. Wherein the reaction equation of esterification reaction and saponification reaction is as follows: [0004] 1. Esterification reaction: [0005] Main reaction: PCl 3 +3C2H5OH→(C 2 h 5 ) 2 POH+C 2 h 5 Cl+2HCl [0006] Side reaction: PCl 3 +3C 2 h 5 OH→3C 2 h 5 Cl+2H 3 PO 3 [0007] 2. Saponification reaction: [0008] Main response: [0009] Side reaction: HCl+NaOH→NaCl+H 2 O. [0010] Concentrated crystalliz...

Claims

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Application Information

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IPC IPC(8): C07F9/06
CPCC07F9/06
Inventor 周少华徐俊平江晓飞胡菁许康林范素珍范莲生
Owner ZHEJIANG JIAHUA CHEM