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Synthetic method for thiophosphate

A synthetic method, a technology of phosphorothioate, which is applied in the field of intermediate preparation and can solve problems such as low reaction yield

Inactive Publication Date: 2014-12-10
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the content of ammonium salt in its waste water is still as high as 3%, and the reaction yield is only 88%-90%

Method used

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  • Synthetic method for thiophosphate
  • Synthetic method for thiophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 100g of ammonium thiophosphate salt with a mass fraction of 52%, was added with 49.3g of methyl chloroacetate at a molar ratio of 1:1.5, and the reaction temperature was controlled at 60°C. After 2.0 hours of reaction, 80.3g of the oil phase and 68g of the water phase were separated. The ammonium sulfate phosphate content in the waste water is 3.8%. The oil phase was vacuum distilled to separate methyl chloroacetate, and the mass fraction of phosphorothioate was 89.8%, and the yield of phosphorothioate was 90.4%.

Embodiment 2

[0033] 100g of sodium thiophosphate with a mass fraction of 50%, 61.5g of methyl chloroacetate was added at a molar ratio of 1:2.0, the reaction temperature was controlled at 58°C, and the reaction was carried out for 2.5 hours to separate 90.2g of the oil phase and 70.3g of the water phase , the sodium phosphoric acid sulfur content in the waste water is 2.9%. The oil phase was vacuum distilled to separate methyl chloroacetate to obtain a mass fraction of phosphorothioate of 90.1%, and a yield of phosphorothioate of 91.3%.

Embodiment 3

[0035] Get 68g of the water phase after the reaction in Example 1, add 49.3g of methyl chloroacetate in the first step, control the reaction temperature to be 60°C, and react for 60 minutes to separate 51.5g of the methyl chloroacetate phase, and the sulfur in the waste water The content of ammonium phosphate is 1.1%, and it will be discharged after wastewater treatment. In the second step, 51.5 g of the methyl chloroacetate phase obtained in the first step is added to 100 g of 52% ammonium sulfuric acid phosphate, the controlled reaction temperature is 58 ° C, and the reaction time is 80 minutes. 82.4g of the oil phase, and the water phase is recycled for the next reaction. The oil phase is distilled at a temperature lower than 115°C and the vacuum degree is higher than 0.095Mpa to separate methyl chloroacetate by distillation to obtain phosphorothioate. The reaction was repeated ten times to obtain an average mass fraction of phosphorothioate of 90.4%, and an average yield ...

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Abstract

The invention discloses a synthetic method for thiophosphate. The synthetic method comprises the following steps: after taking thiophosphate aqueous liquor and methyl chloroacetate as raw materials to carry out primary reaction on thiophosphate and methyl chloroacetate, separating to obtain an oil phase and a water phase, carrying out continuous cyclic synthesis by virtue of the following two-step reaction: a first step, namely adding methyl chloroacetate into a water phase, reacting, and after reacting, separating to obtain oil phase of thiophosphate-containing methyl chloroacetate and water phase capable of being subjected to posttreatment and exhausted, and a second step, namely adding thiophosphate aqueous liquor into the oil phase of thiophosphate-containing methyl chloroacetate to react, and after the reacting, separating to obtain the oil phase containing thiophosphate and excessive methyl chloroacetate and the water phase, wherein methyl chloroacetate is separated from the oil phase containing thiophosphate and excessive methyl chloroacetate by virtue of distillation to obtain the thiophosphate, and circulating the water phase to the first step. The synthetic method is high in yield, short in synthesis time and low in cost, capable of effectively utilizing various raw materials and products and lowering the content of the thiophosphate in wastewater, and environmentally friendly.

Description

technical field [0001] The invention belongs to the field of intermediate preparation, and in particular relates to a synthesis method of phosphorothioate. Background technique [0002] Dimethoate is an excellent organic phosphorus insecticide and acaricide with high efficiency, low toxicity, low residue and systemic property. It was created in Italy in the early 1950s and was successfully trial-produced by Beijing Agricultural University in China. Pesticide factory introduces trial production, because its raw material is easy to get, and drug effect is good, and cost is low, still has extensive market prospect at present, and thionate is as the important intermediate of dimethoate synthesis, and its quality has directly determined dimethoate quality and yield. [0003] At present, the synthetic method of phosphorothioate mainly utilizes ammonium phosphate phosphoric acid or sodium salt to react with methyl chloroacetate, and its reaction principle is as follows: [0004] ...

Claims

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Application Information

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IPC IPC(8): C07F9/17
Inventor 艾秋红文敬滨罗和安袁峰游奎一刘平乐黄荣辉
Owner XIANGTAN UNIV
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