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Method for preparing Anilofos by recycled ammonium thiophosphate salt from phosphorus-containing wastewater

A technology of phosphorothioate ammonium salt and saponin, which is applied in the field of chemical pesticide preparation to achieve the effects of cheap and easy-to-obtain raw materials, convenient operation, and easy industrial production

Inactive Publication Date: 2019-09-06
潍坊新绿化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] However, in the malathion production project, a large amount of phosphorus-containing wastewater will be produced. From a global perspective, phosphorus-containing wastewater has always been a problem in environmental protection. Therefore, there is an urgent need for a method to turn phosphorus-containing wastewater into fertilizer.

Method used

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  • Method for preparing Anilofos by recycled ammonium thiophosphate salt from phosphorus-containing wastewater
  • Method for preparing Anilofos by recycled ammonium thiophosphate salt from phosphorus-containing wastewater

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Embodiment 1

[0028] A method for preparing saponin by reclaiming phosphorothioate ammonium salt from phosphorus-containing wastewater, comprising the following steps:

[0029] (1) after the malathion synthetic reaction finishes, add the pure water of malathion process oil weight 10% in the malathion process oil, slowly add massfraction 25% ammoniacal liquor, temperature is controlled below 20 ℃, Ammonia water was added dropwise until the pH of the reaction system was 9, then the dropwise addition was completed, and after standing for 80 minutes, an aqueous methyl sulfide ammonium salt solution was obtained, which was filtered, extracted with toluene, dehydrated by a low-temperature evaporation system, and centrifuged in a centrifuge. , obtain the methyl sulfide ammonium salt solid, wherein the quality of the methyl sulfide ammonium salt solid obtained is as shown in Table 1:

[0030] project purity,% Moisture, % Methyl sulfide ammonium salt solid 96 1

[0031] (2) ...

Embodiment 2

[0036] A method for preparing saponin by reclaiming phosphorothioate ammonium salt from phosphorus-containing wastewater, comprising the following steps:

[0037] (1) after the synthetic reaction of malathion finishes, add the pure water of malathion process oil weight 10% in the malathion process oil, slowly add massfraction 25% ammoniacal liquor, temperature is controlled below 20 ℃, Ammonia water is added dropwise until the pH of the reaction system is 9, the dropwise addition is completed, and after standing for 100 minutes to separate layers, an aqueous solution of methyl sulfide ammonium salt is obtained, which is filtered, extracted with toluene, dehydrated by a low-temperature evaporation system, and centrifuged in a centrifuge. , obtain the methyl sulfide ammonium salt solid, wherein the quality of the methyl sulfide ammonium salt solid obtained is as shown in Table 2:

[0038] project purity,% Moisture, % Methyl sulfide ammonium salt solid 97 1 ...

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Abstract

The invention discloses a method for preparing Anilofos by recycled ammonium thiophosphate salt from phosphorus-containing wastewater, the method comprises the following operation steps: (1) after themalathion synthesis reaction is finished, quantitative pure water is added into malathion process oil, ammonia water is slowly dripped, and the mixture is left standing for layering to obtain methylsulfide ammonium salt solution; (2) adding p-chloronitrobenzene, acetone, catalyst and solvent methanol into a high-pressure reaction kettle in sequence, and introducing hydrogen to enable the internal pressure to reach 0.20-0.35 MPa; and (3) N-isopropyl p-chloroaniline and chloroacetyl chloride are reacted to generate an intermediate N-isopropyl-N-chloroacetyl p-chloroaniline, and finally N-isopropyl-N-chloroacetyl p-chloroaniline is subjected to solid reaction with methyl sulfide ammonium salt to finally prepare the Anilofos. The method for preparing the Anilofos by the recycled ammonium thiophosphate salt from the phosphorus-containing wastewater is simple to operate, and is green and environment-friendly, and the prepared intermediate of the ammonium thiophosphate salt can be completely used for synthesizing the Anilofos without affecting the quality of the final product.

Description

technical field [0001] The technical field of chemical pesticide preparation of the present invention particularly relates to a method for preparing saponin by reclaiming phosphorothioate ammonium salt from phosphorus-containing wastewater. Background technique [0002] Barnyard Phosphate, glyphosate, and Aminafos are three organophosphorus herbicides that are widely used in my country at present. Grass, Flutter Grass) and Carex. In the prior art, the synthetic route of saponin is mainly as follows: [0003] (1) generate intermediate (A) N-isopropyl p-chloroaniline by p-chloroaniline and 2-chloropropane reaction: [0004] [0005] (2) generate intermediate (B) N-isopropyl-N-chloroacetyl p-chloroaniline by intermediate (A) and chloroacetyl chloride reaction: [0006] [0007] (3) Finally, the intermediate (B) reacts with sulfurized phosphoric acid ester ammonium salt, and the product is saponin: [0008] [0009] However, in the malathion production project, a lar...

Claims

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Application Information

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IPC IPC(8): C07F9/165A01N57/14A01P13/00
CPCA01N57/14C07F9/165
Inventor 于登博田俊杰杜凯杨洪强姜东升
Owner 潍坊新绿化工有限公司
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