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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  • Abstract
  • Description
  • Claims
  • Application Information

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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

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

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Example Embodiment

[0027] Example 1

[0028] A method for preparing sarcophos by recovering phosphorothioate ammonium salt from phosphorous wastewater, including the following operation steps:

[0029] (1) After the malathion synthesis reaction is over, add 10% pure water by weight of malathion process oil to the malathion process oil, slowly add 25% mass fraction of ammonia water dropwise, and the temperature is controlled below 20°C. Ammonia was dripped into the reaction system when the pH was 9, then the dripping was ended. After standing for 80 minutes, the aqueous solution of methyl sulfide ammonium salt was obtained, which was filtered, extracted with toluene, dehydrated by a low-temperature evaporation system, and centrifuged. , The methyl sulfide ammonium salt solid is obtained, and the quality of the obtained methyl sulfide ammonium salt solid is shown in Table 1:

[0030] project purity,% Moisture,% Methyl sulfide ammonium salt solid961

[0031] (2) In the autoclave, add p-chloronitroben...

Example Embodiment

[0035] Example 2

[0036] A method for preparing sarcophos by recovering phosphorothioate ammonium salt from phosphorous wastewater, including the following operation steps:

[0037] (1) After the malathion synthesis reaction is over, add 10% pure water by weight of malathion process oil to the malathion process oil, slowly add 25% mass fraction of ammonia water dropwise, and the temperature is controlled below 20°C. Ammonia was dripped into the reaction system when the pH was 9, then the dripping was finished. After standing for 100 minutes, the aqueous solution of methyl sulfide ammonium salt was obtained, which was filtered, extracted with toluene, dehydrated by a low-temperature evaporation system, and centrifuged. , The methyl sulfide ammonium salt solid is obtained, and the quality of the obtained methyl sulfide ammonium salt solid is shown in Table 2:

[0038] project purity,% Moisture,% Methyl sulfide ammonium salt solid971

[0039] (2) In the autoclave, add p-chloronitr...

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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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