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Method for extracting and recovering methylpyrimidinol by using nitrogen heterocyclic functionalized ionic liquid

A technology of methylpyrimidinol and ionic liquid, which is applied in the field of extraction and recovery of methylpyrimidinol by nitrogen-heterocyclic functionalized ionic liquid, which can solve the problems of resource utilization of valuable components and no significant advantages. , to achieve the effect of repeated utilization, fast process and good separation effect

Active Publication Date: 2021-04-16
HUNAN HAILI HIGH TECH IND GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In terms of extraction and separation, more emphasis is placed on the selective extraction ability of the extractant for the extraction object. The extraction efficiency of the broad-spectrum ionic liquid for the extraction object is not significantly superior to that of traditional solvent extraction.
In addition, so far, there have been no relevant research reports on the use of ionic liquids in the treatment of pyrimidine pesticide wastewater and the resource utilization of valuable components in wastewater.

Method used

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  • Method for extracting and recovering methylpyrimidinol by using nitrogen heterocyclic functionalized ionic liquid

Examples

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Effect test

Embodiment 1

[0043] A method for extracting and recovering methylpyrimidinol by using nitrogen-heterocyclic functionalized ionic liquid, specifically using azocyclopentanetriethyl quaternary ammonium hexafluorophosphate ionic liquid to extract and recover methylpyrimidinol in waste water, Include the following steps:

[0044] (1) Synthesis of azacyclopentane triethyl quaternary ammonium hexafluorophosphate ionic liquid: by the molar ratio of triethylamine, hexafluorophosphoric acid, cyanamide, 1,2-dichloroethane 1.2: 1:1:1.2, the azacyclopentanetriethyl quaternary ammonium hexafluorophosphate ionic liquid was prepared.

[0045] Step 1: Add triethylamine (0.36mol) into a 250mL three-necked round-bottomed flask, place it in an ice-water bath (0°C to 5°C), and slowly drop it at a rate of 1mL / min under stirring Add an aqueous solution of hexafluorophosphoric acid with a mass concentration of 50% (the solution contains 0.3 mol of hexafluorophosphoric acid) to carry out a neutralization reactio...

Embodiment 2

[0053] A method for extracting and recovering methylpyrimidinol by using nitrogen-heterocyclic functionalized ionic liquid, specifically using azacyclohexanetriethyl quaternary ammonium hexafluorophosphate ionic liquid to extract and recover methylpyrimidinol in wastewater, Include the following steps:

[0054] (1) Synthesis of azacyclohexane triethyl quaternary ammonium hexafluorophosphate ionic liquid: according to the molar ratio of triethylamine, hexafluorophosphoric acid, cyanamide, 1,3-dichloropropane 1.5:1 : 1: 1.5 to prepare an azacyclohexanetriethyl quaternary ammonium hexafluorophosphate ionic liquid.

[0055] Step 1: Add triethylamine (0.45mol) into a 250mL three-necked round-bottomed flask, place it in an ice-water bath (0°C-5°C), and slowly add mass at a rate of 2mL / min under stirring A 50% hexafluorophosphoric acid aqueous solution (the solution contains 0.3 mol hexafluorophosphoric acid) was neutralized for 1 hour to obtain triethylamine hexafluorophosphate ion...

Embodiment 3

[0063] A method for extracting and recovering methylpyrimidinol by using nitrogen-heterocyclic functionalized ionic liquid, specifically using azepanetriethyl quaternary ammonium hexafluorophosphate ionic liquid to extract and recover methylpyrimidinol in wastewater, Include the following steps:

[0064] (1) Synthesis of azepanetriethyl quaternary ammonium hexafluorophosphate ionic liquid: by the molar ratio of triethylamine, hexafluorophosphoric acid, cyanamide, 1,4-dichlorobutane 2: 1:1:2, the azepanotriethyl quaternary ammonium hexafluorophosphate ionic liquid was prepared.

[0065] Step 1: Add triethylamine (0.6mol) into a 250mL three-necked round-bottomed flask, place it in an ice-water bath (0°C-5°C), and slowly add mass at a rate of 3mL / min under stirring A 50% hexafluorophosphoric acid aqueous solution (the solution contains 0.3 mol hexafluorophosphoric acid) was neutralized for 2 hours to obtain triethylamine hexafluorophosphate ionic liquid.

[0066] The second ste...

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Abstract

The invention discloses a method for extracting and recovering methylpyrimidinol by using a nitrogen heterocyclic functionalized ionic liquid. The method comprises the following steps: dissolving the nitrogen heterocyclic functionalized ionic liquid in a non-water-soluble organic solvent to obtain an extractant; mixing an extracting agent with wastewater containing methylpyrimidinol, extracting, and standing to obtain an extracted organic phase; mixing the extracted organic phase with an acidic solution, carrying out back extraction, and standing to obtain back extraction liquid and an extraction agent; and adjusting the pH value of the strip liquor to 4-9, separating out pyrimidinol salt precipitate, and carrying out centrifugal separation to complete recovery of methylpyrimidinol. According to the method for extracting and recovering the methylpyrimidinol by using the nitrogen heterocyclic functionalized ionic liquid, efficient recovery of the methylpyrimidinol is realized, cyclic utilization of the nitrogen heterocyclic functionalized ionic liquid is also realized, the whole process is rapid, efficient and pollution-free, the technical performance is excellent, the method has the advantages of low cost, high extraction efficiency, good separation effect, greenness, no pollution and the like, and has a wide application prospect.

Description

technical field [0001] The invention relates to a method for extracting and recovering methylpyrimidinol by utilizing nitrogen heterocycle functionalized ionic liquid. Background technique [0002] Pirimiphos-methyl (alias Andre, PP511) is a pyrimidine insecticide, which is recommended by the World Health Organization (WHO) and the United Nations Food and Agriculture Organization (FAO) as a safe pesticide variety for grain storage and household hygiene pest control . Compared with highly toxic aluminum phosphide, pirimiphos-methyl has a broad insecticidal spectrum, rapid action, and a drug effect of up to 45-70 weeks. It has gradually become an excellent substitute for highly toxic organophosphorus pesticides. [0003] However, the water pollution problem in the production process of pirimiphos-methyl is serious, and the wastewater components are complex, containing high concentrations of pyrimidinol, various small molecular organic amines, thiophosphoryl chloride and other...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/36C07D239/14
Inventor 曹金艳陈灿陈明干兴利张海涛刘欢钟若楠秦岳军张燕马林
Owner HUNAN HAILI HIGH TECH IND GRP
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