Method for extracting and separating acetyl spermine in acylation reaction liquid

A technique for acetylspermine and acylation reaction, applied in chemical instruments and methods, separation/purification of carboxylic acid amides, separation/purification of carboxylic acid compounds, etc., can solve waste of resources, reduce crystal purity of acephate, and pollution Environmental and other issues, to achieve the effect of reducing waste water production, chemical stability and thermal stability, and reducing pollution

Active Publication Date: 2017-03-15
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] And there is no record of the technology of separation and recovery of acephate at present. Acetyl spermine and acephate are co-crystallized or directly discharged into the environment, which will reduce the crystallization purity of acephate on the one hand, and on the other hand, acephate directly Discharged into the environment, causing a waste of resources and polluting the environment

Method used

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  • Method for extracting and separating acetyl spermine in acylation reaction liquid
  • Method for extracting and separating acetyl spermine in acylation reaction liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Take 150g of acephate content and be 49.57%, acetic acid content is 27.85%, and the acylation reaction solution that acetylspermine content is 5.74% is put into the mixing tank of extraction device, and 150g petroleum ether extractant is carried out 5 grades of countercurrent extraction experiments After extraction, 186.6 g of the upper extract phase and 97.4 g of the lower raffinate phase were obtained. Through liquid chromatography analysis, the mass percentages of the upper layer of the extract phase are respectively 13.03% of acephate, 16.60% of acetic acid, and 3.08% of acetylspermine, and the mass percentages of the lower raffinate phase are respectively 51.14% of acephate and 10.92% of acetic acid. %, acetylspermine 2.97%. Compared with acephate, the selectivity coefficient of acetic acid was calculated to be 5.97, and the selectivity coefficient of acetylspermine to be 4.07. The total recovery rate was 94.67%. Put the extract phase in a rotary evaporator with ...

Embodiment 2

[0055] Getting 150g acephate content is 53.40%, and acetic acid content is 31.72%, and the acylation reaction liquid that acetylspermine content is 5.86% is put into the mixing tank of extraction device, carries out 5 grades of countercurrent extraction experiments with 150g toluene extractant, After extraction, 176.3 g of the upper extract phase and 104.6 g of the lower raffinate phase were obtained. Through liquid chromatography analysis, the mass percentages of the upper layer extract phase are respectively 13.15% of acephate, 18.76% of acetic acid, and 4.07% of acetylspermine, and the mass percentages of the lower raffinate phase are respectively 54.36% of acephate and 13.41% of acetic acid. %, acetylspermine 1.62%. Compared with acephate, the selectivity coefficient of acetic acid is 5.78, the selectivity coefficient of acetylspermine is 10.39, and the total recovery rate is 93.63%. Put the extraction phase in a rotary evaporator with a rotating speed of 70rmp, and disti...

Embodiment 3

[0057] Get 150g of acephate content and be 49.68%, acetic acid content is 34.24%, and the acylation reaction solution that acetyspermine content is 5.32% is put into the mixing tank of extraction device, carries out 5 grades of countercurrent continuous extractions with 150g xylene extractant In the experiment, 180.1 g of the upper extract phase and 106.7 g of the lower raffinate phase were obtained after extraction. Through liquid chromatography analysis, the mass percentages of the upper layer of the extract phase are respectively 8.76% of acephate, 20.12% of acetic acid, and 3.41% of acetylspermine, and the mass percentages of the lower raffinate phase are respectively 54.84% of acephate and 14.15% of acetic acid. %, acetylspermine 1.08%. Compared with acephate, the selectivity coefficient of acetic acid is 8.30, the selectivity coefficient of acetylspermine is 12.11, and the total recovery rate is 95.6%. Put the extract phase in a rotary evaporator with a rotating speed o...

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Abstract

The invention provides a method for extracting and separating acetyl spermine in an acylation reaction liquid. The method comprises the following steps: I, taking the acylation reaction liquid as a raw material liquid, adding an extraction agent, and performing multi-stage countercurrent continuous extraction on the raw material liquid to obtain an extraction phase and a raffinate phase, wherein the extraction phase comprises a main amount of the acetyl spermine and acetic acid of the raw material liquid, and the raffinate phase comprises a main amount of acephate in the raw material liquid; II, separating the extraction phase and the raffinate phase, thereby obtaining coarse crystal of the acetyl spermine and coarse crystal of acephate. By adopting the method provided by the invention, the crystallization purity of the acephatethe can be increased while the acetyl spermine is recycled, and moreover as the acetic acid is recycled in a rectification manner, the method is simple and convenient to operate and good in separation effect; and the acetyl spermine can be prevented from being discharged into wastewater, so that the environment pollution can be reduced.

Description

[0001] 【Technical field】 [0002] The invention relates to a method for separating an acylation reaction liquid, in particular to a method for extracting and separating acetylspermine in an acylation reaction liquid. [0003] 【Background technique】 [0004] my country is a large agricultural country based on agriculture. However, with global warming, land desertification is becoming more and more serious, and rootland degradation and other problems have appeared, the supply of food is becoming more and more tense. In order to ensure food security and increase food production On the one hand, chemical pesticides play an important role. In my country, chemical pesticides are also an important means of resisting and controlling pests. Therefore, the development of high-efficiency and low-toxic chemical pesticides and the development of simple and efficient synthesis processes have extremely important practical significance. [0005] Acephate (acephate), the chemical name is O, S-d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/36C07C51/48C07C51/44C07C53/08C07F9/24
CPCC07C51/44C07C51/48C07C231/24C07F9/2408C07C233/36C07C53/08
Inventor 艾秋红刘伟罗和安黄荣辉
Owner XIANGTAN UNIV
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