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Separation method for acetic acid in acylation reaction liquid

A technology of acylation reaction and separation method, which is applied in the field of separation of acetic acid in acylation reaction liquid, to achieve the effects of reduced decomposition loss, high recovery rate of acetic acid, and good separation effect

Inactive Publication Date: 2016-05-04
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to solve the problems in the above separation method, the present invention provides a method for directly separating and recovering acetic acid, which can reduce the generation of waste water, avoid solvent mixing and equipment corrosion, and at the same time, the method has the advantages of simple operation, short time consumption and high separation effect. advantages, and the method can directly recycle acetic acid, which can meet the needs of industry

Method used

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  • Separation method for acetic acid in acylation reaction liquid
  • Separation method for acetic acid in acylation reaction liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Put 200 grams of acylation reaction solution with acephate content of 54% and acetic acid content of 28.4% in a stirred crystallization kettle, cool down from 29°C to 5°C within 4 hours, crystallize for 15 hours, and obtain acetyl form Amidophos crystals and first filtrate. Put the filtrate for the first time in a rotary evaporator, distill at 40°C and -0.1mpa, obtain acetic acid after the gaseous stream is condensed, and put the liquid phase stream back into the crystallization tank with stirring, within 4 hours from Cool down from 50°C to 5°C, crystallize for 2 hours, separate acephate crystals and the second filtrate, put the second filtrate in a rotary evaporator, distill at 40°C and -0.1mpa, and condense the gas phase stream To obtain acetic acid, the acetic acid obtained by the filtrate vacuum distillation for the first time and the acetic acid obtained by the filtrate vacuum distillation for the second time are mixed. Obtained through measurement, the purity of ...

Embodiment 2

[0051] Put 200 grams of acylation reaction solution with acephate content of 60% and acetic acid content of 27.93% in a stirred crystallization kettle, cool down from 40°C to 5°C in 3 hours, crystallize for 10 hours, and obtain acephate Crystals and first filtrate. Put the filtrate for the first time in a rotary evaporator, and distill it at -0.1mpa at 70°C. The gaseous phase stream is condensed to obtain acetic acid, and the liquid phase stream is recycled to the crystallization tank with stirring, and the temperature is lowered from 45°C for 3 hours. to 5°C, crystallized for 0.5h, separated to obtain acephate crystals and the second filtrate, put the second filtrate in a rotary evaporator, and distilled at -0.03mpa at 70°C, and obtained acetic acid after condensation of the gas phase stream , the acetic acid obtained by the filtrate decompression distillation for the first time and the acetic acid obtained by the filtrate decompression distillation for the second time are mi...

Embodiment 3

[0053] Put 200 grams of acylation reaction solution with acephate content of 60% and acetic acid content of 28.51% in a stirred crystallization kettle, cool down from 38°C to 2°C in 2 hours, crystallize for 5 hours, and obtain acephate Crystals and first filtrate. Put the filtrate for the first time in a rotary evaporator, and distill it at -0.1mpa at 50°C. The gaseous phase stream is condensed to obtain acetic acid, and the liquid phase stream is recycled to the crystallization tank with stirring, and the temperature is lowered from 38°C for 2 hours. to 2°C, crystallized for 5 hours, separated to obtain acephate crystals and the second filtrate, put the second filtrate in a rotary evaporator, and distilled at -0.05mpa at 50°C, and obtained acetic acid after the gaseous stream was condensed. The acetic acid obtained by the filtrate decompression distillation for the first time and the acetic acid obtained by the filtrate decompression distillation for the second time are mixed...

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Abstract

The invention provides a separation method for acetic acid in acylation reaction liquid. The method comprises the following steps of 1, performing cooling crystallization on the acylation reaction liquid to separate coarse crystals and filtrate by adopting a cooling crystallization process; 2, performing reduced pressure distillation on the filtrate to separate a gas-phase material flow and a liquid-phase material flow by adopting a reduced pressure distillation process, and condensing the obtained gas-phase material flow to obtain acetic acid; 3, recycling acetic acid from the liquid-phase material flow obtained in Step 2 by adopting an ammonia water neutralization method. According to the acetic acid separation method, most of acetic acid is directly recycled from the acylation reaction liquid by reduced pressure distillation, and a small amount of acetic acid is recycled by the ammonia water neutralization method, so that introduction of a water phase in an acetic acid direct recycling process is avoided, and production of wastewater and decomposition loss of acephate are reduced. The acetic acid separation method has a good separation effect, and an industrial requirement can be met.

Description

【Technical field】 [0001] The invention relates to a method for separating acetic acid in an acylation reaction solution, in particular to a method for separating acetic acid in acephate reaction solution or acetylspermine reaction solution synthesized by acetylation. 【Background technique】 [0002] my country is a large agricultural country based on agriculture. However, with global warming, land desertification is becoming more and more serious, and problems such as cultivated land degradation appear, the supply of food is becoming more and more tense. In terms of ensuring food security and increasing food production Chemical pesticides play an important role, and chemical pesticides are also an important means of resisting and controlling pests in our country. 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. [0003] Acephate (acep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43C07C51/44C07C53/08
CPCC07C51/43C07C51/44C07C53/08
Inventor 艾秋红汪伟罗和安黄荣辉
Owner XIANGTAN UNIV
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