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Method for recovery and application of reaction solvent ethanol in the process of producing 4-aminotrifluorotoluene

A technology of aminotrifluorotoluene and reaction solvent, which is applied in the field of recovery and application of reaction solvent ethanol, can solve problems such as high consumption, high economic cost, environmental pollution, etc., and achieve good effect, large economic benefit, and reduced operating cost Effect

Inactive Publication Date: 2015-12-09
NANTONG HAISHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] For a long time, in the process of producing 4-aminotrifluorotoluene, the amount of solvent ethanol used in ammonification has remained high, and the receiving solution from ammoniation stripping contains about 50% solvent ethanol. If this part finally contains The receiving solution of ethanol, whether it is used as wastewater or hazardous solid waste, will cause great pollution to the environment, and it will also cost a lot of money to buy solvent ethanol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The method for recovering the reaction solvent ethanol in the process of producing 4-aminotrifluorotoluene comprises the following steps: a feeding step, an ammonia passing step, a pressure relief and pressing step, a precipitating step and a precipitating receiving liquid recovery step;

[0017] The feeding steps are as follows: into the high-pressure ammoniation kettle, sequentially input recovered ethanol containing 550 parts by mass of ethanol, 750 parts by mass of p-chlorobenzotrifluoride (correspondingly deducting the mass parts of p-chlorobenzotrifluoride contained in recovered ethanol) and 100 parts by mass of Catalyst cuprous chloride;

[0018] The ammonia passing step is as follows: the temperature is controlled at 25°C, 350 parts by mass of liquid ammonia is passed into the high-pressure ammoniation kettle, and then the temperature is raised to 155°C, and the temperature is kept for 10 hours;

[0019] The steps of pressure relief and material pressing are: af...

Embodiment 2

[0023] The method for recovering the reaction solvent ethanol in the process of producing 4-aminotrifluorotoluene comprises the following steps: a feeding step, an ammonia passing step, a pressure relief and pressing step, a precipitating step and a precipitating receiving liquid recovery step;

[0024] The feeding steps are as follows: into the high-pressure ammoniation kettle, sequentially input recovered ethanol containing 600 parts by mass of ethanol, 800 parts by mass of p-chlorobenzotrifluoride (correspondingly deducting the mass parts of p-chlorobenzotrifluoride contained in recovered ethanol) and 150 parts by mass of The catalyst potassium fluoride;

[0025] The ammonia passing step is as follows: the temperature is controlled at 28°C, 380 parts by mass of liquid ammonia is passed into the high-pressure ammoniation kettle, and then the temperature is raised to 160°C, and the temperature is kept for 11 hours;

[0026] The steps of pressure relief and material pressing a...

Embodiment 3

[0030] The method for recovering the reaction solvent ethanol in the process of producing 4-aminotrifluorotoluene comprises the following steps: a feeding step, an ammonia passing step, a pressure relief and pressing step, a precipitating step and a precipitating receiving liquid recovery step;

[0031] The feeding steps are as follows: into the high-pressure ammoniation kettle, sequentially input recovered ethanol containing 650 parts by mass of ethanol, 850 parts by mass of p-chlorobenzotrifluoride (correspondingly deducting the mass parts of p-chlorobenzotrifluoride contained in recovered ethanol) and 200 parts by mass of Catalyst cuprous chloride;

[0032] The ammonia passing step is as follows: the temperature is controlled at 30°C, 400 parts by mass of liquid ammonia is passed into the high-pressure ammoniation kettle, and then the temperature is raised to 165°C, and the temperature is kept for 12 hours;

[0033] The steps of pressure relief and material pressing are: af...

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PUM

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Abstract

The invention discloses a recycling and reusing method for a reaction dissolvent alcohol in a production process of 4- aminotrifluorotoluene, which comprises the steps of material feeding, ammonia introducing, pressure reliefing, and material pressing, desolvation and desolvation receiving liquid recovering. Recycled alcohol, 4-chlorobenzotrifluoride and a catalyzer are sequentially put into a high-pressure ammoniation kettle; the desolvation kettle is up to the final temperature of 105-110 DEG C for 30-40 minutes; when a receiving pot view mirror shows that receiving liquid is cloudy, the desolvation is over. The desolvation receiving solution mainly comprises components including the dissolventethanol and 4-chlorobenzotrifluoride of which partial ammoniation does not react completely, the desolvation receiving solutions (recycled ethanol) can be used as dissolvents and reaction materials, and are continuously fed in the next batch, as a result, wastewater drainage amount is reduced and wastewater treatment pressure is relieved, the total drainage amount is controlled, the wastewater treatment effect is good, the running cost is lowered, and meanwhile, the yield of all intermediates and the product can be remarkably improved, and higher economic benefits are realized.

Description

technical field [0001] The invention relates to a recovery and application method of reaction solvent ethanol in the process of producing 4-aminotrifluorotoluene. Background technique [0002] For a long time, in the process of producing 4-aminotrifluorotoluene, the amount of solvent ethanol used in ammonification has remained high, and the receiving solution from ammoniation stripping contains about 50% solvent ethanol. If this part finally contains The receiving solution of ethanol will cause great pollution to the environment no matter it is used as waste water or hazardous solid waste, and it will also cost a lot of money to buy solvent ethanol in large quantities. Through feasibility analysis to the reuse of the precipitation receiving solution, it is found that in addition to containing most of the solvent ethanol, there is also a part of unreacted initial raw material p-chlorobenzotrifluoride. If the receiving solution can be recycled, it can not only reduce the The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/52C07C209/10
Inventor 江耀田杨劲松朱春雷盛海涛陈虹
Owner NANTONG HAISHENG PHARMA
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