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Method for recovering copper-containing mother liquid in 4-aminotrifluorotoluene production technology

A technology of aminotrifluorotoluene and recovery method, which is applied in the field of recovery of copper-containing mother liquor, can solve the problems of discarding copper-containing substances, wasting intermediates or products, and no longer using them, so as to reduce waste water discharge and control the total discharge , the effect of reducing operating costs

Inactive Publication Date: 2013-09-04
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, the amount of copper-containing catalyst used in the amination of 4-aminotrifluorotoluene has remained high. In the end, this part of copper-containing matter will cause serious pollution to the environment no matter whether it is used as wastewater or hazardous solid waste, and it is necessary to purchase a large amount of catalysts. It costs a lot of money. One of the reasons is that these copper-containing substances are discarded directly and are no longer used. This not only increases the treatment difficulty and operating cost of the sewage treatment station, but also wastes some intermediates or products. , if it is used as solid waste, it will have to pay more economic costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The recovery method of copper-containing mother liquor in the production of 4-aminotrifluorotoluene process of the present invention comprises the following steps: feeding step, ammonia passing step, pressure relief and pressing step, defiltration step and press filtration washing step,

[0033] The feeding steps are as follows: drop in 550kg of ethanol, 750kg of p-chlorobenzotrifluoride and 100kg of copper-containing catalyst in sequence;

[0034] The ammonia passing step is as follows: the temperature is controlled at 25°C, 350kg of liquid ammonia is introduced, then the temperature is raised to 155°C, and the temperature is kept for 10 hours;

[0035] The pressure relief and material pressing steps are: after the heat preservation is completed, the pressure is released, and then the material is pressed to the precipitation kettle;

[0036] The defiltration steps are: control the appropriate residual pressure of 0.4Mpa to press the material, the steam temperature belo...

Embodiment 2

[0043] The recovery method of copper-containing mother liquor in the production of 4-aminotrifluorotoluene process of the present invention comprises the following steps: feeding step, ammonia passing step, pressure relief and pressing step, defiltration step and press filtration washing step,

[0044] The feeding steps are as follows: input 600kg of ethanol, 800kg of p-chlorobenzotrifluoride and 150kg of copper-containing catalyst in sequence;

[0045] The ammonia passing step is as follows: the temperature is controlled at 28°C, 380kg of liquid ammonia is introduced, and then the temperature is raised to 160°C, and the temperature is kept for 10 hours;

[0046] The pressure relief and material pressing steps are: after the heat preservation is completed, the pressure is released, and then the material is pressed to the precipitation kettle;

[0047] The defiltration steps are: control the appropriate residual pressure of 0.4Mpa to press the material, the temperature of the s...

Embodiment 3

[0054] The recovery method of copper-containing mother liquor in the production of 4-aminotrifluorotoluene process of the present invention comprises the following steps: feeding step, ammonia passing step, pressure relief and pressing step, defiltration step and press filtration washing step,

[0055] The feeding steps are as follows: 650kg of ethanol, 850kg of p-chlorobenzotrifluoride and 200kg of copper-containing catalyst are dropped in sequence;

[0056] The ammonia passing step is as follows: the temperature is controlled at 30°C, 400kg of liquid ammonia is introduced, and then the temperature is raised to 165°C, and the temperature is kept for 10 hours;

[0057] The pressure relief and material pressing steps are: after the heat preservation is completed, the pressure is released, and then the material is pressed to the precipitation kettle;

[0058] The defiltration steps are: control the appropriate residual pressure of 0.4Mpa to press the material, the steam temperat...

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PUM

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Abstract

The invention discloses a method for recovering a copper-containing mother liquid in a 4-aminotrifluorotoluene production technology. The method is characterized in that the method comprises the following steps: 1, feeding: sequentially adding 550-650 parts by mass of ethanol, 750-850 parts by mass of 4-chlorobenzotrifluoride and 100-200 parts by mass of a copper-containing catalyst; 2, ammonia feeding: letting in 350-400 parts by mass of liquid ammonia, heating to 155-165DEG C, and carrying out heat insulation for 10h; 3, decompression and material pressing: decompressing after the heat insulation is ended, and pressing the obtained material to a desolventizing kettle; 4, defiltration: pressing the material under a controlled excess pressure, and desolventizing; and 5, filter pressing and material washing: preparing before the filter pressing and material washing, filter-pressing, washing the material, and discharging filter residues. The method allows copper-containing water and the water-containing filter residues to be continuously fed as process water or a catalyst, so the discharge amount of wastewater is reduced, and a large economic benefit is obtained.

Description

technical field [0001] The invention relates to a method for recovering copper-containing mother liquor in the process of producing 4-aminotrifluorotoluene. Background technique [0002] For a long time, the amount of copper-containing catalyst used in the amination of 4-aminotrifluorotoluene has remained high. In the end, this part of copper-containing matter will cause serious pollution to the environment no matter whether it is used as wastewater or hazardous solid waste, and it is necessary to purchase a large amount of catalysts. It costs a lot of money. One of the reasons is that these copper-containing substances are discarded directly and are no longer used. This not only increases the treatment difficulty and operating cost of the sewage treatment station, but also wastes some intermediates or products. , if it is regarded as solid waste, more economic costs will be paid for the transfer. Therefore, in order to solve the above problems, a new technical solution is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/10C07C209/84
Inventor 江耀田杨劲松冯进盛海涛陈虹
Owner NANTONG HAISHENG PHARMA