Purification technology for trichloroacetone

A technology of trichloroacetone and process, which is applied in the field of purification process of trichloroacetone, which can solve the problems of filter cake irritation, low purity of trichloroacetone, poor purification effect, etc., achieve less impurity content, reduce contact and reduce damage Effect

Inactive Publication Date: 2015-12-09
JIHENG PHARMA HENGSHUI CITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the technical problems in the prior art that the purity of trichloroacetone is low, the existing purification process is likely to cause environmental pollution, the

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take a 250ml flask as a reaction kettle, set a filter screen at the discharge port at the bottom of the reaction kettle, add 50ml of crude trichloroacetone with a concentration of 52%, 10ml of water, and 50ml of petroleum ether into the flask, and stir in the reaction kettle at room temperature 20min, then slowly cool down to 0°C with cold brine, and stir at 0°C for 2h, after the recrystallization is complete, pressurize the reactor to 0.1MPa, and discharge the filtrate to the filtrate storage tank through the discharge port at the bottom of the reactor Inside, after the filtrate flows out, add sherwood oil to the reaction kettle to wash the filter cake, and then perform a water wash, the filtrate after washing is discharged into the filtrate storage tank, after the washing is finished, close the discharge port at the bottom of the reaction kettle to obtain The wet product of trichloroacetone is dissolved in water to obtain the aqueous solution of trichloroacetone, the G...

Embodiment 2

[0025] Take a 250ml flask as a reaction kettle, set a filter screen at the discharge port at the bottom of the reaction kettle, add 50ml of crude trichloroacetone with a concentration of 50%, 12ml of water, and 90ml of petroleum ether into the flask, and stir in the reaction kettle at room temperature 23min, then slowly cool down to 0°C with cold brine, and stir at 0°C for 2.3h. After the recrystallization is complete, pressurize the reactor to 0.12MPa, and discharge the filtrate through the discharge port at the bottom of the reactor to the filtrate storage In the tank, after the filtrate has flowed out, add petroleum ether to the reactor to wash the filter cake, and then perform a water wash, and the washed filtrate is discharged into the filtrate storage tank. After washing, close the discharge port at the bottom of the reactor. The wet product of trichloroacetone was obtained, and the wet product of trichloroacetone was dissolved in water to obtain an aqueous solution of tr...

Embodiment 3

[0028] Take a 250ml flask as a reaction kettle, set a filter screen at the discharge port at the bottom of the reaction kettle, add 50ml of crude trichloroacetone with a concentration of 50%, 10ml of water, and 20ml of petroleum ether into the flask, and stir in the reaction kettle at room temperature 17min, then slowly cool down to 0°C with cold brine, and stir at 0°C for 1.6h. After the recrystallization is complete, pressurize the reactor to 0.14MPa, and discharge the filtrate to the filtrate storage through the discharge port at the bottom of the reactor. In the tank, after the filtrate has flowed out, add petroleum ether to the reactor to wash the filter cake, and then perform a water wash, and the washed filtrate is discharged into the filtrate storage tank. After washing, close the discharge port at the bottom of the reactor. The wet product of trichloroacetone was obtained, and the wet product of trichloroacetone was dissolved in water to obtain an aqueous solution of t...

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PUM

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Abstract

The invention provides a purification technology for trichloroacetone, and belongs to the technical field of compound purification. According to the technology, crude trichloroacetone with the purity of 42-53% is adopted as the raw materials, recrystallization is performed on the crude trichloroacetone through mixed solvent of water and petroleum ether in a reaction kettle, filtering and washing are performed, and then the purified trichloroacetone is obtained; washing is directly performed in the reaction kettle by adopting a filtering mode through closed washing, a filter screen is arranged at a discharging opening in the bottom of the reaction kettle, filtrate is drained into a filtrate storage tank through the discharging opening in the bottom of the reaction kettle after recrystallization is completed, filter cake washing is performed by adding the petroleum ether into the reaction kettle after the filtrate is drained completely, washing is performed for once again, the washed filtrate is drained into the filtrate storage tank, the discharging opening in the bottom of the reaction kettle is closed after washing is completed, and the purified trichloroacetone is obtained. According to the purification technology, the purity of the trichloroacetone is high, and compared with the prior art, the yield can be improved by 2% when the purified trichloroacetone is applied to folic acid production.

Description

technical field [0001] The invention belongs to the technical field of compound purification and relates to the purification of polychloroacetone, in particular to a process for the purification of trichloroacetone. The purified trichloroacetone by the process has high purity and is used to produce folic acid, which can obviously increase the folic acid output. Background technique [0002] Trichloroacetone is the main raw material of folic acid crude product, and its stable quality is the guarantee of folic acid quality, but the content of trichloroacetone on the domestic market is mostly about 50%, and the price of high-quality trichloroacetone is lower than that of ordinary trichloroacetone. 2 times more. In actual production, trichloroacetone is extracted with water to remove high chlorine and low chlorine in trichloroacetone, which not only consumes a lot of water, but also contains a part of low chlorine in the trichloroacetone aqueous extract, which affects the reacti...

Claims

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Application Information

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IPC IPC(8): C07C49/16C07C45/78C07C45/81
CPCC07C45/81C07C45/78C07C49/16
Inventor 马胜义魏晶磊杜文峰张志强蔡颂公李希明庄士千徐亚威董永广焦银蕾
Owner JIHENG PHARMA HENGSHUI CITY
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