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Continuous esterification process based on acyclovir intermediate production mother liquor

A technology of intermediates and mother liquor, applied in the field of continuous esterification process, can solve the problems of inability to realize the recycling of mother liquor, inability to recycle catalysts, and huge production equipment, so as to reduce energy consumption, complete reaction, efficient recycling and comprehensive utilization Effect

Pending Publication Date: 2020-09-29
潍坊奥通药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method also has problems such as huge production equipment and catalysts that cannot be recycled.
And utilize existing esterification method, can't realize the recycling of the mother liquor that acyclovir produces

Method used

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  • Continuous esterification process based on acyclovir intermediate production mother liquor

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Effect test

Embodiment 1

[0048] Such as figure 1 Shown, is the device used in the continuous esterification process based on the production of mother liquor of acyclovir intermediate of the present invention: a continuous production device in which esterification and rectification operations are carried out in combination, separated by reaction unit and rectification Unit composition, the reaction unit is used to realize the esterification reaction, and the rectification separation unit is used to realize the separation of the product ester from other materials. The gas phase material produced by the reaction unit is directly condensed and separated through the rectification unit to realize continuous esterification.

[0049] The reaction unit includes an esterification reactor 101 with a jacket structure and a stirring system. The upper part of the esterification reactor is equipped with a liquid feed port 102 and a liquid feed port 103 , a solid catalyst feed port 104 and a large-diameter gas phase ...

Embodiment 2

[0064] According to the production device set forth in Example 1, the trial production operation of the reclaimed mother liquor of the acyclovir intermediate diacetylguanine is as follows, the quality of the reclaimed mother liquor consists of 48% acetic acid, 51% acetic anhydride, and 1% of other organic matter (mainly guanine, xanthine, etc.), the mass percentage of used recovered ethanol is 94.5%.

[0065] First put 20Kg of sodium bisulfate, 100Kg of recovered mother liquor, and 90Kg of recovered ethanol into a 500L reactor, turn on stirring, jacket steam heating, and the power switch of the oil-water phase discriminator, and adjust the reflux ratio to the full reflux state to control the reactor The temperature is 90-100°C.

[0066] When the temperature at the top of the rectification tower is stable at 70.0 to 75.0°C (in this embodiment, the temperature at the top of the tower is stable at 70 to 71°C), the quantitative feeding system for recovering the mother liquor and e...

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Abstract

The invention discloses a continuous esterification process based on acyclovir intermediate production mother liquor. The process comprises the following steps: (I) respectively and continuously introducing acyclovir intermediate production mother liquor and ethanol / recovered ethanol into a reaction kettle filled with a catalyst, and carrying out an esterification reaction; (II) introducing a gas-phase material generated by esterification into a rectifying tower for rectification; (III) introducing a gas-phase material generated at the top of the rectifying tower into a water segregator with acondenser, layering condensate in the water segregator, and collecting an esterification product from the ester outlet of the water segregator, and returning materials at the bottom of the rectifyingtower back to the esterification reaction kettle; and (IV) returning part of water generated in the water segregator back to the rectifying tower, and collecting the other part of water. By adoptingthe process, the acyclovir intermediate (diacetyl guanine) mother liquor can be efficiently recovered, and meanwhile, a high-quality ethyl acetate product is obtained, so that the wastewater treatmentcost is reduced, and the income is increased due to generated ethyl acetate.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and in particular relates to a continuous esterification process for producing mother liquor based on an acyclovir intermediate. Background technique [0002] During the production of acyclovir, a large amount of mother liquor containing mixed solvents such as acetic acid, acetic anhydride, and / or toluene is produced. These mother liquors are equipped with traditional separation methods, and it is difficult to obtain pure products / or solvents with low pollutant emissions. [0003] The traditional ethyl acetate synthesis process is generally divided into two steps: reaction process and rectification purification process. During the reaction process, it is necessary to add an acid catalyst, and it is necessary to continuously remove by-product water during the reaction process. The reaction product ester is mixed with an excess of a raw material (acid / or alcohol), and a small amo...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/14C07C67/54C07D473/18
CPCC07C67/08C07C67/54C07D473/18C07C69/14
Inventor 杨栽根刘晓磊晏金华魏海鹏
Owner 潍坊奥通药业有限公司
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