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Method and apparatus for producing formic esters by comprehensively utilizing metronidazole hydroxylation synthesis wastewater

A technology for the hydroxylation and chemical synthesis of metronidazole is applied in the field of comprehensive recycling and utilization of chemical synthesis pharmaceutical production wastewater, which can solve the problems of formic acid consumption and waste, difficult treatment of hydroxylation synthesis production wastewater, etc. Excellent quality of by-products and the effect of eliminating formic acid waste gas

Active Publication Date: 2015-10-28
黄冈银河阿迪药业有限公司
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Problems solved by technology

The consumption of formic acid in the production process of metronidazole can be said to be all wasted, and at the same time it brings the problem of wastewater treatment in the production of hydroxylation synthesis

Method used

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  • Method and apparatus for producing formic esters by comprehensively utilizing metronidazole hydroxylation synthesis wastewater

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Embodiment 1

[0037] After the hydroxylation synthesis reaction is completed, the material is transferred to the esterification reactor 4 to prepare for the esterification reaction. Assuming that the quality of formic acid added when the hydroxylation synthesis reaction takes place is Q (Kg), the amount of methyl alcohol to be added is calculated as follows: W 甲醇 =1.05×Q / 46×32, then slowly add it into the esterification reaction kettle 4, after the feeding is completed, control the temperature to be greater than or equal to 60°C, reflux for 2 hours, and after the reaction is completed, transfer the material to No. Distillation, the distilled mixed gas is directly sent to the rectification tower 8 (the rectification tower is a single-tower process) for rectification separation, and the distillation operation temperature is controlled at 88 ± 2°C until all the methyl formate and methanol are distilled out and sent to enter the rectification tower for rectification separation, obtain methyl fo...

Embodiment 2

[0042] The technological process of embodiment 2 is with embodiment 1.

[0043] The difference is that:

[0044] (1) The alcohols that join in the esterification reactor 4 are ethanol, and the esterification product that obtains is ethyl formate.

[0045] (2) Ethyl formate and water have an azeotropic point (54.23°C), and the rectification process must adopt a double-tower (or three-tower) process. The double-tower process is to use the rectification tower 8 to distill ethyl formate and ethanol first, and then use The dehydration of the desiccant skips the azeotropic point, and then continues the rectification and separation in the rectification tower 8, and intercepts the fraction at 54±0.5°C at the top of the tower to obtain more than 99% of the ethyl formate product; what is obtained at the bottom of the tower is ethanol And the distillate entrainment composition when the previous process evaporates, discharges to the ethanol aqueous solution storage tank 14, and then send...

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Abstract

The invention discloses a method and an apparatus for producing methyl formate or ethyl formate by comprehensively utilizing metronidazole hydroxylation synthesis wastewater, and solves the problems of high formic acid waste, difficulty for mixed salt treatment, very high difficulty for hydroxylation synthesis wastewater treatment, serious environmental pollution due to direct discharge and the like in the prior art. According to the process, alcohols are added for producing an esterification reaction to recover formic acid in the wastewater; and technological processes of distillation, rectification, crystallization, centrifugation and the like are added for separating and recovering formic acid in the wastewater on the premise of not influencing metronidazole preparation by a product, so that the difficult problem of metronidazole production wastewater treatment is radically solved, the metronidazole production cost is reduced, and the metronidazole yield is increased. The method has very good environmental, social and economic benefits, can be widely applied to metronidazole enterprises and has important practical significance.

Description

technical field [0001] The present invention belongs to the comprehensive recovery and utilization of chemical synthesis pharmaceutical production wastewater, specifically refers to a method and device for the comprehensive utilization of metronidazole hydroxylation synthesis wastewater to produce formic esters, the formic esters described in the present invention are only methyl formate and ethyl formate. Background technique [0002] Metronidazole is an antimicrobial agent and has been used by the World Health Organization as the drug of choice against anaerobic bacteria. The raw materials used for the hydroxylation of metronidazole are as follows: take formic acid as a catalyst, and sulfuric acid as an adjustment solvent; 2-methyl-5-nitroimidazole (nitrate) is a precursor compound; oxirane is a hydroxyethylation reagent ( hydroxylating agent). [0003] Metronidazole hydroxylation synthesis chemical reaction formula is as follows: [0004] C 4 h 5 N 3 o 2 +C 2 h 4...

Claims

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Application Information

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IPC IPC(8): C07C69/06C07C67/08C07C67/54
CPCC07C67/08C07C67/54C07C69/06
Inventor 张懿黄刚明张怀松
Owner 黄冈银河阿迪药业有限公司
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