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

Method used

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

Examples

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Example Embodiment

[0036] Example 1:

[0037] After the hydroxylation synthesis reaction is completed, the materials are transferred to the esterification reactor 4 to prepare for the esterification reaction. Assuming that the mass of formic acid added during the hydroxylation synthesis reaction is Q (Kg), calculate the amount of methanol to be added as follows: W Methanol =1.05×Q / 46×32, and then slowly added to the esterification reactor 4, after the addition is completed, control the temperature to be greater than or equal to 60℃, reflux for 2 hours, after the reaction is completed, then transfer the materials to the No. 1 distillation kettle 7 Distillation, the mixed gas that is distilled is directly sent to 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 methyl formate and methanol are distilled out, and then sent Into the rectifying tower for rectification and ...

Example Embodiment

[0041] Example 2:

[0042] The process of Example 2 is the same as that of Example 1.

[0043] The difference is that:

[0044] (1) The alcohol added to the esterification reactor 4 is ethanol, and the obtained esterification product is ethyl formate.

[0045] (2) Ethyl formate and water have an azeotropic point (54.23℃). The rectification process must adopt a double-tower (or three-tower) process. The double-tower process uses rectification tower 8 to distill ethyl formate and ethanol first, and then use The desiccant dehydration skips the azeotropic point, and then continues rectification and separation in the rectification tower 8. The fraction at 54±0.5°C is intercepted at the top of the tower to obtain more than 99% ethyl formate product; ethanol is obtained at the bottom of the tower And the entrained components of the distillate during evaporation in the previous process are discharged to the ethanol aqueous solution storage tank 14, and then sent to the sewage treatment stati...

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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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