CN104774143B - The circulation recovery method of formic acid solvent in metronidazole production process - Google Patents
The circulation recovery method of formic acid solvent in metronidazole production process Download PDFInfo
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- CN104774143B CN104774143B CN201410015717.3A CN201410015717A CN104774143B CN 104774143 B CN104774143 B CN 104774143B CN 201410015717 A CN201410015717 A CN 201410015717A CN 104774143 B CN104774143 B CN 104774143B
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Abstract
The invention belongs to the recovery method of dilute formic acid, especially relate to the circulation recovery method of formic acid solvent in a kind of metronidazole production process.It is characterized in that technological process is as follows: the moisture content in (1) thermal dehydration still removing phosphoric acid,diluted obtains thick polyphosphoric acid；(2) by thick polyphosphoric acid press-in water suction top of tower, dilution tailing edge packing layer dirty, after gradually become phosphoric acid,diluted flow to phosphoric acid,diluted storage still；(3) with pump, phosphoric acid,diluted is sent into dehydrating kettle；(4) the dilute formic acid steam that mass concentration is 20～80% is evaporated to obtain；(5) allow formic acid vapor first pass through the packing layer of vaporizer, remove solid entrainment in formic acid vapor；(6) then by there being the water suction tower of thick polyphosphoric acid to remove the moisture content in formic acid vapor；(7) formic acid vapor after concentrating is condensed into concentration formic acid and high liquid.Can be widely applied to Chemical Manufacture enterprise and a large amount of dilute formic acid solution produced are carried out dehydration recovery.
Description
One, technical field
This practicality invention belongs to the recovery method of dilute formic acid, especially relates to the circulation recovery method of formic acid solvent in a kind of metronidazole production process.
Two, background technology
Metronidazole is a kind of Effective Anti trichomoniasis, also various types of amebiasis, acne and vinasse nose can be treated, in recent years as a kind of antimicrobial, especially as anti-anaerobic agent, have has a broad antifungal spectrum, evident in efficacy, the medicine of resistance to bacterium strain is few, the feature that various administrations the most easily absorb and are distributed, by World Health Organization (WHO) (WHO) as the choice drug of anaerobe resistant.
At present it has been reported that the method for synthesis metronidazole be: 2-5-nitro imidazole is dissolved in formic acid solvent, gradually adds oxirane and sulphuric acid, react and to obtain hydroxylation liquid.First heating evaporation hydroxylation liquid obtains dilute formic acid aqueous solution, after add water and adjust pH with sodium hydroxide, place and cool down, crystallize, filter to obtain metronidazole.
Formic acid, also referred to as formic acid, molecular formula is HCOOH, colourless and have penetrating odor, and is corrosive, redness of bubbling after human skin contact.Formic acid is important industrial chemicals and solvent, is widely used in the industry such as pesticide, leather, dyestuff, medicine and rubber.In above-mentioned industrial process (such as metronidazole production process), produce substantial amounts of dilute formic acid solution.Owing to the boiling-point difference of formic acid Yu water only has 0.7 DEG C, and form constant boiling point with water, so being difficult to concentrate dilute formic acid with conventional rectificating method.How to concentrate dilute formic acid, existing way is a lot.Such as patent of invention " apparatus and method of intermittent azeotropic rectifying method purifying formic acid solution ", CN101596371A, perhaps pine forest etc..Its main thought is for make entrainer initially with hexamethylene, by dilute formic acid aqueous solution initial concentration that mass concentration is 10% to 30%；Re-using chlorobenzene and make entrainer, tower top the most constantly extraction chlorobenzene and the azeotropic mixture of water, the mixing composition of extraction chlorobenzene-formic acid-water when tower top temperature is at 95 DEG C-102 DEG C, after split-phase, the mass fraction of formic acid is up to 60%-70%；Finally using compression rectification, control pressure is at 4atm, and tower reactor can reach the concentration formic acid and high solution of about 80-85%；And for example patent of invention " new method that a kind of formic acid purifies ", CN101391945A, fourth Cheng Rong etc..Its thinking is the water sloughing in formic acid with anhydrous calcium chloride, and then distillation obtains concentration formic acid and high.But both schemes, the former cost of equipment is big, inferior separating effect, and the latter's intermittently operated labour cost is big, has acid mist pollution environment.Above-mentioned similar technique only has a small amount of production application, does not the most promote, and causes and has a large amount of dilute formic acid supply on market, cheap.Dilute formic acid is made direct discharging of waste water by some chemical enterprises, causes environmental pollution.
Three, summary of the invention
Present invention aim to solve above-mentioned technical problem, provide that a kind of equipment is simple, it is little to invest, yield is high for chemical enterprise, continuous production, the circulation recovery method of formic acid solvent in easy to operate metronidazole production process.
The technical scheme is that in metronidazole production process, the technological process of the circulation recovery method of formic acid solvent is as follows:
(1) utilize phosphoric acid circulation to concentrate the thermal dehydration still of dilute formic acid device, the moisture content in removing phosphoric acid,diluted, obtain thick polyphosphoric acid；
(2) by thick polyphosphoric acid press-in water suction top of tower, absorb moisture content dilution after, dirty along packing layer, after gradually become phosphoric acid,diluted, flow to phosphoric acid,diluted storage still；
(3) with pump, phosphoric acid,diluted is sent into dehydrating kettle.
(4) use evaporator evaporation hydroxylation liquid, obtain the dilute formic acid steam that mass concentration is 20～80%；
(5) allow formic acid vapor first pass through cold filling layer above vaporizer or have the dirty packing layer of charging dilute formic acid solution, remove solid entrainment in formic acid vapor；
(6) by there being the water suction tower of thick polyphosphoric acid, the most of moisture content in formic acid vapor is removed；
(7) formic acid vapor after concentrating becomes concentration formic acid and high liquid by condensing tube condensation.
Described phosphoric acid circulation concentrates dilute formic acid device, and (I has applied for utility model patent, Application No.: 201320486117.6) it is made up of parts such as vaporizer, storage still, water suction tower, condenser and storagetanks, filler and inlet valve is set above vaporizer, communicated by pipeline with between storage still above vaporizer filler, water suction tower is set above storage still, setting filler in water suction tower, top sets shower nozzle, is provided above dehydrating kettle.Leakage fluid dram is set bottom dehydrating kettle, it is connected with shower nozzle by the pipeline of band phosphoric acid valve, water suction tower side arranges venthole at tower top, it is connected by the air intake of pipeline with the condensing tube in condenser, the port of export of condensing tube is connected with formic acid storagetank by the pipeline of band product valve, condenser sets cooling water water intaking valve, and top sets coolant outlet；Storage still bottom discharging opening arranges Phosphoric Acid Circulating Pump, and its inlet tube accesses phosphoric acid storage still inner bottom part, and outlet inserts in dehydrating kettle, and dehydrating kettle upper side wall arranges Crude product input valve, and lower wall arranges and adds thermal medium inlet valve.
Having the beneficial effects that of patent of the present invention: owing to using phosphoric acid circulation dehydration, the recovery making formic acid solvent in metronidazole production process realizes continuous operation, can be widely applied to Chemical Manufacture enterprise and a large amount of dilute formic acid solution produced carry out dehydration recovery, its popularization and application will bring abundant economic benefit for enterprise.
Four, accompanying drawing explanation
Fig. 1 is the structural representation of the present invention
In figure: 1 is evaporating kettle, 2 is valve of slagging tap, and 3 is outlet valve, and 4 is inlet valve, 5 is steam valve, and 6 is pipeline, and 7 is storage still, and 8 is water suction tower, 9 is filler, and 10 is shower nozzle, and 11 is phosphoric acid valve, and 12 is condenser, 13 is condensing tube, and 14 is water intaking valve, and 15 is product valve, 16 is storagetank, and 17 is Crude product input valve, and 18 for adding thermal medium inlet valve, 19 is dehydrating kettle, and 20 is circulating pump, and 21 is filler.
Five, detailed description of the invention
When implementing the present invention, first add phosphoric acid,diluted to dehydrating kettle 19, open Crude product input valve 17 and add thermal medium inlet valve 18, the moisture in heating removing phosphoric acid,diluted；When still liquid temp to be drained off is raised to 150 350 DEG C, phosphoric acid,diluted becomes polyphosphoric acid；Then opening phosphoric acid valve 11, allow thick polyphosphoric acid flow into packing layer, while flow downward, limit absorbs moisture content, finally flows to phosphoric acid storage still 7.Then add to vaporizer 1 and be hydroxylated liquid in right amount, open heating steam valve 5 and cooling water water intaking valve 14 the most successively.After a while, the hydroxylation liquid boiling in vaporizer 1, the steam of generation rises to packing layer 21, removes solid entrainment, then from connecting bottom pipeline 6 entrance water suction tower 8.Steam is in water suction tower 8 during flowing, and the polyphosphoric acid on filled 9 surfaces of moisture content and highly concentrated phosphoric acid absorb.The steam rising to water suction tower 8 top enters the condensing tube 13 in condenser 12, is condensed into dense formic acid, flows to formic acid storagetank 16.When vaporizer 1 liquid level is less than discharging opening, open outlet valve 3 and inlet valve 4, and by hydroxylation liquid feed rate with add thermal medium inlet Flow-rate adjustment to certain value.When the phosphoric acid,diluted liquid level stored in still 7 reaches 1/2 to 2/3, automatically start circulating pump 20, phosphoric acid,diluted is sent into dehydrating kettle 19.
Claims (2)
1. the circulation recovery method of formic acid solvent in a metronidazole production process, it is characterised in that: technological process is as follows:
(1) utilize phosphoric acid circulation to concentrate the thermal dehydration still of dilute formic acid device, the moisture content in removing phosphoric acid,diluted, obtain thick polyphosphoric acid；
(2) by thick polyphosphoric acid press-in water suction top of tower, absorb moisture content dilution after, dirty along packing layer, after gradually become phosphoric acid,diluted, flow to phosphoric acid,diluted storage still；
(3) with pump, phosphoric acid,diluted is sent into dehydrating kettle；
(4) use evaporator evaporation hydroxylation liquid, obtain the dilute formic acid steam that mass concentration is 20～80%；
(5) allow formic acid vapor first pass through cold filling layer above vaporizer or have the dirty packing layer of charging dilute formic acid solution, remove solid entrainment in formic acid vapor；
(6) by there being the water suction tower of thick polyphosphoric acid, the most of moisture content in formic acid vapor is removed；
(7) formic acid vapor after concentrating becomes concentration formic acid and high liquid by condensing tube condensation.
The circulation recovery method of formic acid solvent in metronidazole production process the most according to claim 1, it is characterized in that: it is by vaporizer that the most described phosphoric acid circulation concentrates dilute formic acid device, storage still, water suction tower, condenser and storagetank part composition, filler and inlet valve is set above vaporizer, communicated by pipeline with between storage still above vaporizer filler, water suction tower is set above storage still, filler is set in water suction tower, top sets shower nozzle, it is provided above dehydrating kettle, leakage fluid dram is set bottom dehydrating kettle, it is connected with shower nozzle by the pipeline of band phosphoric acid valve, water suction tower side arranges venthole at tower top, it is connected by the air intake of pipeline with the condensing tube in condenser, the port of export of condensing tube is connected with formic acid storagetank by the pipeline of band product valve, condenser sets cooling water water intaking valve, top sets coolant outlet；Storage still bottom discharging opening arranges Phosphoric Acid Circulating Pump, and its inlet tube accesses phosphoric acid storage still inner bottom part, and outlet inserts in dehydrating kettle, and dehydrating kettle upper side wall arranges Crude product input valve, and lower wall arranges and adds thermal medium inlet valve.
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| CN201410015717.3A CN104774143B (en) | 2014-01-14 | 2014-01-14 | The circulation recovery method of formic acid solvent in metronidazole production process |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0652203A1 (en) * | 1994-04-07 | 1995-05-10 | Glitsch, Inc. | Method and apparatus for recovering carboxylic acids from dilute solutions |
| CN101391945A (en) * | 2008-10-27 | 2009-03-25 | 浙江工业大学 | Novel purification method for formic acid |
| CN102249203A (en) * | 2011-04-29 | 2011-11-23 | 南通京通石墨设备有限公司 | Phosphoric acid evaporation process and device thereof |
| CN103408082A (en) * | 2013-08-10 | 2013-11-27 | 黄冈师范学院 | Recovery method and device for formic acid solvent during metronidazole production |
-
2014
- 2014-01-14 CN CN201410015717.3A patent/CN104774143B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0652203A1 (en) * | 1994-04-07 | 1995-05-10 | Glitsch, Inc. | Method and apparatus for recovering carboxylic acids from dilute solutions |
| CN101391945A (en) * | 2008-10-27 | 2009-03-25 | 浙江工业大学 | Novel purification method for formic acid |
| CN102249203A (en) * | 2011-04-29 | 2011-11-23 | 南通京通石墨设备有限公司 | Phosphoric acid evaporation process and device thereof |
| CN103408082A (en) * | 2013-08-10 | 2013-11-27 | 黄冈师范学院 | Recovery method and device for formic acid solvent during metronidazole production |
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Inventor after: Zeng Zhouhua Inventor after: Ni Yong Inventor after: Xu Zhenqiang Inventor after: Chen Wen Inventor after: Wang Hainan Inventor after: Xie Yuqiao Inventor before: Zeng Zhouhua Inventor before: Xu Zhenqiang Inventor before: Chen Wen Inventor before: Wang Hainan Inventor before: Xie Yuqiao |
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Effective date of registration: 20161018 Address after: 438000 Huanggang Development Zone, Xingang, No. two, No. Road, No. 146 Patentee after: Huanggang Normal University Address before: 438000 Huanggang Development Zone, Xingang, No. two, No. Road, No. 146 Patentee before: Zeng Zhouhua |
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Effective date of registration: 20170601 Address after: 510000, No. 1 Industrial Avenue, new industrial park, Zengcheng District, Guangzhou, Guangdong Patentee after: Guangzhou Ouhua Pharmaceutical Co., Ltd. Address before: 438000 Huanggang Development Zone, Xingang, No. two, No. Road, No. 146 Patentee before: Huanggang Normal University |