CN103319309A - Interrupted extraction, rectification and separation method of methanol-nitromethane azeotrope - Google Patents
Interrupted extraction, rectification and separation method of methanol-nitromethane azeotrope Download PDFInfo
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- CN103319309A CN103319309A CN201310270986XA CN201310270986A CN103319309A CN 103319309 A CN103319309 A CN 103319309A CN 201310270986X A CN201310270986X A CN 201310270986XA CN 201310270986 A CN201310270986 A CN 201310270986A CN 103319309 A CN103319309 A CN 103319309A
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- nitromethane
- methanol
- nitromethane 99min
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Abstract
The invention discloses an interrupted extraction, rectification and separation method of a methanol-nitromethane azeotrope. The method belongs to a separation technology of the methanol-nitromethane azeotrope. According to the method, pentanol, ethylene glycol, 1, 2-propanediol, 1, 3-propanediol, glycerol or N, N-dimethylformamide is taken as an extraction agent, an extraction and rectification tower is operated at normal pressure or reduced pressure, the weight ratio of the extraction agent to distillates at the top of the tower is 0.5: 1-10: 1, the feeding temperature of the extraction agent is 20-60 DEG C, the different temperatures and the different reflux ratios at the top of the extraction and rectification tower are controlled, and a methanol product, a methanol-nitromethane transition section I, a nitromethane product and a nitromethane-extraction agent transition section II are respectively produced; and when the composition of the extraction agent of a heating kettle achieves the requirements, the extraction agent is pumped into a high-level storage tank, and feeding is performed for performing the next batch of interrupted extraction, rectification and separation. The method disclosed by the invention has the advantages that, the extraction agent is adopted for damaging a methanol-nitromethane azeotropic system, the high-purity methanol and the nitromethane products are separated, the single tower is flexible to operate, and the cost of equipment is low.
Description
Technical field
The present invention relates to the intermittent extraction, distillation and separation method of a kind of methyl alcohol-Nitromethane 99Min. azeotropic mixture, belong to the isolation technique of methyl alcohol-Nitromethane 99Min. azeotropic mixture.
Background technology
Extracting rectifying is a kind of special extract rectification isolation technique, the separation of applicable azeotropic system.Add continuously extraction agent by the top toward rectifying tower and reach the separation purpose with the relative volatility that changes between stock blend.The batch extracting rectified advantage that has merged batch fractionating and extracting rectifying, flexible operation can separate a plurality of components by a tower, and facility investment is little, is applicable to separating of short run azeotropic system and the system of closely boiling.The chemical structural formula of Nitromethane 99Min. is: CH
3NO
2, be colourless oil liquid, can be used for organic synthesis, also can be used as organic solvent.The methyl alcohol that produces in process of production-Nitromethane 99Min. mixture, owing to forming azeotrope (massfraction of methyl alcohol is 92%), methyl alcohol and Nitromethane 99Min. be difficult to separate, as not reclaiming, not only pollute the environment, and the increase production cost, the separation method of therefore developing methyl alcohol-Nitromethane 99Min. azeotropic mixture has important meaning.About article and the patent of extracting rectifying aspect are a lot, there is not yet the data of the methyl alcohol published-Nitromethane 99Min. azeotropic system separation of extractive distillation aspect.
Summary of the invention
The object of the present invention is to provide the intermittent extraction, distillation and separation method of a kind of methyl alcohol-Nitromethane 99Min. azeotropic mixture.The isolated methyl alcohol of the method, Nitromethane 99Min. product purity are high.
The present invention is realized by following technical proposals.Employing comprises extractive distillation column, heating kettle, and condenser, high-level storage groove, receiving tank, the extracting rectifying device that products pot and vacuum pump consist of, batch extracting rectified separation of methanol-Nitromethane 99Min. azeotropic mixture is characterized in that comprising following process:
With amylalcohol, ethylene glycol, 1,2-propylene glycol, 1, ammediol, glycerol or N, dinethylformamide is extraction agent, extractive distillation column operates with following condition, under normal pressure or decompression, entering the extraction agent of extractive distillation column and the mass ratio of this overhead product is 0.5:1-10:1, and the feeding temperature of extraction agent is 20-60 ℃.When extracting rectifying cat head temperature is 64.2-66 ℃, with reflux ratio 1:1-6:1 by the qualified methanol product of overhead extraction methanol content; When extracting rectifying cat head temperature is 66-100.2 ℃, by overhead extraction methyl alcohol-Nitromethane 99Min. transition section I, and stop to add extraction agent with reflux ratio 3:1-10:1; When extracting rectifying cat head temperature is 100.2-102 ℃, with reflux ratio 0.5:1-6:1 by the overhead extraction Nitromethane 99Min.; When extracting rectifying cat head temperature surpasses 102 ℃, by overhead extraction Nitromethane 99Min.-extraction agent transition section II, if the boiling point of extraction agent equals and is higher than 160 ℃, select the rectification under vacuum operation, working pressure 10 with reflux ratio 1:1-12:1
3-10
5Pa; When the extraction agent of heating kettle forms when reaching requirement, the cooling of stopping pumps into high-level storage groove with extraction agent, heating kettle pack into new a collection of methyl alcohol-Nitromethane 99Min. mixture and transition section I and transition section II, lower batch of batch extracting rectified separation.
The idiographic flow (see photo): methyl alcohol-Nitromethane 99Min. mixture adds in the heating kettle 3, open the thermal source of heating kettle and the low-temperature receiver of condenser 4, until the extracting rectifying cat head reflux and tower top temperature stable after, extraction agent is introduced into extractive distillation column 2 tops from high-order storage tank 1, total reflux for some time, discharging when methanol content reaches requirement, enter receiving tank 4, when methanol content is lower than product requirement in the extracting rectifying cat head overhead product, the material of overhead extraction enters transition section I receiving tank 6(when methanol content forms less than azeotropic in the extracting rectifying cat head overhead product, stop to add extraction agent), when Nitromethane 99Min. content reaches product requirement in the extracting rectifying cat head overhead product, the material of extraction enters receiving tank 7, when Nitromethane 99Min. content is lower than product requirement in the extracting rectifying cat head overhead product, the material of extraction enters transition section II receiving tank 8, when the composition of heating kettle extraction agent reaches requirement, stops.Heating kettle is high-purity extraction agent, squeezes into high-level storage groove 1 and recycles.The material of transition section I and II is put in the heating kettle 3 during next batch rectifying again.
The invention has the advantages that and use rationally effectively extraction agent destruction methyl alcohol-Nitromethane 99Min. azeotropic system, isolate high-purity methyl alcohol, Nitromethane 99Min. product, adopt single tower operation, flexible operation, cost of equipment less investment.
Description of drawings
Fig. 1 is apparatus of the present invention and schematic flow sheet.Among the figure: 1-high-level storage groove, 2-extractive distillation column, 3-heating kettle, 4-condenser, 5-methanol product receiving tank, 6-transition section I receiving tank, 7-Nitromethane 99Min. product receiving tank, 8-transition section II receiving tank, 9-vacuum pump.
Embodiment
Embodiment 1: adopt batch extraction rectification device, (wherein methyl alcohol 92% to drop into 500 L methyl alcohol-Nitromethane 99Min. azeotropic mixture at heating kettle, Nitromethane 99Min. 8%, be mass percent), testing selected extraction agent is amylalcohol, open heating kettle thermal source and condenser low-temperature receiver, after the extracting rectifying cat head refluxed for some time, tower top temperature was stable, add extraction agent, the cat head place is being closed in the extractant feed position, and the control extraction agent adds speed 500 L/h, total reflux operation, when extracting rectifying cat head temperature is 64.2-66 ℃, methanol content in the overhead product 〉=99% beginning discharging, reflux ratio is 3:1, discharging speed is 200 L/h.When extracting rectifying cat head temperature is 66-100.2 ℃, extraction methyl alcohol-Nitromethane 99Min. transition section, and stop to add extraction agent, reflux ratio is 9:1, when extracting rectifying cat head temperature is 100.2-102 ℃, during Nitromethane 99Min. content in the overhead product 〉=99%, receive Nitromethane 99Min., reflux ratio is 4:1, when extracting rectifying cat head temperature surpasses 102 ℃, reflux ratio 5:1, extraction Nitromethane 99Min.-amylalcohol transition section II, when amylalcohol content in the extracting rectifying cat head overhead product 〉=99%, stop, heating kettle is high-purity amylalcohol.
Embodiment 2: adopt batch extraction rectification device, (wherein methyl alcohol 91% to drop into 500 L methyl alcohol-Nitromethane 99Min. azeotropic mixture at heating kettle, Nitromethane 99Min. 9%, be mass percent), testing selected extraction agent is ethylene glycol, open heating kettle thermal source and condenser low-temperature receiver, after the extracting rectifying cat head refluxed for some time, tower top temperature was stable, add extraction agent, the cat head place is being closed in the extractant feed position, and the control extraction agent adds speed 800 L/h, total reflux operation, when extracting rectifying cat head temperature is 64.2-66 ℃, methanol content in the overhead product 〉=99% beginning discharging, reflux ratio is 2:1, discharging speed is 300 L/h.When extracting rectifying cat head temperature is 66-100.2 ℃, extraction methyl alcohol-Nitromethane 99Min. transition section, and stop to add extraction agent, reflux ratio is 10:1, when extracting rectifying cat head temperature is 100.2-102 ℃, during Nitromethane 99Min. content in the overhead product 〉=99%, receive Nitromethane 99Min., reflux ratio is 4:1, when extracting rectifying cat head temperature above 102 ℃, reflux ratio 6:1, extraction Nitromethane 99Min.-ethylene glycol transition section II, when the heating kettle temperature above 160 ℃, stop, naturally cooling when still temperature to be heated drops to 50 ℃, is opened heating kettle, decompression operation, vacuum degree control is at 70000Pa, and behind the trim the top of column, total reflux operation is after 30 minutes, with reflux ratio 9:1 discharging, when ethylene glycol content in the extracting rectifying cat head overhead product 〉=99%, stop, heating kettle is high-purity ethylene glycol.
Embodiment 3: experimental installation and working method are with embodiment two, and extraction agent adopts 1,2-PD.
Embodiment 4: experimental installation and working method are with embodiment two, and extraction agent adopts 1,3-PD.
Embodiment 5: experimental installation and working method are with embodiment two, and extraction agent adopts glycerol.
Embodiment 6: experimental installation and working method are with embodiment one, and extraction agent adopts DMF.
Claims (3)
1. the intermittent extraction, distillation and separation method of methyl alcohol-Nitromethane 99Min. azeotropic mixture, the method adopts and comprises extractive distillation column, heating kettle, condenser, high-level storage groove, receiving tank, the extracting rectifying device that products pot and vacuum pump consist of, batch extracting rectified separation of methanol-Nitromethane 99Min. azeotropic mixture.
2. the intermittent extraction, distillation and separation method of a kind of methyl alcohol as claimed in claim 1-Nitromethane 99Min. azeotropic mixture is characterized in that take amylalcohol, ethylene glycol, 1,2-PD, 1,3-PD, glycerol or DMF as extraction agent.
3. the intermittent extraction, distillation and separation method of a kind of methyl alcohol as claimed in claim 1-Nitromethane 99Min. azeotropic mixture, it is characterized in that comprising following process: extractive distillation column operates with following condition, under normal pressure or decompression, entering the extraction agent of extractive distillation column and the mass ratio of this overhead product is 0.5:1-10:1, the feeding temperature of extraction agent is 20-60 ℃, when extracting rectifying cat head temperature is 64.2-66 ℃, with reflux ratio 1:1-6:1 by the qualified methanol product of overhead extraction methanol content; When extracting rectifying cat head temperature is 66-100.2 ℃, by overhead extraction methyl alcohol-Nitromethane 99Min. transition section I, and stop to add extraction agent with reflux ratio 3:1-10:1; When extracting rectifying cat head temperature is 100.2-102 ℃, with reflux ratio 0.5:1-6:1 by the overhead extraction Nitromethane 99Min.; When extracting rectifying cat head temperature surpasses 102 ℃, by overhead extraction Nitromethane 99Min.-extraction agent transition section II, if the boiling point of extraction agent equals and is higher than 160 ℃, select the rectification under vacuum operation, working pressure 10 with reflux ratio 1:1-12:1
3-10
5Pa; When the extraction agent of heating kettle forms when reaching requirement, the cooling of stopping pumps into high-level storage groove with extraction agent, heating kettle pack into new a collection of methyl alcohol-Nitromethane 99Min. mixture and transition section I and transition section II, lower batch of batch extracting rectified separation.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237404A (en) * | 2015-09-17 | 2016-01-13 | 湖北远大富驰医药化工股份有限公司 | Recovery method for water-phase nitromethane |
| CN106995375A (en) * | 2017-04-18 | 2017-08-01 | 青岛科技大学 | It is a kind of to be thermally integrated the method that variable-pressure rectification separates nitre methane methanol hexamethylene azeotropic mixture |
| CN113214086A (en) * | 2021-05-26 | 2021-08-06 | 山东中盛药化设备有限公司 | Continuous rectification and purification process of nitromethane |
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| CN102527072A (en) * | 2012-03-23 | 2012-07-04 | 济南大学 | Batch extraction distillation separation method for propyl alcohol-propyl formate azeotropic mixture |
| CN102584525A (en) * | 2012-03-23 | 2012-07-18 | 济南大学 | Intermittent extractive distillation separation method of methanol-methyl propionate azeotropic mixtures |
| CN102627536A (en) * | 2012-03-23 | 2012-08-08 | 济南大学 | Batch extractive distillation separation method of methylal-methanol azeotropic mixture |
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2013
- 2013-07-01 CN CN201310270986XA patent/CN103319309A/en active Pending
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| CN102527072A (en) * | 2012-03-23 | 2012-07-04 | 济南大学 | Batch extraction distillation separation method for propyl alcohol-propyl formate azeotropic mixture |
| CN102584525A (en) * | 2012-03-23 | 2012-07-18 | 济南大学 | Intermittent extractive distillation separation method of methanol-methyl propionate azeotropic mixtures |
| CN102627536A (en) * | 2012-03-23 | 2012-08-08 | 济南大学 | Batch extractive distillation separation method of methylal-methanol azeotropic mixture |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237404A (en) * | 2015-09-17 | 2016-01-13 | 湖北远大富驰医药化工股份有限公司 | Recovery method for water-phase nitromethane |
| CN105237404B (en) * | 2015-09-17 | 2018-01-09 | 湖北远大富驰医药化工股份有限公司 | A kind of aqueous phase nitromethane recovery method |
| CN106995375A (en) * | 2017-04-18 | 2017-08-01 | 青岛科技大学 | It is a kind of to be thermally integrated the method that variable-pressure rectification separates nitre methane methanol hexamethylene azeotropic mixture |
| CN113214086A (en) * | 2021-05-26 | 2021-08-06 | 山东中盛药化设备有限公司 | Continuous rectification and purification process of nitromethane |
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Application publication date: 20130925 |