CN103304371A - Intermittent extracting, distilling and separating method of methanol-methyl acrylate azeotropic mixture - Google Patents
Intermittent extracting, distilling and separating method of methanol-methyl acrylate azeotropic mixture Download PDFInfo
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- CN103304371A CN103304371A CN2013102713189A CN201310271318A CN103304371A CN 103304371 A CN103304371 A CN 103304371A CN 2013102713189 A CN2013102713189 A CN 2013102713189A CN 201310271318 A CN201310271318 A CN 201310271318A CN 103304371 A CN103304371 A CN 103304371A
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Abstract
The invention discloses an intermittent extracting, distilling and separating method of a methanol-methyl acrylate azeotropic mixture, and belongs to a separating technology of the methanol-methyl acrylate azeotropic mixture. The method comprises the steps of: taking ethylene glycol, methylbenzene, chlorobenzene, methyl-phenoxide or phenol as extracting agents, wherein the operation conditions of an extracting distillation tower are that: the mass ratio of the extracting agent to an overhead product is (0.5-1) to (10:1) at normal pressure or reduced pressure; the feeding temperature of the extracting agent is 20-60 DEG C, controlling different temperature and different reflux ratios of the extracting distillation tower, respectively extracting a methanol product, a methanol-methyl acrylate transition section I, a methyl acrylate product, and a methyl acrylate-extracting agent transition section II from the top of the extracting distillation tower; pumping the extracting agent into a high-level storage slot when the extracting agent components of a heating kettle achieve the requirements; feeding to carrying out next batch of intermittent extracting, distilling and separating. The intermittent extracting, distilling and separating method has the advantages that the methanol-methyl acrylate azeotropic system is destroyed by adopting the extracting agent; high-purity methanol and a methyl acrylate product are separated out; operation on the single tower is flexible; the equipment cost is low.
Description
Technical field
The present invention relates to the intermittent extraction, distillation and separation method of a kind of methyl alcohol-methyl acrylate azeotropic mixture, belong to the isolation technique of methyl alcohol-methyl acrylate 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 methyl acrylate is: C
4H
6O
2, can be used as organic synthesis intermediate, also be the monomer of synthesising macromolecule copolymer.The methyl alcohol that produces in process of production-methyl acrylate mixture, owing to forming azeotrope (massfraction of methyl alcohol is 54%), methyl alcohol and methyl acrylate 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-methyl acrylate 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-methyl acrylate 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-methyl acrylate azeotropic mixture.The isolated methyl alcohol of the method, methyl acrylate product purity are high.
The present invention is realized by following technical proposals.Employing 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-methyl acrylate azeotropic mixture, it is characterized in that comprising following process: take ethylene glycol, toluene, chlorobenzene, methyl-phenoxide or phenol as 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 66-79 ℃, by overhead extraction methyl alcohol-methyl acrylate transition section I, and stop to add extraction agent with reflux ratio 3:1-10:1; When extracting rectifying cat head temperature is 79-80.5 ℃, with reflux ratio 0.5:1-6:1 by the overhead extraction methyl acrylate; When extracting rectifying cat head temperature surpasses 80.5 ℃, by overhead extraction methyl acrylate-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-methyl acrylate mixture and transition section I and transition section II, lower batch of batch extracting rectified separation.
The idiographic flow (see photo): methyl alcohol-methyl acrylate 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 methyl acrylate content reaches product requirement in the extracting rectifying cat head overhead product, the material of extraction enters receiving tank 7, when methyl acrylate 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-methyl acrylate azeotropic system, isolate high-purity methyl alcohol, methyl acrylate 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-methyl acrylate product receiving tank, 8-transition section II receiving tank, 9-vacuum pump.
Embodiment
Embodiment 1: adopt batch extraction rectification device, (wherein methyl alcohol 54% to drop into 500 L methyl alcohol-methyl acrylate azeotropic mixture at heating kettle, methyl acrylate 46%, be mass percent), testing selected extraction agent is toluene, open heating kettle thermal source and condensation 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 66-79 ℃, extraction methyl alcohol-methyl acrylate transition section, and stop to add extraction agent, reflux ratio is 9:1, when extracting rectifying cat head temperature is 79-80.5 ℃, during methyl acrylate content in the overhead product 〉=99%, receive methyl acrylate, reflux ratio is 4:1, when extracting rectifying cat head temperature surpasses 80.5 ℃, reflux ratio 5:1, extraction methyl acrylate-toluene transition section II, when toluene level in the extracting rectifying cat head overhead product 〉=99%, stop, heating kettle is high purity toluene.
Embodiment 2: adopt batch extraction rectification device, (wherein methyl alcohol 53% to drop into 500 L methyl alcohol-methyl acrylate azeotropic mixture at heating kettle, methyl acrylate 47%, 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 66-79 ℃, extraction methyl alcohol-methyl acrylate transition section, and stop to add extraction agent, reflux ratio is 10:1, when extracting rectifying cat head temperature is 79-80.5 ℃, during methyl acrylate content in the overhead product 〉=99%, receive methyl acrylate, reflux ratio is 4:1, when extracting rectifying cat head temperature above 80.5 ℃, reflux ratio 6:1, extraction methyl acrylate-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 one, and extraction agent adopts chlorobenzene.
Embodiment 4: experimental installation and working method are with embodiment one, and extraction agent adopts methyl-phenoxide.
Embodiment 5: experimental installation and working method are with embodiment two, and extraction agent adopts phenol.
Claims (3)
1. the intermittent extraction, distillation and separation method of methyl alcohol-methyl acrylate 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-methyl acrylate azeotropic mixture.
2. the intermittent extraction, distillation and separation method of a kind of methyl alcohol as claimed in claim 1-methyl acrylate azeotropic mixture is characterized in that take ethylene glycol, toluene, chlorobenzene, methyl-phenoxide or phenol as extraction agent.
3. the intermittent extraction, distillation and separation method of a kind of methyl alcohol as claimed in claim 1-methyl acrylate 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 66-79 ℃, by overhead extraction methyl alcohol-methyl acrylate transition section I, and stop to add extraction agent with reflux ratio 3:1-10:1; When extracting rectifying cat head temperature is 79-80.5 ℃, with reflux ratio 0.5:1-6:1 by the overhead extraction methyl acrylate; When extracting rectifying cat head temperature surpasses 80.5 ℃, by overhead extraction methyl acrylate-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-methyl acrylate mixture and transition section I and transition section II, lower batch of batch extracting rectified separation.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311418A (en) * | 2014-11-06 | 2015-01-28 | 旭阳化学技术研究院有限公司 | Azeotropic distillation separating and treatment method for methanol and methyl acrylate mixture |
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2013
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| CN104311418A (en) * | 2014-11-06 | 2015-01-28 | 旭阳化学技术研究院有限公司 | Azeotropic distillation separating and treatment method for methanol and methyl acrylate mixture |
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Application publication date: 20130918 |