CN102527072B - Batch extraction distillation separation method for propyl alcohol-propyl formate azeotropic mixture - Google Patents
Batch extraction distillation separation method for propyl alcohol-propyl formate azeotropic mixture Download PDFInfo
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- CN102527072B CN102527072B CN201210078711.1A CN201210078711A CN102527072B CN 102527072 B CN102527072 B CN 102527072B CN 201210078711 A CN201210078711 A CN 201210078711A CN 102527072 B CN102527072 B CN 102527072B
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Abstract
The invention discloses a batch extraction distillation separation method for a propyl alcohol-propyl formate azeotropic mixture, which belongs to the separation technique for the propyl alcohol-propyl formate azeotropic mixture. The method comprises utilizing isobutanol as extractant, enabling an extraction distillation tower to operate under the following conditions that the mass ratio of the extractant to tower top distillate is 0.5:1-10:1 and material inlet temperature of the extractant is 20-60 DEG C, controlling the extraction distillation tower top to have different temperatures and different reflux ratios, respectively extracting a propyl formate product, a propyl alcohol-propyl formate transition section I, a propyl alcohol product and a propyl alcohol- extractant transition section II, pumping the extractant into a high-position tank when extractant compositions of a heating kettle reach the requirements, and feeding materials to perform next batch extraction distillation separation. The batch extraction distillation separation method has the advantages that the single-tower equipment is low in cost and flexible in operation, and the extractant is utilized to destroy a propyl alcohol-propyl formate azeotropic system to separate out high-purity propyl alcohol and propyl formate products.
Description
Technical field
The present invention relates to a kind of intermittent extraction, distillation and separation method of propyl alcohol-propyl formate azeotropic mixture, belong to the isolation technics of propyl alcohol-propyl formate azeotropic mixture.
Background technology
Extracting rectifying is a kind of special extract rectification isolation technics, the separation of applicable azeotropic system.By the top toward rectifying column, add continuously extractant to reach separated object with the relative volatility changing between stock blend.The batch extracting rectified advantage that has merged batch fractionating and extracting rectifying, flexible operation, can separated a plurality of components by a tower, and equipment investment is little, is applicable to the separated of small lot azeotropic system and the system of closely boiling.The chemical structural formula of propyl formate is: C4H8O2, as solvent and manufacture spices, also can be used as organic synthesis intermediate.Propyl alcohol-propyl formate the mixture producing in process of production, because propyl alcohol and propyl formate form azeotropic mixture (mass fraction of propyl alcohol is 9.8%), be difficult to separated, if do not reclaimed, not only pollute the environment, and increase production cost, the separation method of therefore developing propyl alcohol-propyl formate azeotropic mixture has important meaning.About article and the patent of extracting rectifying aspect are a lot, there is not yet the data of propyl alcohol-propyl formate azeotropic system separation of extractive distillation aspect of publishing.
Summary of the invention
The object of the present invention is to provide a kind of intermittent extraction, distillation and separation method of propyl alcohol-propyl formate azeotropic mixture.The isolated propyl alcohol of the method, propyl formate 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 vavuum pump form, batch extracting rectified separated propyl alcohol-propyl formate azeotropic mixture, is characterized in that comprising following process:
Take isobutanol as extractant, and extractive distillation column operates with following condition, and under normal pressure or decompression, entering the extractant of extractive distillation column and the mass ratio of this overhead is 0.5: 1-10: 1, and the feeding temperature of extractant is 20-60 ℃.When extracting rectifying tower top temperature is 80.9-81.6 ℃, with reflux ratio 1: 1-6: 1 by the qualified propyl formate product of overhead extraction propyl formate content; When extracting rectifying tower top temperature is 81.6-96.8 ℃, with reflux ratio 3: 1-10: 1 by overhead extraction propyl alcohol-propyl formate changeover portion I, and stops adding extractant; When extracting rectifying tower top temperature is 96.8-97.5 ℃, with reflux ratio 0.5: 1-6: 1 by overhead extraction propyl alcohol; When extracting rectifying tower top temperature surpasses 97.5 ℃, with reflux ratio 1: 1-12: 1 by overhead extraction propyl alcohol-extractant changeover portion II; When the extractant composition of heating kettle reaches requirement, stop cooling, extractant is pumped into high-level storage groove, heating kettle packs new a collection of propyl alcohol-propyl formate mixture and changeover portion I and changeover portion II into, lower batch of batch extracting rectified separation.
Idiographic flow (see photo): propyl alcohol-propyl formate mixture adds in heating kettle 3, open the thermal source of heating kettle and the low-temperature receiver of condenser 4, until extracting rectifying tower top reflux and tower top temperature stable after, extractant is introduced into extractive distillation column 2 tops from high-order storage tank 1, infinite reflux a period of time, discharging when propyl formate content reaches requirement, enter receiving tank 4, when in extracting rectifying tower top distillate, propyl formate content is lower than product requirement, the material of overhead extraction enters changeover portion I receiving tank 6 (when propyl formate content is less than azeotropic composition in extracting rectifying tower top distillate, stop adding extractant), when in extracting rectifying tower top distillate, propyl alcohol content reaches product requirement, the material of extraction enters receiving tank 7, when in extracting rectifying tower top distillate, propyl alcohol content is lower than product requirement, the material of extraction enters changeover portion II receiving tank 8, when the composition of heating kettle extractant reaches requirement, stop.Heating kettle is high-purity extractant, squeezes into high-level storage groove 1 and recycles.The material of changeover portion I and II is put in heating kettle 3 during next group rectifying again.
The invention has the advantages that and use rationally effectively extractant to destroy propyl alcohol-propyl formate azeotropic system, isolate high-purity propyl alcohol, propyl formate product, adopt single tower operation, flexible operation, cost of equipment less investment.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention and schematic flow sheet.
In figure: 1-high-level storage groove, 2-extractive distillation column, 3-heating kettle, 4-condenser, 5-propyl formate product receiving tank, 6-changeover portion I receiving tank, 7-propyl alcohol product receiving tank, 8-changeover portion II receiving tank, 9-vavuum pump.
The specific embodiment
Embodiment mono-
Adopt batch extraction rectification device, (wherein propyl alcohol 48% at heating kettle, to drop into 500L propyl alcohol-propyl formate azeotropic mixture, propyl formate 52%, be mass percent), extractant is isobutanol, open heating kettle thermal source and condenser low-temperature receiver, until extracting rectifying tower top, reflux after a period of time, tower top temperature is stable, add extractant, tower top place is being closed in extractant feed position, control extractant and add speed 500L/h, total reflux operation, when extracting rectifying tower top temperature is 80.9-81.6 ℃, in distillate, propyl formate content >=99% starts discharging, reflux ratio is 3: 1, discharging speed is 200L/h.When extracting rectifying tower top temperature is 81.6-96.8 ℃, extraction propyl alcohol-propyl formate changeover portion, and stop adding extractant, reflux ratio is 9: 1, when extracting rectifying tower top temperature is 96.8-97.5 ℃, in overhead during propyl alcohol content >=99%, receive propyl alcohol, reflux ratio is 4: 1, when extracting rectifying tower top temperature surpasses 97.5 ℃, reflux ratio 5: 1, extraction propyl alcohol-isobutanol changeover portion II, in extracting rectifying tower top distillate, during isobutanol content >=99%, stop, heating kettle is high-purity isobutanol.
Embodiment bis-
Adopt batch extraction rectification device, (wherein propyl alcohol 10% at heating kettle, to drop into 500L propyl alcohol-propyl formate azeotropic mixture, propyl formate 90%, be mass percent), extractant is isobutanol, open heating kettle thermal source and condenser low-temperature receiver, until extracting rectifying tower top, reflux after a period of time, tower top temperature is stable, add extractant, tower top place is being closed in extractant feed position, control extractant and add speed 800L/h, total reflux operation, when extracting rectifying tower top temperature is 80.9-81.6 ℃, in distillate, propyl formate content >=99% starts discharging, reflux ratio is 2: 1, discharging speed is 300L/h.When extracting rectifying tower top temperature is 81.6-96.8 ℃, extraction propyl alcohol-propyl formate changeover portion, and stop adding extractant, reflux ratio is 10: 1, when extracting rectifying tower top temperature is 96.8-97.5 ℃, in overhead during propyl alcohol content >=99%, receive propyl alcohol, reflux ratio is 4: 1, when extracting rectifying tower top temperature surpasses 97.5 ℃, reflux ratio 6: 1, extraction propyl alcohol-isobutanol changeover portion II, in extracting rectifying tower top distillate, during isobutanol content >=99%, stop, heating kettle is high-purity isobutanol.
Claims (1)
1. the intermittent extraction, distillation and separation method of propyl alcohol-propyl formate 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 vavuum pump form, batch extracting rectified separated propyl alcohol-propyl formate azeotropic mixture, it is characterized in that take that isobutanol is as extractant, comprise following process: extractive distillation column operates with following condition, under normal pressure or decompression, entering the extractant of extractive distillation column and the mass ratio of overhead is 0.5: 1-10: 1, the feeding temperature of extractant is 20-60 ℃, when extracting rectifying tower top temperature is 80.9-81.6 ℃, with reflux ratio 1: 1-6: 1 by the qualified propyl formate product of overhead extraction propyl formate content, when extracting rectifying tower top temperature is 81.6-96.8 ℃, with reflux ratio 3: 1-10: 1 by overhead extraction propyl alcohol-propyl formate changeover portion I, and stops adding extractant, when extracting rectifying tower top temperature is 96.8-97.5 ℃, with reflux ratio 0.5: 1-6: 1 by overhead extraction propyl alcohol, when extracting rectifying tower top temperature surpasses 97.5 ℃, with reflux ratio 1: 1-12: 1 by overhead extraction propyl alcohol-extractant changeover portion II, when the extractant composition of heating kettle reaches requirement, stop cooling, extractant is pumped into high-level storage groove, heating kettle packs new a collection of propyl alcohol-propyl formate mixture and changeover portion I and changeover portion II into, lower batch of batch extracting rectified separation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210078711.1A CN102527072B (en) | 2012-03-23 | 2012-03-23 | Batch extraction distillation separation method for propyl alcohol-propyl formate azeotropic mixture |
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| CN201210078711.1A CN102527072B (en) | 2012-03-23 | 2012-03-23 | Batch extraction distillation separation method for propyl alcohol-propyl formate azeotropic mixture |
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| CN102527072B true CN102527072B (en) | 2014-08-13 |
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| CN103304371A (en) * | 2013-07-01 | 2013-09-18 | 济南大学 | Intermittent extracting, distilling and separating method of methanol-methyl acrylate azeotropic mixture |
| CN103319309A (en) * | 2013-07-01 | 2013-09-25 | 济南大学 | Interrupted extraction, rectification and separation method of methanol-nitromethane azeotrope |
| CN105968006B (en) * | 2016-05-24 | 2019-01-25 | 济南大学 | A kind of separation method of propyl acetate-allyl alcohol mixture |
| CN110681173A (en) * | 2019-10-23 | 2020-01-14 | 广州首联环境工程有限公司 | Multifunctional waste organic solvent recovery device and application thereof |
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| US5458741A (en) * | 1994-01-14 | 1995-10-17 | Lloyd Berg | Separation of benzene from close boiling hydrocarbons by extractive distillation |
| CN100531845C (en) * | 2007-12-05 | 2009-08-26 | 天津大学 | Salt-adding intermittent extraction, rectified separation method of acetonitrile-water azeotropic mixture |
| CN102180791A (en) * | 2011-04-13 | 2011-09-14 | 天津大学 | Method for separating methyl acetate-methanol mixture by ionic liquid intermittent extractive rectification |
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