CN102527072A - 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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- CN102527072A CN102527072A CN2012100787111A CN201210078711A CN102527072A CN 102527072 A CN102527072 A CN 102527072A CN 2012100787111 A CN2012100787111 A CN 2012100787111A CN 201210078711 A CN201210078711 A CN 201210078711A CN 102527072 A CN102527072 A CN 102527072A
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- propyl alcohol
- propyl formate
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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 the intermittent extraction, distillation and separation method of a kind 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, is suitable for the separation of azeotropic system.Add extractant continuously through top and reach the separation purpose with the relative volatility that changes between stock blend toward rectifying column.The batch extracting rectified advantage that has merged batch fractionating and extracting rectifying, flexible operation can separate a plurality of components through a tower, and equipment investment is little, is applicable to separating of the small lot azeotropic system and the system of closely boiling.The chemical structural formula of propyl formate is: C4H8O2 as solvent and manufacturing spices, also can be used as organic synthesis intermediate.Propyl alcohol-propyl formate the mixture that produces in process of production; Owing to forming azeotropic mixture (mass fraction of propyl alcohol is 9.8%), propyl alcohol and propyl formate be difficult to separate; As do not reclaim; 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 the article and the patent of extracting rectifying aspect a lot, the data of the propyl alcohol that Shang Weijian publishes-propyl formate azeotropic system extracting rectifying separation 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 propyl alcohol-propyl formate azeotropic mixture.The isolated propyl alcohol of this method, propyl formate product purity height.
The present invention realizes through following technical proposals.Employing comprises extractive distillation column, heating kettle, and condenser, high-level storage groove, receiving tank, the extracting rectifying device that product jar and vavuum pump constitute, batch extracting rectified separation propyl alcohol-propyl formate azeotropic mixture is characterized in that comprising following process:
With the isobutanol is extractant, and extractive distillation column is operated with following condition, and under normal pressure or decompression, getting into 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 cat head temperature is 80.9-81.6 ℃, with reflux ratio 1: 1-6: 1 by the qualified propyl formate product of cat head extraction propyl formate content; When extracting rectifying cat head temperature is 81.6-96.8 ℃, with reflux ratio 3: 1-10: 1 by cat head extraction propyl alcohol-propyl formate changeover portion I, and stops to add extractant; When extracting rectifying cat head temperature is 96.8-97.5 ℃, with reflux ratio 0.5: 1-6: 1 by cat head extraction propyl alcohol; When extracting rectifying cat head temperature surpasses 97.5 ℃, with reflux ratio 1: 1-12: 1 by cat head extraction propyl alcohol-extractant changeover portion II; Form when reaching requirement when the extractant of heating kettle, the cooling of stopping pumps into high-level storage groove with extractant, heating kettle pack into new a collection of propyl alcohol-propyl formate mixture and changeover portion I and changeover portion II, following batch of batch extracting rectified separation.
Idiographic flow (seeing accompanying drawing): propyl alcohol-propyl formate mixture adds in the heating kettle 3, opens the thermal source and the low-temperature receiver of condenser 4 of heating kettle, treats that the extracting rectifying cat head refluxes and after tower top temperature stablizes; Extractant is introduced into extractive distillation column 2 tops, infinite reflux a period of time, discharging when propyl formate content reaches requirement from high-order storage tank 1; Get into receiving tank 4; When propyl formate content was lower than product requirement in the extracting rectifying cat head distillate, the material of cat head extraction got into changeover portion I receiving tank 6 (when propyl formate content is formed less than azeotropic in the extracting rectifying cat head distillate, stopping to add extractant); When propyl alcohol content reaches product requirement in the extracting rectifying cat head distillate; The material of extraction gets into receiving tank 7, and when propyl alcohol content was lower than product requirement in the extracting rectifying cat head distillate, the material of extraction got into 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 the heating kettle 3 during next group rectifying again.
The invention has the advantages that and use the rational and effective 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.
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-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 one
Adopt batch extraction rectification device, drop into 500L propyl alcohol-propyl formate azeotropic mixture (wherein propyl alcohol 48%, and propyl formate 52% is mass percent) at heating kettle; Extractant is an isobutanol, opens heating kettle thermal source and condenser low-temperature receiver, treats that the extracting rectifying cat head is after backflow a period of time; Tower top temperature is stable, adds extractant, and the cat head place is being closed in the extractant feed position; The control extractant adds speed 500L/h, and total reflux operation is when extracting rectifying cat head temperature is 80.9-81.6 ℃; Propyl formate content in the distillate >=99% beginning discharging, reflux ratio is 3: 1, discharging speed is 200L/h.When extracting rectifying cat head temperature is 81.6-96.8 ℃, extraction propyl alcohol-propyl formate changeover portion, and stop to add extractant, reflux ratio is 9: 1; When extracting rectifying cat head temperature is 96.8-97.5 ℃, propyl alcohol content >=99% o'clock in the overhead receives propyl alcohol, and reflux ratio is 4: 1; When extracting rectifying cat head temperature surpasses 97.5 ℃, reflux ratio 5: 1, extraction propyl alcohol-isobutanol changeover portion II; When isobutanol content in the extracting rectifying cat head distillate >=99%, stop, heating kettle is high-purity isobutanol.
Embodiment two
Adopt batch extraction rectification device, drop into 500L propyl alcohol-propyl formate azeotropic mixture (wherein propyl alcohol 10%, and propyl formate 90% is mass percent) at heating kettle; Extractant is an isobutanol, opens heating kettle thermal source and condenser low-temperature receiver, treats that the extracting rectifying cat head is after backflow a period of time; Tower top temperature is stable, adds extractant, and the cat head place is being closed in the extractant feed position; The control extractant adds speed 800L/h, and total reflux operation is when extracting rectifying cat head temperature is 80.9-81.6 ℃; Propyl formate content in the distillate >=99% beginning discharging, reflux ratio is 2: 1, discharging speed is 300L/h.When extracting rectifying cat head temperature is 81.6-96.8 ℃, extraction propyl alcohol-propyl formate changeover portion, and stop to add extractant; Reflux ratio is 10: 1, when extracting rectifying cat head temperature is 96.8-97.5 ℃, and propyl alcohol content >=99% o'clock in the overhead; Receive propyl alcohol, reflux ratio is 4: 1, when extracting rectifying cat head temperature above 97.5 ℃; Reflux ratio 6: 1, extraction propyl alcohol-isobutanol changeover portion II is when isobutanol content in the extracting rectifying cat head distillate >=99%; Stop, heating kettle is high-purity isobutanol.
Claims (3)
1. the intermittent extraction, distillation and separation method of propyl alcohol-propyl formate azeotropic mixture; This method adopts and comprises extractive distillation column, heating kettle, condenser; High-level storage groove; Receiving tank, the extracting rectifying device that product jar and vavuum pump constitute, batch extracting rectified separation propyl alcohol-propyl formate azeotropic mixture.
2. the intermittent extraction, distillation and separation method of a kind of propyl alcohol as claimed in claim 1-propyl formate azeotropic mixture is characterized in that with the isobutanol being extractant.
3. the intermittent extraction, distillation and separation method of a kind of propyl alcohol as claimed in claim 1-propyl formate azeotropic mixture; It is characterized in that comprising following process: extractive distillation column is operated with following condition; Under normal pressure or decompression; Getting into 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 cat head temperature is 80.9-81.6 ℃, with reflux ratio 1: 1-6: 1 by the qualified propyl formate product of cat head extraction propyl formate content; When extracting rectifying cat head temperature is 81.6-96.8 ℃, with reflux ratio 3: 1-10: 1 by cat head extraction propyl alcohol-propyl formate changeover portion I, and stops to add extractant; When extracting rectifying cat head temperature is 96.8-97.5 ℃, with reflux ratio 0.5: 1-6: 1 by cat head extraction propyl alcohol; When extracting rectifying cat head temperature surpasses 97.5 ℃, with reflux ratio 1: 1-12: 1 by cat head extraction propyl alcohol-extractant changeover portion II; Form when reaching requirement when the extractant of heating kettle, the cooling of stopping pumps into high-level storage groove with extractant, heating kettle pack into new a collection of propyl alcohol-propyl formate mixture and changeover portion I and changeover portion II, following batch of batch extracting rectified separation.
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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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| 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105968006A (en) * | 2016-05-24 | 2016-09-28 | 济南大学 | Separation method for 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5458741A (en) * | 1994-01-14 | 1995-10-17 | Lloyd Berg | Separation of benzene from close boiling hydrocarbons by extractive distillation |
| CN101254358A (en) * | 2007-12-05 | 2008-09-03 | 天津大学 | Adding salt intermittent extraction rectification 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 |
-
2012
- 2012-03-23 CN CN201210078711.1A patent/CN102527072B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5458741A (en) * | 1994-01-14 | 1995-10-17 | Lloyd Berg | Separation of benzene from close boiling hydrocarbons by extractive distillation |
| CN101254358A (en) * | 2007-12-05 | 2008-09-03 | 天津大学 | Adding salt intermittent extraction rectification 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105968006A (en) * | 2016-05-24 | 2016-09-28 | 济南大学 | Separation method for 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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| CN102527072B (en) | 2014-08-13 |
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