CN103288581A - Batch extractive distillation separation method of benzene-propyl alcohol azeotropic mixture - Google Patents
Batch extractive distillation separation method of benzene-propyl alcohol azeotropic mixture Download PDFInfo
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- CN103288581A CN103288581A CN2013102713193A CN201310271319A CN103288581A CN 103288581 A CN103288581 A CN 103288581A CN 2013102713193 A CN2013102713193 A CN 2013102713193A CN 201310271319 A CN201310271319 A CN 201310271319A CN 103288581 A CN103288581 A CN 103288581A
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Abstract
The invention discloses a batch extractive distillation separation method of a benzene-propyl alcohol azeotropic mixture, and belongs to a separation technology of benzene-propyl alcohol azeotropic mixtures. According to the method, dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF) or an arbitrary mixture of the two ingredients is used as an extraction agent, the operating condition of an extractive distillation tower is that the mass ratio of the extraction agent to a tower top distillate is 0.5:(1-10):1, different temperatures and different reflux ratios at the top of the extractive distillation tower are controlled, and a transition segment I of benzene and benzene-propyl alcohol and a transition segment II of propyl alcohol and propyl alcohol-extraction agent are respectively extracted from the top of the extractive distillation tower; when the extraction agent composition of the tower kettle meets the demand, the extraction agent is pumped into a high-level storage tank so as to be recycled. The batch extractive distillation separation method disclosed by the invention has the advantages that the extraction agent is used for breaking the benzene-propyl alcohol azeotropic system to separate out benzene and propyl alcohol products with high purity, the single tower operation is flexible and the equipment cost is low.
Description
Technical field
The present invention relates to a kind of intermittent extraction, distillation and separation method of benzene-propanol azeotrope, belong to the isolation technique of benzene-propanol azeotrope.
Background technology
Extracting rectifying is a kind of special extract rectification isolation technique, is suitable for the separation of azeotropic system.Add extraction agent continuously 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 propyl alcohol is: CH
3CH
2CH
2OH, industrial being widely used.Benzene-the propanol mixture of Chan Shenging in process of production, owing to forming azeotrope (massfraction of benzene is 83.1%), benzene and propyl alcohol be difficult to separate, as not reclaiming, not only pollute the environment, and the increase production cost, the separation method of therefore developing benzene-propanol azeotrope has important meaning.About article and the patent of extracting rectifying aspect a lot, the data of the benzene that Shang Weijian publishes-propyl alcohol azeotropic system extracting rectifying separation aspect.
Summary of the invention
The object of the present invention is to provide a kind of intermittent extraction, distillation and separation method of benzene-propanol azeotrope.The isolated benzene of this method, propyl alcohol product purity height.
The present invention is realized by following technical proposals.Employing comprises extractive distillation column, heating kettle, and condenser, high-level storage groove, the extracting rectifying device that receiving tank and product jar constitute, batch extracting rectified separation of benzene-propanol azeotrope is characterized in that comprising following process:
With the inferior maple (DMSO) of diformazan, N, dinethylformamide (DMF) or the two any composition mixture are extraction agent, extractive distillation column is operated with following condition, under normal pressure, 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 79.5-81 ℃, with reflux ratio 1:1-6:1 by the qualified benzaldehyde product of cat head extraction benzene content; When extracting rectifying cat head temperature is 81-96.5 ℃, by cat head extraction benzene-propyl alcohol transition section I, and stop to add extraction agent with reflux ratio 3:1-10:1; When extracting rectifying cat head temperature is 96.5-97.6 ℃, with reflux ratio 0.5:1-6:1 by cat head extraction propyl alcohol; When extracting rectifying cat head temperature surpasses 97.6 ℃, with reflux ratio 1:1-12:1 by cat head extraction propyl alcohol-extraction agent transition section II; Form when reaching requirement when the extraction agent of heating kettle, the cooling of stopping pumps into high-level storage groove with extraction agent, heating kettle pack into new a collection of benzene-propanol mixture and transition section I and transition section II, following batch of batch extracting rectified separation.
Idiographic flow (seeing accompanying drawing): benzene-propanol mixture adds in the heating kettle 3, open the thermal source of heating kettle and the low-temperature receiver of condenser 4, after treating that the backflow of extracting rectifying cat head and tower top temperature are stable, extraction agent is introduced into extractive distillation column 2 tops from high-order storage tank 1, total reflux for some time, discharging when benzene content reaches requirement, enter receiving tank 4, when benzene content is lower than product requirement in the extracting rectifying cat head overhead product, the material of cat head extraction enters transition section I receiving tank 6(when benzene content is formed less than azeotropic in the extracting rectifying cat head overhead product, stop to add extraction agent), when propyl alcohol content reaches product requirement in the extracting rectifying cat head overhead product, the material of extraction enters receiving tank 7, when propyl alcohol 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 the rational and effective extraction agent to destroy benzene-propyl alcohol azeotropic system, isolate high pure benzene, propyl alcohol 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-benzaldehyde product receiving tank, 6-transition section I receiving tank, 7-propyl alcohol product receiving tank, 8-transition section II receiving tank.
Embodiment
Embodiment 1: adopt batch extraction rectification device, (wherein benzene 80% to drop into 500 L benzene-propanol azeotrope at heating kettle, propyl alcohol 20%, be mass percent), testing selected extraction agent is methyl-sulphoxide, open heating kettle thermal source and condenser low-temperature receiver, treat the extracting rectifying cat head after backflow for some time, tower top temperature is 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 79.5-81 ℃, benzene 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 81-96.5 ℃, extraction benzene-propyl alcohol transition section, and stop to add extraction agent, reflux ratio is 9:1, when extracting rectifying cat head temperature is 96.5-97.6 ℃, and propyl alcohol content 〉=99% o'clock in the overhead product, receive propyl alcohol, reflux ratio is 4:1, when extracting rectifying cat head temperature surpasses 97.6 ℃, reflux ratio 5:1, extraction propyl alcohol-methyl-sulphoxide transition section II, when methyl-sulphoxide content in the extracting rectifying cat head overhead product 〉=99%, stop, heating kettle is high-purity methyl-sulphoxide.
Embodiment 2: experimental installation and working method are with embodiment 1, and extraction agent adopts N, dinethylformamide.
Embodiment 3: experimental installation and working method are with embodiment 1, and extraction agent adopts methyl-sulphoxide and N, the equal-volume mixture of dinethylformamide.
Claims (3)
1. the intermittent extraction, distillation and separation method of a benzene-propanol azeotrope, this method adopt and comprise extractive distillation column, heating kettle, condenser, high-level storage groove, the extracting rectifying device that receiving tank and product jar constitute, batch extracting rectified separation of benzene-propanol azeotrope.
2. the intermittent extraction, distillation and separation method of a kind of benzene-propanol azeotrope as claimed in claim 1 is characterized in that dinethylformamide (DMF) or the two any composition mixture are extraction agent with the inferior maple (DMSO) of diformazan, N.
3. the intermittent extraction, distillation and separation method of a kind of benzene-propanol azeotrope as claimed in claim 2, it is characterized in that comprising following process: extractive distillation column is operated with following condition, under normal pressure, 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 79.5-81 ℃, with reflux ratio 1:1-6:1 by the qualified benzaldehyde product of cat head extraction benzene content; When extracting rectifying cat head temperature is 81-96.5 ℃, by cat head extraction benzene-propyl alcohol transition section I, and stop to add extraction agent with reflux ratio 3:1-10:1; When extracting rectifying cat head temperature is 96.5-97.6 ℃, with reflux ratio 0.5:1-6:1 by cat head extraction propyl alcohol; When extracting rectifying cat head temperature surpasses 97.6 ℃, with reflux ratio 1:1-12:1 by cat head extraction propyl alcohol-extraction agent transition section II; Form when reaching requirement when the extraction agent of heating kettle, the cooling of stopping pumps into high-level storage groove with extraction agent, heating kettle pack into new a collection of benzene-propanol mixture and transition section I and transition section II, following batch of batch extracting rectified separation.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610021A (en) * | 2015-01-12 | 2015-05-13 | 济南大学 | Method for continuous extractive distillation and separation of ethanol-toluene azeotrope with mixed solvent |
| CN104876788A (en) * | 2015-05-21 | 2015-09-02 | 济南大学 | Benzene-propyl alcohol azeotrope continuous extractive distillation technology based on choline chloride/urea low co-melting solvent |
| CN104926605A (en) * | 2015-05-21 | 2015-09-23 | 济南大学 | Benzene-propanol azeotrope rectification separation method based on choline chloride further-co-melting solvent |
| CN105037112A (en) * | 2015-05-21 | 2015-11-11 | 济南大学 | Batch extractive distillation separation method of ethyl tert-butyl ether/tert-butyl alcohol azeotropic mixture |
| CN105198701A (en) * | 2015-09-10 | 2015-12-30 | 青岛科技大学 | Method of separating mixture of tert-amyl alcohol and benzene by extractive distillation |
| CN105646146A (en) * | 2016-01-17 | 2016-06-08 | 济南大学 | Propyl alcohol-triethylamine azeotropic mixture extraction and rectification method |
| CN112778087A (en) * | 2021-01-14 | 2021-05-11 | 山东科技大学 | Method for separating methanol-toluene azeotrope through continuous extractive distillation |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610021A (en) * | 2015-01-12 | 2015-05-13 | 济南大学 | Method for continuous extractive distillation and separation of ethanol-toluene azeotrope with mixed solvent |
| CN104876788A (en) * | 2015-05-21 | 2015-09-02 | 济南大学 | Benzene-propyl alcohol azeotrope continuous extractive distillation technology based on choline chloride/urea low co-melting solvent |
| CN104926605A (en) * | 2015-05-21 | 2015-09-23 | 济南大学 | Benzene-propanol azeotrope rectification separation method based on choline chloride further-co-melting solvent |
| CN105037112A (en) * | 2015-05-21 | 2015-11-11 | 济南大学 | Batch extractive distillation separation method of ethyl tert-butyl ether/tert-butyl alcohol azeotropic mixture |
| CN105198701A (en) * | 2015-09-10 | 2015-12-30 | 青岛科技大学 | Method of separating mixture of tert-amyl alcohol and benzene by extractive distillation |
| CN105198701B (en) * | 2015-09-10 | 2017-09-01 | 青岛科技大学 | A kind of method of separation of extractive distillation tert-pentyl alcohol and benzol mixture |
| CN105646146A (en) * | 2016-01-17 | 2016-06-08 | 济南大学 | Propyl alcohol-triethylamine azeotropic mixture extraction and rectification method |
| CN105646146B (en) * | 2016-01-17 | 2017-12-01 | 济南大学 | A kind of propyl alcohol triethylamine azeotropic mixture extraction rectifying method |
| CN112778087A (en) * | 2021-01-14 | 2021-05-11 | 山东科技大学 | Method for separating methanol-toluene azeotrope through continuous extractive distillation |
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Application publication date: 20130911 |