CN101306982A - Method for intermittently extracting, rectifying and separating ethanol and xylol mixture - Google Patents
Method for intermittently extracting, rectifying and separating ethanol and xylol mixture Download PDFInfo
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- CN101306982A CN101306982A CNA2008100537285A CN200810053728A CN101306982A CN 101306982 A CN101306982 A CN 101306982A CN A2008100537285 A CNA2008100537285 A CN A2008100537285A CN 200810053728 A CN200810053728 A CN 200810053728A CN 101306982 A CN101306982 A CN 101306982A
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- diethylbenzene
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Abstract
The invention relates to a method for the intermittent extraction rectification separation of an ethanol-xylene mixture. The method adopts a rectification device consisting of an extraction rectification tower, a heating kettle arranged at the bottom of the extraction rectification tower, a condenser connected with the top of the extraction rectification tower, a high-level storage tank and a receiving tank so as to separate the ethanol-xylene mixture through intermittent operation. Moreover, the method comprises the following steps that: p-diethylbenzene is taken as an extraction agent under ordinary pressure, and intermittent operation is carried out inside the extraction rectification tower; different temperatures and different reflux ratios at the top of the extraction rectification tower are controlled; and ethanol product, ethanol-xylene transition section, xylene product, xylene-p-diethylbenzene transition section and extraction agent p-diethylbenzene are respectively collected from the top of the extraction rectification tower. The method has the advantages that: due to taking p-diethylbenzene as extraction agent, the method increases the relative volatility of ethanol-xylene; moreover, the method adopts mono-tower operation and has flexible operation and less cost of equipment.
Description
Technical field
The present invention relates to a kind of intermittent extraction, distillation and separation method of ethanol-xylene mixture, belong to the isolation technique of ethanol-xylene mixture.
Background technology
Extracting rectifying is to add the high boiling point additive continuously to rectifying tower top, changes the relative volatility between separated component in the feed liquid, makes conventional distillation be difficult to isolating liquid mixture and becomes and be easy to isolating a kind of special extract rectification method.To ethanol-dimethylbenzene system, conventional separation method is to adopt atmospheric distillation, it can satisfy general separation requirement, but when ethanol-dimethylbenzene system when ethanol content surpasses 92%, relative volatility approaches 1, is difficult to obtain content greater than 92% ethanol with conventional separation method.
Summary of the invention
The object of the present invention is to provide a kind of intermittent extraction, distillation and separation method of ethanol-xylene mixture.With the isolated alcohol product purity of this method height, and equipment is simple, and is easy to operate.
The present invention is realized by following technical proposals.A kind of intermittent extraction, distillation and separation method of ethanol-xylene mixture, this method adopts and comprises extractive distillation column, heating kettle at the bottom of the extracting rectifying Tata, the rectifier unit that condenser that the extracting rectifying column overhead connects and high-order basin and receiving tank constitute, periodical operation separating alcohol-xylene mixture, it is characterized in that comprising following process: the employing p-diethylbenzene is an extraction agent, extractive distillation column is operated with following condition: under normal pressure, the extraction agent that the steam that still to be heated produces rises to extractive distillation column adds when entering the mouth, under the normal temperature, the extraction agent p-diethylbenzene is introduced extractive distillation column top from high-order basin, extractive distillation column is carried out total reflux operation, the volume ratio of the add-on of extraction agent p-diethylbenzene and extracting rectifying cat head liquid return amount is 1-5: 1 is adding under the situation of p-diethylbenzene continuously, when extracting rectifying cat head temperature is 78.6-80.5 ℃, with reflux ratio 1-3: 1 operation, be higher than 99% alcohol product to the alcohol product jar by extracting rectifying cat head extraction ethanol mass content, when the ethanol mass content is lower than 98.0% in the extractive distillation column overhead product, stop to add the extraction agent p-diethylbenzene to extractive distillation column, and from the extracting rectifying cat head with reflux ratio 1-5: 1 extraction ethanol-dimethylbenzene transition section fraction is to transition fraction receiving tank, when extracting rectifying cat head temperature reaches 138-144 ℃, extraction dimethylbenzene is to the dimethylbenzene receiving tank, after tower top temperature is higher than 144 ℃, extraction dimethylbenzene-p-diethylbenzene transition section is to transition fraction receiving tank, when extracting rectifying cat head temperature reaches 188 ℃, reach 99.8% p-diethylbenzene extraction agent with 1: 1 extraction mass content of reflux ratio.
The invention has the advantages that, adopt the p-diethylbenzene extraction agent to increase the relative volatility of ethanol-dimethylbenzene system, isolate the product of ethanol mass content more than 99%, and adopt single tower operation, flexible operation, cost of equipment less investment.
Description of drawings
The rectifier unit schematic flow sheet of Fig. 1 for realizing that the inventive method adopts.
Among the figure: the high-order basin of 1-, 2-extractive distillation column, 3-heating kettle, the 4-condenser, 5-alcohol product basin, 6-ethanol-dimethylbenzene transition section fraction receiving tank, 7-dimethylbenzene receiving tank, 8-dimethylbenzene-p-diethylbenzene transition section fraction receiving tank, 9-p-diethylbenzene receiving tank.
Embodiment
The idiographic flow of Fig. 1: ethanol-xylene mixture adds in the heating kettle 3, open the thermal source of heating kettle and the low-temperature receiver of condenser 4, treat that the extraction agent that the interior rising steam of extractive distillation column rises to extractive distillation column adds when entering the mouth, the extraction agent p-diethylbenzene is introduced into extractive distillation column top from high-order basin 1, extractive distillation column carries out total reflux operation, when the tower top temperature of extractive distillation column is stabilized in 78.6 ℃, beginning extraction mass content reaches 99% ethanol from extracting rectifying column overhead fraction, enter alcohol product basin 5, when ethanol content in the extracting rectifying cat head fraction is lower than 98.0% is that the extractive distillation column tower top temperature is when reaching 80.6 ℃, enter from the transition section fraction of the ethanol-dimethylbenzene of extracting rectifying cat head extraction that ethanol-dimethylbenzene transition section fraction receiving tank 6 (at this moment, stop to add extraction agent), the extractive distillation column tower top temperature reached 138 ℃-144 ℃ to dimethylbenzene in extracting rectifying cat head fraction (comprise three kinds of isomer and) when mass content reached 95%, extraction dimethylbenzene, enter dimethylbenzene receiving tank 7, when xylene content in the overhead product is lower than 94.5% is that tower top temperature is when being higher than 144 ℃, extraction dimethylbenzene-p-diethylbenzene transition section, enter dimethylbenzene-p-diethylbenzene transition fraction receiving tank 8, it is extractive distillation column tower top temperature when reaching 188 ℃ that p-diethylbenzene extraction agent mass content reaches 99%, and the p-diethylbenzene of extraction enters p-diethylbenzene receiving tank 9 and recycles.The transition section fraction joins in the heating kettle when the next batch extracting rectifying and recycles.
Embodiment one
With flow path device shown in Figure 1, adopt periodical operation separating alcohol-xylene mixture, detailed process is as follows: the diameter of the extractive distillation column of employing is φ 40mm, interior dress Dixon ring filler, bed stuffing height is 1.15m, and the extraction agent import is at distance cat head 0.15m place.Drop into 1300ml ethanol-xylene mixture (wherein ethanol 90.13%, dimethylbenzene 9.82%, all the other be impurity, are mass percent) at heating kettle, get extraction agent p-diethylbenzene 1200ml adding extraction agent storage tank.Open heating kettle thermal source and condenser low-temperature receiver, extractive distillation column brings into operation, treat that the interior rising steam of extractive distillation column rises to extraction agent and adds when entering the mouth, extraction agent is added in the extractive distillation column by the extraction agent import, drips extraction agent, total reflux operation, when extracting rectifying cat head temperature is 78.6 ℃, stop total reflux, be operation in 2: 1 with reflux ratio, begin the extraction mass content from cat head and be higher than 98.5% ethanol, enter the alcohol product jar.When the ethanol mass content of extraction is lower than 98%, stop to add the extraction agent p-diethylbenzene, and with reflux ratio be 4: 1 the operation, by extracting rectifying column overhead extraction ethanol-dimethylbenzene transition section fraction, when extracting rectifying cat head temperature reaches 138-144 ℃, extraction dimethylbenzene enters the dimethylbenzene receiving tank, after tower top temperature is higher than 144 ℃, extraction dimethylbenzene-p-diethylbenzene transition section enters transition fraction receiving tank, when extracting rectifying cat head temperature reaches 188 ℃, with reflux ratio is operation in 1: 1, by extracting rectifying column overhead extraction extraction agent p-diethylbenzene, during end in the tower still content of extraction agent also up to 99.6%, as following batch of rectifying use.
Claims (1)
1. the intermittent extraction, distillation and separation method of an ethanol-xylene mixture, this method adopts and comprises extractive distillation column, heating kettle at the bottom of the extracting rectifying Tata, the rectifier unit that condenser that the extracting rectifying column overhead connects and high-order basin and receiving tank constitute, periodical operation separating alcohol-xylene mixture, it is characterized in that comprising following process: the employing p-diethylbenzene is an extraction agent, extractive distillation column is operated with following condition: under normal pressure, the extraction agent that the steam that still to be heated produces rises to extractive distillation column adds when entering the mouth, under the normal temperature, the extraction agent p-diethylbenzene is introduced extractive distillation column top from high-order basin, extractive distillation column is carried out total reflux operation, the volume ratio of the add-on of extraction agent p-diethylbenzene and extracting rectifying cat head liquid return amount is 1-5: 1 is adding under the situation of p-diethylbenzene continuously, when extracting rectifying cat head temperature is 78.6-80.5 ℃, with reflux ratio 1-3: 1 operation, be higher than 99% alcohol product to the alcohol product jar by extracting rectifying cat head extraction ethanol mass content, when the ethanol mass content is lower than 98.0% in the extractive distillation column overhead product, stop to add the extraction agent p-diethylbenzene to extractive distillation column, and from the extracting rectifying cat head with reflux ratio 1-5: 1 extraction ethanol-dimethylbenzene transition section fraction is to transition fraction receiving tank, when extracting rectifying cat head temperature reaches 138-144 ℃, extraction dimethylbenzene is to the dimethylbenzene receiving tank, after tower top temperature is higher than 144 ℃, extraction dimethylbenzene-p-diethylbenzene transition section is to transition fraction receiving tank, when extracting rectifying cat head temperature reaches 188 ℃, reach 99.8% p-diethylbenzene extraction agent with 1: 1 extraction mass content of reflux ratio.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100537285A CN101306982B (en) | 2008-07-02 | 2008-07-02 | Method for intermittently extracting, rectifying and separating ethanol and xylol mixture |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100537285A CN101306982B (en) | 2008-07-02 | 2008-07-02 | Method for intermittently extracting, rectifying and separating ethanol and xylol mixture |
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| Publication Number | Publication Date |
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| CN101306982A true CN101306982A (en) | 2008-11-19 |
| CN101306982B CN101306982B (en) | 2011-03-16 |
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| CN2008100537285A Expired - Fee Related CN101306982B (en) | 2008-07-02 | 2008-07-02 | Method for intermittently extracting, rectifying and separating ethanol and xylol mixture |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992930A (en) * | 2012-12-15 | 2013-03-27 | 福州大学 | Recovery process and separation device of toluene solvent in production process of alpha-acetyl-gamma butyrolactone |
| CN104628522A (en) * | 2015-01-12 | 2015-05-20 | 济南大学 | Intermittent extractive distillation process for ethanol-methylbenzene azeotropic mixture |
| CN110052052A (en) * | 2019-05-29 | 2019-07-26 | 天津赫普菲乐新材料有限公司 | Multicomponent batch fractionating intelligence control system and control method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5800681A (en) * | 1997-04-21 | 1998-09-01 | Berg; Lloyd | Separation of ethanol, isopropanol and water mixtures by extractive distillation |
| US5876569A (en) * | 1998-06-29 | 1999-03-02 | Berg; Lloyd | Separation of methyl ethyl ketone from ethanol by extractive distillation |
-
2008
- 2008-07-02 CN CN2008100537285A patent/CN101306982B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992930A (en) * | 2012-12-15 | 2013-03-27 | 福州大学 | Recovery process and separation device of toluene solvent in production process of alpha-acetyl-gamma butyrolactone |
| CN102992930B (en) * | 2012-12-15 | 2014-12-31 | 福州大学 | Recovery process and separation device of toluene solvent in production process of alpha-acetyl-gamma butyrolactone |
| CN104628522A (en) * | 2015-01-12 | 2015-05-20 | 济南大学 | Intermittent extractive distillation process for ethanol-methylbenzene azeotropic mixture |
| CN110052052A (en) * | 2019-05-29 | 2019-07-26 | 天津赫普菲乐新材料有限公司 | Multicomponent batch fractionating intelligence control system and control method |
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| CN101306982B (en) | 2011-03-16 |
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