CN106178571A - A kind of Azeotrope separation technique - Google Patents
A kind of Azeotrope separation technique Download PDFInfo
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- CN106178571A CN106178571A CN201610788105.7A CN201610788105A CN106178571A CN 106178571 A CN106178571 A CN 106178571A CN 201610788105 A CN201610788105 A CN 201610788105A CN 106178571 A CN106178571 A CN 106178571A
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- rectifying column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
A kind of Azeotrope separation technique, this technique comprises the steps: 1) add raw materials into extraction kettle, add extractant, after stirring certain time, stand split-phase, be divided into aqueous phase and oil phase；2) going in rectifying still by the phase in aqueous phase or oil phase, after being heated by rectifying still reboiler, vapour phase rises in rectifying column；3) vapour phase in rectifying column rises to tower top and is condensed into liquid, after infinite reflux is stable, sets suitable reflux ratio, first extraction foreshot, then extraction product, last extraction interim fraction.This Azeotrope separation technique has merged the advantage of batch fractionating and extracting rectifying, flexible operation, good stability, and equipment investment is little, it is adaptable to azeotropic system and the separation of nearly system of boiling.
Description
Technical field
The present invention relates to a kind of Azeotrope separation technique, belong to the separating-purifying field of azeotropic mixture.
Background technology
During petrochemicals separate, often two kinds of boiling points product closely is separated, if using general
Logical rectificating method, the theoretical cam curve of needs and reflux ratio are the biggest, and investment and operating cost are higher.
Extracting rectifying is a kind of special extract rectification isolation technics, is suitable for the separation of azeotropic system.By the top toward rectifying column
It is continuously added to extractant and reaches to separate purpose to change the relative volatility between stock blend.By extraction is existed with rectification combination
Together, the advantage having merged batch fractionating and extracting rectifying, flexible operation, equipment investment is little, saves expense, it is adaptable to azeotropic body
System and the separation of nearly system of boiling, such as: the azeotropic composition of acetonitrile and water (acetonitrile :～85%, remaining is water), dichloromethane and first
The azeotropic of azeotropic composition (dichloromethane :～94%, remaining be methanol), toluene and the methanol of alcohol form (toluene :～31%, its
Remaining is methanol) and other azeotropic composition systems.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, comprehensive extraction and distillation technology, it is provided that a kind of Azeotrope separation work
Skill.
The technical scheme is that a kind of Azeotrope separation technique, this technique include as
Lower step:
1) add raw materials into extraction kettle, add extractant, after stirring certain time, stand split-phase, be divided into aqueous phase and oil
Phase；
2) according to the character of material to be separated, the phase in aqueous phase or oil phase is gone in rectifying still, by rectifying still again
After boiling device heating, vapour phase rises in rectifying column；
3) vapour phase in rectifying column rises to tower top and is condensed into liquid, after tower top infinite reflux is stable, according to overhead product
Analysis result, sets suitable reflux ratio, first extraction foreshot, then extraction product, last extraction interim fraction.
Described rectifying column uses plate column, packed tower, board-like and fill out the combined column of formula.
Wherein, step 2) can leave out according to practical situation, the step of this Azeotrope separation technique is as follows:
1) add raw materials into extraction kettle, add extractant, after stirring certain time, stand split-phase, be divided into aqueous phase and oil
Phase；
2) according to the character of material to be separated, go to the phase in aqueous phase or oil phase rectifying column carries out atmosphere intermission essence
Evaporate；After being heated by rectifying column reboiler, vapour phase rises to tower top, and overhead vapor phase is condensed into liquid, after infinite reflux is stable, and root
According to overhead product analysis result, set suitable reflux ratio, first extraction foreshot, then extraction product, last extraction transition
Fraction.
As the further improvement of this programme, the present invention provides a kind of Azeotrope separation device, this Azeotrope separation device
Including rectifying still, rectifying column, extraction kettle；Described extraction kettle bottom is provided with aqueous phase and receives tank and oil phase reception tank；Aqueous phase receives tank
Tank bottoms and rectifying still, rectifying column connect respectively；Oil phase reception tank is tank bottoms and rectifying still, rectifying column connect respectively；Described rectifying still
It is connected with tower bottom of rectifying tower；Described rectifying column tower top is provided with return tank, and return tank is connected with extraction kettle.
Further, described rectifying still bottom is connected to the residual barrelling of still.
Further, described return tank is provided with product and receives tank, is provided with front-end volatiles side by side and connects between return tank and extraction kettle
Closed cans, interim fraction receive tank, extractant tank.
Further, it is provided with condenser between described rectifying column and return tank.
Further, receive tank at described front-end volatiles, interim fraction receives tank, extractant tank, product receive tank and return tank
Between pipeline be provided with cooler.
Further, described condenser connects has tail cooler, the described tail cooler other end to connect front-end volatiles reception tank, mistake respectively
Cross fraction and receive tank, extractant tank, product reception tank.
Further, described tower bottom of rectifying tower is provided with rectifying column reboiler.
Further, described rectifying still bottom is provided with rectifying still reboiler.
The present invention has the feature of low energy consumption, low stain, high-recovery, high product purities, have significant practicality and
Economic benefit.
Accompanying drawing explanation
Fig. 1 is Azeotrope separation apparatus structure schematic diagram.
Wherein, 1, rectifying still；2, rectifying column；3, extraction kettle；4, aqueous phase receives tank；5, oil phase receives tank；6, return tank；7、
Product receives tank；8, front-end volatiles receive tank；9, interim fraction receives tank；10, extractant tank；11, condenser；12, cooler；
13, tail cooler；14, the residual barrelling of still；15, rectifying still reboiler；16, rectifying column reboiler.
Detailed description of the invention
Being described principle and the feature of the present invention below in conjunction with accompanying drawing, example is served only for explaining the present invention, and
Non-for limiting the scope of the present invention.
Embodiment 1
Pretreated raw material is mainly acetonitrile, water
Raw material initially enters extraction kettle 3, is subsequently adding extractant, after opening stirring certain time, stands split-phase, and aqueous phase is adopted
Go out to wastewater treatment working section；Oil phase goes in rectifying still 1, and after being heated by rectifying still reboiler 15, vapour phase rises to rectifying column 2
In, condensed by overhead condenser 11, after tower top infinite reflux is stable, according to overhead product analysis result, set suitable backflow
Ratio, first extraction foreshot (extractant and the azeotropic mixture of water, the interim fraction of extractant and acetonitrile), as extractant can with under
Batch returns extraction kettle and recycles；Then extraction acetonitrile product is to product pans 7.
Embodiment 2
Pretreated raw material is mainly dichloromethane, methanol
Raw material initially enters extraction kettle 3, is subsequently adding extractant, after opening stirring certain time, stands split-phase, after split-phase
Obtain oil phase (dichloromethane product) and aqueous phase (methanol aqueous solution, the dichloromethane containing a small amount of), aqueous phase (methanol aqueous solution,
Dichloromethane containing a small amount of) go in rectifying still 1, after being heated by rectifying still reboiler 15, vapour phase rises to rectifying column 2
In, condensed by overhead condenser 11, after tower top infinite reflux is stable, according to overhead product analysis result, set suitable backflow
Ratio, successively extraction front-end volatiles (methylene chloride/methanol/water), methanol, water；Water can recycle as the extractant of this workshop section.
Embodiment 3
Pretreated raw material is mainly toluene, methanol
By extraction kettle 3, carry out liquid-liquid extraction, after split-phase, obtain toluene product；Aqueous phase is that methanol aqueous solution goes to rectification
In still 1, after being heated by rectifying still reboiler 15, vapour phase rises to, in rectifying column 2, be condensed by overhead condenser 11, tower top
After infinite reflux is stable, according to overhead product analysis result, setting suitable reflux ratio, a small amount of front-end volatiles of extraction, methanol produce successively
Product, interim fraction (first alcohol and water)；After in rectifying column 2 overhead distillate without methanol, heating can be stopped.Technique waste water in still
Can use as the extractant recirculated water of this technique after cooling.
A kind of Azeotrope separation device used in this Azeotrope separation technique, as it is shown in figure 1, this Azeotrope separation device
Including rectifying still 1, rectifying column 2, extraction kettle 3；Described extraction kettle 3 bottom is provided with aqueous phase and receives tank 4 and oil phase reception tank 5；Aqueous phase
Reception tank 4 is tank bottoms and rectifying still 1, rectifying column 2 connect respectively；Oil phase reception tank 5 is tank bottoms and rectifying still 1, rectifying column 2 connect respectively
Connect；Described rectifying still 1 is connected with rectifying column 2 tower reactor；Described rectifying column 2 tower reactor is provided with rectifying column reboiler 16, rectifying column 2 tower top
Being provided with return tank 6, return tank 6 is connected with extraction kettle 3.
Described rectifying still 1 bottom is provided with rectifying still reboiler 15, and rectifying still 1 bottom is connected to the residual barrelling of still 14；Described backflow
Tank 6 is provided with product and receives tank 7, is provided with front-end volatiles side by side and receives tank 8, interim fraction reception tank between return tank 6 and extraction kettle 3
9, extractant tank 10；It is provided with condenser 11 between described rectifying column 2 and return tank 6；Receive tank 8 at described front-end volatiles, transition evaporates
The pipeline that tap closed cans 9, extractant tank 10, product receive between tank 7 and return tank 6 is provided with cooler 12；Described front-end volatiles
Receive tank 8, interim fraction receives tank 9, extractant tank 10, product receive the pipeline between tank 7 and condenser 11 to be provided with tail cold
Device 13.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (9)
1. an Azeotrope separation technique, it is characterised in that this technique comprises the steps:
1) add raw materials into extraction kettle, add extractant, after stirring certain time, stand split-phase, be divided into aqueous phase and oil phase；
2) going in rectifying still by the phase in aqueous phase or oil phase, after being heated by rectifying still reboiler, vapour phase rises to rectification
In tower；
3) vapour phase in rectifying column rises to tower top and is condensed into liquid, after infinite reflux is stable, sets suitable reflux ratio, first
Extraction foreshot, then extraction product, last extraction interim fraction.
A kind of Azeotrope separation technique the most according to claim 1, it is characterised in that: rectifying column uses plate column, filler
Tower, board-like and fill out the combined column of formula.
3. a kind of Azeotrope separation device used in claim 1, it is characterised in that: this Azeotrope separation device includes rectification
Still, rectifying column, extraction kettle；Described extraction kettle bottom is provided with aqueous phase and receives tank and oil phase reception tank；It is tank bottoms and smart that aqueous phase receives tank
Evaporate still, rectifying column connects respectively；Oil phase reception tank is tank bottoms and rectifying still, rectifying column connect respectively；Described rectifying still and rectifying column
Tower reactor is connected；Described rectifying column tower top is provided with return tank, and return tank is connected with extraction kettle.
A kind of Azeotrope separation device the most according to claim 3, it is characterised in that: described return tank is provided with product and connects
Closed cans, is provided with front-end volatiles side by side and receives tank, interim fraction reception tank, extractant tank between return tank and extraction kettle.
A kind of Azeotrope separation device the most according to claim 3, it is characterised in that: between described rectifying column and return tank
It is provided with condenser.
A kind of Azeotrope separation device the most according to claim 4, it is characterised in that: receive tank, mistake at described front-end volatiles
Cross the pipeline that fraction receives tank, extractant tank, product receive between tank and return tank and be provided with cooler.
A kind of Azeotrope separation device the most according to claim 5, it is characterised in that: described condenser connects has tail cold
Device, the described tail cooler other end connects front-end volatiles respectively and receives tank, interim fraction reception tank, extractant tank, product reception tank.
A kind of Azeotrope separation device the most according to claim 3, it is characterised in that: described tower bottom of rectifying tower is provided with rectification
Tower reboiler.
A kind of Azeotrope separation device the most according to claim 3, it is characterised in that: described rectifying still bottom is provided with rectification
Still reboiler.
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| CN201610788105.7A CN106178571B (en) | 2016-08-31 | 2016-08-31 | Azeotrope separation process |
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| CN201610788105.7A CN106178571B (en) | 2016-08-31 | 2016-08-31 | Azeotrope separation process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840808A (en) * | 2017-10-30 | 2018-03-27 | 烟台国邦化工机械科技有限公司 | Continuous reaction rectification production cyanoacetate compound, malonate compound device and its production technology |
| CN107998678A (en) * | 2017-10-30 | 2018-05-08 | 烟台国邦化工机械科技有限公司 | A kind of environment-protecting clean device and process for separating organic azeotropic mixture |
| CN108046992A (en) * | 2017-12-29 | 2018-05-18 | 山东华安新材料有限公司 | A kind of method of purification and its equipment of 2,2- difluoroethanols |
| CN109231635A (en) * | 2018-11-20 | 2019-01-18 | 江苏九天高科技股份有限公司 | A kind of dichloroethanes/ethane nitrile wastewater New Process for Treatment |
| CN112661731A (en) * | 2019-10-15 | 2021-04-16 | 中国石油化工股份有限公司 | Device and method for decoloring and purifying maleic anhydride refined heavy components |
| CN113461568A (en) * | 2021-06-24 | 2021-10-01 | 索闻特环保科技(上海)有限公司 | Method for treating toluene in acetonitrile waste liquid |
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| CN101492391A (en) * | 2008-01-25 | 2009-07-29 | 天津普莱化工技术有限公司 | Process for separating ethane nitrile wastewater with combination of abstraction and distillation |
| CN201279398Y (en) * | 2008-10-09 | 2009-07-29 | 上海宝钢化工有限公司 | Rectifier |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107840808A (en) * | 2017-10-30 | 2018-03-27 | 烟台国邦化工机械科技有限公司 | Continuous reaction rectification production cyanoacetate compound, malonate compound device and its production technology |
| CN107998678A (en) * | 2017-10-30 | 2018-05-08 | 烟台国邦化工机械科技有限公司 | A kind of environment-protecting clean device and process for separating organic azeotropic mixture |
| CN107998678B (en) * | 2017-10-30 | 2023-08-18 | 烟台国邦化工机械科技有限公司 | Environment-friendly cleaning device and process method for separating organic azeotrope |
| CN108046992A (en) * | 2017-12-29 | 2018-05-18 | 山东华安新材料有限公司 | A kind of method of purification and its equipment of 2,2- difluoroethanols |
| CN108046992B (en) * | 2017-12-29 | 2021-02-02 | 山东华安新材料有限公司 | Method and equipment for purifying 2, 2-difluoroethanol |
| CN109231635A (en) * | 2018-11-20 | 2019-01-18 | 江苏九天高科技股份有限公司 | A kind of dichloroethanes/ethane nitrile wastewater New Process for Treatment |
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| CN112661731A (en) * | 2019-10-15 | 2021-04-16 | 中国石油化工股份有限公司 | Device and method for decoloring and purifying maleic anhydride refined heavy components |
| CN112661731B (en) * | 2019-10-15 | 2022-08-05 | 中国石油化工股份有限公司 | Device and method for decoloring and purifying maleic anhydride refined heavy components |
| CN113461568A (en) * | 2021-06-24 | 2021-10-01 | 索闻特环保科技(上海)有限公司 | Method for treating toluene in acetonitrile waste liquid |
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