CN104447636A - Method and device for separating ethanol-tetrahydrofuran by extractive distillation by using dividing tower - Google Patents
Method and device for separating ethanol-tetrahydrofuran by extractive distillation by using dividing tower Download PDFInfo
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- CN104447636A CN104447636A CN201410619853.3A CN201410619853A CN104447636A CN 104447636 A CN104447636 A CN 104447636A CN 201410619853 A CN201410619853 A CN 201410619853A CN 104447636 A CN104447636 A CN 104447636A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/04—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D307/06—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D307/08—Preparation of tetrahydrofuran
-
- 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
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/40—Extractive distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for separating ethanol-tetrahydrofuran by extractive distillation by using a dividing tower, belonging to a separating technology of a tetrahydrofuran-ethanol azeotropic mixture. According to the method, 1,4-butanediol is by preferably selected as an extraction agent, and the used device is an extracting and rectifying tower with a dividing wall, wherein the tower is structurally characterized in that the dividing wall is installed on the upper part of a common rectifying tower to divide the tower into regions I, III, III and IV while a dividing plate is installed in the region II to divide the region III and the region II; the region I is an extracting and rectifying region in which a tower plate is mainly installed, materials and an extraction agent enter from the middle and upper part of the region I, and tetrahydrofuran and heavy components are mainly separated in the region I; the region II is an extraction agent recovery area in which the tower plate is further installed, and secondary light component ethanol is extracted from the top; the region IV is a common withdrawal section of the regions I and II; and the region III is not provided with any tower plates, and the height of the region II is controlled by the dividing plate, so that the tower plates are saved. High-purity tetrahydrofuran and ethanol are extracted by the dividing wall rectifying tower, and meanwhile the extraction agent is recovered from the kettle bottom. The process equipment can ensure the recovery rate of tetrahydrofuran and reduce the energy consumption and equipment expense in the process of extracting tetrahydrofuran to a great extent, so that the method has remarkable economical and practical benefits.
Description
Technical field
The present invention relates to method and the device of a kind of next door rectifying tower extracting rectifying tetrahydrofuran (THF), belong to the isolation technique of the azeotrope of tetrahydrofuran-ethyl alcohol.
Background technology
In pharmaceutical industry, ethanol, tetrahydrofuran (THF) are important solvents, but the two can form binary azeotropic system, and separating difficulty is larger.Original technique adopts multitower rectifying separation, and facility investment is high, energy consumption is large, can not adapt to energy-conservation, efficient chemical separating processing requirement.
For the recovery of tetrahydrofuran (THF), domesticly carry out a large amount of research work, proposed multiple technologies scheme, comprising: three tower continuous rectifications, azeotropic distillation and batch extracting rectified.
Adopt batch extracting rectified, the extraction agent adopted is ethylene glycol, and the purity of the tetrahydrofuran (THF) of this extraction agent extraction is lower, and this patent adopts batch extracting rectified, therefore it at least needs two single tower expenses large.
Rectifying tower with bulkhead establishes a vertical wall by rectifying tower middle and upper part, tower is divided into the one of the integrated tower of complete heat of epimere, hypomere, the rectifying feed zone separated by dividing plate and the tetrameric novel texture of rectifying extraction section.With rectifying tower with bulkhead, binary mixture is separated into pure product and only needs a tower, reboiler, two condensers and two reflux splitters, energy consumption and facility investment can be minimized.Therefore the application of rectifying tower with bulkhead gets more and more in recent years.US5335504 and US5709780 discloses a kind of technology adopting rectifying tower with bulkhead Separation and Recovery carbonic acid gas; European patent EP 1413571, EP1371633 and US Patent No. 20030230476 disclose a kind of technology adopting rectifying tower with bulkhead to be separated TDI; UOP company has applied for the novel process of multinomial employing rectifying tower with bulkhead, as US6395950, US6395951, US6407303 and US6472578 disclose the technology adopting rectifying tower with bulkhead separation simulation moving-bed fractionation by adsorption isomerization high-octane rating raffinate; Total more than about 70 rectifying tower with bulkheads in the current whole world have carried out comercial operation.Although can adopt the rectifying tower with bulkhead of any number of side take-off in theory, in fact industrialized divided wall column only has a lateral line discharging, and is located at the bulkhead section side contrary with opening for feed.There is not been reported for the bulkhead rectifier unit combined with bulkhead section lateral line discharging by conventional lateral line discharging, also has no report rectifying tower with bulkhead being used for ethanol, tetrahydrofuran (THF) separation.
In above-mentioned existing ethanol, tetrahydrofuran (THF) isolation technique, all adopt independent knockout tower to reclaim tetrahydrofuran (THF), needs at least two knockout towers, investment is large, and energy consumption is high, and the tetrahydrofuran (THF) of recovery and ethanol to go out purity low.
Summary of the invention
Technical problem to be solved by this invention is in the sepn process of ethanol and tetrahydrofuran (THF) in the waste liquid of existing pharmaceutical industry, conventional distillation or interrupted extraction extractive distillation column number of units many, investment is large, energy consumption is high and reclaim the low technical problem of tetrahydrofuran (THF) purity, provides a kind of bulkhead type rectification column be separated for ethanol, tetrahydrofuran (THF) newly.With the material that this bulkhead type rectification column is separated containing ethanol and tetrahydrofuran (THF), there is less investment, the advantage that energy consumption is low and product purity is high.
In order to solve the problem, technical scheme of the present invention is as follows:
The present invention is used for the portion of energy integrated separation system of ethanol-tetrahydrofuran (THF), and for the situation that ethanol content in raw material is more, it is integrated rectifying tower and extraction agent knockout tower to be carried out portion of energy; In a divided wall column, complete portion of energy coupling rectification be separated.
What the present invention adopted is a kind of novel rectifying tower-divided wall column (DWC), it is the rectifying separation completing direct part Energy Coupling in a divided wall column, and the structure of this tower is: the top of tower is installed one piece of dividing wall and tower is divided into I, II, III, IV 4 regions (as shown in Figure 1).Wherein the Ith region is extracting rectifying district, and install tower tray in its main body with column plate, raw material and extraction agent enter from this region, the overhead extraction tetrahydrofuran (THF) in this region; IIth region is extraction agent recovery zone, also installs column plate in main body, the top extraction ethanol in this region; IIIth region is public stripping section, and being provided with two condensers at the top in the Ith, the IIth region is respectively used to gaseous stream condensation simultaneously, and be provided with reboiler at the bottom of tower for providing upflowing vapor for full tower, the extraction agent of rectifying is BDO.
The working method of direct sequence structure division Energy Coupling rectifying separation system is: the pressure of divided wall column is 101.325kpa, adopt atmospheric distillation, the stage number in region I is 20 ~ 27 blocks of plates, head temperature controls at 65 DEG C, control of reflux ratio is 4 ~ 7, extraction agent adds from tower top, and material adds from 16 ~ 13 blocks of plates; The stage number in region II is 11 ~ 20 blocks of plates, and head temperature is 70 DEG C, and control of reflux ratio is 3 ~ 6; The stage number in region III is 3 ~ 10 blocks of plates.
The extraction agent that the present invention adopts is BDO, and it is raw material important in chemical process, by simple addition reaction just getable BDO and effect of extracting is better.
The present invention adopts the method for diaphragm structure and Energy Coupling, be not only applicable to the separation of ethanol-tetrahydrofuran (THF), also be applicable to the separation of other approximate thing simultaneously, and adopt a divided wall column can complete the separation task of three common rectifying towers, greatly save investment.Meanwhile, adopt bulkhead distillation technology compared with the common rectification under vacuum of employing, tower reactor thermal load and tower top refrigeration duty can reduce by 15 ~ 30%, and purity >=99.9% of tetrahydrofuran (THF) product.Therefore, adopt technology of the present invention can solve technical problem in existing tetrahydrofuran (THF) rectification process preferably, achieve good technique effect.
Accompanying drawing illustrates:
Fig. 1 is device of the present invention and schematic flow sheet.
Fig. 2 is the schematic flow sheet of traditional extraction rectifying tower.
Embodiment
Further illustrate effect of the present invention with embodiment below, in embodiment and comparative example, selecting of extraction agent does not have special requirement.Described solvent ratio is the mass ratio of tetrahydrofuran (THF)-water.
Embodiment 1:
Raw material (tetrahydrofuran (THF): 35wt%, ethanol: 65wt%), extraction agent BDO (99.9%), adopt flow process shown in Fig. 1, temperature of charge is 20 DEG C, and flow is 100kg/h, extraction agent temperature is 30 DEG C, and flow is 220kg/h, and overhead condensation actuator temperature controls at 45 DEG C; Tower reactor thermal load is 64Kw, first total reflux one hour, then at the overhead extraction tetrahydrofuran (THF) in the Ith region, at the overhead extraction ethanol in the IIth region, from tower reactor extraction extraction agent BDO after rectifying for some time simultaneously, then extraction agent uses through interchanger heat exchange Posterior circle.Separating resulting lists in table 1.
Comparative example 1: raw material (tetrahydrofuran (THF): 35wt%, ethanol: 65wt%), extraction agent ethylene glycol (99.9m%), the operating parameters of comparative example 1 and the equipment adopted identical with embodiment 1, but adopt ethylene glycol extraction rectification technique.Separating resulting lists in table 1.
Embodiment 2
By the flow process shown in Fig. 1, other conditions are constant.Compare for convenience, separating resulting also lists in table 1.
Comparative example 2
The operating parameters of comparative example 2 and the extraction agent adopted identical with embodiment 2, but adopt traditional extraction rectification process, as shown in Figure 2, extractive distillation column 31 pieces of theoretical stages, solvent recovery tower 21 pieces of theoretical stages, raw material enters extractive distillation column after heating, and feed entrance point is the 12nd piece of theoretical stage, extraction agent 1,4-butyleneglycol enters the 2nd piece of theoretical stage after heating, high pure tetrahydrofuran is from extractive distillation column overhead extraction, and ethanol is from solvent recovery tower overhead extraction, and extraction agent recycles from extraction at the bottom of tower.Separating resulting lists in table 2.
Table 1 adopts the tetrahydrofuran (THF) separation simulation calculation result of bulkhead distillation technology
Table 2 adopts the tetrahydrofuran (THF) separation simulation calculation result of traditional extraction distillation technology
Claims (2)
1. the method utilizing rectifying tower with bulkhead extracting rectifying to extract the tetrahydrofuran (THF) in waste liquid, the method adopts the rectifying tower with dividing wall, namely in the vertical direction of common rectifying tower, one dividing wall is installed, tower is divided into four parts, wherein the Ith region is extracting rectifying region, main body installs column plate, is mainly used to assign to tetrahydrofuran (THF) and heavy constituent; IIth region is extraction agent recovery zone, and install tower tray and column plate in this region, the IVth region is the public stripping section in the Ith region and the IIth region; IIIth region is without any column plate, and the height being controlled the IIth region by division board is saved column plate with this and so both improve product purity and also save cost simultaneously; The method is: the waste liquid lower than azeotropic composition enters the Ith extracting rectifying district, region from opening for feed, the top temperature control in condenser the Ith region is provided with at 45 DEG C above the Ith region tower top, the control of reflux ratio in the Ith region is 4 ~ 7, highly purified tetrahydrofuran (THF) is from the top extraction in the Ith region, extraction agent adds from the tower top in the Ith region, and the mass ratio of extraction agent and waste liquid controls about 1 ~ 3; Install condenser at the top in the IIth region, head temperature controls at 50 DEG C, the IIth top, region extraction ethanol; Tower reactor extraction extraction agent, by continuing to recycle after interchanger heat exchange.
2. the method for abstraction distillation separation of tetrahydrofuran-ethyl alcohol as claimed in claim 1, is characterized in that the extraction agent selected is BDO.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410619853.3A CN104447636A (en) | 2014-11-07 | 2014-11-07 | Method and device for separating ethanol-tetrahydrofuran by extractive distillation by using dividing tower |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410619853.3A CN104447636A (en) | 2014-11-07 | 2014-11-07 | Method and device for separating ethanol-tetrahydrofuran by extractive distillation by using dividing tower |
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| CN104447636A true CN104447636A (en) | 2015-03-25 |
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| CN201410619853.3A Pending CN104447636A (en) | 2014-11-07 | 2014-11-07 | Method and device for separating ethanol-tetrahydrofuran by extractive distillation by using dividing tower |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110393940A (en) * | 2018-04-25 | 2019-11-01 | 杨祖杰 | A kind of next door tower aromatic hydrocarbons extraction rectifier unit |
| CN112876432A (en) * | 2021-01-30 | 2021-06-01 | 上海化工研究院有限公司 | Device and method for removing trace impurities in tetrahydrofuran |
| CN113181681A (en) * | 2021-05-24 | 2021-07-30 | 烟台大学 | Device and method for separating butane and butene from mixed carbon four through partition wall extractive distillation |
| CN113262515A (en) * | 2021-05-18 | 2021-08-17 | 河南中托力合化学有限公司 | Partition rectifying tower for separating mixed fraction of C8-C11 normal paraffins |
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| US5437770A (en) * | 1994-09-13 | 1995-08-01 | Lloyd Berg | Separation of ethanol from isopropanol by azeotropic distillation |
| CN1660828A (en) * | 2004-12-21 | 2005-08-31 | 哈尔滨工程大学 | Method for retrieving tetrahydrofuran from waste of pharmacy |
| CN103408513A (en) * | 2013-07-22 | 2013-11-27 | 青岛科技大学 | Method for separation of ethanol-tetrahydrofuran azeotrope by high-low pressure double-tower distillation |
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2014
- 2014-11-07 CN CN201410619853.3A patent/CN104447636A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5437770A (en) * | 1994-09-13 | 1995-08-01 | Lloyd Berg | Separation of ethanol from isopropanol by azeotropic distillation |
| CN1660828A (en) * | 2004-12-21 | 2005-08-31 | 哈尔滨工程大学 | Method for retrieving tetrahydrofuran from waste of pharmacy |
| CN103408513A (en) * | 2013-07-22 | 2013-11-27 | 青岛科技大学 | Method for separation of ethanol-tetrahydrofuran azeotrope by high-low pressure double-tower distillation |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110393940A (en) * | 2018-04-25 | 2019-11-01 | 杨祖杰 | A kind of next door tower aromatic hydrocarbons extraction rectifier unit |
| CN112876432A (en) * | 2021-01-30 | 2021-06-01 | 上海化工研究院有限公司 | Device and method for removing trace impurities in tetrahydrofuran |
| CN113262515A (en) * | 2021-05-18 | 2021-08-17 | 河南中托力合化学有限公司 | Partition rectifying tower for separating mixed fraction of C8-C11 normal paraffins |
| CN113262515B (en) * | 2021-05-18 | 2022-06-24 | 河南中托力合化学有限公司 | Partition rectifying tower for separating mixed fraction of C8-C11 normal paraffins |
| CN113181681A (en) * | 2021-05-24 | 2021-07-30 | 烟台大学 | Device and method for separating butane and butene from mixed carbon four through partition wall extractive distillation |
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