CN111888792A - Device and method for separating tetrahydrofuran-ethanol-water azeotrope system by extractive distillation - Google Patents
Device and method for separating tetrahydrofuran-ethanol-water azeotrope system by extractive distillation Download PDFInfo
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- 238000000895 extractive distillation Methods 0.000 title claims abstract description 101
- NNCLVCFOZHJMDL-UHFFFAOYSA-N 2-(oxolan-2-yl)ethanol;hydrate Chemical compound O.OCCC1CCCO1 NNCLVCFOZHJMDL-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000000926 separation method Methods 0.000 claims abstract description 69
- 238000010992 reflux Methods 0.000 claims abstract description 46
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 19
- 239000011344 liquid material Substances 0.000 claims description 17
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 13
- 238000000605 extraction Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 101000797623 Homo sapiens Protein AMBP Proteins 0.000 description 23
- 102100032859 Protein AMBP Human genes 0.000 description 23
- 101100225106 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) EDC2 gene Proteins 0.000 description 19
- 230000008878 coupling Effects 0.000 description 5
- 238000010168 coupling process Methods 0.000 description 5
- 238000005859 coupling reaction Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- BTVWZWFKMIUSGS-UHFFFAOYSA-N dimethylethyleneglycol Natural products CC(C)(O)CO BTVWZWFKMIUSGS-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229940053934 norethindrone Drugs 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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
- B01D3/34—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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- 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
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or 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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- 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
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Furan Compounds (AREA)
Abstract
The invention belongs to the field of separation and purification in the chemical industry, and relates to a device and a method for separating tetrahydrofuran-ethanol-water azeotrope system by extractive distillation. The invention adopts a method of pre-separation and two-time extractive distillation, adopts ethylene glycol as an extracting agent, and realizes the complete separation of tetrahydrofuran-ethanol-water azeotrope system through a pre-separation rectifying tower and two extractive rectifying towers. The device mainly comprises a pre-separation tower, a cooler, a flow divider, two extractive distillation towers, three condensers, three reflux tanks and three reboilers. The invention saves energy consumption cost and ensures the quality of products; the process device is reasonable; the method is also suitable for separating other similar ternary systems.
Description
Technical Field
The invention belongs to the field of separation and purification in the chemical industry, relates to a device and a method for separating a tetrahydrofuran-ethanol-water azeotropic system by extractive distillation, and further relates to a device and a method for separating the tetrahydrofuran-ethanol-water azeotropic system by using ethylene glycol as an extracting agent and adopting a pre-separation tower and two extractive distillation towers.
Background
Tetrahydrofuran and ethanol are important chemical raw materials and are widely applied to the industries of pharmacy, organic synthesis and the like. In the industrial production process of the norethindrone, the effective separation of the tetrahydrofuran-ethanol-water ternary system has great economic benefit for enterprises.
The tetrahydrofuran-ethanol-water system can form three binary azeotropes under normal pressure and exist in three rectification areas, and effective separation of the three azeotropes is difficult to realize by conventional rectification, so a special rectification method is required to separate the mixture of the three azeotropes. Chinese patent CN106967017A discloses a conventional extractive distillation method for separating tetrahydrofuran-ethanol-water mixture with mixed extractant, which comprises mixing dimethyl sulfoxide and ethylene glycol in a certain proportion to form the mixed extractant to separate tetrahydrofuran-ethanol-water mixture.
A method for separating a tetrahydrofuran-ethanol-water mixture by thermal coupling extractive distillation is reported in the literature (Zhao Y, Ma K, Bai W, et al, Energy-saving thermal coupling purification process by combining with mixed inlet distillation bio-ethanol [ J ]. Energy,2018, 148: 296. 308, 2018.), and the method has poor controllability in the actual industry.
The prior art for separating the tetrahydrofuran-ethanol-water ternary azeotropic system can be mainly divided into a conventional extraction and rectification process and a thermal coupling extraction and rectification process, and the problems of high energy consumption and poor economical efficiency exist in the conventional extraction and rectification process, and the problems of poor operability and controllability exist in the thermal coupling extraction and rectification process.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a device and a method for separating a tetrahydrofuran-ethanol-water mixture by three-tower extractive distillation coupled with pre-separation. The invention realizes the separation of the tetrahydrofuran-ethanol-water mixture and reduces the energy consumption of the process by coupling the three-tower extraction rectification technology of pre-separation. The invention adopts a pre-separation method and adopts a side-draw method to extract a product in advance, thereby avoiding the back-mixing effect to a certain extent and simultaneously directly introducing high-temperature streams into the pre-separation tower to further reduce the energy consumption.
The invention is realized by the following technical scheme:
a device for separating tetrahydrofuran-ethanol-water azeotrope by extractive distillation comprises a pre-separation tower, a cooler, a flow divider, two extractive distillation towers, three condensers, three reflux tanks and three reboilers.
The first reboiler R1, the second reboiler R2 and the third reboiler R3 are respectively connected with the bottoms of the pre-separation column PFT, the first extractive distillation column EDC1 and the second extractive distillation column EDC2, and are circularly reboiled at the bottoms of the respective columns; meanwhile, after the first reboiler R1 is connected with the cooler E, the cooler E is connected with the splitter S, and after being split by the splitter S, the cooler E is respectively connected with the middle parts of the first extractive distillation column EDC1 and the second extractive distillation column EDC 2; the second reboiler R2 is connected with the lower part of the second extractive distillation column EDC 2; the third reboiler R3 was connected to the lower part of the pre-separation column PFT.
The inlet end of the first condenser C1 is connected with the top of the pre-separation column PFT, the outlet end is connected with the inlet end of a first reflux tank D1, the outlet end of the first reflux tank D1 is divided into two paths, and the two paths are respectively connected with the top of the pre-separation column PFT and the middle part of a first extractive distillation column EDC 1; the inlet end of the second condenser C2 is connected with the top of the first extractive distillation column EDC1, the outlet end is connected with the inlet end of the second reflux tank D2, the outlet end of the second reflux tank D2 is divided into two paths, one path is connected with the top of the first extractive distillation column EDC1, and the other path is output as a product; the inlet end of the third condenser C3 is connected with the top of the second extractive distillation column EDC2, the outlet end is connected with the inlet end of the third reflux tank D3, the outlet end of the third reflux tank D3 is divided into two paths, one path is connected with the top of the second extractive distillation column EDC2, and the other path is output as a product.
A method for separating tetrahydrofuran-ethanol-water azeotrope system by extractive distillation adopts the device, and comprises the following steps:
step (1), feeding the tetrahydrofuran-ethanol-water ternary mixture and the bottom material from the EDC2 of the second extractive distillation tower into a pre-separation tower PFT from different tower plates, condensing overhead vapor of the pre-separation tower PFT through a first condenser C1, and then feeding the overhead vapor into a first reflux tank D1; one part of the material in the first reflux tank D1 enters a pre-separation column PFT through reflux, and the other part of the material and a first extraction agent flow into a first extractive distillation column EDC1 from different trays;
step (2), one part of liquid material at the bottom of the pre-separation tower PFT enters the pre-separation tower PFT after being reboiled by a first reboiler R1, the other part of liquid material is taken as an extractant, and the liquid material is divided into two parts after sequentially passing through a cooler E and a splitter S and then enters a first extractive distillation tower EDC1 and a second extractive distillation tower EDC2 for recycling;
step (3), liquid materials are extracted through a side line in a pre-separation tower PFT to obtain product water;
step (4), after a part of materials and a first strand of extracting agent in the first reflux tank D1 flow into the first extractive distillation tower EDC1 from different tower plates, separation is carried out, steam at the top of the first extractive distillation tower EDC1 is condensed by a second condenser C2 and collected by a second reflux tank D2, a part of materials reflux to the top of the first extractive distillation tower EDC1, and the other part of materials are taken as tetrahydrofuran products;
in the step (5), part of the bottom liquid material in the first extractive distillation column EDC1 is reboiled by a second reboiler R2 and then enters the first extractive distillation column EDC1, and the other part of the bottom liquid material as a material and a second strand of extractant flows into the second extractive distillation column EDC2 from different trays for separation;
step (6), after the bottom material of the first extractive distillation tower EDC1 enters a second extractive distillation tower EDC2, contacting with a second strand of extractant, separating, condensing the top steam of the second extractive distillation tower EDC2 through a third condenser C3, collecting the steam through a third reflux tank D3, refluxing a part of material to the top of the second extractive distillation tower EDC2, and collecting the other part of material as an ethanol product;
and (4) reboiling part of the bottom liquid material in the EDC2 of the second extractive distillation column in the step (7) by a third reboiler R3, then feeding the reboiled bottom liquid material into EDC2 of the second extractive distillation column, and feeding the other part of the bottom liquid material serving as the material and raw materials into a pre-separation column PFT from different trays for continuous separation.
The extractant is ethylene glycol.
The tetrahydrofuran-ethanol-water mixture can be mixed in any proportion, and the energy-saving effect of mixing with high-concentration water is more obvious.
The number of the trays of the pre-separation tower PFT is 50-54, the feeding position of the tetrahydrofuran-ethanol-water ternary mixture is 16-20 trays, the feeding position of the circulating stream is 36-40 trays, the lateral line extraction position is 26-30 trays, and the reflux ratio is 2.20-2.60; the EDC1 plate number of the first extractive distillation tower is 50-55, the feeding position of the extracting agent is 4-8 tower plates, the feeding position of the fresh raw material is 28-32 tower plates, and the reflux ratio is 2.21-4.39; the EDC2 plate number of the second extractive distillation column is 41-47, the feed position of the extracting agent is 12-18 th plate, the feed position of the top effluent of the pre-separation column PFT is 35-41 th plate, and the reflux ratio is 0.11-1.82; the operating pressure of the pre-separation column PFT, the first extractive distillation column EDC1 and the second extractive distillation column EDC2 is normal pressure; the temperature of the top of the pre-separation tower PFT is 67.80-68.02 ℃, and the temperature of the bottom of the pre-separation tower PFT is 207.21-207.93 ℃; the top temperature of the EDC1 of the first extractive distillation tower is 65.95-65.97 ℃, and the bottom temperature is 118.83-138.22 ℃; the top temperature of the EDC2 of the second extractive distillation tower is 78.19-78.28 ℃, and the bottom temperature is 179.78-198.53 ℃.
The molar ratio of the total amount of the extractant to the tetrahydrofuran-ethanol-water mixture is 1.59-2.35;
the mole ratio of the dosage of the extracting agent of the EDC1 of the first extractive distillation column to the molar ratio of the extracting agent of the EDC2 of the second extractive distillation column is 8.4-16.7.
The purity range of the tetrahydrofuran product obtained by the method is 99.65-99.93 mol%, and the yield is 99.66-99.93 mol%; the purity range of the ethanol product is 99.51 mol% -99.91 mol%, and the yield is 99.51 mol% -99.92 mol%; the purity range of the aquatic product is 99.95 mol% -99.99 mol%, and the yield is 99.95 mol% -99.99 mol%. The product has high purity and high yield.
Compared with the prior art, the invention mainly has the following beneficial effects:
(1) the method has simple process and convenient operation, and can successfully separate the tetrahydrofuran-ethanol-water mixture to obtain a high-purity product.
(2) Compared with the traditional separation process, the invention adopts the pre-separation and side-draw technology, reduces back mixing to a certain extent, fully utilizes the energy of the high-temperature extracting agent, reduces the energy consumption of the whole process, improves the energy utilization rate and saves the operation cost.
(3) The invention is also applicable to the separation of other similar ternary systems.
Drawings
FIG. 1 is a flow chart of an apparatus and a process for separating tetrahydrofuran-ethanol-water azeotrope by extractive distillation according to the present invention.
In the figure: a PFT pre-separation column; EDC1 first extractive distillation column; EDC2 second extractive distillation column;
D1-D3 first-third reflux drum; C1-C3 first-third condenser; R1-R3 first-third reboiler;
e, a cooler; and S, a current divider.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
The device and the method for separating the tetrahydrofuran-ethanol-water ternary azeotrope by extraction and rectification are shown in figure 1, and three specific examples are adopted to explain the process and the effect of the invention.
Example 1
Feed flow 200kmol/h, temperature 50 ℃, pressure 1atm (absolute), molar composition: tetrahydrofuran 20%, ethanol 20% and water 60%. The number of theoretical plates of the PFT of the pre-separation tower is 52, fresh materials are fed on the 18 th tray, circulating materials are fed on the 38 th tray, side-stream liquid is extracted on the 28 th tray, the reflux ratio is 2.20, the operation pressure is normal pressure, the temperature at the top of the tower is 68.02 ℃, and the temperature at the bottom of the tower is 207.57 ℃. The number of theoretical plates of EDC1 of the first extractive distillation column is 50, the material extracted from the top of the PFT of the pre-separation column is fed in the 28 th tray, the first circulating extractant is fed in the 6 th tray, the flow rate of the extractant is 300kmol/h, the reflux ratio is 4.39, the temperature at the top of the column is 65.95 ℃, the temperature at the bottom of the column is 118.83 ℃, and the operation pressure is normal pressure. The number of theoretical plates of EDC2 of the second extractive distillation column is 45, the material extracted from the bottom of EDC1 of the first extractive distillation column is fed at the 39 th tray, the second circulating extractant is fed at the 16 th tray, the flow rate of the extractant is 18kmol/h, the reflux ratio is 1.82, the temperature at the top of the column is 78.19 ℃, the temperature at the bottom of the column is 179.78 ℃, and the operating pressure is normal pressure.
After separation: the molar purity of the tetrahydrofuran product reaches 99.65 percent; the molar purity of the ethanol product reaches 99.51 percent; the molar purity of water is 99.95%; the yield of the tetrahydrofuran product reaches 99.66 percent; the yield of the ethanol product reaches 99.51 percent; the yield of aquatic products reaches 99.95 percent.
Example 2:
feed flow 100kmol/h, temperature 50 ℃, pressure 1atm (absolute), molar composition: tetrahydrofuran 20%, ethanol 20% and water 60%. The number of theoretical plates of the PFT of the pre-separation tower is 54, fresh materials are fed on a 20 th tray, circulating materials are fed on a 40 th tray, side-stream liquid is extracted on a 30 th tray, the reflux ratio is 2.40, the operation pressure is normal pressure, the temperature of the top of the tower is 67.96 ℃, and the temperature of the bottom of the tower is 207.93 ℃. The number of EDC1 theoretical plates of the first extractive distillation column is 52, the material extracted from the top of the PFT pre-separation column is fed at the 30 th tray, the first circulating extractant is fed at the 8 th tray, the flow rate of the extractant is 200kmol/h, the reflux ratio is 3.27, the temperature at the top of the column is 65.96 ℃, the temperature at the bottom of the column is 127.59 ℃, and the operation pressure is normal pressure. The number of theoretical plates of EDC2 of the second extractive distillation column is 47, the material extracted from the bottom of EDC1 of the first extractive distillation column is fed at 41 th tray, the second circulating extractant is fed at 18 th tray, the flow rate of the extractant is 20kmol/h, the reflux ratio is 0.28, the temperature at the top of the column is 78.23 ℃, the temperature at the bottom of the column is 189.12 ℃, and the operation pressure is normal pressure.
After separation: the purity of the tetrahydrofuran product reaches 99.77 percent; the molar purity of the ethanol product reaches 99.75 percent; the molar purity of water is 99.98%; the yield of the tetrahydrofuran product reaches 99.77 percent; the yield of the ethanol product reaches 99.75 percent; the yield of aquatic products reaches 99.98 percent.
Example 3:
feed flow 100kmo/h, temperature 50 ℃, pressure 1atm (absolute), molar composition: tetrahydrofuran 15%, ethanol 15% and water 70%. The theoretical plate number of the pre-separation tower (PFT) is 50, the fresh material is fed in the 16 th tray, the circulating material is fed in the 36 th tray, the side liquid is extracted in the 26 th tray, the reflux ratio is 2.60, the operation pressure is normal pressure, the temperature at the top of the tower is 67.80 ℃, and the temperature at the bottom of the tower is 207.21 ℃. The number of theoretical plates of EDC1 of the first extractive distillation column is 55, the material extracted from the top of the PFT of the pre-separation column is fed at the 32 th tray, the first circulation extractant is fed at the 4 th tray, the flow rate of the extractant is 210kmol/h, the reflux ratio is 2.21, the temperature at the top of the column is 65.97 ℃, the temperature at the bottom of the column is 138.22 ℃, and the operation pressure is normal pressure. The number of theoretical plates of EDC2 of the second extractive distillation column is 41, the material extracted from the bottom of EDC1 of the first extractive distillation column is fed in the 35 th tray, the second circulating extractant is fed in the 12 th tray, the flow rate of the extractant is 25kmol/h, the reflux ratio is 0.11, the temperature at the top of the column is 78.28 ℃, the temperature at the bottom of the column is 198.53 ℃, and the operation pressure is normal pressure.
After separation: the purity of the tetrahydrofuran product reaches 99.93 percent; the molar purity of the ethanol product reaches 99.92 percent; the molar purity of water is 99.99%; the yield of the tetrahydrofuran product reaches 99.93 percent; the yield of the ethanol product reaches 99.92 percent; the yield of aquatic products reaches 99.99 percent.
Claims (6)
1. The device for separating the tetrahydrofuran-ethanol-water azeotrope system by extraction and rectification is characterized by comprising a pre-separation tower, a cooler, a flow divider, two extraction and rectification towers, three condensers, three reflux tanks and three reboilers;
the first reboiler (R1), the second reboiler (R2) and the third reboiler (R3) are respectively connected with the bottoms of the pre-separation column (PFT), the first extractive distillation column (EDC1) and the second extractive distillation column (EDC2) and are circularly reboiled at the bottoms of the respective columns; meanwhile, after the first reboiler (R1) is connected with the cooler (E), the cooler (E) is connected with the splitter (S), split by the splitter (S) and then respectively connected with the middle parts of the first extractive distillation column (EDC1) and the second extractive distillation column (EDC 2); a second reboiler (R2) connected to the lower portion of a second extractive distillation column (EDC 2); a third reboiler (R3) connected to the lower part of the pre-separation column (PFT);
the inlet end of the first condenser (C1) is connected with the top of the pre-separation column (PFT), the outlet end of the first condenser is connected with the inlet end of a first reflux tank (D1), and the outlet end of the first reflux tank (D1) is divided into two paths and is respectively connected with the top of the pre-separation column (PFT) and the middle part of a first extractive distillation column (EDC 1); the inlet end of a second condenser (C2) is connected with the top of the first extractive distillation column (EDC1), the outlet end of the second condenser is connected with the inlet end of a second reflux tank (D2), the outlet end of the second reflux tank (D2) is divided into two paths, one path is connected with the top of the first extractive distillation column (EDC1), and the other path is output as a product; the inlet end of the third condenser (C3) is connected with the top of the second extractive distillation column (EDC2), the outlet end is connected with the inlet end of the third reflux tank (D3), the outlet end of the third reflux tank (D3) is divided into two paths, one path is connected with the top of the second extractive distillation column (EDC2), and the other path is output as a product.
2. The method for separating the tetrahydrofuran-ethanol-water azeotrope system by extractive distillation, which adopts the device of claim 1, is characterized by comprising the following steps:
step (1), feeding the tetrahydrofuran-ethanol-water ternary mixture and a material from the bottom of a second extractive distillation column (EDC2) into a pre-separation column (PFT) from different trays, condensing overhead steam of the pre-separation column (PFT) through a first condenser (C1), and then feeding the overhead steam into a first reflux tank (D1); one part of the material in the first reflux tank (D1) flows back to a pre-separation column (PFT) and the other part flows into a first extractive distillation column (EDC1) from different trays as the material and a first stream of extractant;
step (2), one part of liquid material at the bottom of the pre-separation column (PFT) enters the pre-separation column (PFT) after being reboiled by a first reboiler (R1), the other part of liquid material is taken as an extractant, and the liquid material is divided into two parts after sequentially passing through a cooler (E) and a splitter (S) and enters a first extractive distillation column (EDC1) and a second extractive distillation column (EDC2) for recycling;
in the step (3), liquid materials are extracted through a strand of lateral line in a pre-separation tower (PFT) to obtain product water;
step (4), after a part of materials and a first strand of extracting agent in a first reflux tank (D1) flow into a first extractive distillation column (EDC1) from different tower plates, separating, condensing overhead steam of the first extractive distillation column (EDC1) through a second condenser (C2), collecting through a second reflux tank (D2), refluxing a part of materials to the top of the first extractive distillation column (EDC1), and collecting the other part of materials as tetrahydrofuran products;
in the step (5), part of the bottom liquid material in the first extractive distillation column (EDC1) is reboiled by a second reboiler (R2) and enters the first extractive distillation column (EDC1), and the other part of the bottom liquid material as a material and a second strand of extractant flow into the second extractive distillation column (EDC2) from different trays for separation;
step (6), after the bottom material of the first extractive distillation column (EDC1) enters a second extractive distillation column (EDC2), contacting with a second strand of extractant, separating, condensing the overhead steam of the second extractive distillation column (EDC2) through a third condenser (C3), collecting through a third reflux tank (D3), refluxing a part of material to the top of the second extractive distillation column (EDC2), and collecting the other part of material as an ethanol product;
and (3) reboiling part of the bottom liquid material in the step (7) and the second extractive distillation column (EDC2) by a third reboiler (R3), then entering the second extractive distillation column (EDC2), and taking the other part of the bottom liquid material as a material and a raw material to flow into a pre-separation column (PFT) from different trays for continuous separation.
3. The method for separating the tetrahydrofuran-ethanol-water azeotrope by extractive distillation according to claim 2,
the extractant is ethylene glycol;
the tetrahydrofuran-ethanol-water mixture is mixed in any proportion.
4. The method for extractive distillation separation of tetrahydrofuran-ethanol-water azeotrope according to claim 2 or 3,
the number of the pre-separation tower (PFT) trays is 50-54, the feeding position of the tetrahydrofuran-ethanol-water ternary mixture is 16-20 trays, the feeding position of the circulating stream is 36-40 trays, the lateral line extraction position is 26-30 trays, and the reflux ratio is 2.20-2.60; the number of plates of the first extractive distillation column (EDC1) is 50-55, the feeding position of the extracting agent is 4-8 tower plates, the feeding position of the fresh raw material is 28-32 tower plates, and the reflux ratio is 2.21-4.39; the number of plates of the second extractive distillation column (EDC2) is 41-47, the feed position of the extracting agent is 12-18 th plates, the feed position of the top effluent of the pre-separation column (PFT) is 35-41 th plates, and the reflux ratio is 0.11-1.82; the operating pressure of the pre-separation column (PFT), the first extractive distillation column (EDC1) and the second extractive distillation column (EDC2) is normal pressure; the temperature of the top of the pre-separation tower (PFT) is 67.80-68.02 ℃, and the temperature of the bottom of the pre-separation tower (PFT) is 207.21-207.93 ℃; the temperature of the top of a first extractive distillation column (EDC1) is 65.95-65.97 ℃, and the temperature of the bottom of the first extractive distillation column is 118.83-138.22 ℃; the top temperature of the second extractive distillation column (EDC2) is 78.19-78.28 ℃, and the bottom temperature is 179.78-198.53 ℃.
5. The method for extractive distillation separation of tetrahydrofuran-ethanol-water azeotrope according to claim 2 or 3,
the molar ratio of the total amount of the extractant to the tetrahydrofuran-ethanol-water mixture is 1.59-2.35;
the mole ratio of the extractant of the first extractive distillation column (EDC1) to the extractant of the second extractive distillation column (EDC2) is 8.4-16.7.
6. The method for extractive distillation separation of tetrahydrofuran-ethanol-water azeotrope according to claim 2 or 3,
the molar ratio of the total amount of the extractant to the tetrahydrofuran-ethanol-water mixture is 1.59-2.35;
the mole ratio of the extractant of the first extractive distillation column (EDC1) to the extractant of the second extractive distillation column (EDC2) is 8.4-16.7.
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Application publication date: 20201106 Assignee: Dalian Tongjia Technology Co.,Ltd. Assignor: DALIAN University OF TECHNOLOGY Contract record no.: X2023980049187 Denomination of invention: Device and Method for Extractive Distillation Separation of Tetrahydrofuran Ethanol Water Azeotropic System Granted publication date: 20210518 License type: Common License Record date: 20231130 |