CN109111337B - Separation equipment and method for mixed solvent containing toluene, ethyl acetate, ethanol and the like - Google Patents
Separation equipment and method for mixed solvent containing toluene, ethyl acetate, ethanol and the like Download PDFInfo
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- CN109111337B CN109111337B CN201811286607.5A CN201811286607A CN109111337B CN 109111337 B CN109111337 B CN 109111337B CN 201811286607 A CN201811286607 A CN 201811286607A CN 109111337 B CN109111337 B CN 109111337B
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 873
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 680
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 title claims abstract description 605
- 239000012046 mixed solvent Substances 0.000 title claims abstract description 67
- 238000000926 separation method Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000007670 refining Methods 0.000 claims abstract description 327
- 238000000605 extraction Methods 0.000 claims abstract description 236
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims description 79
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 239000000463 material Substances 0.000 claims description 46
- 238000004064 recycling Methods 0.000 claims description 19
- 239000000284 extract Substances 0.000 claims description 17
- 239000000945 filler Substances 0.000 claims description 17
- 230000008859 change Effects 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 12
- 230000000630 rising effect Effects 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 6
- 108700002808 N-Me-Phe(3)- morphiceptin Proteins 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims 1
- 238000011027 product recovery Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 110
- 239000012071 phase Substances 0.000 description 78
- 239000000203 mixture Substances 0.000 description 15
- OMQHDIHZSDEIFH-UHFFFAOYSA-N 3-Acetyldihydro-2(3H)-furanone Chemical compound CC(=O)C1CCOC1=O OMQHDIHZSDEIFH-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000003944 tolyl group Chemical group 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 101000954570 Mus musculus V-type proton ATPase 16 kDa proteolipid subunit c Proteins 0.000 description 1
- 229930003451 Vitamin B1 Natural products 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229960003495 thiamine Drugs 0.000 description 1
- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
- 239000011691 vitamin B1 Substances 0.000 description 1
- 235000010374 vitamin B1 Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/10—Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids
Abstract
The invention belongs to the field of solvent recovery, and particularly relates to separation equipment and a separation method for a mixed solvent containing toluene, ethyl acetate, ethanol and the like. The invention comprises an extraction tower, an ethanol light component removal tower condenser, an ethanol light component removal tower reboiler, an ethanol light component removal tower layering device, an ethanol product tower condenser, an ethanol product tower reboiler, an extractant cooler, a toluene refining tower condenser, a toluene refining tower reboiler, an ethyl acetate refining tower condenser, an ethyl acetate refining tower reboiler and an ethyl acetate refining tower layering device. The device can be used for separating the mixed solvent containing toluene, ethyl acetate, ethanol and the like, and has low energy consumption and high recovery purity; the method does not introduce other impurities additionally, and can effectively reduce energy consumption and equipment investment.
Description
Technical Field
The invention belongs to the field of solvent recovery, and particularly relates to separation equipment and a separation method for a mixed solvent containing toluene, ethyl acetate, ethanol and the like.
Background
Alpha-acetyl-gamma-butyrolactone, ABL for short, of formula: c (C) 6 H 8 O 3 Molecular weight: 128.13 CAS number:517-23-7, is a colorless transparent liquid with ester smell, and is mainly used for synthesizing vitamin B1 and pesticide. The main route for producing the alpha-acetyl-gamma-butyrolactone at present is to take gamma-butyrolactone and ethyl acetate as raw materials, sodium as a catalyst and toluene as a solvent, the production process produces ethanol as a byproduct, and meanwhile, a small amount of water exists in the raw materials, and in the subsequent product distillation and purification process, the solvent needs to be distilled out firstly, and the distilled mixed solvent comprises the following components: 30-34% toluene, 32-38% ethyl acetate, 30-33.5% ethanol and 0.5-2.0% water. The mixed solvent is required to be separated, so that the solvent toluene: purity greater than 99.6%, ethanol content less than 400ppm and moisture less than 400ppm, raw material ethyl acetate: the purity is more than 99.6%, the ethanol content is less than 400ppm and the water content is less than 400ppm so as to meet the recycling requirement, and the ethanol reaches the industrial ethanol standard for sale.
The separation and purification of the generated mixed solvent is a very difficult problem, because the system has a plurality of groups of binary azeotropes and ternary azeotropes under normal pressure, the ethanol content in the binary azeotropes of ethanol and water is 95.6%, and the azeotropes temperature is 78.2 ℃; the content of ethanol in the binary azeotropic composition of ethanol and toluene is 68 percent, and the azeotropic temperature is 76.7 ℃; the content of ethanol in the binary azeotropic composition of ethanol and ethyl acetate is 31 percent, and the azeotropic temperature is 71.8 ℃; the ethanol content in the binary azeotropic composition of ethyl acetate and water is 91.5 percent, and the azeotropic temperature is 70.4 ℃; the toluene content in the binary azeotropic composition of toluene and water is 86.5%, and the azeotropic temperature is 84.1 ℃; the ternary azeotropic composition of ethyl acetate, ethanol and water has the ethyl acetate content of 78.3 percent, the ethanol content of 13.1 percent and the azeotropic temperature of 70.2 ℃, so that the separation of the mixed solvent is difficult to realize by common rectification.
The patent CN102992930B discloses a toluene solvent recovery process and separation equipment thereof in the production process of alpha-acetyl-gamma-butyrolactone, the method adopts an extraction rectification process, ketone substances are used as an extractant to separate toluene from mixed solvents containing toluene, ethyl acetate, ethanol and the like through twice extraction rectification, and alcohol substances are further used as the extractant to separate a mixture of ethyl acetate and ethanol. Although the method realizes the separation of the mixed solvent, the method adopts two kinds of extracting agents, and two additional other components are introduced in the separation process, so that other impurities are inevitably introduced into three separated products (toluene, ethyl acetate and ethanol respectively), thereby affecting the quality of ABL.
Disclosure of Invention
In view of the above, the invention aims to provide a separation device and a separation method for mixed solvents containing toluene, ethyl acetate, ethanol and the like, and the separation device can be used for separating the mixed solvents containing toluene, ethyl acetate, ethanol and the like, and has the advantages of low energy consumption and high recovery purity; the method does not introduce other impurities additionally, and can effectively reduce energy consumption and equipment investment.
The scheme of the separation equipment is as follows:
a separation device containing mixed solvents such as toluene, ethyl acetate, ethanol and the like comprises an extraction tower, an ethanol light-off tower condenser, an ethanol light-off tower reboiler, an ethanol light-off tower layering device, an ethanol product tower condenser, an ethanol product tower reboiler, an extractant cooler, a toluene refining tower condenser, a toluene refining tower reboiler, an ethyl acetate refining tower condenser, an ethyl acetate refining tower reboiler and an ethyl acetate refining tower layering device;
the top of the extraction tower is provided with an extraction phase discharge port of the extraction tower, the upper part of the extraction tower is provided with an extraction agent feed port of the extraction tower, the bottom of the extraction tower is provided with an extraction raffinate phase discharge port of the extraction tower, and the lower part of the extraction tower is provided with a mixed solvent feed port; the top of the ethanol light component removing tower is provided with an ethanol light component removing tower azeotrope circulating extraction outlet, the upper part is provided with an ethanol light component removing tower reflux port, the middle part is provided with an ethanol light component removing tower raffinate phase feed inlet, the lower part is provided with an ethanol light component removing tower reboiling inlet, and the bottom is provided with an ethanol light component removing tower extraction outlet and an ethanol light component removing tower reboiling outlet; the top of the ethanol product tower is provided with an ethanol product tower reflux port and an ethanol product outlet, the middle part is provided with an ethanol product tower feed inlet, the lower part is provided with an ethanol product tower reboiling inlet, and the bottom is provided with an ethanol product tower outlet and an ethanol product tower reboiling outlet; the top of the toluene refining tower is provided with a toluene refining tower reflux port and a toluene refining tower outlet, the middle part is provided with a toluene refining tower extract phase feed port, the lower part is provided with a toluene refining tower reboiling inlet, and the bottom is provided with a toluene refining tower toluene product outlet and a toluene refining tower reboiling outlet; the top of the ethyl acetate refining tower is provided with an ethyl acetate refining tower reflux port and an ethyl acetate refining tower azeotrope recycling outlet, the middle part is provided with an ethyl acetate refining tower feed inlet, the lower part is provided with an ethyl acetate refining tower reboiling inlet, and the bottom is provided with an ethyl acetate product outlet and an ethyl acetate refining tower reboiling outlet;
The top of the toluene refining tower is provided with a toluene refining tower reflux port and a toluene refining tower outlet, the middle part of the toluene refining tower is provided with a toluene refining tower extract phase feed port, the lower part of the toluene refining tower is provided with a toluene refining tower reboiling inlet, and the bottom of the toluene refining tower is provided with a toluene refining tower toluene product outlet and a toluene refining tower reboiling outlet; the top of the ethyl acetate refining tower is provided with an ethyl acetate refining tower reflux port and an ethyl acetate refining tower azeotrope recycling outlet, the middle of the ethyl acetate refining tower is provided with an ethyl acetate refining tower feed port, the lower of the ethyl acetate refining tower is provided with an ethyl acetate refining tower reboiling inlet, and the bottom of the ethyl acetate refining tower is provided with an ethyl acetate product outlet and an ethyl acetate refining tower reboiling outlet;
the extraction tower raffinate phase discharge port at the bottom of the extraction tower is connected with the extraction tower raffinate phase feed port at the middle part of the ethanol light-removal tower through an extraction tower raffinate phase discharge pipe, and the extraction tower extract phase discharge port at the top of the extraction tower is connected with the toluene refining tower extract phase feed port at the middle part of the toluene refining tower through an extraction tower extract phase discharge pipe;
The device comprises an extraction tower, an alcohol stripping tower top vapor pipe, an alcohol stripping tower condenser, an alcohol stripping tower top extraction pipe, an alcohol stripping tower layering device oil phase discharging pipe, an azeotrope circulating total material pipe and a total mixed solvent feeding pipe which are sequentially connected, wherein the alcohol stripping tower azeotrope circulating extraction outlet at the top of the alcohol stripping tower is connected to the mixed solvent feeding port at the lower part of the extraction tower, the alcohol stripping tower reflux port at the upper part of the alcohol stripping tower is connected with the outlet of the alcohol stripping tower condenser through the alcohol stripping tower top reflux pipe, the alcohol stripping tower extraction outlet at the bottom of the alcohol stripping tower is connected with the alcohol product tower feeding port at the middle part of the alcohol product tower through the alcohol stripping tower bottom extraction pipe, and the alcohol stripping tower reboiling outlet at the bottom of the alcohol stripping tower is connected with the gas phase reflux pipe at the lower part through the alcohol stripping tower bottom reboiler inlet and the alcohol stripping tower reboiler which are sequentially connected;
the ethanol product tower extraction outlet at the bottom of the ethanol product tower is connected to an extraction tower extractant feed inlet at the upper part of the extraction tower through a ethanol product tower kettle extraction pipe, an extractant cooler, an extractant circulating pipe and a total extractant feed pipe which are sequentially connected, and the ethanol product tower reboiling outlet at the bottom of the ethanol product tower is connected with an ethanol product tower reboiling inlet at the lower part of the ethanol product tower through an ethanol product tower kettle reboiler inlet pipe, an ethanol product tower reboiler and an ethanol product tower kettle gas phase reflux pipe which are sequentially connected;
The toluene refining tower extraction port at the top of the toluene refining tower is connected to the ethyl acetate refining tower feed inlet at the middle part of the ethyl acetate refining tower through a toluene refining tower top steam pipe, a toluene refining tower condenser and a toluene refining tower top extraction pipe which are sequentially connected, the toluene refining tower reflux port at the top of the toluene refining tower is connected with the toluene refining tower condenser outlet, the toluene product extraction port at the bottom of the toluene refining tower is extracted through a toluene refining tower kettle extraction pipe, and the toluene refining tower reboiling outlet at the bottom of the toluene refining tower is connected with the toluene refining tower reboiling inlet at the lower part of the toluene refining tower through a toluene refining tower kettle reboiler pipe, a toluene refining tower reboiler and a toluene refining tower kettle reflux pipe which are sequentially connected;
the ethyl acetate refining tower azeotrope recycling extraction outlet at the top of the ethyl acetate refining tower is connected to the mixed solvent feed inlet at the lower part of the extraction tower through a vapor pipe at the top of the ethyl acetate refining tower, a condenser at the top of the ethyl acetate refining tower, a extraction pipe at the top of the ethyl acetate refining tower, an ethyl acetate refining tower layering device, an oil phase discharge pipe of the ethyl acetate refining tower layering device, an azeotrope recycling total material pipe and a total mixed solvent feed pipe which are sequentially connected, the ethyl acetate refining tower reflux inlet at the top of the ethyl acetate refining tower is connected with the outlet of the condenser at the top of the ethyl acetate refining tower, the ethyl acetate product extraction outlet at the bottom of the ethyl acetate refining tower is extracted through a extraction pipe at the bottom of the ethyl acetate refining tower,
And the reboiling outlet of the ethyl acetate refining tower at the bottom of the ethyl acetate refining tower is connected with the reboiling inlet of the ethyl acetate refining tower at the lower part of the ethyl acetate refining tower through a reboiler inlet pipe, an ethyl acetate refining tower reboiler and a gas phase backflow pipe of the ethyl acetate refining tower kettle which are connected in sequence.
Further, for better extraction effect, the lower middle part of the extraction tower is provided with a circulating discharge port, the extraction tower is also provided with at least one circulating feed port positioned on the upper side of the circulating discharge port, and the circulating discharge port of the extraction tower is connected with the circulating feed port through a circulating discharge pipe.
Further, in order to achieve better extraction effect, the number of the circulating feed inlets of the extraction tower is two, wherein one circulating feed inlet is positioned at the middle upper part of the extraction tower, and the other circulating feed inlet is positioned at the upper part of the extraction tower; the circulating discharge port of the extraction tower is connected with one of the circulating feed ports through a circulating discharge pipe; the circulating discharge port of the extraction tower is connected with the circulating feed pipe through a circulating discharge pipe between the circulating discharge port and the other circulating feed port.
Further, the type of column internals of the extraction column is a column plate or packing, and the theoretical plate number is 16-25.
Further, the ethanol light component removing tower consists of a rectifying section above a raffinate phase feed inlet and a stripping section below the raffinate phase feed inlet, wherein tower plates or fillers are arranged as tower internals, the theoretical plate number of the rectifying section is 12-25, and the theoretical plate number of the stripping section is 18-28.
Further, the ethanol product tower consists of a rectifying section above the feed inlet and a stripping section below the feed inlet, wherein tower internals are tower plates or fillers, the theoretical plates of the rectifying section are 20-35, and the theoretical plates of the stripping section are 15-26.
Further, the toluene refining tower consists of a rectifying section above the feed inlet of the extraction phase and a stripping section below the feed inlet of the extraction phase, wherein the type of tower internals is tower plates or packing, the theoretical plate number of the rectifying section is 16-26, and the theoretical plate number of the stripping section is 25-36.
Further, the ethyl acetate refining tower consists of a rectifying section above a feed inlet and a stripping section below the feed inlet, wherein tower plates or fillers are arranged as tower internals, the theoretical plates of the rectifying section are 18-24, and the theoretical plates of the stripping section are 26-35.
The method for separating the mixed solvent containing toluene, ethyl acetate, ethanol and the like comprises the following steps:
step S1: the mixed solvent containing toluene, ethyl acetate, ethanol and the like enters the lower part of the extraction tower from a mixed solvent feed inlet through a total mixed solvent feed pipe, and the extractant enters the upper part of the extraction tower from a total extractant feed pipe;
Step S2: the raffinate phase at the bottom of the extraction tower enters an ethanol light-removal tower through a raffinate phase discharging pipe of the extraction tower to carry out rectification, the ascending steam at the top of the ethanol light-removal tower is subjected to phase change through a condenser, the materials obtained by condensation are ternary azeotrope containing ethyl acetate, ethanol and water and binary azeotrope of toluene and water, one part of the materials flows back into the tower from a reflux port of the ethanol light-removal tower at the top of the ethanol light-removal tower, the other part of the materials enters an ethanol light-removal tower layering device from a recycling extracting port of the ethanol light-removal tower at the top of the ethanol light-removal tower through an extracting pipe at the top of the ethanol light-removal tower, a lower water phase is discharged through a water phase discharging pipe of the ethanol light-removal tower layering device, and an upper oil phase returns to a mixed solvent feeding port at the lower part of the extraction tower for recycling through an oil phase discharging pipe of the ethanol light-removal tower layering device;
step S3: materials at the bottom of an ethanol light component removal tower kettle enter an ethanol product tower through a extraction pipe at the bottom of the ethanol light component removal tower kettle to be rectified, steam rising at the top of the ethanol product tower is subjected to phase change through a condenser, one part of the steam flows back into the tower from a reflux port of the ethanol product tower at the top of the ethanol product tower, the other part of the steam flows back into the tower from a extraction port of the ethanol light component removal tower at the top of the ethanol product tower through an extraction pipe extraction system at the top of the ethanol product tower, and an extractant separated from the bottom of the ethanol product tower is cooled by an extractant cooler and then returns to an extraction tower feed port at the upper part of the extraction tower from an extractant circulation pipe to be recycled; condensing the obtained material into an industrial ethanol product with the concentration of 95%;
Step S4: the extraction phase at the top of the extraction tower enters a toluene refining tower through an extraction phase discharging pipe of the extraction tower for rectification, the vapor rising at the top of the toluene refining tower is subjected to phase change through a condenser, the condensed material is a mixture of ethyl acetate, a small amount of water and trace toluene, one part of the condensed material flows back into the toluene refining tower from a reflux port at the top of the toluene refining tower, the other part of the condensed material enters the ethyl acetate refining tower from a recovery port at the top of the toluene refining tower through a recovery pipe at the top of the toluene refining tower, and the product obtained at the bottom of the toluene refining tower is recovered from a recovery pipe system at the bottom of the toluene refining tower; (the product obtained in the tower kettle is toluene product with purity of more than 99.6 percent)
Step S5: materials from a top extraction outlet of the toluene refining tower enter the ethyl acetate refining tower to be rectified, steam rising at the top of the ethyl acetate refining tower is subjected to phase change through a condenser, the condensed materials are mixtures of ethyl acetate, water azeotropes and toluene and water azeotropes, one part of the condensed materials flows back into the ethyl acetate refining tower from a reflux port of the ethyl acetate refining tower at the top of the ethyl acetate refining tower, the other part of the condensed materials circulate the ethyl acetate refining tower from the extraction outlet of the ethyl acetate refining tower to enter an ethyl acetate refining tower layering device through an extraction pipe at the top of the ethyl acetate refining tower to be layered, a lower water phase is discharged through an aqueous phase discharge pipe of the ethyl acetate refining tower layering device, an upper oil phase is returned to a lower feed port of the extraction tower to be recycled, and a product obtained from an ethyl acetate refining tower kettle is discharged through an extraction pipe at the bottom of the ethyl acetate refining tower. The ethyl acetate product with the purity of more than 99.6% is obtained in the ethyl acetate refining tower kettle.
Further, the extractant is water;
the operating conditions within the extraction column are set to: the pressure at the top of the tower is normal pressure, the operating temperature is normal temperature, the volume ratio of the extractant entering from the total extractant feed pipe to the mixed acid wastewater entering from the total mixed solvent feed pipe is 0.4-1.2, and the volume ratio of the middle-lower part circulating discharge port to the extractant is 1.0-4.0;
the operating conditions in the ethanol light ends column are set as follows: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 66-73 ℃, the temperature at the bottom of the tower is 80-90 ℃, and the reflux ratio at the top of the tower is 1.2-4.5;
the operating conditions within the ethanol product column are set to: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 77-80 ℃, the temperature at the bottom of the tower is 99-101 ℃, and the reflux ratio at the top of the tower is 1.8-8.0;
the operating conditions in the toluene refining column were set as follows: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 73-79 ℃, the temperature at the bottom of the tower is 112-118 ℃, and the reflux ratio at the top of the tower is 1.0-5.0;
the operating conditions in the ethyl acetate refining column were set as follows: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 67-73 ℃, the temperature at the bottom of the tower is 75-79 ℃, and the reflux ratio at the top of the tower is 2.0-7.0.
The invention has the remarkable advantages that:
(1) The existing component water in the mixed solvent is selected as an extracting agent, and the separation of toluene, ethyl acetate, ethanol and water in the mixed solvent is effectively realized by adopting an extraction and rectification coupling process, so that the difficult problem of separation of a plurality of groups of azeotropes in the system is solved, and the influence of other components is avoided, which is introduced to influence the quality of the separated solvent.
(2) Compared with the five-tower extraction rectification process adopted by the patent CN102992930B, the method for separating the mixed solvent containing toluene, ethyl acetate, ethanol and water by adopting the extraction and rectification coupling process has the advantages that the first tower is an extraction tower, steam is not required to be consumed, the other towers are all normal-pressure rectification, and reduced-pressure rectification is not required, so that the energy consumption and equipment investment of separation are effectively reduced, the energy consumption can be saved by 20-35%, and the equipment investment can be saved by 17-28%.
(3) With the method of the invention, the recovered toluene: purity greater than 99.6%, ethanol content less than 400ppm and moisture less than 400ppm; recovered ethyl acetate: purity greater than 99.6%, ethanol content less than 400ppm and moisture content less than 400ppm; recovered ethanol: the purity is more than 95 percent, and the industrial ethanol standard is achieved.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
The reference numerals in the figures are illustrated as follows: t1-extraction tower, T2-ethanol light component removing tower, T3-ethanol product tower, T4-toluene refining tower and T5-ethyl acetate refining tower; an E1-ethanol light component removal tower condenser, an E2-ethanol light component removal tower reboiler, an E3-ethanol product tower condenser, an E4-ethanol product tower reboiler, an E5-extractant cooler, an E6-toluene refining tower condenser, an E7-toluene refining tower reboiler, an E8-ethyl acetate refining tower condenser, an E9-ethyl acetate refining tower reboiler, an ethanol light component removal tower layering device (V1) and an ethyl acetate refining tower layering device (V2); PL 1-fresh mixed solvent feeding pipe, PL 2-total mixed solvent feeding pipe, PL 3-supplementary extractant feeding pipe, PL 4-total extractant feeding pipe, PL 5-extraction column raffinate discharging pipe, PL 6-extraction column extract discharging pipe, PL 7-extraction column middle and lower circulating discharging pipe, PL 8-extraction column middle and upper circulating feeding pipe, PL 9-extraction column upper circulating feeding pipe, PL 10-alcohol stripping column top steam pipe, PL 11-alcohol stripping column top reflux pipe, PL 12-alcohol stripping column top extracting pipe, PL 13-alcohol stripping column separator water phase discharging pipe, PL 14-alcohol stripping column separator oil phase discharging pipe, PL 15-alcohol stripping column kettle feeding reboiler pipe, PL 16-alcohol stripping column kettle gas phase reflux pipe, PL 17-alcohol stripping column kettle extracting pipe, PL 18-alcohol product column top steam pipe, PL 19-alcohol product column top reflux pipe, PL 20-alcohol product column top extracting pipe, PL 21-ethanol product tower kettle reboiler inlet pipe, PL 22-ethanol product tower kettle gas phase reflux pipe, PL 23-ethanol product tower kettle extraction pipe, PL 24-extractant circulation pipe, PL 25-toluene refining tower top steam pipe, PL 26-toluene refining tower top reflux pipe, PL 27-toluene refining tower top extraction pipe, PL 28-toluene refining tower kettle reboiler inlet pipe, PL 29-toluene refining tower kettle gas phase reflux pipe, PL 30-toluene refining tower kettle extraction pipe, PL 31-ethyl acetate refining tower top steam pipe, PL 32-ethyl acetate refining tower top reflux pipe, PL 33-ethyl acetate refining tower top extraction pipe, PL 34-ethyl acetate refining tower separator water phase discharge pipe, PL 35-ethyl acetate refining tower separator oil phase discharge pipe, PL 36-azeotrope circulation total pipe, PL 37-ethyl acetate refining tower kettle reboiler inlet pipe, PL 38-ethyl acetate refining tower kettle gas phase reflux pipe, PL 39-ethyl acetate refining tower bottom extraction pipe.
Detailed Description
The invention will be further described with reference to the accompanying drawings and examples.
Example 1
As shown in fig. 1, the present embodiment provides a separation apparatus for a mixed solvent containing toluene, ethyl acetate, ethanol and the like, which comprises an extraction column T1, an ethanol light-off column T2, an ethanol light-off column condenser E1, an ethanol light-off column reboiler E2, an ethanol light-off column separator V1, an ethanol product column T3, an ethanol product column condenser E3, an ethanol product column reboiler E4, an extractant cooler E5, a toluene refining column T4, a toluene refining column condenser E6, a toluene refining column reboiler E7, an ethyl acetate refining column T5, an ethyl acetate refining column condenser E8, an ethyl acetate refining column reboiler E9, and an ethyl acetate refining column separator V2;
the top of the extraction tower T1 is provided with an extraction phase discharge port of the extraction tower, the upper part of the extraction phase discharge port is provided with an extraction agent feed port of the extraction tower, the bottom of the extraction tower is provided with a raffinate phase discharge port of the extraction tower, and the lower part of the extraction tower is provided with a mixed solvent feed port; the top of the ethanol light component removal tower T2 is provided with an ethanol light component removal tower azeotrope circulating extraction outlet, the upper part is provided with an ethanol light component removal tower reflux port, the middle part is provided with an ethanol light component removal tower raffinate phase feed inlet, the lower part is provided with an ethanol light component removal tower reboiling inlet, and the bottom is provided with an ethanol light component removal tower extraction outlet and an ethanol light component removal tower reboiling outlet; the top of the ethanol product tower T3 is provided with an ethanol product tower reflux port and an ethanol product outlet, the middle part is provided with an ethanol product tower feed inlet, the lower part is provided with an ethanol product tower reboiling inlet, and the bottom is provided with an ethanol product tower outlet and an ethanol product tower reboiling outlet; the top of the toluene refining tower T4 is provided with a toluene refining tower reflux port and a toluene refining tower outlet, the middle part is provided with a toluene refining tower extract phase feed port, the lower part is provided with a toluene refining tower reboiling inlet, and the bottom is provided with a toluene refining tower toluene product outlet and a toluene refining tower reboiling outlet; the top of the ethyl acetate refining tower T5 is provided with an ethyl acetate refining tower reflux port and an ethyl acetate refining tower azeotrope recycling outlet, the middle part is provided with an ethyl acetate refining tower feed inlet, the lower part is provided with an ethyl acetate refining tower reboiling inlet, and the bottom is provided with an ethyl acetate product outlet and an ethyl acetate refining tower reboiling outlet;
The top of the toluene refining tower T4 is provided with a toluene refining tower reflux port and a toluene refining tower outlet, the middle part of the toluene refining tower T4 is provided with a toluene refining tower extract phase feed port, the lower part of the toluene refining tower T4 is provided with a toluene refining tower reboiling inlet, and the bottom of the toluene refining tower T4 is provided with a toluene refining tower toluene product outlet and a toluene refining tower reboiling outlet; the top of the ethyl acetate refining tower T5 is provided with an ethyl acetate refining tower reflux port and an ethyl acetate refining tower azeotrope recycling outlet, the middle part of the ethyl acetate refining tower T5 is provided with an ethyl acetate refining tower feed port, the lower part of the ethyl acetate refining tower T5 is provided with an ethyl acetate refining tower reboiling inlet, and the bottom of the ethyl acetate refining tower T5 is provided with an ethyl acetate product outlet and an ethyl acetate refining tower reboiling outlet;
the extraction tower raffinate phase discharge port at the bottom of the extraction tower T1 is connected with the extraction tower raffinate phase feed port in the middle of the ethanol light ends removal tower T2 through an extraction tower raffinate phase discharge pipe PL5, and the extraction tower extract phase discharge port at the top of the extraction tower T1 is connected with the toluene refining tower extract phase feed port in the middle of the toluene refining tower T4 through an extraction tower extract phase discharge pipe PL 6;
The azeotropic mixture circulation extraction port of the ethanol stripping tower at the top of the ethanol stripping tower T2 is connected with the mixed solvent feed port at the lower part of the extraction tower T1 through a steam pipe PL10 at the top of the ethanol stripping tower, a condenser E1 of the ethanol stripping tower, a extraction pipe PL12 at the top of the ethanol stripping tower, an ethanol stripping tower separator V1, an oil phase discharge pipe PL14 of the ethanol stripping tower separator, an azeotropic mixture circulation total pipe PL36 and a total mixed solvent feed pipe PL2 which are sequentially connected, the reflux port of the ethanol stripping tower at the upper part of the ethanol stripping tower T2 is connected with the outlet of the condenser E1 of the ethanol stripping tower through a reflux pipe PL11 at the top of the ethanol stripping tower, the ethanol stripping tower extraction port at the bottom of the ethanol stripping tower T2 is connected with the ethanol product tower feed port at the middle part of the ethanol product tower T3 through a recovery pipe PL17 of the ethanol stripping tower kettle, and the reflux port of the ethanol stripping tower at the bottom of the ethanol stripping tower T2 is connected with the reflux pipe PL16 of the ethanol stripping tower through a reboiler at the bottom of the ethanol stripping tower T2;
an ethanol product tower top steam pipe PL18, an ethanol product tower condenser E3 and an ethanol product tower top extraction pipe PL20 are sequentially connected outside an ethanol product extraction port at the top of the ethanol product tower T3, the ethanol product tower extraction port at the bottom of the ethanol product tower T3 is connected to an extraction tower extractant feed inlet at the upper part of the extraction tower T1 through an ethanol product tower kettle extraction pipe PL23, an extractant cooler E5, an extractant circulating pipe PL24 and a total extractant feed pipe PL4 which are sequentially connected, and an ethanol product tower reboiling outlet at the bottom of the ethanol product tower T3 is connected with an ethanol product tower reboiling inlet at the lower part of the ethanol product tower T3 through an ethanol product tower kettle reboiler pipe PL21, an ethanol product tower reboiler E4 and an ethanol product tower kettle gas phase reflux pipe PL22 which are sequentially connected;
The toluene refining tower extraction port at the top of the toluene refining tower T4 is connected to the ethyl acetate refining tower feed port in the middle of the ethyl acetate refining tower T5 through a toluene refining tower top steam pipe PL25, a toluene refining tower condenser E6 and a toluene refining tower top extraction pipe PL27 which are sequentially connected, the toluene refining tower reflux port at the top of the toluene refining tower T4 is connected with the outlet of the toluene refining tower condenser E6, the toluene product extraction port at the bottom of the toluene refining tower T4 is extracted through a toluene refining tower bottom extraction pipe PL30, and the toluene refining tower reboiling outlet at the bottom of the toluene refining tower T4 is connected with a toluene refining tower bottom reboiler pipe PL28, a toluene refining tower reboiler E7 and a toluene refining tower bottom gas phase reflux pipe PL29 which are sequentially connected;
the ethyl acetate refining tower azeotrope recycling extraction outlet at the top of the ethyl acetate refining tower T5 is connected to the mixed solvent feed inlet at the lower part of the extraction tower T1 through an ethyl acetate refining tower top steam pipe PL31, an ethyl acetate refining tower condenser E8, an ethyl acetate refining tower top extraction pipe PL33, an ethyl acetate refining tower separator V2, an ethyl acetate refining tower separator oil phase discharge pipe PL35, an azeotrope recycling total material pipe PL36 and a total mixed solvent feed pipe PL2 which are sequentially connected, the ethyl acetate refining tower reflux inlet at the top of the ethyl acetate refining tower T5 is connected with the outlet of the ethyl acetate refining tower condenser E8, and the ethyl acetate product extraction outlet at the bottom of the ethyl acetate refining tower T5 is extracted through an ethyl acetate refining tower bottom extraction pipe PL 39;
The reboiling outlet of the ethyl acetate refining tower at the bottom of the ethyl acetate refining tower T5 is connected with the reboiling inlet of the ethyl acetate refining tower at the lower part of the ethyl acetate refining tower through a reboiler inlet pipe PL37, an ethyl acetate refining tower reboiler E9 and a gas phase backflow pipe PL38 of the ethyl acetate refining tower kettle which are connected in sequence.
The lower part of the extraction tower T1 is provided with a circulating discharge port, the extraction tower T1 is also provided with at least one circulating feed port positioned on the upper side of the circulating discharge port, and the circulating discharge port and the circulating feed port of the extraction tower T1 are connected with a circulating feed pipe PL8 through a circulating discharge pipe PL 7.
The number of the circulating feed inlets of the extraction tower T1 is two, one circulating feed inlet is positioned at the middle upper part of the extraction tower T1, and the other circulating feed inlet is positioned at the upper part of the extraction tower T1; the circulating discharge port of the extraction tower T1 is connected with one of the circulating feed ports through a circulating discharge pipe PL7 and a circulating feed pipe PL 8; the circulating discharge port and the other circulating feed port of the extraction tower T1 are connected with a circulating feed pipe PL9 through a circulating discharge pipe PL 7. In this embodiment, the circulation discharge port or more circulation discharge ports may not be provided.
The type of column internals of the extraction column T1 is column plates or packing, and the theoretical plate number is 16-25; the ethanol light component removal tower T2 consists of a rectifying section above a raffinate phase feed inlet and a stripping section below the raffinate phase feed inlet, wherein tower plates or fillers are arranged as tower internals, the theoretical plate number of the rectifying section is 12-25, and the theoretical plate number of the stripping section is 18-28; the ethanol product tower T3 consists of a rectifying section above a feed inlet and a stripping section below the feed inlet, wherein tower internals are tower plates or fillers, the theoretical plate number of the rectifying section is 20-35, and the theoretical plate number of the stripping section is 15-26; the toluene refining tower T4 consists of a rectifying section above an extraction phase feed inlet and a stripping section below the extraction phase feed inlet, wherein tower plates or fillers are arranged as tower internals, the theoretical plate number of the rectifying section is 16-26, and the theoretical plate number of the stripping section is 25-36; the ethyl acetate refining tower T5 consists of a rectifying section above a feed inlet and a stripping section below the feed inlet, wherein tower internals are tower plates or fillers, the theoretical plates of the rectifying section are 18-24, and the theoretical plates of the stripping section are 26-35.
A method for separating a mixed solvent containing toluene, ethyl acetate, ethanol and the like comprises the following steps:
Step S1: the mixed solvent to be separated containing toluene, ethyl acetate, ethanol and a small amount of water enters the lower part of an extraction tower T1 from a mixed solvent feed inlet through a total mixed solvent feed pipe PL2, an extracting agent enters the upper part of the extraction tower T1 from a total extracting agent feed pipe PL4, a middle lower circulating discharge port of the extraction tower T1 extracts a flow to circulate to a middle upper feed inlet and an upper feed inlet of the extraction tower T1, and the flow is respectively connected with a middle upper circulating feed pipe PL8 and an upper circulating feed pipe PL9 of the extraction tower through a middle lower circulating discharge pipe PL7 of the extraction tower;
step S2: the raffinate phase at the bottom of the extraction tower T1 enters the ethanol light-removal tower T2 through a raffinate phase discharge pipe PL5 of the extraction tower to carry out rectification, the rising steam at the top of the ethanol light-removal tower T2 realizes phase change through a condenser E1, the materials obtained by condensation are ternary azeotrope containing ethyl acetate, ethanol and water and binary azeotrope of toluene and water, one part of the materials flows back into the tower from a reflux port at the top of the ethanol light-removal tower T2, the other part of materials enters an ethanol light-removal tower layering device V1 from an azeotrope circulating extraction port at the top of the ethanol light-removal tower T2 through an extract pipe PL12 at the top of the ethanol light-removal tower to be layered, a lower water phase is discharged out of the system through an aqueous phase discharge pipe PL13 of the ethanol light-removal tower layering device, and an upper oil phase returns to a feed port at the lower part of the extraction tower T1 through an oil phase discharge pipe PL14 for circulating use;
Step S3: the mixture of ethanol and water separated from the tower kettle of the ethanol light-removal tower T2 enters an ethanol product tower T3 through a extraction pipe PL17 at the tower kettle of the ethanol light-removal tower for rectification, the rising steam at the tower top of the ethanol product tower T3 realizes phase change through a condenser E3, the condensed material is an industrial ethanol product with the concentration of 95 percent, one part of the industrial ethanol product flows back into the tower from a reflux port at the top of the ethanol product tower T3, the other part of the industrial ethanol product flows out of the system from a extraction port at the top of the ethanol light-removal tower T2 through a extraction pipe PL20 at the tower top of the ethanol product tower, and the extractant separated from the tower kettle of the ethanol product tower T3 is cooled by an extractant cooler E3 and then returns to a feed port at the upper part of the extraction tower T1 from an extractant circulation pipe PL24 for recycling;
step S4: the extraction phase at the top of the extraction tower T1 enters a toluene refining tower T4 through an extraction phase discharging pipe PL6 of the extraction tower for rectification, the rising steam at the top of the toluene refining tower T4 realizes phase change through a condenser E6, the condensed material is a mixture of ethyl acetate, a small amount of water and trace toluene, one part of the condensed material flows back into the toluene refining tower T4 from a reflux port at the top of the toluene refining tower T4, the other part of the condensed material enters an ethyl acetate refining tower T5 from a collecting outlet at the top of the toluene refining tower T4 through a collecting outlet PL27 at the top of the toluene refining tower, and a toluene product with purity of more than 99.6% is obtained at the bottom of the toluene refining tower T4 and is discharged from a system through a collecting outlet PL30 at the bottom of the toluene refining tower;
Step S5: the material from the top extraction port of the ethyl acetate refining tower T4 enters the ethyl acetate refining tower T5 for rectification, the phase change of the vapor rising from the top of the ethyl acetate refining tower T5 is realized through a condenser E8, the material obtained by condensation is a mixture of ethyl acetate, water azeotropes and toluene and water azeotropes, one part of the material flows back into the ethyl acetate refining tower T5 from a reflux port at the top of the ethyl acetate refining tower T5, the other part of the material enters an ethyl acetate refining tower separator V2 for layering from an azeotrope circulation extraction port at the top of the ethyl acetate refining tower T5 through an ethyl acetate refining tower top extraction pipe PL33, the lower water phase is discharged from a system through an ethyl acetate refining tower separator water phase discharge pipe PL34, the upper oil phase is returned to a lower feed port of the extraction tower T1 for circulation through an ethyl acetate refining tower separator oil phase discharge pipe PL35, and the ethyl acetate product with purity of more than 99.6% is obtained from the ethyl acetate refining tower T4 kettle through an ethyl acetate refining tower kettle extraction pipe PL 39.
The extractant is water which is the existing component in the mixed solvent.
The operating conditions in the extraction column T1 are set as follows: the pressure at the top of the tower is normal pressure, the operating temperature is normal temperature, the volume ratio of the extractant entering from the total extractant feed pipe to the mixed acid wastewater entering from the total mixed solvent feed pipe is 0.4-1.2, and the volume ratio of the middle-lower part circulating discharge port to the extractant is 1.0-4.0;
The operating conditions in the ethanol light ends column T2 are set as follows: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 66-73 ℃, the temperature at the bottom of the tower is 80-90 ℃, and the reflux ratio at the top of the tower is 1.2-4.5;
the operating conditions within the ethanol product column T3 are set to: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 77-80 ℃, the temperature at the bottom of the tower is 99-101 ℃, and the reflux ratio at the top of the tower is 1.8-8.0;
the operating conditions in the toluene refining column T4 were set as follows: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 73-79 ℃, the temperature at the bottom of the tower is 112-118 ℃, and the reflux ratio at the top of the tower is 1.0-5.0;
the operating conditions in the ethyl acetate refining column T5 were set as follows: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 67-73 ℃, the temperature at the bottom of the tower is 75-79 ℃, and the reflux ratio at the top of the tower is 2.0-7.0.
Specifically, the material of the tower body of the extraction tower T1 is SUS304, the tower is filled with MELLAPAKPL 752Y regular silk screen filler, the tower diameter is 500mm, and the theoretical plate number is 18. The ethanol light component removal tower T2 body is made of SUS304, the tower is filled with MELLAPAKPL 752Y regular silk screen filler, the tower diameter is 400mm, the theoretical plate number is 50, and the 22 nd theoretical plate is fed. The material of the tower body of the ethanol product tower T3 is SUS304, the tower is filled with MELLAPAKPL 752Y regular silk screen filler, the tower diameter is 600mm, the number of theoretical plates is 58, and the 34 th theoretical plate is fed. The toluene refining tower T4 has SUS304 as the tower body material, MELLAPAKPL 752Y regular silk screen stuffing as the tower inside, 500mm diameter, 52 theoretical plates and 24 th theoretical plates as the material. The ethyl acetate refining tower T5 body is made of SUS304, a tower is filled with MELLAPAKPL 752Y regular silk screen filler, the tower diameter is 300mm, the theoretical plate number is 48, and the 20 th theoretical plate is fed.
The feeding flow of the mixed solvent is 1000kg/h, the mixed solvent enters from a feeding port at the lower part of the extraction tower T1, the feeding temperature is 32 ℃, and the feeding composition is as follows: 32% toluene, 35% ethyl acetate, 32.5% ethanol, 0.5% water; the feeding amount of extractant water is 600kg/h, and the extractant water enters from a feeding port at the upper part of the extraction tower T1; extraction column T1 operating conditions: the operation pressure is 101kPa, the temperature of the top of the tower is 36.9 ℃, the temperature of the bottom of the tower is 36.4 ℃, and the flow rate of a middle-lower circulating discharge hole is 1800kg/h; ethanol light ends column T2 operating conditions: the operation pressure is 101kPa, the tower top temperature is 70.1 ℃, the tower bottom temperature is 85.8 ℃, and the tower top reflux ratio is 3; ethanol product column T3 operating conditions: the operation pressure is 101kPa, the tower top temperature is 77.8 ℃, the tower bottom temperature is 99.6 ℃, and the tower top reflux ratio is 5; toluene refining column T4 operating conditions: the operating pressure is 101kPa, the tower top temperature is 75.4 ℃, the tower bottom temperature is 113.4 ℃, and the tower top reflux ratio is 2; ethyl acetate refining column T5 operating conditions: the operating pressure was 101kPa, the overhead temperature was 70.5 ℃, the bottom temperature was 76.8 ℃, and the overhead reflux ratio was 4.
Under the above conditions, ethanol product at the top of ethanol product column T3: purity 95.2%; toluene product of tower kettle of toluene refining tower T4: purity 99.6%, ethanol content 348ppm and moisture 356ppm; ethyl acetate product of ethyl acetate refining tower T5 tower kettle: purity 99.6%, ethanol content 302ppm and moisture 348ppm.
Example 2:
unlike the above examples, the process shown in FIG. 1 was adopted, the material of the column body of the extraction column T1 was SUS304, the column was filled with MELLAPAKPL 752Y structured gauze packing, the column diameter was 500mm, and the number of theoretical plates was 18. The ethanol light component removal tower T2 body is made of SUS304, the tower is filled with MELLAPAKPL 752Y regular silk screen filler, the tower diameter is 400mm, the theoretical plate number is 50, and the 22 nd theoretical plate is fed. The material of the tower body of the ethanol product tower T3 is SUS304, the tower is filled with MELLAPAKPL 752Y regular silk screen filler, the tower diameter is 600mm, the number of theoretical plates is 58, and the 34 th theoretical plate is fed. The toluene refining tower T4 has SUS304 as the tower body material, MELLAPAKPL 752Y regular silk screen stuffing as the tower inside, 500mm diameter, 52 theoretical plates and 24 th theoretical plates as the material. The ethyl acetate refining tower T5 body is made of SUS304, a tower is filled with MELLAPAKPL 752Y regular silk screen filler, the tower diameter is 300mm, the theoretical plate number is 48, and the 20 th theoretical plate is fed.
The feeding flow of the mixed solvent is 1000kg/h, the mixed solvent enters from a feeding port at the lower part of the extraction tower T1, the feeding temperature is 32 ℃, and the feeding composition is as follows: 31% toluene, 36% ethyl acetate, 31% ethanol, 2.0% water; the feeding amount of extractant water is 800kg/h, and the extractant water enters from a feeding port at the upper part of the extraction tower T1; extraction column T1 operating conditions: the operation pressure is 101kPa, the temperature of the top of the tower is 37.2 ℃, the temperature of the bottom of the tower is 37.0 ℃, and the flow rate of a circulating discharge hole at the middle lower part is 2200kg/h; ethanol light ends column T2 operating conditions: the operating pressure is 101kPa, the tower top temperature is 69.1 ℃, the tower bottom temperature is 84.2 ℃, and the tower top reflux ratio is 2.5; ethanol product column T3 operating conditions: the operating pressure is 101kPa, the temperature of the top of the tower is 78.0 ℃, the temperature of the bottom of the tower is 99.4 ℃, and the reflux ratio of the top of the tower is 4.6; toluene refining column T4 operating conditions: the operating pressure is 101kPa, the tower top temperature is 74.1 ℃, the tower bottom temperature is 113.2 ℃, and the tower top reflux ratio is 2.6; ethyl acetate refining column T5 operating conditions: the operating pressure was 101kPa, the overhead temperature was 69.2 ℃, the bottom temperature was 77.1 ℃, and the overhead reflux ratio was 3.8.
Under the above conditions, ethanol product at the top of ethanol product column T3: purity 95.1%; toluene product of tower kettle of toluene refining tower T4: purity 99.7%, ethanol content 315ppm and moisture 338ppm; ethyl acetate product of ethyl acetate refining tower T5 tower kettle: purity 99.7%, ethanol content 282ppm and moisture 315ppm.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. A separation device containing toluene, ethyl acetate and ethanol mixed solvent is characterized in that: the device comprises an extraction tower (T1), an ethanol light-off tower (T2), an ethanol light-off tower condenser (E1), an ethanol light-off tower reboiler (E2), an ethanol light-off tower layered machine (V1), an ethanol product tower (T3), an ethanol product tower condenser (E3), an ethanol product tower reboiler (E4), an extractant cooler (E5), a toluene refining tower (T4), a toluene refining tower condenser (E6), a toluene refining tower reboiler (E7), an ethyl acetate refining tower (T5), an ethyl acetate refining tower condenser (E8), an ethyl acetate refining tower reboiler (E9) and an ethyl acetate refining tower layered machine (V2);
the top of the extraction tower (T1) is provided with an extraction phase discharge port of the extraction tower, the upper part of the extraction phase discharge port is provided with an extraction agent feed port of the extraction tower, the bottom of the extraction tower is provided with an extraction raffinate phase discharge port, and the lower part of the extraction tower is provided with a mixed solvent feed port; the top of the ethanol light component removing tower (T2) is provided with an ethanol light component removing tower azeotrope circulating extraction outlet, the upper part is provided with an ethanol light component removing tower reflux port, the middle part is provided with an ethanol light component removing tower raffinate phase feeding port, the lower part is provided with an ethanol light component removing tower reboiling inlet, and the bottom is provided with an ethanol light component removing tower extraction outlet and an ethanol light component removing tower reboiling outlet; the top of the ethanol product tower (T3) is provided with an ethanol product tower reflux port and an ethanol product outlet, the middle part is provided with an ethanol product tower feed port, the lower part is provided with an ethanol product tower reboiling inlet, and the bottom is provided with an ethanol product tower outlet and an ethanol product tower reboiling outlet; the top of the toluene refining tower (T4) is provided with a toluene refining tower reflux port and a toluene refining tower outlet, the middle part is provided with a toluene refining tower extract phase feed port, the lower part is provided with a toluene refining tower reboiling inlet, and the bottom is provided with a toluene refining tower toluene product outlet and a toluene refining tower reboiling outlet; the top of the ethyl acetate refining tower (T5) is provided with an ethyl acetate refining tower reflux port and an ethyl acetate refining tower azeotrope recycling outlet, the middle part is provided with an ethyl acetate refining tower feed inlet, the lower part is provided with an ethyl acetate refining tower reboiling inlet, and the bottom is provided with an ethyl acetate product outlet and an ethyl acetate refining tower reboiling outlet;
The extraction tower raffinate phase discharge port at the bottom of the extraction tower (T1) is connected with the extraction tower raffinate phase feed port at the middle part of the ethanol light-off tower (T2) through an extraction tower raffinate phase discharge pipe (PL 5), and the extraction tower extract phase discharge port at the top of the extraction tower (T1) is connected with the toluene refining tower extract phase feed port at the middle part of the toluene refining tower (T4) through an extraction tower extract phase discharge pipe (PL 6);
the method comprises the steps that an ethanol light component removing tower azeotrope recycling outlet at the top of an ethanol light component removing tower (T2) is connected to a mixed solvent feed inlet at the lower part of an extraction tower (T1) through an ethanol light component removing tower top steam pipe (PL 10), an ethanol light component removing tower condenser (E1), an ethanol light component removing tower top extraction pipe (PL 12), an ethanol light component removing tower layering device (V1), an ethanol product tower oil phase discharge pipe (PL 14), an azeotrope recycling total feed pipe (PL 36) and a total mixed solvent feed pipe (PL 2) which are sequentially connected, an ethanol light component removing tower reflux inlet at the upper part of the ethanol light component removing tower (T2) is connected with an ethanol light component removing tower outlet at the bottom of the ethanol light component removing tower (T2) through an ethanol light component removing tower top reflux pipe (PL 11), an ethanol product tower feed inlet at the middle part of an ethanol product tower (T3) is connected with an ethanol product tower light component removing tower outlet at the bottom of the ethanol product tower (T2) through an ethanol light component removing tower outlet pipe (PL 17), and an ethanol component removing tower reboiler outlet at the bottom of the lower part of the ethanol component removing tower (T2) is sequentially connected with an ethanol component removing tower bottom reflux tower (PL 16) through an ethanol component removing tower reflux pipe (PL 16);
The ethanol product recovery outlet at the bottom of the ethanol product tower (T3) is connected to an extraction tower extractant feed inlet at the upper part of the extraction tower (T1) through an ethanol product tower kettle recovery pipe (PL 23), an extractant cooler (E5), an extractant circulating pipe (PL 24) and a total extractant feed pipe (PL 4) which are sequentially connected, and an ethanol product tower reboiling outlet at the bottom of the ethanol product tower (T3) is connected to an ethanol product tower kettle inlet reboiler pipe (PL 21), an ethanol product tower reboiler (E4) and an ethanol product tower kettle gas phase boiling reflux pipe (PL 22) which are sequentially connected;
the toluene refining tower extraction port at the top of the toluene refining tower (T4) is connected to the ethyl acetate refining tower feed port at the middle part of the ethyl acetate refining tower (T5) through a toluene refining tower top steam pipe (PL 25), a toluene refining tower condenser (E6) and a toluene refining tower top extraction pipe (PL 27) which are sequentially connected, the toluene refining tower reflux port at the top of the toluene refining tower (T4) is connected with the outlet of the toluene refining tower condenser (E6), the toluene product extraction port at the bottom of the toluene refining tower (T4) is extracted through a toluene refining tower kettle extraction pipe (PL 30), and the toluene refining tower reboiling outlet at the bottom of the toluene refining tower (T4) is connected with a toluene refining tower kettle reboiler inlet pipe (PL 28), a toluene refining tower reboiler (E7) and a toluene refining tower gas phase reflux pipe (PL 29) which are sequentially connected;
The ethyl acetate refining tower azeotrope recycling extraction outlet at the top of the ethyl acetate refining tower (T5) is connected to the mixed solvent feed inlet at the lower part of the extraction tower (T1) through an ethyl acetate refining tower top steam pipe (PL 31), an ethyl acetate refining tower condenser (E8), an ethyl acetate refining tower top extraction pipe (PL 33), an ethyl acetate refining tower layering device (V2), an ethyl acetate refining tower layering device oil phase discharge pipe (PL 35), an azeotrope recycling total material pipe (PL 36) and a total mixed solvent feed pipe (PL 2) which are sequentially connected, the ethyl acetate refining tower reflux inlet at the top of the ethyl acetate refining tower (T5) is connected with the outlet of the ethyl acetate refining tower condenser (E8), and the ethyl acetate product extraction outlet at the bottom of the ethyl acetate refining tower (T5) is extracted through an ethyl acetate refining tower kettle extraction pipe (PL 39);
the reboiling outlet of the ethyl acetate refining tower at the bottom of the ethyl acetate refining tower (T5) is connected with the reboiling inlet of the ethyl acetate refining tower at the lower part of the ethyl acetate refining tower through a reboiler inlet pipe (PL 37), an ethyl acetate refining tower reboiler (E9) and a gas phase backflow pipe (PL 38) of the ethyl acetate refining tower kettle which are connected in sequence.
2. The separation device of the mixed solvent of toluene, ethyl acetate and ethanol according to claim 1, wherein: the lower part of the extraction tower (T1) is provided with a circulating discharge hole, the extraction tower (T1) is also provided with at least one circulating feed hole positioned on the upper side of the circulating discharge hole, and the circulating discharge hole of the extraction tower (T1) is connected with a circulating feed pipe (PL 8) through a circulating discharge pipe (PL 7).
3. The separation device of the mixed solvent of toluene, ethyl acetate and ethanol according to claim 2, wherein: the number of the circulating feed inlets of the extraction tower (T1) is two, one circulating feed inlet is positioned at the middle upper part of the extraction tower (T1), and the other circulating feed inlet is positioned at the upper part of the extraction tower (T1); the circulating discharge port of the extraction tower (T1) is connected with one of the circulating feed ports through a circulating discharge pipe (PL 7) and a circulating feed pipe (PL 8); the circulating discharge port of the extraction tower (T1) is connected with the circulating feed pipe (PL 9) through a circulating discharge pipe (PL 7) between the circulating discharge port and the other circulating feed port.
4. The separation device of the mixed solvent of toluene, ethyl acetate and ethanol according to claim 1, wherein:
The type of column internals of the extraction column (T1) is a column plate or a packing, and the theoretical plate number is 16-25.
5. The separation device of the mixed solvent of toluene, ethyl acetate and ethanol according to claim 1, wherein:
the ethanol light component removing tower (T2) consists of a rectifying section above a raffinate phase feed inlet and a stripping section below the raffinate phase feed inlet, wherein tower plates or fillers are arranged as tower internals, the theoretical plate number of the rectifying section is 12-25, and the theoretical plate number of the stripping section is 18-28.
6. The separation device of the mixed solvent of toluene, ethyl acetate and ethanol according to claim 1, wherein: the ethanol product tower (T3) consists of a rectifying section above a feed inlet and a stripping section below the feed inlet, wherein tower plates or fillers are arranged as tower internals, the theoretical plates of the rectifying section are 20-35, and the theoretical plates of the stripping section are 15-26.
7. The separation device of the mixed solvent of toluene, ethyl acetate and ethanol according to claim 1, wherein: the toluene refining tower (T4) consists of a rectifying section above the feed inlet of the extraction phase and a stripping section below the feed inlet of the extraction phase, wherein the type of tower internals is tower plates or packing, the theoretical plate number of the rectifying section is 16-26, and the theoretical plate number of the stripping section is 25-36.
8. The separation device of the mixed solvent of toluene, ethyl acetate and ethanol according to claim 1, wherein: the ethyl acetate refining tower (T5) consists of a rectifying section above a feed inlet and a stripping section below the feed inlet, wherein tower plates or fillers are arranged as tower internals, the theoretical plates of the rectifying section are 18-24, and the theoretical plates of the stripping section are 26-35.
9. The method for separating a mixed solvent containing toluene, ethyl acetate and ethanol by using the apparatus according to any one of claims 1 to 8, wherein: the method comprises the following steps:
step S1: the mixed solvent containing toluene, ethyl acetate and ethanol enters the lower part of the extraction tower (T1) from a mixed solvent feed inlet through a total mixed solvent feed pipe (PL 2), and the extractant enters the upper part of the extraction tower (T1) from a total extractant feed pipe (PL 4);
step S2: the raffinate phase at the bottom of the extraction tower (T1) enters the ethanol light-removal tower (T2) through a raffinate phase discharge pipe (PL 5) of the extraction tower to carry out rectification, the vapor rising at the top of the ethanol light-removal tower (T2) is subjected to phase change through a condenser (E1), the materials obtained by condensation are ternary azeotrope containing ethyl acetate, ethanol and water and binary azeotrope of toluene and water, one part of the materials returns into the tower from an ethanol light-removal tower reflux port at the top of the ethanol light-removal tower (T2), the other part of the materials returns into the mixed solvent feed port at the lower part of the extraction tower (T1) from an ethanol light-removal tower azeotrope circulating discharge port at the top of the ethanol light-removal tower (T2) through an ethanol light-removal tower top discharge pipe (PL 12), the lower water phase enters an ethanol light-removal tower separator (V1) to be layered, the lower water phase passes through an ethanol light-removal tower separator water phase discharge pipe (PL 13) to discharge the system, and the upper oil phase returns to the mixed solvent feed port at the lower part of the extraction tower (T1) through an ethanol light-removal tower separator oil phase discharge pipe (PL 14) to be recycled;
Step S3: materials at the bottom of a tower kettle of the ethanol light component removal tower (T2) enter the ethanol product tower (T3) for rectification through a tower kettle extraction pipe (PL 17) of the ethanol light component removal tower, steam rising from the tower top of the ethanol product tower (T3) is subjected to phase change through a condenser (E3), one part of the steam flows back into the tower from a reflux port of the ethanol product tower at the top of the ethanol product tower (T3), the other part of the steam flows out of a system from a light component removal tower extraction port at the top of the ethanol product tower (T2) through a tower top extraction pipe (PL 20), and an extractant separated from the tower kettle of the ethanol product tower (T3) is cooled through an extractant cooler (E5) and then returns to an extraction tower feed port at the upper part of the extraction tower (T1) from an extractant circulation pipe (PL 24) for recycling;
step S4: the extraction phase at the top of the extraction tower (T1) flows into an extraction phase discharging pipe (PL 6) of the extraction tower to enter a toluene refining tower (T4) for rectification, the rising steam at the top of the toluene refining tower (T4) is subjected to phase change through a condenser (E6), one part of condensed materials flows back into the toluene refining tower (T4) from a reflux port at the top of the toluene refining tower, the other part of condensed materials enters an ethyl acetate refining tower (T5) from a collecting outlet at the top of the toluene refining tower (T4) through a toluene refining tower top collecting pipe (PL 27), and the product obtained from a toluene refining tower (T4) tower kettle is discharged from a system through a toluene refining tower kettle collecting pipe (PL 30);
Step S5: materials from a top extraction port of the toluene refining tower (T4) enter an ethyl acetate refining tower (T5) for rectification, steam rising from the top of the ethyl acetate refining tower (T5) is subjected to phase change through a condenser (E8), part of the condensed materials flow back into the ethyl acetate refining tower from a reflux port of the ethyl acetate refining tower at the top of the ethyl acetate refining tower (T5), the other part of the condensed materials flow back into the ethyl acetate refining tower from an azeotrope circulating ethyl acetate refining tower extraction port at the top of the ethyl acetate refining tower (T5) and enter an ethyl acetate refining tower layering device (V2) for layering through an ethyl acetate refining tower top extraction pipe (PL 33), a lower water phase is discharged out of the system through an ethyl acetate refining tower layering device water phase discharge pipe (PL 34), an upper oil phase is returned to a lower feed port of the extraction tower (T1) for recycling through an ethyl acetate refining tower layering device oil phase discharge pipe (PL 35), and a product obtained from an ethyl acetate refining tower (T5) kettle is discharged out of the system through an ethyl acetate refining tower kettle extraction pipe (PL 39);
the extractant is water.
10. The method for separating a mixed solvent containing toluene, ethyl acetate and ethanol according to claim 9, wherein: the extractant is water;
the operating conditions in the extraction column (T1) are set as: the pressure at the top of the tower is normal pressure, the operating temperature is normal temperature, the volume ratio of the extractant entering from a total extractant feeding pipe to the mixed acid wastewater entering from a total mixed solvent feeding pipe is 0.4-1.2, and the volume ratio of the discharged material of a middle-lower part circulating discharge hole to the fed material of the extractant entering from the total extractant feeding pipe is 1.0-4.0;
The operating conditions within the ethanol light ends column (T2) are set to: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 66-73 ℃, the temperature at the bottom of the tower is 80-90 ℃, and the reflux ratio at the top of the tower is 1.2-4.5;
the operating conditions within the ethanol product column (T3) are set to: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 77-80 ℃, the temperature at the bottom of the tower is 99-101 ℃, and the reflux ratio at the top of the tower is 1.8-8.0;
the operating conditions in the toluene refining column (T4) are set as follows: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 73-79 ℃, the temperature at the bottom of the tower is 112-118 ℃, and the reflux ratio at the top of the tower is 1.0-5.0;
the operating conditions in the ethyl acetate refining column (T5) are set as follows: the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 67-73 ℃, the temperature at the bottom of the tower is 75-79 ℃, and the reflux ratio at the top of the tower is 2.0-7.0.
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| CN110156556A (en) * | 2019-06-03 | 2019-08-23 | 新中天环保股份有限公司 | A kind of coating solvent slop withdrawal technique |
| CN110483230A (en) * | 2019-09-12 | 2019-11-22 | 新中天环保股份有限公司 | A method of recycling toluene from pharmacy class toluene solvent slop |
| CN110483296A (en) * | 2019-09-12 | 2019-11-22 | 新中天环保股份有限公司 | A kind of recovery method of pharmacy class ethyl acetate solvent slop |
| CN111747817A (en) * | 2020-08-11 | 2020-10-09 | 江西泽嵘化工有限公司 | Method for separating ethyl ester toluene organic waste liquid containing small amount of water |
| CN115304458B (en) * | 2022-07-08 | 2024-02-23 | 陕西延长石油（集团）有限责任公司 | System and process for separating and refining acetaldehyde by ethanol dehydrogenation |
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