CN117339233A - Device and method for separating sec-butyl alcohol from sec-butyl alcohol-water-containing waste liquid - Google Patents
Device and method for separating sec-butyl alcohol from sec-butyl alcohol-water-containing waste liquid Download PDFInfo
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- CN117339233A CN117339233A CN202311646134.6A CN202311646134A CN117339233A CN 117339233 A CN117339233 A CN 117339233A CN 202311646134 A CN202311646134 A CN 202311646134A CN 117339233 A CN117339233 A CN 117339233A
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- butyl alcohol
- tower
- distillation tower
- butanol
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- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 title claims abstract description 285
- 239000002699 waste material Substances 0.000 title claims abstract description 58
- 239000007788 liquid Substances 0.000 title claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 20
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 132
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 74
- 238000010992 reflux Methods 0.000 claims abstract description 71
- 239000000463 material Substances 0.000 claims abstract description 48
- 238000004821 distillation Methods 0.000 claims abstract description 27
- 238000012546 transfer Methods 0.000 claims abstract description 13
- 239000002351 wastewater Substances 0.000 claims abstract description 9
- 238000004064 recycling Methods 0.000 claims abstract description 8
- 238000005191 phase separation Methods 0.000 claims description 29
- DYXGOCQNHOIWHO-UHFFFAOYSA-N butan-2-ol hydrate Chemical compound O.CCC(C)O DYXGOCQNHOIWHO-UHFFFAOYSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 8
- MHYCRLGKOZWVEF-UHFFFAOYSA-N ethyl acetate;hydrate Chemical compound O.CCOC(C)=O MHYCRLGKOZWVEF-UHFFFAOYSA-N 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 5
- 230000014759 maintenance of location Effects 0.000 claims description 5
- 208000028659 discharge Diseases 0.000 claims description 4
- 239000010865 sewage Substances 0.000 claims description 4
- 238000011084 recovery Methods 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 3
- 125000004122 cyclic group Chemical group 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- MOLPUWBMSBJXER-YDGSQGCISA-N bilobalide Chemical compound O([C@H]1OC2=O)C(=O)[C@H](O)[C@@]11[C@@](C(C)(C)C)(O)C[C@H]3[C@@]21CC(=O)O3 MOLPUWBMSBJXER-YDGSQGCISA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229930184727 ginkgolide Natural products 0.000 description 2
- SQOJOAFXDQDRGF-WJHVHIKBSA-N ginkgolide B Natural products O=C1[C@@H](C)[C@@]2(O)[C@@H]([C@H](O)[C@]34[C@@H]5OC(=O)[C@]23O[C@H]2OC(=O)[C@H](O)[C@@]42[C@H](C(C)(C)C)C5)O1 SQOJOAFXDQDRGF-WJHVHIKBSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 235000011201 Ginkgo Nutrition 0.000 description 1
- 241000218628 Ginkgo Species 0.000 description 1
- 235000008100 Ginkgo biloba Nutrition 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- FPUXKXIZEIDQKW-MFJLLLFKSA-N ginkgolide A Natural products O=C1[C@H](C)[C@@]2(O)[C@@H](O1)C[C@]13[C@@H]4OC(=O)[C@]21O[C@@H]1OC(=O)[C@H](O)[C@]31[C@@H](C(C)(C)C)C4 FPUXKXIZEIDQKW-MFJLLLFKSA-N 0.000 description 1
- FPUXKXIZEIDQKW-VKMVSBOZSA-N ginkgolide-a Chemical compound O[C@H]([C@]12[C@H](C(C)(C)C)C[C@H]3OC4=O)C(=O)O[C@H]2O[C@]24[C@@]13C[C@@H]1OC(=O)[C@@H](C)[C@]21O FPUXKXIZEIDQKW-VKMVSBOZSA-N 0.000 description 1
- SQOJOAFXDQDRGF-MMQTXUMRSA-N ginkgolide-b Chemical compound O[C@H]([C@]12[C@H](C(C)(C)C)C[C@H]3OC4=O)C(=O)O[C@H]2O[C@]24[C@@]13[C@@H](O)[C@@H]1OC(=O)[C@@H](C)[C@]21O SQOJOAFXDQDRGF-MMQTXUMRSA-N 0.000 description 1
- 239000004434 industrial solvent Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- B01D3/146—Multiple effect distillation
-
- 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
- B01D3/36—Azeotropic distillation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- 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
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a device and a method for separating sec-butyl alcohol from a sec-butyl alcohol-water-containing waste liquid, wherein the device comprises an azeotropic rectifying tower and a sec-butyl alcohol rectifying tower which are sequentially arranged; the bottom of the azeotropic distillation tower is connected with the middle part of the sec-butyl alcohol distillation tower through a material transfer pump and is used for transferring the treated material into the sec-butyl alcohol distillation tower. An entrainer is added into the azeotropic distillation tower and is used for separating a wastewater part in the waste liquid containing the sec-butyl alcohol; the sec-butyl alcohol rectifying tower is used for separating sec-butyl alcohol from the materials and recovering the entrainer; the entrainer is ethyl acetate; the sec-butyl alcohol separated after the treatment is extracted from the bottom of the sec-butyl alcohol rectifying tower. The invention has the advantages that: ethyl acetate is adopted as an entrainer, so that the azeotrope form of sec-butyl alcohol-water in the waste liquid can be well destroyed, and the waste water is separated in advance; finally obtaining a high-purity sec-butyl alcohol product, wherein the entrainer can be reused in the forms of recovery, reflux and the like; the recycling efficiency of sec-butyl alcohol is high, and the cyclic utilization rate of the entrainer is high.
Description
Technical Field
The invention belongs to the field of extraction and separation, and particularly relates to a device and a method for separating sec-butyl alcohol from a sec-butyl alcohol-water-containing waste liquid.
Background
Sec-butyl alcohol is an important industrial chemical and solvent, has wide application, can be used as an emulsifier, a dehydrating agent and a detergent, and belongs to common organic solvents in the traditional Chinese medicine industry; CN201210121252.0 discloses a method for extracting and separating ginkgolide, wherein the total extraction amount of ginkgolide, ginkgolide A, ginkgolide B and Yinbheng cool C can be more than 95%; the method has realized industrialized batch use.
In the extraction process of bilobalide, water saturated sec-butyl alcohol solvents are required to be used for extracting enzymes in ginkgo for many times, so that a large amount of sec-butyl alcohol-water-containing waste liquid can be generated in the batch production process, sec-butyl alcohol and water in the waste liquid are partially mutually dissolved under normal pressure, an azeotrope can be formed during distillation, and compared with other waste liquids taking a single organic solvent as a main component, the separation efficiency of the waste liquid is lower by adopting a common rectification method, and the waste liquid containing sec-butyl alcohol-water which is not completely treated is always directly discharged or the residue is incinerated after being evaporated, but the treatment mode causes environmental pollution on one hand and increases the treatment cost for enterprises on the other hand; therefore, it is necessary to provide a device and a method which are simple in operation and can efficiently separate and recycle sec-butanol in waste liquid.
Disclosure of Invention
Aiming at the problem that the treatment of the waste liquid of the sec-butyl alcohol is difficult in the traditional Chinese medicine extraction process in the prior art, the invention provides a method and a device for separating the sec-butyl alcohol from the waste liquid containing the sec-butyl alcohol-water.
The technical scheme of the invention is as follows: an apparatus for separating sec-butanol from a sec-butanol-water containing waste liquid, comprising: the azeotropic rectifying tower and the sec-butyl alcohol rectifying tower are sequentially arranged; the bottom of the azeotropic distillation tower is connected with the middle part of the sec-butyl alcohol distillation tower through a material transfer pump and is used for transferring the treated material into the sec-butyl alcohol distillation tower;
the middle part of the azeotropic distillation tower is provided with a first feed inlet and a second feed inlet, wherein the first feed inlet is used for entering waste liquid containing sec-butyl alcohol, and the second feed inlet is used for entering entrainer; the top of the azeotropic distillation tower is connected with a first condenser, a first cooler, a phase-splitting tank and a first reflux tank in sequence through pipelines; the phase separation tank is used for separating the materials entering the phase separation tank, the light phase after phase separation enters the first reflux tank, the materials in the first reflux tank are driven by the first reflux pump and are connected with the upper part of the azeotropic distillation tower, so that the light phase separated by the phase separation tank enters the azeotropic distillation tower body again; the heavy phase is directly subjected to pollution discharge treatment after phase separation; the entrainer is ethyl acetate;
the top of the sec-butyl alcohol rectifying tower is sequentially connected with a second condenser and a second reflux tank through pipelines, and part of materials in the second reflux tank enter from the upper part of the sec-butyl alcohol rectifying tower through a second reflux pump; the second reflux tank is connected with a second cooler, and the entrainer is collected through the second cooler for reuse; the sec-butyl alcohol separated after the treatment is extracted from the bottom of the sec-butyl alcohol rectifying tower.
Further, the second feed port is located above the first feed port.
Further, the lower part of the azeotropic distillation tower is connected with a first reboiler, and partial materials at the bottom of the azeotropic distillation tower enter the first reboiler and are heated and then returned into the azeotropic distillation tower; the lower part of the sec-butyl alcohol rectifying tower is connected with a second reboiler, and partial materials at the bottom of the sec-butyl alcohol rectifying tower enter the second reboiler and are heated and then returned into the sec-butyl alcohol rectifying tower.
Further, the second condenser is also connected with the tail condenser; the tail condenser is used for further condensing the gas which is not condensed in the condenser so as to reduce the content of organic gas in the exhaust gas.
The invention also provides a method for separating the sec-butyl alcohol in the sec-butyl alcohol-water-containing waste liquid, which adopts the device for separating the sec-butyl alcohol in the sec-butyl alcohol-water-containing waste liquid to separate, and specifically comprises the following steps:
s1, adding a waste liquid containing sec-butyl alcohol into an azeotropic distillation tower through a first feed port, adding ethyl acetate into the azeotropic distillation tower through a second feed port, and performing azeotropic treatment in the azeotropic distillation tower;
s2, ethyl acetate-water constant boiling substance steam generated in the azeotropic distillation tower is condensed by a first condenser, and enters a phase separation tank after being cooled, wherein a light phase in the phase separation tank is ethyl acetate, the light phase enters the azeotropic distillation tower through a first reflux tank to be refluxed and reused, and a heavy phase in the phase separation tank is wastewater containing ethyl acetate and can be recycled or directly discharged to a sewage treatment system;
s3, after the treatment of S2, the sec-butyl alcohol and ethyl acetate remained at the bottom of the azeotropic distillation tower are transferred into the sec-butyl alcohol distillation tower through a transfer pump through a third feed port, after the sec-butyl alcohol distillation tower is rectified, the ethyl acetate is gasified and transferred into a second reflux tank through a second condenser, part of high-purity ethyl acetate in the second reflux tank is collected through a second cooler and then recycled, and the other part of material is refluxed into the sec-butyl alcohol distillation tower through a second reflux pump for recycling;
s4, collecting the separated sec-butyl alcohol from the bottom of the sec-butyl alcohol rectifying tower after the S3 treatment.
Further, the pressure of the azeotropic distillation tower is 101 to 150kPa, and the tower top temperature is: the temperature of the tower bottom is between 82 and 99 ℃ and the retention time of the materials in the azeotropic distillation tower is between 30 and 60 minutes at the temperature of between 69 and 72 ℃.
Further, the pressure of the sec-butyl alcohol rectifying tower is 101 to 150kPa, and the tower top temperature is: the temperature of the bottom of the tower is between 75 and 77 ℃, the temperature of the bottom of the tower is between 98 and 99 ℃, and the retention time of the materials in a sec-butyl alcohol rectifying tower is between 30 and 60 minutes.
Further, the feeding temperature of the first feeding port is 10-60 ℃; the feeding temperature of the second feeding hole is 10-60 ℃.
Further, the mass ratio of the ethyl acetate to the waste liquid containing the sec-butyl alcohol in the step S1 is 0.5-1:1.
Further, in the step S2, the reflux ratio of the ethyl acetate-water constant boiling substance to the azeotropic distillation column is 1-7:1, and in the step S3, the reflux ratio of the ethyl acetate to the sec-butyl alcohol distillation column is 1-3:1.
The invention has the advantages that: the ethyl acetate is used as an entrainer of the sec-butyl alcohol waste liquid, so that each component in the waste liquid is easier to form an azeotropic substance, the azeotrope form of sec-butyl alcohol-water in the waste liquid can be well destroyed, and the waste water is separated in advance; separating high-purity sec-butyl alcohol product by rectification, wherein the entrainer can be reused in the forms of recovery, reflux and the like; the recovery efficiency of the sec-butyl alcohol is high, the purity of the separated sec-butyl alcohol is high, and the cyclic utilization rate of the entrainer is high. Solves the problem of waste liquid treatment commonly existing in the production of the pharmaceutical industry, on one hand, avoids the environmental pollution caused by direct discharge, on the other hand, separates the sec-butyl alcohol for reuse, reduces the production cost of enterprises, saves the energy consumption and improves the weight of products. The treatment process is a continuous and stable process, is convenient for realizing automatic control, can be suitable for a separation process with a large scale, and can obviously improve economic benefit.
Drawings
FIG. 1 is a schematic diagram of an apparatus for separating sec-butanol from a sec-butanol-water containing waste stream.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The device for separating sec-butyl alcohol from the sec-butyl alcohol-water-containing waste liquid provided by the invention comprises: the device comprises a first reboiler 1, an azeotropic distillation column 2, a first condenser 3, a first cooler 5, a phase separation tank 4, a first reflux tank 6, a first reflux pump 7, a transfer pump 8, a second reboiler 9, a sec-butyl alcohol distillation column 10, a second condenser 11, a tail condenser 12, a second reflux tank 13, a second reflux pump 14 and a second cooler 15.
The first reboiler 1, the azeotropic rectifying tower 2, the first condenser 3, the first cooler 5, the phase separation tank 4, the first reflux tank 6 and the first reflux pump 7 are used as relatively independent azeotropic systems and are mainly used for separating a wastewater part in the sec-butyl alcohol-containing waste liquid; the second reboiler 9, the sec-butyl alcohol rectifying tower 10, the second condenser 11, the tail condenser 12, the second reflux tank 13, the second reflux pump 14 and the second cooler 15 are used as a sec-butyl alcohol rectifying system and are mainly used for separating sec-butyl alcohol from materials and recovering entrainers. The material treated by the azeotropic system is transferred to a sec-butyl alcohol rectifying system through a transfer pump 8.
As shown in fig. 1, the top of the azeotropic distillation tower 2 is communicated with a first condenser 3 through a pipeline, the first condenser 3 is communicated with a first cooler 5, the first cooler 5 is used for further cooling the liquid in the first condenser 3, and the first cooler 5 is communicated with a phase separation tank 4; the materials entering the phase separation tank 4 are separated; the light phase after phase separation enters a first reflux tank 6, and materials in the first reflux tank 6 are driven by a first reflux pump 7 and are connected with the upper part of the azeotropic distillation tower 2, so that the light phase separated by the phase separation tank 4 enters the azeotropic distillation tower main body 2 again; and the heavy phase is directly subjected to pollution discharge treatment after phase separation.
The middle part of the azeotropic distillation tower 2 is provided with a first feed inlet 201 and a second feed inlet 202, wherein the first feed inlet is used for entering waste liquid containing sec-butyl alcohol, the second feed inlet 202 is used for entering entrainer, and the second feed inlet 202 is positioned above the first feed inlet 201. The lower part of the azeotropic distillation tower 2 is connected with a first reboiler 1, and partial materials at the bottom of the azeotropic distillation tower 2 enter the first reboiler 1 and return to the azeotropic distillation tower 2 after being heated; the bottom of the azeotropic distillation tower 2 is connected with the middle part of the sec-butyl alcohol distillation tower 10 through a transfer pump 8 and is used for transferring the treated material into the sec-butyl alcohol distillation tower 10.
The lower part of the sec-butyl alcohol rectifying tower 10 is connected with a second reboiler 9, and partial materials at the bottom of the sec-butyl alcohol rectifying tower 10 enter the second reboiler 9 and are heated and then returned into the sec-butyl alcohol rectifying tower 10; the middle part of the sec-butyl alcohol rectifying tower 10 is provided with a third feed inlet 1001, and a transfer pump 8 transfers the bottom material of the azeotropic rectifying tower 2 to the third feed inlet 1001 to enter the sec-butyl alcohol rectifying tower 10. The top of the sec-butyl alcohol rectifying tower 10 is communicated with a second condenser 11 through a pipeline; the second condenser 11 is connected with a second reflux tank 13, and part of materials in the second reflux tank 13 enter from the upper part of the sec-butyl alcohol rectifying tower 10 through a second reflux pump 14.
The second reflux tank 13 is connected with a second cooler 15, and the entrainer is collected by the second cooler 15 for reuse; the sec-butanol separated after the treatment is extracted from the bottom of the sec-butanol rectifying column 10. The second condenser 11 is also connected with a tail condenser 12; the tail condenser 12 is used for further condensing the gas which is not condensed in the condenser 11 so as to reduce the content of organic gas in the exhaust gas and reduce the COD value in the exhaust gas.
According to the invention, the entrainer is ethyl acetate, and the ethyl acetate is continuously added into the middle upper part of the azeotropic distillation tower 2, so that the ethyl acetate is easier to add and forms an azeotropic substance with the water phase part in the waste liquid, the azeotrope form of sec-butyl alcohol-water in the waste liquid can be well destroyed, the water phase part in the waste liquid can be driven to evaporate according to the corresponding proportion in the form of the azeotropic substance, and the waste water is separated in advance; and then separating the high-purity sec-butyl alcohol product through rectification, wherein the entrainer can be reused in the forms of recovery, reflux and the like.
The pressure of the azeotropic distillation tower 2 is 101-150 kPa, and the tower top temperature is: 69-72 ℃, and the bottom temperature is 82-99 ℃; the pressure of the sec-butyl alcohol rectifying tower 10 is 101-150 kPa, and the tower top temperature is: 75-77 deg.c and tower bottom temperature of 98-99 deg.c.
The feeding temperature at the first feeding port 201 is 10-60 ℃; the feeding temperature at the second feeding port 202 is 10-60 ℃.
The method for separating the sec-butyl alcohol from the sec-butyl alcohol-water-containing waste liquid comprises the following steps of:
s1, continuously feeding waste liquid taking sec-butyl alcohol-water as a main component into an azeotropic distillation tower 2 through a first feed inlet 201, continuously feeding ethyl acetate into the azeotropic distillation tower 2 through a second feed inlet 202, and performing azeotropic treatment in the azeotropic distillation tower 2;
s2, ethyl acetate-water constant boiling substance steam generated in the azeotropic distillation tower 2 is condensed by the first condenser 3, and enters the phase separation tank 4 after being cooled, wherein the light phase in the phase separation tank 4 is ethyl acetate, the light phase enters the azeotropic distillation tower 2 through the first reflux tank 6 for reflux and reutilization, and the heavy phase in the phase separation tank 4 is wastewater containing ethyl acetate and can be recycled or directly discharged to a sewage treatment system;
s3, after the treatment of S2, sec-butyl alcohol and ethyl acetate remained at the bottom of the azeotropic distillation tower 2 are transferred into the sec-butyl alcohol distillation tower 10 through a transfer pump 8 through a third feed port 1001, after rectification in the sec-butyl alcohol distillation tower 10, the ethyl acetate is gasified and transferred into a second reflux tank 13 through a second condenser 11, part of high-purity ethyl acetate in the second reflux tank 13 is collected through a second cooler 15 and then recycled, and the other part of material is refluxed into the sec-butyl alcohol distillation tower 10 through a second reflux pump 14 for recycling.
S4, collecting the separated sec-butyl alcohol from the bottom of the sec-butyl alcohol rectifying tower 10 after the S3 treatment.
Wherein the mass ratio of the ethyl acetate to the waste liquid containing sec-butyl alcohol-water in the step S1 is 0.5-1:1; the retention time of the material in the azeotropic distillation tower 2 is 30-60min; in the step S2, the reflux ratio of the ethyl acetate-water azeotropic mixture to the azeotropic distillation tower 2 is 1-7:1; in the step S3, the reflux ratio of ethyl acetate to the secondary butanol rectifying tower is 1-3:1; the material stays in the sec-butyl alcohol rectifying tower 10 for 30-60min.
The technical effects of the present invention are further illustrated by the following specific examples.
The diameters of the azeotropic distillation tower 2 and the sec-butyl alcohol distillation tower 10 adopted in the embodiment are 40mm, theta-ring packing is filled in the azeotropic distillation tower, the heights of the packing are 1.5m respectively, wherein the position 0.5m away from the top of the azeotropic distillation tower is provided with a second feed inlet 202, and the position 0.5m away from the bottom of the azeotropic distillation tower is provided with a first feed inlet 201; the waste liquid to be treated is derived from Chengdu scientific and technological pharmaceutical Co.
Example 1
The mass fraction of the sec-butyl alcohol in the waste liquid containing sec-butyl alcohol-water to be treated is about 80%; the weight of the waste liquid is 50kg, and the specific treatment steps are as follows:
s1, enabling the waste liquid containing sec-butyl alcohol-water to enter an azeotropic distillation tower 2 from a first feed inlet 201 at a flow rate of 1kg/h, and adding an ethyl acetate entrainer into the azeotropic distillation tower through a second feed inlet 202, wherein the flow rate of the entrainer is 3-5kg/h;
s2, material steam (ethyl acetate-water constant boiling substance) sequentially passes through a first condenser 3 and a first cooler 5 to be condensed and cooled at the top of the azeotropic distillation tower 2, and then enters a phase separation tank 4; after separation in the phase separation tank 4, the light phase enters a first reflux tank 6, and then is pumped into the azeotropic distillation tower 2 for reflux through a first reflux pump 7, the heavy phase in the phase separation tank 4 is water phase, and is directly discharged into a sewage treatment system;
the temperature of the top of the azeotropic rectifying tower 2 is 69-72 ℃, and the temperature of the bottom of the tower kettle 2 is 82-99 ℃; the material remained in the azeotropic distillation tower 2 for 40min.
S3, pumping a material at the bottom of the azeotropic distillation tower 2 into the middle part of the sec-butyl alcohol distillation tower 10 from a third feed inlet 1001 through a transfer pump 8, condensing a gas phase material (mainly ethyl acetate) generated at the top of the sec-butyl alcohol distillation tower 10 through a second condenser 11, and then entering a second reflux tank 13, pumping part of the material in the second reflux tank 13 into the sec-butyl alcohol distillation tower 10 through a second reflux pump 14 for reflux, extracting the other part of high-purity ethyl acetate entrainer from the bottom of the second reflux tank 13, and recycling, wherein the purity of the extracted ethyl acetate reaches 99.9%; the recycling rate of the ethyl acetate in the whole system is 95%.
The reflux ratio in the sec-butyl alcohol rectifying tower 10 is controlled to be 3:1, and the tower top temperature is as follows: the temperature of the bottom of the tower is between 75 and 77 ℃, the temperature of the bottom of the tower is between 98 and 99 ℃, and the material stays in the sec-butyl alcohol rectifying tower 10 for 30 minutes.
S4, qualified sec-butyl alcohol is extracted from the tower kettle of the sec-butyl alcohol rectifying tower 10, the purity of the sec-butyl alcohol reaches 99.9%, and the recovery rate of the sec-butyl alcohol is 97%.
Example 2
100t of waste liquid containing sec-butyl alcohol-water to be treated, wherein the mass fraction of sec-butyl alcohol is about 68%; the specific processing steps are as follows:
s1, enabling the waste liquid containing sec-butyl alcohol-water to enter an azeotropic distillation tower 2 from a first feed inlet 201 at a flow rate of 1t/h, and adding an ethyl acetate entrainer into the azeotropic distillation tower through a second feed inlet 202, wherein the flow rate of the entrainer is 5-6t/h;
the temperature of the top of the azeotropic rectifying tower 2 is 69-72 ℃, the temperature of the bottom of the tower kettle 2 is 82-99 ℃, and the material stays in the azeotropic rectifying tower 2 for 60min.
S3, pumping a material at the bottom of the azeotropic distillation tower 2 into the middle part of the sec-butyl alcohol distillation tower 10 from a third feed inlet 1001 through a transfer pump 8, condensing a gas phase material (mainly ethyl acetate) generated at the top of the sec-butyl alcohol distillation tower 10 through a second condenser 11, and then entering a second reflux tank 13, pumping part of the material in the second reflux tank 13 into the sec-butyl alcohol distillation tower 10 through a second reflux pump 14 for reflux, extracting the other part of high-purity ethyl acetate entrainer from the bottom of the second reflux tank 13, and recycling, wherein the purity of the extracted ethyl acetate reaches 99.9%; the recycling rate of the ethyl acetate in the whole system is 95%.
The reflux ratio in the sec-butyl alcohol rectifying tower 10 is controlled to be 3:1, and the tower top temperature is as follows: the temperature of the bottom of the tower is between 75 and 77 ℃, the temperature of the bottom of the tower is between 98 and 99 ℃, and the material stays in the sec-butyl alcohol rectifying tower 10 for 40 minutes.
S4, qualified sec-butyl alcohol is extracted from the tower kettle of the sec-butyl alcohol rectifying tower 10, the purity of the sec-butyl alcohol reaches 99.9%, and the recovery rate of the sec-butyl alcohol is 98%.
Comparative example
The common rectification means are adopted to classify sec-butyl alcohol and wastewater, and only an azeotropic rectification tower is used.
The mass fraction of the sec-butyl alcohol in the waste liquid containing sec-butyl alcohol-water to be treated is about 80%; the weight of the waste liquid is 50kg, and the specific treatment steps are as follows:
s1, enabling the waste liquid containing sec-butyl alcohol-water to enter an azeotropic distillation column 2 from a first feed inlet 201 at a flow rate of 1kg/h, wherein an ethyl acetate entrainer is not added;
s2, at the top of the azeotropic distillation tower 2, material steam (sec-butyl alcohol-water azeotrope) sequentially passes through the first condenser 3 and the first cooler 5 to be condensed and cooled, then enters the first reflux tank 6, is pumped into the azeotropic distillation tower 2 through the first reflux pump 7 to be partially refluxed, and after the material stays in the azeotropic distillation tower 2 for 60min, sec-butyl alcohol is extracted from the tower kettle.
The temperature of the top of the azeotropic distillation tower 2 is 88.5 ℃, and the temperature of the bottom of the tower kettle 2 is 99 ℃.
The reflux ratio in the azeotropic distillation tower 2 is controlled at 5:1.
The purity of the extracted sec-butyl alcohol is 68 percent (the sec-butyl alcohol and water form an azeotrope under the normal temperature condition, the azeotropic composition is that the sec-butyl alcohol content is 68 percent and the water content is 32 percent), and the purity of the sec-butyl alcohol extracted from the tower kettle is 99 percent; the recovery rate of sec-butyl alcohol is 38%.
The mode of adding the ethyl acetate entrainer can be adopted to well destroy the azeotrope form of sec-butyl alcohol-water in the waste liquid, and the recovery efficiency of sec-butyl alcohol is obviously improved.
The foregoing description is only illustrative of the preferred embodiment of the present invention, and is not to be construed as limiting the invention, but is to be construed as limiting the invention to any and all simple modifications, equivalent variations and adaptations of the embodiments described above, which are within the scope of the invention, may be made by those skilled in the art without departing from the scope of the invention.
Claims (10)
1. The device for separating the sec-butyl alcohol from the sec-butyl alcohol-water-containing waste liquid is characterized by comprising an azeotropic rectifying tower and a sec-butyl alcohol rectifying tower which are sequentially arranged; the bottom of the azeotropic distillation tower is connected with the middle part of the sec-butyl alcohol distillation tower through a material transfer pump and is used for transferring the treated material into the sec-butyl alcohol distillation tower;
the middle part of the azeotropic distillation tower is provided with a first feed inlet and a second feed inlet, wherein the first feed inlet is used for entering waste liquid containing sec-butyl alcohol, and the second feed inlet is used for entering entrainer; the top of the azeotropic distillation tower is connected with a first condenser, a first cooler, a phase-splitting tank and a first reflux tank in sequence through pipelines; the phase separation tank is used for separating the materials entering the phase separation tank, the light phase after phase separation enters the first reflux tank, the materials in the first reflux tank are driven by the first reflux pump and are connected with the upper part of the azeotropic distillation tower, so that the light phase separated by the phase separation tank enters the azeotropic distillation tower body again; the heavy phase is directly subjected to pollution discharge treatment after phase separation; the entrainer is ethyl acetate;
the top of the sec-butyl alcohol rectifying tower is sequentially connected with a second condenser and a second reflux tank through pipelines, and part of materials in the second reflux tank enter from the upper part of the sec-butyl alcohol rectifying tower through a second reflux pump; the second reflux tank is connected with a second cooler, and the entrainer is collected through the second cooler for reuse; the sec-butyl alcohol separated after the treatment is extracted from the bottom of the sec-butyl alcohol rectifying tower.
2. The apparatus for separating sec-butanol from a sec-butanol-water containing waste stream according to claim 1 wherein the second feed port is located above the first feed port.
3. The apparatus for separating sec-butanol from sec-butanol-water containing waste liquid according to claim 1 or 2, wherein: the lower part of the azeotropic distillation tower is connected with a first reboiler, and part of the material at the bottom of the azeotropic distillation tower enters the first reboiler and returns to the azeotropic distillation tower after being heated; the lower part of the sec-butyl alcohol rectifying tower is connected with a second reboiler, and partial materials at the bottom of the sec-butyl alcohol rectifying tower enter the second reboiler and are heated and then returned into the sec-butyl alcohol rectifying tower.
4. The apparatus for separating sec-butanol from sec-butanol-water containing waste liquid according to claim 1 or 2, wherein: the second condenser is also connected with the tail condenser; the tail condenser is used for further condensing the gas which is not condensed in the condenser so as to reduce the content of organic gas in the exhaust gas.
5. A method for separating sec-butanol from a sec-butanol-water containing waste liquid by using the apparatus for separating sec-butanol from a sec-butanol-water containing waste liquid according to claims 1 to 3, comprising the steps of:
s1, adding a waste liquid containing sec-butyl alcohol into an azeotropic distillation tower through a first feed port, adding ethyl acetate into the azeotropic distillation tower through a second feed port, and performing azeotropic treatment in the azeotropic distillation tower;
s2, ethyl acetate-water constant boiling substance steam generated in the azeotropic distillation tower is condensed by a first condenser, and enters a phase separation tank after being cooled, wherein a light phase in the phase separation tank is ethyl acetate, the light phase enters the azeotropic distillation tower through a first reflux tank to be refluxed and reused, and a heavy phase in the phase separation tank is wastewater containing ethyl acetate and can be recycled or directly discharged to a sewage treatment system;
s3, after the treatment of S2, the sec-butyl alcohol and ethyl acetate remained at the bottom of the azeotropic distillation tower are transferred into the sec-butyl alcohol distillation tower through a transfer pump through a third feed port, after the sec-butyl alcohol distillation tower is rectified, the ethyl acetate is gasified and transferred into a second reflux tank through a second condenser, part of high-purity ethyl acetate in the second reflux tank is collected through a second cooler and then recycled, and the other part of material is refluxed into the sec-butyl alcohol distillation tower through a second reflux pump for recycling;
s4, collecting the separated sec-butyl alcohol from the bottom of the sec-butyl alcohol rectifying tower after the S3 treatment.
6. The method for separating sec-butanol from a sec-butanol-water containing waste liquid according to claim 5, wherein: the pressure of the azeotropic distillation tower is 101-150 kPa, and the temperature of the tower top is: the temperature of the tower bottom is between 82 and 99 ℃ and the retention time of the materials in the azeotropic distillation tower is between 30 and 60 minutes at the temperature of between 69 and 72 ℃.
7. The method for separating sec-butanol from a sec-butanol-water containing waste liquid according to claim 5, wherein: the pressure of the sec-butyl alcohol rectifying tower is 101-150 kPa, and the tower top temperature is: the temperature of the bottom of the tower is between 75 and 77 ℃, the temperature of the bottom of the tower is between 98 and 99 ℃, and the retention time of the materials in a sec-butyl alcohol rectifying tower is between 30 and 60 minutes.
8. The method for separating sec-butanol from a sec-butanol-water containing waste liquid according to claim 5, wherein: the feeding temperature of the first feeding hole is 10-60 ℃; the feeding temperature of the second feeding hole is 10-60 ℃.
9. The method for separating sec-butanol from sec-butanol-water containing waste liquid according to claim 5, wherein the mass ratio of ethyl acetate to sec-butanol-containing waste liquid in step S1 is 0.5 to 1:1.
10. The method for separating sec-butanol from a sec-butanol-water containing waste liquid according to claim 5, wherein in step S2, the reflux ratio of the ethyl acetate-water azeotrope to the azeotropic distillation column is 1 to 7:1; in the step S3, the reflux ratio of ethyl acetate to the secondary butanol rectifying tower is 1-3:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311646134.6A CN117339233A (en) | 2023-12-04 | 2023-12-04 | Device and method for separating sec-butyl alcohol from sec-butyl alcohol-water-containing waste liquid |
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| CN202311646134.6A CN117339233A (en) | 2023-12-04 | 2023-12-04 | Device and method for separating sec-butyl alcohol from sec-butyl alcohol-water-containing waste liquid |
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|---|---|---|---|---|
| FR855762A (en) * | 1938-06-06 | 1940-05-20 | Bataafsche Petroleum | Purification process for organic compounds |
| SU1087146A1 (en) * | 1982-05-20 | 1984-04-23 | Государственный научно-исследовательский институт химии и технологии элементоорганических соединений | Method of separating azeotropic mixture |
| CN1561323A (en) * | 2001-07-30 | 2005-01-05 | 英国石油化学品有限公司 | Process for separating sec-butanol from ethyl acetate |
| CN102060660A (en) * | 2010-12-13 | 2011-05-18 | 上海兖矿能源科技研发有限公司 | Method for separating alcohol compound from Tropsch synthesis reaction water |
| CN110862301A (en) * | 2019-12-05 | 2020-03-06 | 湖南中创化工股份有限公司 | Sec-butyl alcohol refining method and device |
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2023
- 2023-12-04 CN CN202311646134.6A patent/CN117339233A/en not_active Withdrawn
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| FR855762A (en) * | 1938-06-06 | 1940-05-20 | Bataafsche Petroleum | Purification process for organic compounds |
| SU1087146A1 (en) * | 1982-05-20 | 1984-04-23 | Государственный научно-исследовательский институт химии и технологии элементоорганических соединений | Method of separating azeotropic mixture |
| CN1561323A (en) * | 2001-07-30 | 2005-01-05 | 英国石油化学品有限公司 | Process for separating sec-butanol from ethyl acetate |
| CN102060660A (en) * | 2010-12-13 | 2011-05-18 | 上海兖矿能源科技研发有限公司 | Method for separating alcohol compound from Tropsch synthesis reaction water |
| CN110862301A (en) * | 2019-12-05 | 2020-03-06 | 湖南中创化工股份有限公司 | Sec-butyl alcohol refining method and device |
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