CN109111337A - A kind of separation equipment and method containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol - Google Patents
A kind of separation equipment and method containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol Download PDFInfo
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- CN109111337A CN109111337A CN201811286607.5A CN201811286607A CN109111337A CN 109111337 A CN109111337 A CN 109111337A CN 201811286607 A CN201811286607 A CN 201811286607A CN 109111337 A CN109111337 A CN 109111337A
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- tower
- column
- extraction
- ethyl acetate
- toluene
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 649
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 title claims abstract description 615
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 536
- 235000019441 ethanol Nutrition 0.000 title claims abstract description 323
- 239000012046 mixed solvent Substances 0.000 title claims abstract description 61
- 238000000926 separation method Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 260
- 238000000746 purification Methods 0.000 claims abstract description 17
- 238000004064 recycling Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims description 58
- 239000000203 mixture Substances 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 36
- 230000008676 import Effects 0.000 claims description 26
- 239000000945 filler Substances 0.000 claims description 15
- 230000009466 transformation Effects 0.000 claims description 12
- 108700002808 N-Me-Phe(3)- morphiceptin Proteins 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- 101000954570 Mus musculus V-type proton ATPase 16 kDa proteolipid subunit c Proteins 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 114
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 12
- 238000012856 packing Methods 0.000 description 9
- 150000002148 esters Chemical class 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 125000004494 ethyl ester group Chemical group 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 1
- 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
- 229930003451 Vitamin B1 Natural products 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000008901 benefit 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
- 238000005516 engineering process Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- -1 extraction tower Chemical compound 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 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
- 239000013589 supplement Substances 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to solvent recovery fields, and in particular to a kind of separation equipment and method containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol.The present invention includes extraction tower, ethyl alcohol lightness-removing column, ethyl alcohol condenser of light component removal column, ethyl alcohol lightness-removing column reboiler, ethyl alcohol lightness-removing column quantizer, alcohol product tower, alcohol product tower condenser, alcohol product tower reboiler, extractant cooler, toluene treating column, toluene treating column condenser, toluene purification tower reboiler, ethyl acetate treating column, ethyl acetate treating column condenser, ethyl acetate purification tower reboiler, ethyl acetate treating column quantizer.Separation containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol is able to achieve using the equipment, and low energy consumption, recycling purity is high；This method does not additionally introduce other impurities, can be effectively reduced energy consumption and equipment investment.
Description
Technical field
The invention belongs to solvent recovery fields, and in particular to a kind of containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol
Separation equipment and method.
Background technique
α-acetyl group-gamma-butyrolacton, abbreviation ABL, molecular formula: C6H8O3, molecular weight: 128.13, No. CAS: 517-23-7,
It is a kind of colourless transparent liquid with esters smell, is mainly used for synthesizing the processes such as vitamin B1 and pesticide.Current production α-
It is catalyst that acetyl group-gamma-butyrolacton main route, which is using gamma-butyrolacton and ethyl acetate as raw material, sodium, toluene is molten
Agent, the production technology while by-product ethyl alcohol, while there is also a small amount of moisture in raw material, in subsequent product distilation process
In, need first solvent be distilled, the mixed solvent component steamed are as follows: 30~34% toluene, 32~38% ethyl acetate, 30~
33.5% ethyl alcohol, 0.5~2.0% water.Need to separate to above-mentioned mixed solvent, make solvent toluene: purity is greater than 99.6%, second
Alcohol content is less than 400ppm and moisture is less than 400ppm, raw acetic acid ethyl ester: purity is greater than 99.6%, ethanol content and is less than
400ppm and moisture content are less than 400ppm, are required with reaching to be recycled, and ethyl alcohol reaches industrial alcohol standard and carries out outer sells.
Carrying out separating-purifying for the mixed solvent of above-mentioned generation is a very difficult problem, this is because the system
There is multiple groups binary azeotropic and ternary azeotropic under normal pressure, ethanol content is 95.6% in the binary azeotropic composition of ethyl alcohol and water,
Azeotropic temperature is 78.2 DEG C；Ethanol content is 68% in the binary azeotropic of ethyl alcohol and toluene composition, and azeotropic temperature is 76.7 DEG C；Second
Ethanol content is 31% in the binary azeotropic of alcohol and ethyl acetate composition, and azeotropic temperature is 71.8 DEG C；The two of ethyl acetate and water
Ethanol content is 91.5% in first azeotropic composition, and azeotropic temperature is 70.4 DEG C；Toluene contains in the binary azeotropic of toluene and water composition
Amount is 86.5%, and azeotropic temperature is 84.1 DEG C；Ethyl acetate, second alcohol and water ternary azeotropic composition in ethyl acetate content be
78.3%, ethanol content 13.1%, azeotropic temperature are 70.2 DEG C, therefore are directly difficult to realize mixed solvent by conventional distillation
Separation.
Patent CN102992930B discloses a kind of recycling of toluene solvant in α-acetyl group-gamma-butyrolacton production process
Technique and its separation equipment, this method use extraction rectification technique, using letones be extractant process twice extracting rectifying from
Toluene is isolated containing in the mixed solvents such as toluene, ethyl acetate and ethyl alcohol, is further extractant by acetic acid second using alcohols material
The mixture of ester and ethyl alcohol is separated.Although the process employs two kinds the method achieve the separation of mixed solvent
Extractant introduces two kinds of additional other components during the separation process, cause separation after three products (be respectively toluene,
Ethyl acetate and ethyl alcohol) unavoidably introduce other impurities, and then the quality of ABL is influenced, in addition five in the separation method
Separation equipment is rectifying column, and energy consumption is higher.
Summary of the invention
In view of this, the purpose of the present invention is to propose to a kind of separation containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol
Device and method are able to achieve the separation containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol using the equipment, and low energy consumption, return
Receive purity is high；This method does not additionally introduce other impurities, can be effectively reduced energy consumption and equipment investment.
Separation equipment scheme of the invention is as follows:
A kind of separation equipment containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol, including extraction tower, ethyl alcohol lightness-removing column,
Ethyl alcohol condenser of light component removal column, ethyl alcohol lightness-removing column reboiler, ethyl alcohol lightness-removing column quantizer, alcohol product tower, the condensation of alcohol product tower
Device, alcohol product tower reboiler, extractant cooler, toluene treating column, toluene treating column condenser, toluene treating column boil again
Device, ethyl acetate treating column, ethyl acetate treating column condenser, ethyl acetate purification tower reboiler, ethyl acetate treating column point
Layer device；
The tower top of the extraction tower is equipped with extraction tower extraction phase discharge port, and top is equipped with extraction tower extractant feed mouth, tower
Bottom is equipped with extraction tower raffinate phase discharge port, and lower part is equipped with mixed solvent feed inlet；Ethyl alcohol is equipped at the top of the ethyl alcohol lightness-removing column
Lightness-removing column azeotropic mixture circulation extraction mouth, top are equipped with ethyl alcohol lightness-removing column refluxing opening, and middle part is fed equipped with ethyl alcohol lightness-removing column raffinate phase
Mouthful, lower part is equipped with ethyl alcohol lightness-removing column and boils import again, and bottom is equipped with ethyl alcohol lightness-removing column extraction mouth and ethyl alcohol lightness-removing column boils outlet again；Institute
The alcohol product top of tower stated is equipped with alcohol product tower refluxing opening and alcohol product produces mouth, and middle part is fed equipped with alcohol product tower
Mouthful, lower part is equipped with alcohol product tower and boils import again, and bottom is equipped with alcohol product tower extraction mouth and alcohol product tower boils outlet again；Institute
Toluene treating column refluxing opening and toluene treating column extraction mouth are equipped at the top of the toluene treating column stated, middle part extracts equipped with toluene treating column
Phase feed inlet is taken, lower part is equipped with toluene treating column and boils import again, and bottom is equipped with toluene treating column toluene product extraction mouth and toluene
Treating column boils outlet again；It is equipped with ethyl acetate treating column refluxing opening at the top of the ethyl acetate treating column and ethyl acetate refines
Tower azeotropic mixture circulation extraction mouth, middle part be equipped with ethyl acetate treating column feed inlet, lower part be equipped with ethyl acetate treating column boil again into
Mouthful, bottom is equipped with ethyl acetate product extraction mouth and ethyl acetate treating column boils outlet again；
It is equipped with toluene treating column refluxing opening at the top of the toluene treating column and toluene treating column produces mouth, the toluene
Be equipped with toluene treating column extraction phase feed inlet in the middle part for the treatment of column, the toluene treating column lower part be equipped with toluene treating column boil again into
Mouthful, the toluene purification tower bottom is equipped with toluene treating column toluene product extraction mouth and toluene treating column boils outlet again；It is described
Ethyl acetate treating column at the top of be equipped with ethyl acetate treating column refluxing opening and ethyl acetate treating column azeotropic mixture circulation extraction mouth,
It is equipped with ethyl acetate treating column feed inlet in the middle part of the ethyl acetate treating column, the ethyl acetate treating column lower part is equipped with
Ethyl acetate treating column boils import again, and the ethyl acetate purification tower bottom is equipped with ethyl acetate product extraction mouth and acetic acid second
Ester treating column boils outlet again；
Extraction tower in the middle part of the extraction tower raffinate phase discharge port of the extraction tower tower bottom and the ethyl alcohol lightness-removing column extracts
Remaining phase feed inlet by extraction tower raffinate phase discharge nozzle connect, it is described extraction column overhead extraction tower extraction phase discharge port with it is described
Toluene treating column extraction phase feed inlet in the middle part of toluene treating column is connected by extraction tower extraction phase discharge nozzle；
Ethyl alcohol lightness-removing column azeotropic mixture circulation extraction mouth at the top of the ethyl alcohol lightness-removing column is de- by sequentially connected ethyl alcohol
Light column overhead steam pipe, ethyl alcohol condenser of light component removal column, ethyl alcohol lightness-removing column overhead extraction pipe, ethyl alcohol lightness-removing column quantizer, ethyl alcohol are de-
Light tower quantizer oil phase discharge nozzle, azeotropic mixture recycles total expects pipe and total mixed solvent feed pipe is connected to the mixing of extraction tower lower part
On solvent feed mouth, the outlet of the ethyl alcohol lightness-removing column refluxing opening and ethyl alcohol condenser of light component removal column on the ethyl alcohol lightness-removing column top is logical
Cross the connection of ethyl alcohol lightness-removing column overhead reflux pipe, the ethyl alcohol lightness-removing column extraction mouth of the ethyl alcohol lightness-removing column bottom and the ethyl alcohol
Alcohol product tower feed inlet in the middle part of product tower produces pipe connection, the ethyl alcohol lightness-removing column bottom by ethyl alcohol lightness-removing column tower reactor
Ethyl alcohol lightness-removing column boil again outlet and lower part ethyl alcohol lightness-removing column boil again import by sequentially connected ethyl alcohol lightness-removing column tower reactor into
Reboiler pipe, ethyl alcohol lightness-removing column reboiler are connect with ethyl alcohol lightness-removing column tower reactor gas phase return pipe；
The alcohol product top of tower alcohol product extraction mouth outside be connected in turn alcohol product column overhead steam pipe,
Alcohol product tower condenser and alcohol product column overhead extraction pipe, the alcohol product tower of the alcohol product tower bottom produce mouth
Pipe, extractant cooler, extractant circulation pipe and total extractant feed pipe are produced by sequentially connected alcohol product tower tower reactor
It is connected on the extraction tower extractant feed mouth on extraction tower top, the alcohol product tower of the alcohol product tower bottom boils out again
Mouth and the alcohol product tower of the alcohol product tower lower part boil import by sequentially connected alcohol product tower tower reactor into again again
Boiling device pipe, alcohol product tower reboiler are connected with alcohol product tower tower reactor gas phase return pipe；
Toluene treating column extraction mouth at the top of the toluene treating column is steamed by sequentially connected toluene refined tower top
Steam pipe, toluene treating column condenser and toluene refined tower top extraction pipe are connected to the ethyl acetate in the middle part of ethyl acetate treating column
On treating column feed inlet, the outlet of toluene treating column refluxing opening and toluene treating column condenser at the top of the toluene treating column
The toluene product extraction mouth of connection, the toluene purification tower bottom produces pipe extraction by toluene treating column tower reactor, described
The toluene treating column that the toluene treating column of toluene purification tower bottom boils outlet and the toluene treating column lower part again boils import again
Tower reboiler is refined into reboiler pipe, toluene by sequentially connected toluene treating column tower reactor and toluene treating column tower reactor gas phase is returned
Flow tube connection；
Ethyl acetate treating column azeotropic mixture circulation extraction mouth at the top of the ethyl acetate treating column is by being sequentially connected
Ethyl acetate refined tower top steam pipe, ethyl acetate treating column condenser, ethyl acetate refined tower top extraction pipe, acetic acid
Ethyl ester treating column quantizer, ethyl acetate treating column quantizer oil phase discharge nozzle, azeotropic mixture recycle total expects pipe and total mixed solvent
Feed pipe is connected on the mixed solvent feed inlet of extraction tower lower part, the ethyl acetate essence at the top of the ethyl acetate treating column
Tower refluxing opening processed is connect with the outlet of ethyl acetate treating column condenser, the ethyl acetate of the ethyl acetate purification tower bottom
Product produces mouth and produces pipe extraction by ethyl acetate treating column tower reactor,
The ethyl acetate treating column of the ethyl acetate purification tower bottom boils outlet again and refines with the ethyl acetate
The ethyl acetate treating column of tower lower part boils import by sequentially connected ethyl acetate treating column tower reactor into reboiler pipe, acetic acid again
Ethyl ester purification tower reboiler is connected with ethyl acetate treating column tower reactor gas phase return pipe.
Further, in order to which effect of extracting is more preferable, the middle and lower part of the extraction tower is equipped with circulation discharge port, the extraction tower
It is additionally provided at least one recycle feed mouth being located on the upside of circulation discharge port, the circulation discharge port of the extraction tower and recycle feed
It is connect by recycling discharge nozzle with recycle feed pipe between mouthful.
Further, in order to which effect of extracting is more preferable, the quantity of the recycle feed mouth of the extraction tower is two, one of them
Recycle feed mouth is located at the middle and upper part of extraction tower, another recycle feed mouth is located at the top of extraction tower；The extraction tower follows
It is connect by recycling discharge nozzle with recycle feed pipe between ring discharge port and one of recycle feed mouth；The extraction tower follows
It is connect by recycling discharge nozzle with recycle feed pipe between ring discharge port and another recycle feed mouth.
Further, the tower internals type of the extraction tower is column plate or filler, number of theoretical plate 16-25.
Further, the ethyl alcohol lightness-removing column is fed by being located at the rectifying section of raffinate phase feed inlet or more and being located at raffinate phase
Mouth stripping section composition below, tower internals type is column plate or filler, theoretical number of plates of rectifying section 12-25, stripping section theoretical plate
Number is 18-28.
Further, the alcohol product tower is by being located at the rectifying section of feed inlet or more and being located at feed inlet stripping below
Duan Zucheng, tower internals type are column plate or filler, and theoretical number of plates of rectifying section 20-35, stripping section number of theoretical plate is 15-26.
Further, the toluene treating column is fed by being located at the rectifying section of extraction phase feed inlet or more and being located at extraction phase
Mouth stripping section composition below, tower internals type is column plate or filler, theoretical number of plates of rectifying section 16-26, stripping section theoretical plate
Number is 25-36.
Further, the ethyl acetate treating column by be located at feed inlet more than rectifying section and be located at feed inlet it is below
Stripping section composition, tower internals type are column plate or filler, and theoretical number of plates of rectifying section 18-24, stripping section number of theoretical plate is 26-
35。
The method containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol of separation, sequentially includes the following steps:
Step S1: containing the mixed solvents such as toluene, ethyl acetate and ethyl alcohol through total mixed solvent feed pipe from mixed solvent into
Material mouth enters extraction tower lower part, and extractant enters extraction tower top from total extractant feed pipe；
Step S2: the raffinate phase of extraction tower tower bottom enters ethyl alcohol lightness-removing column by extraction tower raffinate phase discharge nozzle and carries out essence
Evaporate, ethyl alcohol lightness-removing column tower top rise steam realize phase transformation through condenser, condense acquisition material be containing ethyl acetate, ethyl alcohol,
The ternary azeotrope and toluene of water and the binary azeotrope of water, a part flow back from the ethyl alcohol lightness-removing column at the top of ethyl alcohol lightness-removing column
Mouth passes back into tower, and another part is from the ethyl alcohol lightness-removing column azeotropic mixture circulation extraction mouth at the top of ethyl alcohol lightness-removing column through ethyl alcohol lightness-removing column
Overhead extraction pipe enters the layering of ethyl alcohol lightness-removing column quantizer, and lower layer's water phase is discharged by ethyl alcohol lightness-removing column quantizer water phase discharge nozzle
System, upper oil phase are back to extraction tower lower part mixed solvent feed inlet circulation by ethyl alcohol lightness-removing column quantizer oil phase discharge nozzle
It uses；
Step S3: the material of ethyl alcohol lightness-removing column tower reactor bottom through ethyl alcohol lightness-removing column tower reactor extraction pipe enter alcohol product tower into
Row rectifying, the steam that alcohol product column overhead rises realize phase transformation, ethyl alcohol of a part from alcohol product top of tower through condenser
Product tower refluxing opening passes back into tower, and another part is from the ethyl alcohol lightness-removing column extraction mouth at the top of ethyl alcohol lightness-removing column through alcohol product tower
Overhead extraction pipe goes out system, and the extractant that alcohol product tower tower reactor is isolated recycles after extractant cooler is cooling from extractant
Pipe is back to the recycling of extraction tower top extraction tower feed inlet；The industrial alcohol product that the material that condensation obtains is 95%；
Step S4: the extraction phase at the top of extraction tower enters toluene treating column by extraction tower extraction phase discharge nozzle and carries out essence
Evaporate, toluene refined tower top rise steam realize phase transformation through condenser, condense acquisition material be ethyl acetate, a small amount of water and
The mixture of trace toluene, a part pass back into tower from the refluxing opening at the top of toluene treating column, and another part is refined from toluene
The extraction mouth of top of tower enters ethyl acetate treating column, the production that toluene treating column tower reactor obtains through toluene refined tower top extraction pipe
Product produce the system of managing out through toluene treating column tower reactor；(product that tower reactor obtains is the toluene product that purity is greater than 99.6%)
Step S5: the material of extraction mouth enters the progress rectifying of ethyl acetate treating column, acetic acid at the top of toluene treating column
The steam that ethyl ester refined tower top rises realizes phase transformation through condenser, condense acquisition material be ethyl acetate and water azeotropic mixture,
The mixture of toluene azeotrope with water object, a part are passed back into from the ethyl acetate treating column refluxing opening at the top of ethyl acetate treating column
In tower, another part is from the azeotropic mixture circulation ethyl acetate treating column extraction mouth at the top of ethyl acetate treating column through ethyl acetate essence
Column overhead extraction pipe processed enters the layering of ethyl acetate treating column quantizer, and lower layer's water phase passes through ethyl acetate treating column quantizer water
Phase discharge nozzle discharge system, upper oil phase by ethyl acetate treating column quantizer oil phase discharge nozzle be back to extraction tower lower part into
Material mouth is recycled, and the product that ethyl acetate purification tower reactor obtains produces the system of managing out through ethyl acetate treating column tower reactor.Acetic acid
The product that ethyl ester purification tower reactor obtains is the ethyl acetate product that purity is greater than 99.6%.
Further, the extractant is water；
Operating condition setting in the extraction tower are as follows: tower top pressure is normal pressure, and operation temperature is room temperature, from total extractant
Feed pipe enter extractant with from total mixed solvent feed pipe enter mixed acid waste water volume ratio be 0.4-1.2, under
It is 1.0~4.0 that portion, which recycles discharge port and the volume ratio of extractant,；
Operating condition setting in the ethyl alcohol lightness-removing column are as follows: tower top pressure is normal pressure, and tower top temperature is 66-73 DEG C, tower
Kettle temperature degree is 80-90 DEG C, and overhead reflux ratio is 1.2-4.5；
Operating condition setting in the alcohol product tower are as follows: tower top pressure is normal pressure, and tower top temperature is 77-80 DEG C, tower
Kettle temperature degree is 99-101 DEG C, and overhead reflux ratio is 1.8-8.0；
Operating condition setting in the toluene treating column are as follows: tower top pressure is normal pressure, and tower top temperature is 73-79 DEG C, tower
Kettle temperature degree is 112-118 DEG C, and overhead reflux ratio is 1.0-5.0；
Operating condition setting in the ethyl acetate treating column are as follows: tower top pressure is normal pressure, tower top temperature 67-73
DEG C, bottom temperature is 75-79 DEG C, and overhead reflux ratio is 2.0-7.0.
Remarkable advantage of the invention is:
(1) select the existing component water of in the mixed solvent as extractant, using extraction with rectifying coupling technique effectively
The separation for realizing in the mixed solvent toluene, ethyl acetate, second alcohol and water solves the system since there are multiple groups azeotropic mixtures
Problem is separated, and avoids the quality for introducing solvent after other components influence separates.
(2) compared with patent CN102992930B is using five tower extraction rectification techniques, using extraction and rectifying coupling technique
The method containing toluene, ethyl acetate, ethyl alcohol and water mixed solvent of separation, since first tower is extraction tower, without consuming steam,
And remaining tower is atmospheric distillation, without using rectification under vacuum, significantly reduces energy consumption, the equipment investment of separation, can save
Energy consumption 20-35% is saved, equipment investment 17-28% is saved.
(3) use method of the invention, the toluene of recycling: purity is greater than 99.6%, ethanol content and is less than 400ppm and water
Divide and is less than 400ppm；The ethyl acetate of recycling: purity is greater than 99.6%, ethanol content less than 400ppm and moisture content is less than
400ppm；The ethyl alcohol of recycling: purity is greater than 95%, reaches industrial alcohol standard.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the embodiment of the present invention.
Figure label is described as follows: T1-extraction tower, T2-ethyl alcohol lightness-removing column, T3-alcohol product tower, T4-toluene essence
Tower processed, T5-ethyl acetate treating column；E1-ethyl alcohol condenser of light component removal column, E2-ethyl alcohol lightness-removing column reboiler, E3-ethyl alcohol produce
Product tower condenser, E4-alcohol product tower reboiler, E5-extractant cooler, E6-toluene treating column condenser, E7-first
Benzene refining tower reboiler, E8-ethyl acetate treating column condenser, E9-ethyl acetate refine tower reboiler, ethyl alcohol lightness-removing column point
Layer device (V1), ethyl acetate treating column quantizer (V2)；The total mixed solvent charging of PL1-fresh mix solvent feed pipe, PL2-
Pipe, the total extractant feed pipe of PL3-supplement extractant feed pipe, PL4-, PL5-extraction tower raffinate phase discharge nozzle, PL6-extraction
Taking tower extraction phase discharge nozzle, PL7-extraction tower middle and lower part recycles discharge nozzle, PL8-extraction tower middle and upper part recycle feed pipe,
PL9-extraction tower top recycle feed pipe, PL10-ethyl alcohol lightness-removing column overhead vapours pipe, PL11-ethyl alcohol lightness-removing column overhead reflux
Pipe, PL12-ethyl alcohol lightness-removing column overhead extraction pipe, PL13-ethyl alcohol lightness-removing column quantizer water phase discharge nozzle, PL14-ethyl alcohol are de- light
Tower quantizer oil phase discharge nozzle, PL15-ethyl alcohol lightness-removing column tower reactor are returned into reboiler pipe, PL16-ethyl alcohol lightness-removing column tower reactor gas phase
Flow tube, PL17-ethyl alcohol lightness-removing column tower reactor extraction pipe, PL18-alcohol product column overhead steam pipe, PL19-alcohol product tower tower
Push up return pipe, PL20-alcohol product column overhead extraction pipe, PL21-alcohol product tower tower reactor is into reboiler pipe, PL22-ethyl alcohol
Product tower tower reactor gas phase return pipe, PL23-alcohol product tower tower reactor extraction pipe, PL24-extractant circulation pipe, PL25-toluene
Refined tower top steam pipe, PL26-toluene refined tower top return pipe, PL27-toluene refined tower top extraction pipe, PL28-
Toluene treating column tower reactor is into reboiler pipe, PL29-toluene treating column tower reactor gas phase return pipe, PL30-toluene treating column tower reactor
Extraction pipe, PL31-ethyl acetate refined tower top steam pipe, PL32-ethyl acetate refined tower top return pipe, PL33-second
Acetoacetic ester refined tower top extraction pipe, PL34-ethyl acetate treating column quantizer water phase discharge nozzle, PL35-ethyl acetate essence
Tower quantizer oil phase discharge nozzle processed, PL36-azeotropic mixture recycle total expects pipe, and PL37-ethyl acetate treating column tower reactor is into reboiler
Pipe, PL38-ethyl acetate treating column tower reactor gas phase return pipe, PL39-ethyl acetate treating column tower reactor extraction pipe.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and embodiments.
Embodiment 1
It is set as shown in Figure 1, present embodiments providing a kind of separation containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol
It is standby, including extraction tower T1, ethyl alcohol lightness-removing column T2, ethyl alcohol condenser of light component removal column E1, ethyl alcohol lightness-removing column reboiler E2, ethyl alcohol lightness-removing column
Quantizer V1, alcohol product tower T3, alcohol product tower condenser E3, alcohol product tower reboiler E4, extractant cooler E5, first
Benzene refining tower T4, toluene treating column condenser E6, toluene purification tower reboiler E7, ethyl acetate treating column T5, ethyl acetate essence
Tower condenser E8 processed, ethyl acetate refine tower reboiler E9, ethyl acetate treating column quantizer V2；
The tower top of the extraction tower T1 is equipped with extraction tower extraction phase discharge port, and top is equipped with extraction tower extractant feed mouth,
Tower bottom is equipped with extraction tower raffinate phase discharge port, and lower part is equipped with mixed solvent feed inlet；It is equipped at the top of the ethyl alcohol lightness-removing column T2
Ethyl alcohol lightness-removing column azeotropic mixture circulation extraction mouth, top are equipped with ethyl alcohol lightness-removing column refluxing opening, and middle part is equipped with ethyl alcohol lightness-removing column raffinate phase
Feed inlet, lower part are equipped with ethyl alcohol lightness-removing column and boil import again, and bottom is equipped with ethyl alcohol lightness-removing column extraction mouth and ethyl alcohol lightness-removing column boils out again
Mouthful；It is equipped with alcohol product tower refluxing opening at the top of the alcohol product tower T3 and alcohol product produces mouth, middle part is produced equipped with ethyl alcohol
Product tower feed inlet, lower part are equipped with alcohol product tower and boil import again, and bottom is equipped with alcohol product tower extraction mouth and alcohol product tower again
Boiling outlet；It is equipped with toluene treating column refluxing opening at the top of the toluene treating column T4 and toluene treating column produces mouth, middle part is equipped with
Toluene treating column extraction phase feed inlet, lower part are equipped with toluene treating column and boil import again, and bottom is equipped with toluene treating column toluene product
Extraction mouth and toluene treating column boil outlet again；Ethyl acetate treating column refluxing opening is equipped at the top of the ethyl acetate treating column T5
Extraction mouth is recycled with ethyl acetate treating column azeotropic mixture, middle part is equipped with ethyl acetate treating column feed inlet, and lower part is equipped with acetic acid second
Ester treating column boils import again, and bottom is equipped with ethyl acetate product extraction mouth and ethyl acetate treating column boils outlet again；
It is equipped with toluene treating column refluxing opening at the top of the toluene treating column T4 and toluene treating column produces mouth, the first
Toluene treating column extraction phase feed inlet is equipped in the middle part of benzene refining tower T4, the toluene lower part treating column T4 is equipped with toluene treating column
Import is boiled again, and the toluene bottom treating column T4 is equipped with toluene treating column toluene product extraction mouth and toluene treating column boils out again
Mouthful；Ethyl acetate treating column refluxing opening is equipped at the top of the ethyl acetate treating column T5 and ethyl acetate treating column azeotropic mixture follows
Ring produces mouth, and ethyl acetate treating column feed inlet, the ethyl acetate essence are equipped in the middle part of the ethyl acetate treating column T5
The lower part tower T5 processed is equipped with ethyl acetate treating column and boils import again, and the ethyl acetate bottom treating column T5 is produced equipped with ethyl acetate
Product extraction mouth and ethyl acetate treating column boil outlet again；
The extraction tower raffinate phase discharge port of the extraction tower T1 tower bottom and the extraction in the middle part of the ethyl alcohol lightness-removing column T2
Tower raffinate phase feed inlet is gone out by extraction tower raffinate phase discharge nozzle PL5 connection, the extraction tower extraction phase of the extraction tower T1 tower top
Material mouth passes through extraction tower extraction phase discharge nozzle PL6 with the toluene treating column extraction phase feed inlet in the middle part of the toluene treating column T4 and connects
It connects；
Ethyl alcohol lightness-removing column azeotropic mixture circulation extraction mouth at the top of the ethyl alcohol lightness-removing column T2 passes through sequentially connected ethyl alcohol
Lightness-removing column overhead vapours pipe PL10, ethyl alcohol condenser of light component removal column E1, ethyl alcohol lightness-removing column overhead extraction pipe PL12, ethyl alcohol lightness-removing column point
Layer device V1, ethyl alcohol lightness-removing column quantizer oil phase discharge nozzle PL14, azeotropic mixture recycle total expects pipe PL36 and total mixed solvent feed pipe
PL2 is connected on the mixed solvent feed inlet of the lower part extraction tower T1, and the ethyl alcohol lightness-removing column on the top ethyl alcohol lightness-removing column T2 returns
Head piece is connect with the outlet of ethyl alcohol condenser of light component removal column E1 by ethyl alcohol lightness-removing column overhead reflux pipe PL11, and the ethyl alcohol is de- light
Ethyl alcohol lightness-removing column extraction mouth and the alcohol product tower feed inlet in the middle part of the alcohol product tower T3 of the bottom tower T2 pass through ethyl alcohol
Lightness-removing column tower reactor produces pipe PL17 connection, and the ethyl alcohol lightness-removing column of the bottom ethyl alcohol lightness-removing column T2 boils the second of outlet and lower part again
Alcohol lightness-removing column boils import by sequentially connected ethyl alcohol lightness-removing column tower reactor into reboiler pipe PL15, ethyl alcohol lightness-removing column reboiler E2 again
It is connect with ethyl alcohol lightness-removing column tower reactor gas phase return pipe PL16；
Alcohol product column overhead steam is connected in turn outside alcohol product extraction mouth at the top of the alcohol product tower T3
Pipe PL18, alcohol product tower condenser E3 and alcohol product column overhead produce pipe PL20, the bottom alcohol product tower T3
Alcohol product tower produces mouth and produces pipe PL23, extractant cooler E5, extractant by sequentially connected alcohol product tower tower reactor
Circulation pipe PL24 and total extractant feed pipe PL4 are connected on the extraction tower extractant feed mouth on the top extraction tower T1, described
The alcohol product tower that the alcohol product tower of the bottom alcohol product tower T3 boils outlet and the lower part alcohol product tower T3 again boils again
Import is by sequentially connected alcohol product tower tower reactor into reboiler pipe PL21, alcohol product tower reboiler E4 and alcohol product tower
Tower reactor gas phase return pipe PL22 connection；
Toluene treating column extraction mouth at the top of the toluene treating column T4 passes through sequentially connected toluene refined tower top
Steam pipe PL25, toluene treating column condenser E6 and toluene refined tower top extraction pipe PL27 are connected to ethyl acetate treating column T5
Toluene treating column refluxing opening and toluene essence on the ethyl acetate treating column feed inlet at middle part, at the top of the toluene treating column T4
The outlet of tower condenser E6 processed connects, and the toluene product extraction mouth of the bottom toluene treating column T4 passes through toluene treating column tower
Kettle produces pipe PL30 extraction, and the toluene treating column of the bottom toluene treating column T4 boils outlet and the toluene treating column again
The toluene treating column of the lower part T4 boils import again and is refined by sequentially connected toluene treating column tower reactor into reboiler pipe PL28, toluene
Tower reboiler E7 is connected with toluene treating column tower reactor gas phase return pipe PL29；
Ethyl acetate treating column azeotropic mixture circulation extraction mouth at the top of the ethyl acetate treating column T5 is by successively connecting
The ethyl acetate refined tower top steam pipe PL31 that connects, ethyl acetate treating column condenser E8, ethyl acetate refined tower top are adopted
Outlet pipe PL33, ethyl acetate treating column quantizer V2, ethyl acetate treating column quantizer oil phase discharge nozzle PL35, azeotropic mixture circulation
Total expects pipe PL36 and total mixed solvent feed pipe PL2 is connected on the mixed solvent feed inlet of the lower part extraction tower T1, the second
Ethyl acetate treating column refluxing opening at the top of acetoacetic ester treating column T5 is connect with the outlet of ethyl acetate treating column condenser E8, institute
The ethyl acetate product extraction mouth for the bottom ethyl acetate treating column T5 stated produces pipe PL39 by ethyl acetate treating column tower reactor
Extraction；
The ethyl acetate treating column of the bottom ethyl acetate treating column T5 boils outlet and the ethyl acetate essence again
The ethyl acetate treating column of tower lower part processed boils import by sequentially connected ethyl acetate treating column tower reactor into reboiler pipe again
PL37, ethyl acetate purification tower reboiler E9 are connected with ethyl acetate treating column tower reactor gas phase return pipe PL38.
The middle and lower part of the extraction tower T1 is equipped with circulation discharge port, and the extraction tower T1 is additionally provided at least one and is located at circulation
Recycle feed mouth on the upside of discharge port passes through circulation discharge nozzle between the circulation discharge port and recycle feed mouth of the extraction tower T1
PL7 is connect with recycle feed pipe PL8.
The quantity of the recycle feed mouth of the extraction tower T1 is two, and one of recycle feed mouth is located at extraction tower T1's
Middle and upper part, another recycle feed mouth are located at the top of extraction tower T1；The circulation discharge port of the extraction tower T1 and one of them
It is connect by recycling discharge nozzle PL7 with recycle feed pipe PL8 between recycle feed mouth；The circulation discharge port of the extraction tower T1 with
It is connect by recycling discharge nozzle PL7 with recycle feed pipe PL9 between another recycle feed mouth.The present embodiment can also be not provided with
Circulation discharge port more recycles discharge port.
The tower internals type of the extraction tower T1 is column plate or filler, number of theoretical plate 16-25；The ethyl alcohol lightness-removing column
T2 is by being located at the rectifying section of raffinate phase feed inlet or more and forming positioned at raffinate phase feed inlet stripping section below, tower internals type
For column plate or filler, theoretical number of plates of rectifying section 12-25, stripping section number of theoretical plate is 18-28；The alcohol product tower T3 is by position
Rectifying section more than feed inlet and it is located at feed inlet stripping section composition below, tower internals type is column plate or filler, rectifying
Section number of theoretical plate is 20-35, and stripping section number of theoretical plate is 15-26；The toluene treating column T4 by be located at extraction phase feed inlet with
On rectifying section and be located at extraction phase feed inlet stripping section below composition, tower internals type is column plate or filler, rectifying section reason
It is 16-26 by plate number, stripping section number of theoretical plate is 25-36；The ethyl acetate treating column T5 is by the essence more than feed inlet
It evaporates section and is located at feed inlet stripping section composition below, tower internals type is column plate or filler, theoretical number of plates of rectifying section 18-
24, stripping section number of theoretical plate is 26-35.
A method of separation is sequentially included the following steps: containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol
Step S1: the mixed solvent to be separated containing toluene, ethyl acetate, ethyl alcohol and a small amount of water is through total mixed solvent feed pipe
PL2 enters the lower part extraction tower T1 from mixed solvent feed inlet, and extractant enters on extraction tower T1 from total extractant feed pipe PL4
The middle and lower part circulation discharge port in portion, extraction tower T1 extracts middle and upper part feed inlet and top that first-class stock is recycled to the extraction tower T1 out
Feed inlet recycles discharge nozzle PL7 respectively and on extraction tower middle and upper part recycle feed pipe PL8 and extraction tower by extraction tower middle and lower part
The PL9 connection of portion's recycle feed pipe；
Step S2: the raffinate phase of extraction tower T1 tower bottom enters ethyl alcohol lightness-removing column T2 by extraction tower raffinate phase discharge nozzle PL5
Rectifying is carried out, the steam that ethyl alcohol lightness-removing column T2 tower top rises realizes phase transformation through condenser E1, and the material for condensing acquisition is containing acetic acid
Ethyl ester, ethyl alcohol, the ternary azeotrope of water and toluene and water binary azeotrope, a part is from returning at the top of ethyl alcohol lightness-removing column T2
Head piece passes back into tower, and another part is adopted from the azeotropic mixture circulation extraction mouth at the top of ethyl alcohol lightness-removing column T2 through ethyl alcohol lightness-removing column tower top
Outlet pipe PL12 enters ethyl alcohol lightness-removing column quantizer V1 layering, and lower layer's water phase passes through ethyl alcohol lightness-removing column quantizer water phase discharge nozzle PL13
Discharge system, upper oil phase are back to the lower part extraction tower T1 feed inlet by ethyl alcohol lightness-removing column quantizer oil phase discharge nozzle PL14 and follow
Ring uses；
Step S3: the mixture that ethyl alcohol lightness-removing column T2 tower reactor isolates second alcohol and water is produced through ethyl alcohol lightness-removing column tower reactor manages
PL17 enters alcohol product tower T3 and carries out rectifying, and the steam that alcohol product tower T3 tower top rises realizes phase transformation through condenser E3, cold
The industrial alcohol product that the solidifying material obtained is 95%, a part pass back into tower from the refluxing opening at the top of alcohol product tower T3,
Another part goes out system, alcohol product tower through alcohol product column overhead extraction pipe PL20 from the extraction mouth at the top of ethyl alcohol lightness-removing column T2
The extractant that T3 tower reactor is isolated is back on extraction tower T1 after extractant cooler E3 is cooling from extractant circulation pipe PL24
Portion's feed inlet is recycled；
Step S4: the extraction phase at the top of extraction tower T1 enters toluene treating column T4 by extraction tower extraction phase discharge nozzle PL6
Rectifying is carried out, the steam that toluene treating column T4 tower top rises realizes phase transformation through condenser E6, and the material for condensing acquisition is acetic acid second
The mixture of ester, a small amount of water and trace toluene, a part pass back into tower from the refluxing opening at the top of toluene treating column T4, another portion
Divide from the extraction mouth at the top of toluene treating column T4 through toluene refined tower top extraction pipe PL27 and enters ethyl acetate treating column T5, first
Benzene refining tower T4 tower reactor obtains toluene product of the purity greater than 99.6% and goes out system through toluene treating column tower reactor extraction pipe PL30；
Step S5: the material of extraction mouth enters ethyl acetate treating column T5 progress rectifying at the top of toluene treating column T4,
The steam that ethyl acetate treating column T5 tower top rises realizes phase transformation through condenser E8, and the material for condensing acquisition is ethyl acetate and water
The mixture of azeotropic mixture, toluene azeotrope with water object, a part pass back into tower from the refluxing opening at the top of ethyl acetate treating column T5,
Another part is produced through ethyl acetate refined tower top from the azeotropic mixture circulation extraction mouth at the top of ethyl acetate treating column T5 and is managed
PL33 enters ethyl acetate treating column quantizer V2 layering, and lower layer's water phase passes through ethyl acetate treating column quantizer water phase discharge nozzle
PL34 discharge system, upper oil phase are back to the lower part extraction tower T1 by ethyl acetate treating column quantizer oil phase discharge nozzle PL35
Feed inlet is recycled, and toluene treating column T4 tower reactor obtains ethyl acetate product of the purity greater than 99.6% and refines through ethyl acetate
Tower tower reactor extraction pipe PL39 goes out system.
The extractant is the existing component water of in the mixed solvent.
Operating condition setting in the extraction tower T1 are as follows: tower top pressure is normal pressure, and operation temperature is room temperature, from total extraction
The volume ratio of the extractant that agent feed pipe enters and the mixed acid waste water entered from total mixed solvent feed pipe is 0.4-1.2, in
It is 1.0~4.0 that lower part, which recycles discharge port and the volume ratio of extractant,；
Operating condition setting in the ethyl alcohol lightness-removing column T2 are as follows: tower top pressure is normal pressure, and tower top temperature is 66-73 DEG C,
Bottom temperature is 80-90 DEG C, and overhead reflux ratio is 1.2-4.5；
Operating condition setting in the alcohol product tower T3 are as follows: tower top pressure is normal pressure, and tower top temperature is 77-80 DEG C,
Bottom temperature is 99-101 DEG C, and overhead reflux ratio is 1.8-8.0；
Operating condition setting in the toluene treating column T4 are as follows: tower top pressure is normal pressure, and tower top temperature is 73-79 DEG C,
Bottom temperature is 112-118 DEG C, and overhead reflux ratio is 1.0-5.0；
Operating condition setting in the ethyl acetate treating column T5 are as follows: tower top pressure is normal pressure, tower top temperature 67-73
DEG C, bottom temperature is 75-79 DEG C, and overhead reflux ratio is 2.0-7.0.
Specifically, extraction tower T1 tower body material is SUS304, fills the regular wire packing of MELLAPAKPL 752Y in tower,
Tower diameter is 500mm, number of theoretical plate 18.Ethyl alcohol lightness-removing column T2 tower body material is SUS304, fills MELLAPAKPL 752Y in tower
Regular wire packing, tower diameter 400mm, number of theoretical plate 50, the 22nd piece of theoretical plate charging.Alcohol product tower T3 tower body material is
SUS304, tower is interior to fill the regular wire packing of MELLAPAKPL 752Y, tower diameter 600mm, number of theoretical plate 58, the 34th piece of reason
It is fed by plate.Toluene treating column T4 tower body material is SUS304, fills the regular wire packing of MELLAPAKPL 752Y, tower in tower
Diameter is 500mm, number of theoretical plate 52, the 24th piece of theoretical plate charging.Ethyl acetate treating column T5 tower body material is SUS304, in tower
Fill the regular wire packing of MELLAPAKPL 752Y, tower diameter 300mm, number of theoretical plate 48, the 20th piece of theoretical plate charging.
The feed rate of mixed solvent is 1000kg/h, is entered from extraction tower T1 lower part feed inlet, 32 DEG C of feeding temperature, into
Material composition: 32% toluene, 35% ethyl acetate, 32.5% ethyl alcohol, 0.5% water；Extractant water inlet amount is 600kg/h, from extraction
Tower T1 upper feed inlet is taken to enter；Extraction tower T1 operating condition: operating pressure 101kPa, 36.9 DEG C of tower top temperature, tower bottom temperature
36.4 DEG C of degree, it is 1800kg/h that middle and lower part, which recycles discharge port flow,；Ethyl alcohol lightness-removing column T2 operating condition: operating pressure 101kPa,
70.1 DEG C of tower top temperature, 85.8 DEG C of column bottom temperature, overhead reflux is than 3；Alcohol product tower T3 operating condition: operating pressure
101kPa, 77.8 DEG C of tower top temperature, 99.6 DEG C of column bottom temperature, overhead reflux is than 5；Toluene treating column T4 operating condition: operation pressure
Power 101kPa, 75.4 DEG C of tower top temperature, 113.4 DEG C of column bottom temperature, overhead reflux is than 2；Ethyl acetate treating column T5 operating condition:
Operating pressure 101kPa, 70.5 DEG C of tower top temperature, 76.8 DEG C of column bottom temperature, overhead reflux is than 4.
Under the above conditions, the alcohol product of alcohol product tower T3 tower top: purity 95.2%；Toluene treating column T4 tower reactor
Toluene product: purity 99.6%, ethanol content 348ppm and moisture 356ppm；The ethyl acetate of ethyl acetate treating column T5 tower reactor
Product: purity 99.6%, ethanol content 302ppm and moisture 348ppm.
Embodiment 2:
Unlike the embodiments above, using attached process flow shown in FIG. 1, extraction tower T1 tower body material is
SUS304, tower is interior to fill the regular wire packing of MELLAPAKPL 752Y, tower diameter 500mm, number of theoretical plate 18.Ethyl alcohol is de- light
Tower T2 tower body material is SUS304, fills the regular wire packing of MELLAPAKPL 752Y, tower diameter 400mm, number of theoretical plate in tower
It is the 50, the 22nd piece of theoretical plate charging.Alcohol product tower T3 tower body material is SUS304, filling MELLAPAKPL 752Y rule in tower
Whole wire packing, tower diameter 600mm, number of theoretical plate 58, the 34th piece of theoretical plate charging.Toluene treating column T4 tower body material is
SUS304, tower is interior to fill the regular wire packing of MELLAPAKPL 752Y, tower diameter 500mm, number of theoretical plate 52, the 24th piece of reason
It is fed by plate.Ethyl acetate treating column T5 tower body material is SUS304, and the filling regular silk screen of MELLAPAKPL 752Y is filled out in tower
Material, tower diameter 300mm, number of theoretical plate 48, the 20th piece of theoretical plate charging.
The feed rate of mixed solvent is 1000kg/h, is entered from extraction tower T1 lower part feed inlet, 32 DEG C of feeding temperature, into
Material composition: 31% toluene, 36% ethyl acetate, 31% ethyl alcohol, 2.0% water；Extractant water inlet amount is 800kg/h, from extraction
Tower T1 upper feed inlet enters；Extraction tower T1 operating condition: operating pressure 101kPa, 37.2 DEG C of tower top temperature, column bottom temperature
37.0 DEG C, it is 2200kg/h that middle and lower part, which recycles discharge port flow,；Ethyl alcohol lightness-removing column T2 operating condition: operating pressure 101kPa, tower
69.1 DEG C of temperature of top, 84.2 DEG C of column bottom temperature, overhead reflux is than 2.5；Alcohol product tower T3 operating condition: operating pressure
101kPa, 78.0 DEG C of tower top temperature, 99.4 DEG C of column bottom temperature, overhead reflux is than 4.6；Toluene treating column T4 operating condition: operation
Pressure 101kPa, 74.1 DEG C of tower top temperature, 113.2 DEG C of column bottom temperature, overhead reflux is than 2.6；Ethyl acetate treating column T5 operation
Condition: operating pressure 101kPa, 69.2 DEG C of tower top temperature, 77.1 DEG C of column bottom temperature, overhead reflux is than 3.8.
Under the above conditions, the alcohol product of alcohol product tower T3 tower top: purity 95.1%；Toluene treating column T4 tower reactor
Toluene product: purity 99.7%, ethanol content 315ppm and moisture 338ppm；The ethyl acetate of ethyl acetate treating column T5 tower reactor
Product: purity 99.7%, ethanol content 282ppm and moisture 315ppm.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (10)
1. a kind of separation equipment containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol, it is characterised in that: including extraction tower
(T1), ethyl alcohol lightness-removing column (T2), ethyl alcohol condenser of light component removal column (E1), ethyl alcohol lightness-removing column reboiler (E2), the layering of ethyl alcohol lightness-removing column
Device (V1), alcohol product tower (T3), alcohol product tower condenser (E3), alcohol product tower reboiler (E4), extractant cooler
(E5), toluene treating column (T4), toluene treating column condenser (E6), toluene refine tower reboiler (E7), ethyl acetate treating column
(T5), ethyl acetate treating column condenser (E8), ethyl acetate refine tower reboiler (E9), ethyl acetate treating column quantizer
(V2)；
The tower top of the extraction tower (T1) is equipped with extraction tower extraction phase discharge port, and top is equipped with extraction tower extractant feed mouth, tower
Bottom is equipped with extraction tower raffinate phase discharge port, and lower part is equipped with mixed solvent feed inlet；It is equipped at the top of the ethyl alcohol lightness-removing column (T2)
Ethyl alcohol lightness-removing column azeotropic mixture circulation extraction mouth, top are equipped with ethyl alcohol lightness-removing column refluxing opening, and middle part is equipped with ethyl alcohol lightness-removing column raffinate phase
Feed inlet, lower part are equipped with ethyl alcohol lightness-removing column and boil import again, and bottom is equipped with ethyl alcohol lightness-removing column extraction mouth and ethyl alcohol lightness-removing column boils out again
Mouthful；It is equipped with alcohol product tower refluxing opening at the top of the alcohol product tower (T3) and alcohol product produces mouth, middle part is equipped with ethyl alcohol
Product tower feed inlet, lower part are equipped with alcohol product tower and boil import again, and bottom is equipped with alcohol product tower extraction mouth and alcohol product tower
Outlet is boiled again；It is equipped with toluene treating column refluxing opening at the top of the toluene treating column (T4) and toluene treating column produces mouth, middle part
Equipped with toluene treating column extraction phase feed inlet, lower part is equipped with toluene treating column and boils import again, and bottom is equipped with toluene treating column toluene
Product extraction mouth and toluene treating column boil outlet again；Ethyl acetate treating column is equipped at the top of the ethyl acetate treating column (T5)
Refluxing opening and ethyl acetate treating column azeotropic mixture circulation extraction mouth, middle part are equipped with ethyl acetate treating column feed inlet, and lower part is equipped with
Ethyl acetate treating column boils import again, and bottom is equipped with ethyl acetate product extraction mouth and ethyl acetate treating column boils outlet again；
Extraction in the middle part of the extraction tower raffinate phase discharge port of described extraction tower (T1) tower bottom and the ethyl alcohol lightness-removing column (T2)
Tower raffinate phase feed inlet is connected by extraction tower raffinate phase discharge nozzle (PL5), the extraction tower extraction of extraction tower (T1) tower top
Phase discharge port is discharged with the toluene treating column extraction phase feed inlet in the middle part of the toluene treating column (T4) by extraction tower extraction phase
Manage (PL6) connection；
Ethyl alcohol lightness-removing column azeotropic mixture circulation extraction mouth at the top of the ethyl alcohol lightness-removing column (T2) is de- by sequentially connected ethyl alcohol
Light column overhead steam pipe (PL10), ethyl alcohol condenser of light component removal column (E1), ethyl alcohol lightness-removing column overhead extraction pipe (PL12), ethyl alcohol are de- light
Tower quantizer (V1), ethyl alcohol lightness-removing column quantizer oil phase discharge nozzle (PL14), azeotropic mixture recycle total expects pipe (PL36) and total mixing
Solvent feed pipe (PL2) is connected on the mixed solvent feed inlet of the lower part extraction tower (T1), on the ethyl alcohol lightness-removing column (T2)
The outlet of the ethyl alcohol lightness-removing column refluxing opening and ethyl alcohol condenser of light component removal column (E1) in portion passes through ethyl alcohol lightness-removing column overhead reflux pipe
(PL11) it connects, in the ethyl alcohol lightness-removing column extraction mouth of described bottom ethyl alcohol lightness-removing column (T2) and the alcohol product tower (T3)
The alcohol product tower feed inlet in portion passes through ethyl alcohol lightness-removing column tower reactor extraction pipe (PL17) connection, described bottom ethyl alcohol lightness-removing column (T2)
The ethyl alcohol lightness-removing column that the ethyl alcohol lightness-removing column in portion boils outlet and lower part again boils import again and passes through sequentially connected ethyl alcohol lightness-removing column tower reactor
It is connect into reboiler pipe (PL15), ethyl alcohol lightness-removing column reboiler (E2) with ethyl alcohol lightness-removing column tower reactor gas phase return pipe (PL16)；
Alcohol product column overhead steam pipe is connected in turn outside alcohol product extraction mouth at the top of the alcohol product tower (T3)
(PL18), alcohol product tower condenser (E3) and alcohol product column overhead extraction pipe (PL20), the alcohol product tower (T3)
The alcohol product tower extraction mouth of bottom produces pipe (PL23), extractant cooler by sequentially connected alcohol product tower tower reactor
(E5), extractant circulation pipe (PL24) and total extractant feed pipe (PL4) are connected to the extraction tower extraction on the top extraction tower (T1)
On agent feed inlet, the alcohol product tower of described bottom alcohol product tower (T3) boils outlet and the alcohol product tower (T3) again
The alcohol product tower of lower part boils import by sequentially connected alcohol product tower tower reactor into reboiler pipe (PL21), alcohol product again
Tower reboiler (E4) and alcohol product tower tower reactor gas phase return pipe (PL22) connection；
Toluene treating column extraction mouth at the top of the toluene treating column (T4) is steamed by sequentially connected toluene refined tower top
Steam pipe (PL25), toluene treating column condenser (E6) and toluene refined tower top extraction pipe (PL27) are connected to ethyl acetate purification
Toluene treating column refluxing opening on ethyl acetate treating column feed inlet in the middle part of tower (T5), at the top of the toluene treating column (T4)
It is connect with the outlet of toluene treating column condenser (E6), the toluene product extraction mouth of described bottom toluene treating column (T4) passes through
Toluene treating column tower reactor extraction pipe (PL30) extraction, the toluene treating column of described bottom toluene treating column (T4) boil again outlet with
The toluene treating column of described lower part toluene treating column (T4) boils import by sequentially connected toluene treating column tower reactor into again again
Boil device pipe (PL28), toluene purification tower reboiler (E7) and toluene treating column tower reactor gas phase return pipe (PL29) connection；
Ethyl acetate treating column azeotropic mixture circulation extraction mouth at the top of the ethyl acetate treating column (T5) is by being sequentially connected
Ethyl acetate refined tower top steam pipe (PL31), ethyl acetate treating column condenser (E8), ethyl acetate refined tower top
Extraction pipe (PL33), ethyl acetate treating column quantizer oil phase discharge nozzle (PL35), is total to ethyl acetate treating column quantizer (V2)
Boiling object recycles total expects pipe (PL36) and total mixed solvent feed pipe (PL2) is connected to the mixed solvent charging of the lower part extraction tower (T1)
Ethyl acetate treating column refluxing opening and ethyl acetate treating column condenser on mouth, at the top of the ethyl acetate treating column (T5)
(E8) the ethyl acetate product extraction mouth of outlet connection, described bottom ethyl acetate treating column (T5) passes through ethyl acetate essence
Tower tower reactor extraction pipe (PL39) extraction processed；
The ethyl acetate treating column of described bottom ethyl acetate treating column (T5) boils outlet again and refines with the ethyl acetate
The ethyl acetate treating column of tower lower part boils import by sequentially connected ethyl acetate treating column tower reactor into reboiler pipe again
(PL37), ethyl acetate purification tower reboiler (E9) and ethyl acetate treating column tower reactor gas phase return pipe (PL38) connection.
2. a kind of separation equipment containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol according to claim 1, feature
Be: the middle and lower part of the extraction tower (T1) be equipped with circulation discharge port, the extraction tower (T1) be additionally provided at least one be located at follow
Recycle feed mouth on the upside of ring discharge port, by recycling between the circulation discharge port and recycle feed mouth of the extraction tower (T1)
Expects pipe (PL7) is connect with recycle feed pipe (PL8).
3. a kind of separation equipment containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol according to claim 2, feature
Be: the quantity of the recycle feed mouth of the extraction tower (T1) is two, and one of recycle feed mouth is located at extraction tower (T1)
Middle and upper part, another recycle feed mouth is located at the top of extraction tower (T1)；The circulation discharge port of the extraction tower (T1) and its
In connect by recycling discharge nozzle (PL7) with recycle feed pipe (PL8) between a recycle feed mouth；The extraction tower (T1)
It is connect by recycling discharge nozzle (PL7) with recycle feed pipe (PL9) between circulation discharge port and another recycle feed mouth.
4. a kind of separation equipment containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol according to claim 1, feature
It is:
The tower internals type of the extraction tower (T1) is column plate or filler, number of theoretical plate 16-25.
5. a kind of separation equipment containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol according to claim 1, feature
It is:
The ethyl alcohol lightness-removing column (T2) is below by the rectifying section more than raffinate phase feed inlet and positioned at raffinate phase feed inlet
Stripping section composition, tower internals type are column plate or filler, and theoretical number of plates of rectifying section 12-25, stripping section number of theoretical plate is 18-
28。
6. a kind of separation equipment containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol according to claim 1, feature
Be: the alcohol product tower (T3) forms by the rectifying section more than feed inlet and positioned at feed inlet stripping section below,
Tower internals type is column plate or filler, and theoretical number of plates of rectifying section 20-35, stripping section number of theoretical plate is 15-26.
7. a kind of separation equipment containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol according to claim 1, feature
Be: the toluene treating column (T4) is below by the rectifying section more than extraction phase feed inlet and positioned at extraction phase feed inlet
Stripping section composition, tower internals type are column plate or filler, and theoretical number of plates of rectifying section 16-26, stripping section number of theoretical plate is 25-
36。
8. a kind of separation equipment containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol according to claim 1, feature
Be: the ethyl acetate treating column (T5) is by being located at the rectifying section of feed inlet or more and being located at feed inlet stripping section group below
At tower internals type is column plate or filler, and theoretical number of plates of rectifying section 18-24, stripping section number of theoretical plate is 26-35.
9. the separation of equipment described in any one of -8 is containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol according to claim 1
Method, it is characterised in that: sequentially include the following steps:
Step S1: containing the mixed solvents such as toluene, ethyl acetate and ethyl alcohol through total mixed solvent feed pipe (PL2) from mixed solvent into
Material mouth enters the lower part extraction tower (T1), and extractant enters the top extraction tower (T1) from total extractant feed pipe (PL4)；
Step S2: the raffinate phase of extraction tower (T1) tower bottom enters ethyl alcohol lightness-removing column by extraction tower raffinate phase discharge nozzle (PL5)
(T2) rectifying is carried out, the steam that ethyl alcohol lightness-removing column (T2) tower top rises realizes phase transformation through condenser (E1), condenses the material of acquisition
It is a part of from ethyl alcohol lightness-removing column for the binary azeotrope containing ethyl acetate, ethyl alcohol, the ternary azeotrope of water and toluene and water
(T2) the ethyl alcohol lightness-removing column refluxing opening at the top of passes back into tower, and another part is from the ethyl alcohol lightness-removing column at the top of ethyl alcohol lightness-removing column (T2)
Azeotropic mixture circulation extraction mouth is layered through ethyl alcohol lightness-removing column overhead extraction pipe (PL12) into ethyl alcohol lightness-removing column quantizer (V1), lower layer
Water phase passes through ethyl alcohol lightness-removing column quantizer water phase discharge nozzle (PL13) discharge system, and upper oil phase passes through ethyl alcohol lightness-removing column quantizer
Oily phase discharge nozzle (PL14) is back to the recycling of extraction tower (T1) lower part mixed solvent feed inlet；
Step S3: the material of ethyl alcohol lightness-removing column (T2) tower reactor bottom produces pipe (PL17) through ethyl alcohol lightness-removing column tower reactor and produces into ethyl alcohol
Product tower (T3) carries out rectifying, and the steam that alcohol product tower (T3) tower top rises realizes phase transformation through condenser (E3), a part of from second
Alcohol product tower refluxing opening at the top of alcohol product tower (T3) passes back into tower, and another part is from the second at the top of ethyl alcohol lightness-removing column (T2)
Alcohol lightness-removing column produces mouth and goes out system, the extraction that alcohol product tower (T3) tower reactor is isolated through alcohol product column overhead extraction pipe (PL20)
Take agent after extractant cooler (E5) is cooling from extractant circulation pipe (PL24) be back to extraction tower (T1) top extraction tower into
Material mouth is recycled；
Step S4: the extraction phase at the top of extraction tower (T1) enters toluene treating column by extraction tower extraction phase discharge nozzle (PL6)
(T4) rectifying is carried out, the steam that toluene treating column (T4) tower top rises realizes phase transformation through condenser (E6), condenses the material of acquisition
A part passes back into tower from the refluxing opening at the top of toluene treating column (T4), and another part is from adopting at the top of toluene treating column (T4)
Outlet produces pipe (PL27) through toluene refined tower top and enters ethyl acetate treating column (T5), and toluene treating column (T4) tower reactor obtains
Product through toluene treating column tower reactor produce pipe (PL30) go out system；
Step S5: the material of extraction mouth enters ethyl acetate treating column (T5) progress rectifying at the top of toluene treating column (T4),
The steam that ethyl acetate treating column (T5) tower top rises realizes phase transformation through condenser (E8), condenses material a part of acquisition from second
Ethyl acetate treating column refluxing opening at the top of acetoacetic ester treating column (T5) passes back into tower, and another part is from ethyl acetate treating column
(T5) the azeotropic mixture circulation ethyl acetate treating column extraction mouth at the top of produces pipe (PL33) through ethyl acetate refined tower top and enters
Ethyl acetate treating column quantizer (V2) layering, lower layer's water phase pass through ethyl acetate treating column quantizer water phase discharge nozzle (PL34)
Discharge system, upper oil phase are back to the lower part extraction tower (T1) by ethyl acetate treating column quantizer oil phase discharge nozzle (PL35)
Feed inlet is recycled, and the product that ethyl acetate treating column (T5) kettle obtains produces pipe (PL39) through ethyl acetate treating column tower reactor
System out.
10. method of the separation containing mixed solvents such as toluene, ethyl acetate and ethyl alcohol according to claim 9, feature exist
In: the extractant is water；
Operating condition setting in the extraction tower (T1) are as follows: tower top pressure is normal pressure, and operation temperature is room temperature, from total extractant
Feed pipe enter extractant with from total mixed solvent feed pipe enter mixed acid waste water volume ratio be 0.4-1.2, under
It is 1.0~4.0 that portion, which recycles the discharging volume of discharge port and the input material volume ratio of the extractant entered from total extractant feed pipe,；
Operating condition setting in the ethyl alcohol lightness-removing column (T2) are as follows: tower top pressure is normal pressure, and tower top temperature is 66-73 DEG C, tower
Kettle temperature degree is 80-90 DEG C, and overhead reflux ratio is 1.2-4.5；
Operating condition setting in the alcohol product tower (T3) are as follows: tower top pressure is normal pressure, and tower top temperature is 77-80 DEG C, tower
Kettle temperature degree is 99-101 DEG C, and overhead reflux ratio is 1.8-8.0；
Operating condition setting in the toluene treating column (T4) are as follows: tower top pressure is normal pressure, and tower top temperature is 73-79 DEG C, tower
Kettle temperature degree is 112-118 DEG C, and overhead reflux ratio is 1.0-5.0；
Operating condition setting in the ethyl acetate treating column (T5) are as follows: tower top pressure is normal pressure, tower top temperature 67-73
DEG C, bottom temperature is 75-79 DEG C, and overhead reflux ratio is 2.0-7.0.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811286607.5A CN109111337B (en) | 2018-10-31 | 2018-10-31 | Separation equipment and method for mixed solvent containing toluene, ethyl acetate, ethanol and the like |
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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 |
| CN115304458A (en) * | 2022-07-08 | 2022-11-08 | 陕西延长石油（集团）有限责任公司 | System and process for separating and refining acetaldehyde prepared by ethanol dehydrogenation |
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| CN109111337B (en) | 2024-04-09 |
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