CN109956866A - A method of from ethyl acetate and normal heptane are separated and recovered in industry in organic sewage - Google Patents
A method of from ethyl acetate and normal heptane are separated and recovered in industry in organic sewage Download PDFInfo
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- CN109956866A CN109956866A CN201910178902.7A CN201910178902A CN109956866A CN 109956866 A CN109956866 A CN 109956866A CN 201910178902 A CN201910178902 A CN 201910178902A CN 109956866 A CN109956866 A CN 109956866A
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- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- 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
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Abstract
The invention discloses a kind of methods for separating and recovering ethyl acetate and normal heptane, belong to field of environment protection.The present invention is to the ethyl acetate and normal heptane organic liquid waste generated in the production processes such as the fields such as chemical industry, weaving, paint and pharmacy, using the tert-butyl alcohol as entrainer through sequence of constant boiling and rectification, the simple process separated using heat pump compression rectification and heat pump rectification under vacuum, obtain the ethyl acetate and normal heptane of high-purity, simultaneously, it converts high-grade heat source for the low-grade heat source of system to utilize again for internal process, to reach energy-efficient purpose.The present invention has simple process, easy to operate；Process continuity is strong, and controllability is high, and low energy consumption；The purity is high of product, impurity are few；Can Resource Recycling Utilization, no exhaust gas, waste liquid and waste sludge discharge, be good for the environment with it is energy saving.The recycling that present invention can be widely used to organic liquid waste in industry, especially suitable for the recycling of the ethyl acetate and normal heptane waste liquid that are generated in large, medium and small type enterprise production process.
Description
Technical field
The invention belongs to field of environment protection, and in particular to a kind of separation and recovery ethyl acetate and normal heptane azeotropic mixture
Method.
Background technique
The preferable solubility property that ethyl acetate and normal heptane have, often by as mixed solvent be applied to chemical industry, weaving,
The fields such as paint and pharmacy, to generate the largely organic liquid waste containing ethyl acetate and normal heptane.Due to ethyl acetate and
Normal heptane forms minimum binary azeotrope under normal pressure, and (azeotropic temperature is 76.18 DEG C, 83wt% containing ethyl acetate, normal heptane
17wt%), conventional rectificating method can not be efficiently separated.In order to avoid environmental pollution, the circulation benefit of resource is realized
With how the waste liquid containing ethyl acetate and normal heptane being efficiently separated, to obtain the product of high-purity, at environmentally friendly work
One of hot spot of author investigation.
It is using N-Methyl pyrrolidone as extractant, to batch extracting rectified separating acetic acid ethyl ester and positive heptan in existing literature
The feasibility and influence factor of alkane azeotropic system are tested, and continuous extraction distillation process is simulated and is optimized.
The result shows that: the number of theoretical plate of extractive distillation column is 34 pieces, and extractant feed position is the 9th block of plate, and solvent ratio is 2.0, reflux
Than being 1.0, the product purity of isolated normal heptane is 98.3%, the rate of recovery 73.4%.The major defect of the method is:
(1) ethyl acetate and normal heptane can not be recycled simultaneously；(2) process controllability is weak；(3) the horizontal impurities affect to product of operation compared with
Greatly；(4) toxicity of extractant is bigger, increases residual risk；(5) dosage of extractant is big, at high cost.
Summary of the invention
The object of the present invention is to provide a kind of from the side for separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method includes condenser, return tank, force (forcing) pump, compressor I, buffering by being sent into containing the organic liquid waste of ethyl acetate and normal heptane
Tank I, compressor II, circulating pump, surge tank II, sequence of constant boiling and rectification tower, kettle type reboiler I, kettle type reboiler II, pressurizing tower, Quan Ning
The processing system of device I, kettle type reboiler III, vacuum tower, complete condenser II and entrainer circulating pump.
It is worth noting that the present invention can form new azeotropic mixture using the tert-butyl alcohol and ethyl acetate, and azeotropic point compares second
Acetoacetic ester/normal heptane azeotropic mixture azeotropic point is low and the pressure-sensitive character of the tert-butyl alcohol and ethyl acetate azeotrope, using azeotropic essence
It evaporates, heat pump compression rectification and heat pump rectification under vacuum efficiently separate ethyl acetate and normal heptane；Meanwhile by the low of system
Grade heat source is converted into high-grade heat source and utilizes again for internal process, to reach energy-efficient purpose.The technology effectively solves
It is difficult that ethyl acetate and normal heptane form Azeotrope separation, and the problem of can not recycle two kinds of products simultaneously, has process flow
Simply, the features such as controllability is strong, and equipment investment is few, easy to maintenance, pollution-free and energy saving.Concrete processing procedure such as S1~S3:
S1) sequence of constant boiling and rectification
S1-1) organic liquid waste by waste liquid feeding pipe be sent into sequence of constant boiling and rectification tower.
Meanwhile the entrainer tert-butyl alcohol is sent into sequence of constant boiling and rectification tower by solvent feed pipeline together.
S1-2) in the isolated normal heptane liquid phase stream of sequence of constant boiling and rectification tower tower bottom, portion of n-heptane liquid phase stream is through pipe
Road is delivered to kettle type reboiler I, after low pressure water vapor is heated as saturated vapor, the liquid that is flowed down with sequence of constant boiling and rectification column overhead
Contact mass transfer step by step, another part are then used as normal heptane product to produce by pipeline.
S1-3) in sequence of constant boiling and rectification column overhead ethyl acetate/tert-butyl alcohol azeotropic mixture vapor phase stream is obtained, pass through Pipeline transport
It is condensed to condenser, by condensed liquid after pipeline to return tank storage, partially liq is flowed back by pipeline
To sequence of constant boiling and rectification column overhead, is contacted with the steam step-by-step that tower bottom rises and carry out mass transfer, another part enters force (forcing) pump.
S2) heat pump compression rectification
S2-1) another part liquid described in S1-3) is pressurizeed by force (forcing) pump after, be delivered to by feeding pipe plus
Press tower.
Meanwhile the azeotropic liquid phase stream of the tert-butyl alcohol and ethyl acetate in S3-3) being passed through to the condensate liquid of circulating pump pressurization,
Compression rectification is carried out by Pipeline transport to pressurizing tower.
S2-2) in the isolated ethyl acetate liquid phase logistics of pressurizing tower tower bottom, portion of ethyl acetate liquid phase stream is by pipe
Road is delivered to kettle type reboiler II, is vaporized into saturated vapor by heat source heating, rising is contacted step by step with liquid in pressurizing tower
Mass transfer, another part ethyl acetate liquid phase logistics are produced as ethyl acetate product by pipeline.
S2-3) in the azeotropic vapor phase stream of pressurization column overhead isolated ethyl acetate and the tert-butyl alcohol, it is delivered to by the road
Compressor I after compression, obtains superheated steam.Superheated steam is through pipeline to tower bottom kettle type reboiler II, as heat source by kettle
Then acetic acid ethyl fluid heat phase in formula reboiler II obtains after complete condenser I is by vapour phase all condensation again at saturated vapor
The azeotropic liquid phase stream of ethyl acetate and the tert-butyl alcohol.
The azeotropic liquid phase stream of portion of ethyl acetate and the tert-butyl alcohol is sent to pressurizing tower tower after being transported to surge tank I by the road
Top carries out contact mass transfer with the vapor phase stream that tower bottom rises.The azeotropic liquid phase stream of another part ethyl acetate and the tert-butyl alcohol into
Enter vacuum tower.
S3) heat pump rectification under vacuum
S3-1) by the azeotropic liquid phase stream of another part ethyl acetate and the tert-butyl alcohol described in S2-3) be sent into vacuum tower into
Row rectifying separation.
S3-2) in the isolated tert-butyl alcohol liquid phase stream of vacuum tower bottoms.Part tert-butyl alcohol liquid phase stream is defeated by pipeline
It send to kettle type reboiler III and saturated vapor is vaporized by heat source heating, contacted step by step with liquid in vacuum tower tower and carry out mass transfer, separately
A part of tert-butyl alcohol liquid phase stream is produced as tert-butyl alcohol product by pipeline, and is sent into sequence of constant boiling and rectification after circulating pump pressurizes
Tower is recycled.
S3-3) in the azeotropic vapor phase stream of decompression the column overhead isolated tert-butyl alcohol and ethyl acetate, it is transported to by the road
After compressor II compression, superheated steam is obtained, tower bottom kettle type reboiler III is transported to, as heat source by the liquid phase of tower bottom
Tert-butyl alcohol heating, then after complete condenser II is condensed, the azeotropic liquid phase stream of the part tert-butyl alcohol and ethyl acetate conveys by the road
It is sent to decompression column overhead after to surge tank II, carries out contact mass transfer with the vapor phase stream that tower bottom rises.Another part tert-butyl alcohol
With the azeotropic liquid phase stream of ethyl acetate then after circulating pump pressurizes, send to compression rectification tower, continue circulation pressurization essence
It evaporates.
Further, S1-1) in, the organic liquid waste is the waste liquid generated in certain enterprise production process, contains acetic acid second
Ester 60mol%~80mol%, normal heptane 20mol%~40mol%, molar flow 1000kmol/h.
Entrainer tert-butyl alcohol molar flow is 428kmol/h~573kmol/h.
The feed entrance point of organic liquid waste is the 30th block of column plate.The feed entrance point of the entrainer tert-butyl alcohol is the 14th~20 piece of tower
Plate, the absolute pressure of sequence of constant boiling and rectification tower operation are 0.1MPa, and total number of plates is 40~50, and operating reflux ratio is 5.5~6.96.
Further, S1-2) in, the isolated temperature of sequence of constant boiling and rectification tower tower bottom is 106.45~108.39 DEG C of normal heptane liquid
Phase logistics.
Further, S1-3) in, condensed fluid temperature is 72.99~73.01 DEG C.
Further, S2-1) in, the partially liq of return tank storage is forced into 0.23~0.45MPa by force (forcing) pump, passes through
Feeding pipe is delivered to the 19th~20 block of column plate of pressurizing tower.
The azeotropic liquid phase stream of the tert-butyl alcohol and ethyl acetate in S3-3) is forced into 0.23 by circulating pump~
The condensate liquid of 0.45MPa carries out compression rectification, by ethyl acetate by the 22nd~23 block of column plate of Pipeline transport to pressurizing tower
It is separated with ethyl acetate/tert-butyl alcohol azeotropic mixture under pressurization, the absolute operating pressures of pressurizing tower are 0.2~0.4MPa, always
The number of plates is 39~41, and operating reflux ratio is 0.999~1.2.
Further, S2-2) in, the acetic acid ethyl fluid for being 103.82~128.6 DEG C in the isolated temperature of pressurizing tower tower bottom
Phase logistics.
Further, S2-3) in, after compressor I is compressed with compression ratio for 5~10, obtaining temperature is 144.8~191
DEG C superheated steam.
Further, S3-1) in, the azeotropic liquid phase stream of portion of ethyl acetate and the tert-butyl alcohol is sent into the 20th~21 of vacuum tower the
The tert-butyl alcohol under the tert-butyl alcohol and decompression is carried out rectifying with ethyl acetate azeotrope and separated by block column plate, the absolute operation of vacuum tower
Pressure is 0.10MPa, and total theoretical cam curve is 39~41 pieces, and operating reflux ratio is 1~1.2.
Further, S3-2) in, the tert-butyl alcohol liquid phase object for being 88.26~88.3 DEG C in the isolated temperature of vacuum tower bottoms
Stream.
Further, S3-3) in, compressor II is compressed with 2.3 compression ratio, and obtaining temperature is 99.4~99.6 DEG C
Superheated steam.
It is mainly had the following effects after the invention adopts the above technical scheme:
(1) purity is high of product, impurity is few, can be with direct circulation reuse.It can be by ethyl acetate using the technology of the present invention
It is efficiently separated with the organic liquid waste of normal heptane, the purity for obtaining normal heptane product is 99.89%~99.92%, and ethyl acetate produces
The purity of product is 98.95%~99.09%, can be with direct circulation reuse.
(2) purity of the isolated entrainer tert-butyl alcohol is very high, and it is useless can be directly recycled for ethyl acetate/normal heptane
It can be the effectively save cost of enterprise in the recovery process of liquid.The technology of the present invention is using the tert-butyl alcohol as entrainer, tert-butyl alcohol energy
The pressure-sensitive that lower azeotropic mixture and the tert-butyl alcohol and ethyl acetate azeotrope are formed with ethyl acetate, using sequence of constant boiling and rectification, heat
Compression rectification and heat pump rectification under vacuum separation are pumped, the tert-butyl alcohol of high-purity can be obtained；It avoids and introduces a large amount of expensive extractions
Contamination of products caused by agent and cost problem are taken, the purity of the obtained entrainer tert-butyl alcohol is 98.78%~98.93%, can
To be directly recycled in the recovery process of ethyl acetate and normal heptane waste liquid.
(3) process flow is simple and easy, and labor intensity is small, easy to operate, and equipment used is simple, and cost performance is high, practical
Strong, the great industry application of property.The sequence of constant boiling and rectification being related in the method for the present invention, heat pump compression rectification and heat pump decompression essence
It the processes such as evaporates and for ease of maintenaince, and equipment is conducive to extend without obvious loss to device therefor to the of less demanding of equipment
Service life reduces production cost.
(4) technical process continuity is strong, and controllability is high, and low energy consumption.The technical process being related in the method for the present invention is to connect
Continuous production, various technic indexs such as temperature, pressure, liquid level and purity etc. are easily controllable, efficiently solve product purity and operated
The problem of level influences, improves the utilization rate of equipment.Meanwhile using heat pump by compression rectification tower and rectification under vacuum column overhead
Steam stream carries out second compression again, and low-grade energy is transformed into high-grade energy, heats the cold object at two rectifying tower bottoms
Stream, realizes the recycling of energy, greatly reduces process energy consumption, technique can save 187.74~224.44MW of heat source.
(5) resource is made full use of, is conducive to protect environment.A kind of separation and recovery ethyl acetate of the method for the present invention and normal heptane
In the method for azeotropic mixture, the group of the organic liquid waste of involved ethyl acetate and normal heptane, which becomes, contains ethyl acetate
60mol%~80mol%, normal heptane 20mol%~40mol%, after treatment ethyl acetate purity be 98.95%~
99.09%, the purity of normal heptane is 99.89%~99.92%, meanwhile, the entrainer tert-butyl alcohol recycled in technical process
Purity is 98.78%~98.93%.Usually by isolated ethyl acetate and normal heptane, it is recycled to be used in target product
Production process, the tert-butyl alcohol of separated obtained high-purity, can be used as folder boiling agent be recycled to be used in ethyl acetate and
In the separating technology of normal heptane waste liquid.This production process is discharged without waste liquid, waste residue and exhaust gas, so that organic liquid waste resource obtains
It makes full use of, is conducive to protect environment.
The recycling that present invention can be widely used to organic liquid waste in industry, it is raw especially suitable for large, medium and small type enterprise
The recycling of the ethyl acetate and normal heptane waste liquid that are generated during producing.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
In figure: condenser (1), return tank (2), force (forcing) pump (3), compressor I (4), surge tank I (5), compressor II (6),
Circulating pump (7), surge tank II (8), sequence of constant boiling and rectification tower (9), kettle type reboiler I (10), kettle type reboiler II (11), pressurizing tower
(12), complete condenser I (13), kettle type reboiler III (14), vacuum tower (15), complete condenser II (16), entrainer circulating pump (17).
Specific embodiment
Below with reference to embodiment, the invention will be further described, but should not be construed the above-mentioned subject area of the present invention only
It is limited to following embodiments.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and used
With means, various replacements and change are made, should all include within the scope of the present invention.
It include condensation by being sent into containing the organic liquid waste of ethyl acetate and normal heptane in the examples below referring to attached drawing
Device (1), return tank (2), force (forcing) pump (3), compressor I (4), surge tank I (5), compressor II (6), circulating pump (7), surge tank
II (8), sequence of constant boiling and rectification tower (9), kettle type reboiler I (10), kettle type reboiler II (11), pressurizing tower (12), complete condenser I (13),
The processing system of kettle type reboiler III (14), vacuum tower (15), complete condenser II (16) and entrainer circulating pump (17) are specific to locate
S1~S3 of for example each embodiment of reason process.
Embodiment 1:
S1) sequence of constant boiling and rectification
S1-1) organic liquid waste is the waste liquid that generates in certain enterprise production process, contain ethyl acetate 60mol%, normal heptane
40mol%, molar flow 1000kmol/h are sent into sequence of constant boiling and rectification tower (9) by waste liquid feeding pipe；
Meanwhile the entrainer tert-butyl alcohol that molar flow is 428kmol/h is sent into azeotropic by solvent feed pipeline together
Rectifying column (9)；The tert-butyl alcohol is from S3-2) in the logistics that is recycled, and the logistics supplemented in molar flow deficiency.
The feed entrance point of organic liquid waste is the 30th block of column plate；The feed entrance point of the entrainer tert-butyl alcohol is the 20th block of column plate, permanent
The absolute pressure for boiling rectifying column (9) operation is 0.1MPa, and total number of plates is 50, operating reflux ratio 6.96.
S1-2) it in the isolated temperature of sequence of constant boiling and rectification tower (9) tower bottom is 108.39 DEG C of normal heptane liquid phase stream, part is just
Heptane liquid phase stream is through pipeline to kettle type reboiler I (10), after low pressure water vapor is heated as saturated vapor, with azeotropic
Contact mass transfer, another part are then used as normal heptane product to produce by pipeline to liquid under rectifying column (9) tower top stream step by step；Point
Product purity from obtained normal heptane reaches 99.90%.
S1-3) in sequence of constant boiling and rectification tower (9) tower top ethyl acetate/tert-butyl alcohol azeotropic mixture vapor phase stream is obtained, pass through pipeline
It is transported to condenser (1) to be condensed, condensed fluid temperature is 73 DEG C, by condensed liquid through pipeline to reflux
After tank (2) storage, partially liq is back to sequence of constant boiling and rectification tower (9) tower top by pipeline, and the steam step-by-step risen with tower bottom contacts
Mass transfer is carried out, another part enters force (forcing) pump (3)；
S2) heat pump compression rectification
S2-1) partially liq of return tank (2) storage is forced into 0.33MPa by force (forcing) pump (3), and it is defeated by feeding pipe
It send to the 19th block of column plate of pressurizing tower (12)；
Meanwhile by the condensate liquid for being forced into 0.33MPa by circulating pump (7) in S3-3), pass through Pipeline transport to pressurization
23rd block of column plate of tower (12) carries out compression rectification, and the ethyl acetate under ethyl acetate and pressurization/tert-butyl alcohol azeotropic mixture is carried out
Separation, the absolute operating pressures of pressurizing tower (12) are 0.3MPa, and total number of plates is 40, operating reflux ratio 1.2.
S2-2) it in the isolated temperature of pressurizing tower (12) tower bottom is 117.71 DEG C of ethyl acetate liquid phase logistics, part second
Acetoacetic ester liquid phase stream to kettle type reboiler II (11), is vaporized into saturated vapor by heat source heating by Pipeline transport, rise with
Contact mass transfer, another part ethyl acetate liquid phase logistics pass through the interior liquid progress of pressurizing tower (12) as ethyl acetate product step by step
Pipeline extraction；
S2-3) in the azeotropic vapor phase stream of pressurizing tower (12) tower top isolated ethyl acetate and the tert-butyl alcohol, it is defeated by the road
It send to compressor I (4), after being compressed with compression ratio for 7, obtains the superheated steam that temperature is 168.9 DEG C；Superheated steam is through pipe
Road is delivered to tower bottom kettle type reboiler II (11), as heat source by the acetic acid ethyl fluid heat phase in kettle type reboiler II (11) at
Then saturated vapor obtains the azeotropic liquid phase object of ethyl acetate and the tert-butyl alcohol after complete condenser I (13) is by vapour phase all condensation again
Stream；
The azeotropic liquid phase stream of portion of ethyl acetate and the tert-butyl alcohol is sent to pressurization after being transported to surge tank I (5) by the road
Tower (12) tower top carries out contact mass transfer with the vapor phase stream that tower bottom rises；The azeotropic liquid of another part ethyl acetate and the tert-butyl alcohol
Phase logistics enters vacuum tower (15)；
S3) heat pump rectification under vacuum
S3-1) the azeotropic liquid phase stream of portion of ethyl acetate and the tert-butyl alcohol is sent into the 21st block of column plate of vacuum tower (15), and it will
The tert-butyl alcohol under the tert-butyl alcohol and decompression carries out rectifying with ethyl acetate azeotrope and separates, and the absolute operating pressures of vacuum tower (15) are
0.10MPa, total theoretical cam curve are 39 pieces, operating reflux ratio 1.2.
S3-2) it in the isolated temperature in vacuum tower (15) bottom is 88.26 DEG C of tert-butyl alcohol liquid phase stream；The part tert-butyl alcohol
Liquid phase stream is vaporized into saturated vapor by heat source heating by Pipeline transport to kettle type reboiler III (14), with vacuum tower (15)
Liquid contacts step by step in tower carries out mass transfer, and another part tert-butyl alcohol liquid phase stream is produced as tert-butyl alcohol product by pipeline, and
Sequence of constant boiling and rectification tower (9) are sent into after circulating pump (17) pressurization, are recycled；
S3-3) in the azeotropic vapor phase stream of vacuum tower (15) tower top isolated tert-butyl alcohol and ethyl acetate, it is defeated by the road
Compressor II (6) are sent to, after being compressed with 2.3 compression ratio, the superheated steam that temperature is 99.4 DEG C is obtained, is transported to
The liquid phase tert-butyl alcohol of tower bottom is heated as heat source, then is condensed through complete condenser II (16) by tower bottom kettle type reboiler III (14)
Afterwards, the azeotropic liquid phase stream of the part tert-butyl alcohol and ethyl acetate is sent to vacuum tower after being transported to surge tank II (8) by the road
(15) tower top carries out contact mass transfer with the vapor phase stream that tower bottom rises；The azeotropic liquid phase of another part tert-butyl alcohol and ethyl acetate
Logistics then after circulating pump (7) pressurization, is sent to compression rectification tower (12) (such as S2-1), continues compression rectification.It separates
Purity to the entrainer tert-butyl alcohol is 98.78%, can save heat source 82.8MW.
Embodiment 2:
The present embodiment major part leads to embodiment 1, unlike:
S1-1) organic liquid waste contains ethyl acetate 70mol%, normal heptane 30mol%, molar flow 1000kmol/h；
Entrainer tert-butyl alcohol molar flow is 500.61kmol/h；
The feed entrance point of organic liquid waste is the 30th block of column plate；The feed entrance point of the entrainer tert-butyl alcohol is the 14th block of column plate, permanent
The absolute pressure for boiling rectifying column (9) operation is 0.1MPa, and total number of plates is 40, operating reflux ratio 5.8.
S1-2) it in the isolated temperature of sequence of constant boiling and rectification tower (9) tower bottom is 106.45 DEG C of normal heptane liquid phase stream.
S1-3) condensed fluid temperature is 73 DEG C；The product purity of isolated normal heptane reaches 99.92%.
S2-1) partially liq of return tank (2) storage is forced into 0.23MPa by force (forcing) pump (3), and it is defeated by feeding pipe
It send to the 20th block of column plate of pressurizing tower (12)；
Meanwhile by the condensate liquid for being forced into 0.23MPa by circulating pump (7) in S3), pass through Pipeline transport to pressurizing tower
(12) the 22nd block of column plate.The absolute operating pressures of pressurizing tower (12) are 0.2MPa, and total number of plates is 39, and operating reflux ratio is
0.999。
S2-2) it in the isolated temperature of pressurizing tower (12) tower bottom is 103.82 DEG C of ethyl acetate liquid phase logistics；It separates
The purity of the ethyl acetate product arrived is 98.95%, can save heat source 112.04MW.
S2-3) compressor I (4) with compression ratio be 5 compressed after, obtaining temperature is 144.8 DEG C of superheated steam；
S3-1) the azeotropic liquid phase stream of portion of ethyl acetate and the tert-butyl alcohol is sent into the 20th block of column plate of vacuum tower (15), and it will
The tert-butyl alcohol under the tert-butyl alcohol and decompression carries out rectifying with ethyl acetate azeotrope and separates, and the absolute operating pressures of vacuum tower (15) are
0.10MPa, total theoretical cam curve are 40 pieces, operating reflux ratio 1.01.
S3-2) it in the isolated temperature in vacuum tower (15) bottom is 88.3 DEG C of tert-butyl alcohol liquid phase stream.
S3-3) after compressor II (6) compressed with 2.3 compression ratio, obtain the superheated steam that temperature is 99.6 DEG C.
The purity of the isolated entrainer tert-butyl alcohol is 98.87%, can save heat source 92.9MW.
Embodiment 3:
The present embodiment major part leads to embodiment 1, unlike:
S1-1) organic liquid waste contains ethyl acetate 80mol%, normal heptane 20mol%, molar flow 1000kmol/h；
Entrainer tert-butyl alcohol molar flow is 573kmol/h；
The feed entrance point of organic liquid waste is the 30th block of column plate；The feed entrance point of the entrainer tert-butyl alcohol is the 15th block of column plate, permanent
The absolute pressure for boiling rectifying column (9) operation is 0.1MPa, and total number of plates is 44, operating reflux ratio 5.5.
S1-2) it in the isolated temperature of sequence of constant boiling and rectification tower (9) tower bottom is 107 DEG C of normal heptane liquid phase stream.
S1-3) condensed fluid temperature is 73.01 DEG C；The product purity of isolated normal heptane reaches 99.89%.
S2-1) partially liq of return tank (2) storage is forced into 0.45MPa by force (forcing) pump (3), and it is defeated by feeding pipe
It send to the 20th block of column plate of pressurizing tower (12)；
Meanwhile by the condensate liquid for being forced into 0.45MPa by circulating pump (7) in S3), pass through Pipeline transport to pressurizing tower
(12) the 23rd block of column plate carries out compression rectification, and ethyl acetate/tert-butyl alcohol azeotropic mixture under ethyl acetate and pressurization is divided
From the absolute operating pressures of pressurizing tower (12) are 0.4MPa, and total number of plates is 41, operating reflux ratio 1.
S2-2) it in the isolated temperature of pressurizing tower (12) tower bottom is 128.6 DEG C of ethyl acetate liquid phase logistics；
S2-3) compressor I (4) with compression ratio be 10 compressed after, obtaining temperature is 191 DEG C of superheated steam；
The purity of isolated ethyl acetate product is 99.09%, can save heat source 129.73MW.
S3-1) the azeotropic liquid phase stream of portion of ethyl acetate and the tert-butyl alcohol is sent into the 20th block of column plate of vacuum tower (15), and it will
The tert-butyl alcohol under the tert-butyl alcohol and decompression carries out rectifying with ethyl acetate azeotrope and separates, and the absolute operating pressures of vacuum tower (15) are
0.10MPa, total theoretical cam curve are 41 pieces, operating reflux ratio 1.
S3-2) it in the isolated temperature in vacuum tower (15) bottom is 88.26~88.3 DEG C of tert-butyl alcohol liquid phase stream.
S3-3) after compressor II (6) compressed with 2.3 compression ratio, obtain the superheated steam that temperature is 99.4 DEG C.
Above-mentioned case study on implementation of the invention is only example to illustrate the invention, and is not to reality of the invention
Apply the restriction of mode.For those of ordinary skill in the art, other can also be made on the basis of the above description
Various forms of variations and variation.Here all embodiments can not be exhaustive.It is all to belong to technical side of the invention
Case changes and variations that derived from are still in the scope of protection of the present invention.
Claims (10)
1. a kind of from the method for separating and recovering ethyl acetate and normal heptane in industry in organic sewage, it is characterised in that:
It include condenser (1), return tank (2), force (forcing) pump by described be sent into containing the organic liquid waste of ethyl acetate and normal heptane
(3), compressor I (4), surge tank I (5), compressor II (6), circulating pump (7), surge tank II (8), sequence of constant boiling and rectification tower (9), kettle
Formula reboiler I (10), kettle type reboiler II (11), pressurizing tower (12), complete condenser I (13), kettle type reboiler III (14), decompression
The processing system of tower (15), complete condenser II (16) and entrainer circulating pump (17), concrete processing procedure such as S1~S3:
S1) sequence of constant boiling and rectification
S1-1) organic liquid waste by waste liquid feeding pipe be sent into sequence of constant boiling and rectification tower (9)；
Meanwhile the entrainer tert-butyl alcohol is sent into sequence of constant boiling and rectification tower (9) by solvent feed pipeline together；
S1-2) in the isolated normal heptane liquid phase stream of sequence of constant boiling and rectification tower (9) tower bottom, portion of n-heptane liquid phase stream is through pipeline
Kettle type reboiler I (10) are delivered to, after low pressure water vapor is heated as saturated vapor, under 9 tower top stream of sequence of constant boiling and rectification tower
Contact mass transfer, another part are then used as normal heptane product to produce by pipeline to liquid step by step；
S1-3) in sequence of constant boiling and rectification tower (9) tower top ethyl acetate/tert-butyl alcohol azeotropic mixture vapor phase stream is obtained, pass through Pipeline transport
It is condensed to condenser (1), by condensed liquid after pipeline to return tank (2) storage, partially liq passes through pipe
Road is back to sequence of constant boiling and rectification tower (9) tower top, contacts with the steam step-by-step that tower bottom rises and carries out mass transfer, another part enters pressurization
It pumps (3)；
S2) heat pump compression rectification
S2-1) another part liquid described in S1-3) is pressurizeed by force (forcing) pump (3) after, be delivered to by feeding pipe plus
It presses tower (12)；
Meanwhile the azeotropic liquid phase stream of the tert-butyl alcohol and ethyl acetate in S3-3) being passed through to the condensate liquid of circulating pump (7) pressurization,
Compression rectification is carried out by Pipeline transport to pressurizing tower (12).
S2-2) in the isolated ethyl acetate liquid phase logistics of pressurizing tower (12) tower bottom, portion of ethyl acetate liquid phase stream is by pipe
Road is delivered to kettle type reboiler II (11), is vaporized into saturated vapor by heat source heating, rises and carry out with pressurizing tower (12) interior liquid
Contact mass transfer step by step, another part ethyl acetate liquid phase logistics are produced as ethyl acetate product by pipeline；
S2-3) in the azeotropic vapor phase stream of pressurizing tower (12) tower top isolated ethyl acetate and the tert-butyl alcohol, it is delivered to by the road
Compressor I (4), after compression, obtains superheated steam；Superheated steam through pipeline to tower bottom kettle type reboiler II (11), as
Heat source by the acetic acid ethyl fluid heat phase in kettle type reboiler II (11) at saturated vapor, then again through complete condenser I (13) by vapour
Mutually the azeotropic liquid phase stream of ethyl acetate and the tert-butyl alcohol all is obtained after condensation；
The azeotropic liquid phase stream of portion of ethyl acetate and the tert-butyl alcohol is sent to pressurizing tower after being transported to surge tank I (5) by the road
(12) tower top carries out contact mass transfer with the vapor phase stream that tower bottom rises；The azeotropic liquid phase of another part ethyl acetate and the tert-butyl alcohol
Logistics enters vacuum tower (15)；
S3) heat pump rectification under vacuum
S3-1) by the azeotropic liquid phase stream of another part ethyl acetate and the tert-butyl alcohol described in S2-3) be sent into vacuum tower (15) into
Row rectifying separation；
S3-2) in the isolated tert-butyl alcohol liquid phase stream in vacuum tower (15) bottom；Part tert-butyl alcohol liquid phase stream is defeated by pipeline
Send to kettle type reboiler III (14) by heat source heating be vaporized into saturated vapor, with liquid in vacuum tower (15) tower contact step by step into
Row mass transfer, another part tert-butyl alcohol liquid phase stream are produced as tert-butyl alcohol product by pipeline, and after circulating pump (17) pressurization
It is sent into sequence of constant boiling and rectification tower (9), is recycled；
S3-3) in the azeotropic vapor phase stream of vacuum tower (15) tower top isolated tert-butyl alcohol and ethyl acetate, it is transported to by the road
After compressor II (6) compression, superheated steam is obtained, tower bottom kettle type reboiler III (14) is transported to, as heat source by tower bottom
The heating of the liquid phase tert-butyl alcohol, then after complete condenser II (16) is condensed, the azeotropic liquid phase stream of the part tert-butyl alcohol and ethyl acetate
It is sent to vacuum tower (15) tower top after being transported to surge tank II (8) by the road, the vapor phase stream risen with tower bottom carries out contact biography
Matter；The azeotropic liquid phase stream of another part tert-butyl alcohol and ethyl acetate then after circulating pump (7) pressurization, is sent to compression rectification tower
(12), continue to recycle compression rectification.
2. according to claim 1 a kind of from the side for separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method, it is characterised in that:
S1-1) in, the organic liquid waste is the waste liquid generated in certain enterprise production process, containing ethyl acetate 60mol%~
80mol%, normal heptane 20mol%~40mol%, molar flow 1000kmol/h；
Entrainer tert-butyl alcohol molar flow is 428kmol/h~573kmol/h；
The feed entrance point of organic liquid waste is the 30th block of column plate；The feed entrance point of the entrainer tert-butyl alcohol is the 14th~20 block of column plate, permanent
The absolute pressure for boiling rectifying column (9) operation is 0.1MPa, and total number of plates is 40~50, and operating reflux ratio is 5.5~6.96.
3. according to claim 1 or 2 a kind of from separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method, it is characterised in that: S1-2) in, the isolated temperature of sequence of constant boiling and rectification tower (9) tower bottom is 106.45~108.39 DEG C of positive heptan
Alkane liquid phase stream.
4. according to claim 1 or 3 a kind of from separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method, it is characterised in that: S1-3) in, condensed fluid temperature is 72.99~73.01 DEG C.
5. according to claim 1 or 3 a kind of from separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method, it is characterised in that:
S2-1) in, the partially liq of return tank (2) storage is forced into 0.23~0.45MPa by force (forcing) pump (3), passes through charging
Pipeline transport to pressurizing tower (12) the 19th~20 block of column plate；
The azeotropic liquid phase stream of the tert-butyl alcohol and ethyl acetate in S3-3) is forced into 0.23~0.45MPa by circulating pump (7)
Condensate liquid compression rectification is carried out by the 22nd~23 block of column plate of Pipeline transport to pressurizing tower (12), by ethyl acetate and plus
The ethyl acetate of pressure/tert-butyl alcohol azeotropic mixture is separated, and the absolute operating pressures of pressurizing tower (12) are 0.2~0.4MPa, always
The number of plates is 39~41, and operating reflux ratio is 0.999~1.2.
6. according to claim 1 or 3 a kind of from separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method, it is characterised in that: S2-2) in, the acetic acid second for being 103.82~128.6 DEG C in the isolated temperature of pressurizing tower (12) tower bottom
Ester liquid phase stream.
7. according to claim 1 or 3 a kind of from separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method, it is characterised in that: S2-3) in, compressor I (4) with compression ratio be 5~10 compressed after, obtain temperature be 144.8~
191 DEG C of superheated steam.
8. according to claim 1 or 3 a kind of from separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method, it is characterised in that: S3-1) in, the azeotropic liquid phase stream of portion of ethyl acetate and the tert-butyl alcohol is sent into the of vacuum tower (15)
The tert-butyl alcohol under the tert-butyl alcohol and decompression is carried out rectifying with ethyl acetate azeotrope and separated by 20~21 blocks of column plates, vacuum tower (15)
Absolute operating pressures be 0.10MPa, total theoretical cam curve be 39~41 pieces, operating reflux ratio be 1~1.2.
9. according to claim 1 or 3 a kind of from separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method, it is characterised in that: S3-2) in, the tert-butyl alcohol liquid for being 88.26~88.3 DEG C in the isolated temperature in vacuum tower (15) bottom
Phase logistics.
10. according to claim 1 or 3 a kind of from separating and recovering ethyl acetate and normal heptane in industry in organic sewage
Method, it is characterised in that: S3-3) in, compressor II (6) is compressed with 2.3 compression ratio, and obtaining temperature is 99.4~99.6
DEG C superheated steam.
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| CN201910178902.7A CN109956866A (en) | 2019-03-11 | 2019-03-11 | A method of from ethyl acetate and normal heptane are separated and recovered in industry in organic sewage |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110903193A (en) * | 2019-12-21 | 2020-03-24 | 山东科技大学 | Method for separating azeotrope of n-heptane and ethyl acetate by extractive distillation |
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| CN107011171A (en) * | 2017-04-14 | 2017-08-04 | 长江师范学院 | The system and method for variable-pressure rectification separating ethyl acetate and n-hexane azeotropic system |
| CN107641083A (en) * | 2017-11-13 | 2018-01-30 | 西南石油大学 | A kind of power-saving technology of azeotropic joint variable-pressure rectification separating ethyl acetate and n-hexane |
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| CN107641083A (en) * | 2017-11-13 | 2018-01-30 | 西南石油大学 | A kind of power-saving technology of azeotropic joint variable-pressure rectification separating ethyl acetate and n-hexane |
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