CN106542990A - A kind of method and system of the recovery of acetic acid from aqueous acetic acid - Google Patents
A kind of method and system of the recovery of acetic acid from aqueous acetic acid Download PDFInfo
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- CN106542990A CN106542990A CN201610891772.8A CN201610891772A CN106542990A CN 106542990 A CN106542990 A CN 106542990A CN 201610891772 A CN201610891772 A CN 201610891772A CN 106542990 A CN106542990 A CN 106542990A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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Abstract
The invention discloses a kind of method and system of the recovery of acetic acid from aqueous acetic acid, a kind of method of the recovery of acetic acid from aqueous acetic acid is employed the following technical solutions：Aqueous acetic acid and extractant carry out liquid-liquid extraction operation into extraction tower；Extraction phase distillation column is entered after extraction phase preheating, and tower bottom distillate is product acetic acid, quantizer is entered after overhead fraction condensation；Extraction phase distillation column is entered after raffinate phase preheating, after overhead fraction condensation, quantizer is entered；Tower bottom distillate is waste water；The heavy phase that quantizer is isolated is extractant, and a part returns Liquid-liquid Extraction Processes, and another part is back to extraction phase still-process, and what quantizer was isolated light phase is back to raffinate phase still-process.Processing technological flow of the present invention is simple, and equipment investment expense is low, good reliability, good separating effect, isolates acetic acid purity height, meets industrial raw material acetic acid requirement.
Description
Technical field
The present invention relates to a kind of method and system of the recovery of acetic acid from aqueous acetic acid, belong to fine chemical technology neck
Domain.
Background technology
Acetic acid is a kind of important Organic Chemicals, is widely used in basic organic synthesis, medicine, dyestuff, spice, agriculture
The industries such as medicine.For a long time, from aqueous acetic acid, recovery of acetic acid is constantly subjected to the attention of people, because which is to each relevant industries
Production technology, economic performance, the utilization of resources and environmental protection are all significant.
Research acetic acid recovery method has rectification method, extraction, esterification process, neutralisation, absorption method, membrance separation both at home and abroad at present
Method etc., and the joint of above each method.Conventional distillation method technical maturity, production capacity are big, wish to get high-purity acetic acid, need a lot
The number of plates and very big reflux ratio, greatly, economic effect is poor, is generally used for thick acetic acid concentration for energy consumption.Azeotropic distillation technique
Maturation, production capacity are big, and energy consumption is less, is not suitable for the low acetum of concentration for the treatment of, more economical, the energy when concentration is more than 80%
Consumption is higher, needs the consumption of precise control nonvariant boiling reagent.Extraction fractional distillation is easy to operate, and production capacity is big, and the number of plates is few, is suitable to medium
Concentration aqueous acetic acid, energy consumption are less, it is important to the screening of suitable solvent.Extraction technical maturity, production capacity are big, energy consumption
It is little, but material consumption is larger, and technique is more complicated, is suitable to low concentration region, and high-purity acetic acid to be obtained will also be through azeotropic distillation, and which is main
Problem is that the extracting power of extractant is not strong enough, the easy emulsifying of solvent reclamation, and processing cost is high.Esterification process technical maturity, produces energy
Power is big, is suitable to low dense acetum, and technique is more complicated, produces spent acid etc. and forms secondary pollution.Membrane separation process good separating effect, fits
In low dense acetum, but film price is higher, and renewal cost is expensive, easily rupturable, and changing affects normal production, the less impact of membrane flux
Yield, and because the stability and regeneration issues of film make large-scale industrial production difficult.Neutralisation process is simple, production capacity are little,
During the process of a small amount of low concentration wastewater, acetate is not typically reclaimed.Absorption method process is simple, it is adaptable to the aqueous acetic acid of low concentration,
Less, production capacity is little for adsorption capacity, and absorption subsequent treatment is difficult.
The content of the invention
It is an object of the invention to provide a kind of processing technological flow is simple, equipment investment expense is low, acetic acid separated effect
The good method and system of recovery of acetic acid from aqueous acetic acid.
The method of recovery of acetic acid from aqueous acetic acid of the present invention is adopted the following technical scheme that：One kind is from aqueous acetic acid
The method of middle recovery of acetic acid, comprises the steps：
（A）Liquid-liquid extraction：Dilute acetic acid aqueous solution and extractant carry out extracting operation into extraction tower, extraction tower tower after extracting operation
Bottom is raffinate phase, and extraction column overhead is extraction phase；
（B）Extraction phase distills：Extraction phase distillation column is entered after extraction phase is preheated, extraction phase distillation column tower bottom distillate is product vinegar
Acid, enters quantizer after the condensation of extraction phase overhead fraction；
（C）Raffinate phase distills：Raffinate phase distillation column is entered after raffinate phase is preheated, the condensation of raffinate phase overhead fraction is laggard
Enter quantizer, raffinate phase distillation column tower bottom distillate is waste water；
（D）Extractant is reclaimed：It is light phase for extractant that quantizer is isolated, and a light phase part returns extraction tower and carries out liquid-liquid extraction
Process, another part are back to extraction phase distillation column and carry out extraction phase still-process, and the heavy phase that quantizer is isolated is back to extraction
Remaining phase distillation column carries out raffinate phase still-process.
In step（A）In,In the dilute acetic acid aqueous solution, acetic acid quality concentration is 10% ~ 80%, and extractant is acetic acid isopropyl
The mixture of ester, butanone and hexane, isopropyl acetate mass fraction are 60% ~ 100%, and butanone mass fraction is 0% ~ 25%,
Hexane mass fraction is 0% ~ 15%；Liquid-liquid extraction operating pressure is 0.1 ~ 1.0MPaG, and operation temperature is 30 ~ 50 DEG C.
In step（A）In, the extraction phase at the top of extraction tower out enters extraction phase storage tank, and extraction phase storage tank upper aqueous phase enters
Enter extraction phase one-level preheater, lower liquid and be back to extraction tower；In step（B）In, extraction phase preheating is preheated using two-stage, and one
Level preheating is and raffinate phase overhead fraction heat exchange that temperature of charge is 80 ~ 95 DEG C after two-stage preheating.
In step（B）In, extraction phase distillation column 0 ~ 0.1MPaG of operating pressure；Extraction phase overhead operation temperature is
65 ~ 100 DEG C, extraction phase distillation column bottom of towe operation temperature is 100 ~ 140 DEG C；The condensed temperature of extraction phase overhead fraction
For 20 ~ 40 DEG C.
In step（C）In, raffinate phase preheating is that raffinate phase carries out heat exchange, raffinate phase with raffinate phase distillation column tower bottom distillate
After preheating, temperature is 70 ~ 100 DEG C；Raffinate phase distillation column 0.05 ~ 0.50MPaG of operating pressure, raffinate phase overhead operation temperature
Spend for 65 ~ 95 DEG C, raffinate phase distillation column bottom of towe operation temperature is 95 ~ 110 DEG C；The condensed temperature of raffinate phase overhead fraction
Spend for 20 ~ 40 DEG C.
In step（D）In, light phase capacity of returns is 0.40 ~ 0.70 with extraction phase overhead fraction amount mass ratio.
The system of recovery of acetic acid from aqueous acetic acid of the present invention is adopted the following technical scheme that：One kind is from aqueous acetic acid
The system of middle recovery of acetic acid, including extraction tower, extraction phase distillation column, raffinate phase distillation column and quantizer, on the extraction tower
Portion is connected by extraction phase pipeline with extraction phase distillation column, is connected with quantizer at the top of extraction phase distillation column, under the extraction tower
Portion is connected with raffinate phase distillation column by raffinate phase pipeline, is connected with quantizer, the layering at the top of the raffinate phase distillation column
Light phase pipeline and heavy phase pipeline are connected with device, are connected with the light phase pipeline and are each led into extraction phase distillation column and extraction
Two laterals of tower, the heavy phase pipeline are passed in raffinate phase distillation column.
The extraction phase pipeline is provided with extraction phase storage tank and extraction phase preheater, and extraction phase preheater includes that one-level is preheated
Device and two grades of preheaters, the raffinate phase overhead are connected with the one-level preheater.
The raffinate phase pipeline is provided with raffinate phase storage tank and raffinate phase preheater, the raffinate phase distillation column bottom of towe and extraction
Remaining phase preheater connection.
Extraction phase overhead condenser, the raffinate phase are provided with the top of the extraction phase distillation column and quantizer between
Raffinate phase overhead condenser is provided with and quantizer between at the top of distillation column, what is connected on the light phase pipeline is passed into extraction
The lateral for taking tower is provided with extractant storage tank, and the extraction phase distillation column bottom of towe is provided with reboiler.
Beneficial effects of the present invention make：Method of the present invention gas separation process is short, equipment investment expense is low, operation letter
Single, heat integration is utilized, good reliability, good separating effect, is isolated acetic acid purity height, is met industrial raw material acetic acid requirement.
Description of the drawings
Fig. 1 is a kind of present invention flow chart of embodiment of the method for recovery of acetic acid from aqueous acetic acid；
Fig. 2 is a kind of present invention system diagram of embodiment of the system of recovery of acetic acid from aqueous acetic acid.
In figure, C-01 is extraction tower, and C-02 is extraction phase distillation column, and C-03 is raffinate phase distillation column, and V-01 is extraction phase
Storage tank, V-02 are extractant storage tank, and V-03 is raffinate phase storage tank, and V-04 is quantizer, and P-01 is extractant feed pump, and P-02 is
Extraction phase feed pump, P-03 are extractant storage tank draining pump, and P-04 is raffinate phase feed pump, and P-05 is waste water pump, and P-06 is to divide
The light phase pump of layer device, P-07 are quantizer heavy phase pump, and E-01 is one-level preheater, and E-02 is two grades of preheaters, and E-03 is extraction phase
Overhead condenser, E-04 are reboiler, and E-05 is raffinate phase preheater, and E-06 is that raffinate phase overhead is condensed
Device.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
As depicted in figs. 1 and 2, present invention method of recovery of acetic acid from aqueous acetic acid is realized by following steps：
（A）Liquid-liquid extraction：Mass concentration is that 10% ~ 80% aqueous acetic acid and extractant carry out liquid liquid extraction into extraction tower C-01
Extract operation.Extractant is the mixture of a certain proportion of isopropyl acetate, butanone and hexane, and isopropyl acetate mass fraction is
60% ~ 100%, butanone mass fraction is 0% ~ 25%, and hexane mass fraction is 0% ~ 15%.Liquid-liquid extraction operating pressure be 0.1 ~
1.0MPaG, preferably 0.2 ~ 0.4MpaG；Operation temperature is 30 ~ 50 DEG C, preferably 37 ~ 43 DEG C.At the top of extraction tower C-01 out
Extraction phase enters extraction phase storage tank V-01, and extraction phase storage tank V-01 upper aqueous phase Jing extraction phase feed pumps P-02 enters extraction phase one
Level preheater E-01, lower liquid Jing extractant storage tank draining pump P-03 are back to extraction tower C-01, and extraction tower C-01 bottoms go out
The raffinate phase for coming enters raffinate phase storage tank V-03.
（B）Extraction phase distills：Two grades of preheater E-02 preheatings of extraction phase Jing extraction phases one-level preheater E-01 and extraction phase
Temperature is 80 ~ 95 DEG C afterwards, and wherein one-level preheating is and raffinate phase distillation column C-03 overhead fraction heat exchanges, extraction phase Jing extraction phases
Extraction phase distillation column C-02 is entered after two grades of preheater E-02 preheatings.Extraction phase distillation column C-02 0 ~ 0.1MPaG of operating pressure, it is excellent
Elect 0.005 ~ 0.02MPaG as；Extraction phase distillation column C-02 bottom of towe arranges reboiler E-04, extraction phase overhead operation temperature
Spend for 65 ~ 100 DEG C, extraction phase distillation column bottom of towe operation temperature is 100 ~ 140 DEG C.Extraction phase distillation column C-02 tower bottom distillates are product
Product acetic acid, extraction phase overhead fraction are entered Jing after extraction phase overhead condenser E-03 is condensed to 20 ~ 40 DEG C and are divided
Layer device V-04.
（C）Raffinate phase distills：Material Jing raffinate phase feed pumps P-04 in raffinate phase storage tank V-03 is preheated into raffinate phase
There is heat exchange with raffinate phase distillation column C-03 tower bottom distillates in device E-05, after preheating, temperature is 70 ~ 100 DEG C and steams into raffinate phase
Evaporate tower C-03.Raffinate phase distillation column 0.05 ~ 0.50MPaG of operating pressure, preferably 0.20 ~ 0.40MPaG；Raffinate phase distillation column tower
Top operation temperature is 65 ~ 95 DEG C, and raffinate phase distillation column bottom of towe operation temperature is 95 ~ 110 DEG C.Raffinate phase distillation column C-03 tower tops evaporate
Point condense to temperature into the preheater E-01 heat exchanges of extraction phase one-level and raffinate phase overhead condenser E-06 is 20 ~ 40
Quantizer V-04 is entered after DEG C；Raffinate phase distillation column C-03 tower bottom distillates be waste water, Jing raffinate phase preheater E-05 heat exchanges return
Discharge after receiving waste heat.
（D）Extractant is reclaimed：Quantizer V-04 isolate it is light phase for extractant, heavy phase be raffinate phase, it is light phase separated
The light phase pump P-06 parts of device are sent into extractant storage tank V-02, another part and are back to extraction phase distillation column C-02, light phase backflow
Amount is 0.40 ~ 0.70 with extraction phase overhead fraction amount mass ratio, and the heavy phase that quantizer V-04 is isolated is separated to think highly of
Phase pump P-07 is back to raffinate phase storage tank V-03.
Embodiment 1
Mass concentration is 30% aqueous acetic acid 50000kg/h and extractant（Extractant is isopropyl acetate, butanone and
The mixture of alkane, wherein isopropyl acetate mass fraction are 85.00%, and butanone mass fraction is 6.50%, hexane mass fraction
For 8.50%）71500kg/h carries out liquid-liquid extraction operation into extraction tower C-01, controls extraction tower C-01 operating pressures and is
0.30MPaG, temperature are 40 DEG C.Extraction phase 96985kg/h at the top of extraction tower C-01 out enters extraction phase storage tank V-01, extraction
Phase storage tank V-01 upper aqueous phases 92330kg/h is taken into extraction phase one-level preheater E-01, lower liquid 4655kg/h Jing extractions
Agent storage tank draining pump P-03 is back to extraction tower C-01.Extraction tower C-01 bottoms raffinate phase 29170kg/h out enters raffinate
Phase storage tank V-03.Extraction phase 92330kg/h is Jing after two grades of preheater E-02 preheatings of extraction phase one-level preheater E-01 and extraction phase
Temperature is 91 DEG C, and wherein one-level preheating is and raffinate phase distillation column C-03 overhead fraction heat exchanges, two grades of extraction phase Jing extraction phases
Enter extraction phase distillation column C-02 after preheater E-02 preheatings, control extraction phase distillation column C-02 operating pressures 0.06 ~
0.09MPaG, extraction phase distillation column C-02 bottom of towe arranges reboiler E-04, and tower top operation temperature is 73 DEG C, and bottom of towe operation temperature is
122℃.Extraction phase distillation column C-02 tower bottom distillates are that acetic acid quality concentration is 99.80 % product acetic acid 14992kg/h, and tower top evaporates
Divide 141963kg/h that quantizer V-04 is entered Jing after extraction phase overhead condenser E-03 is condensed to 30 DEG C.Raffinate phase storage tank
Material 35955kg/h Jing raffinate phase feed pumps P-04 in V-03 enters raffinate phase preheater E-05 and raffinate phase distillation column C-03
There is heat exchange in tower bottom distillate, after preheating, temperature is 85 DEG C and enters raffinate phase distillation column C-03.Raffinate phase distillation column operation pressure
Power 0.20MPaG；Tower top operation temperature is 89 DEG C, and bottom of towe operation temperature is 101 DEG C.Raffinate phase distillation column C-03 overhead fractions (have
Machine amount of substance content enters the preheater E-01 heat exchanges of extraction phase one-level and raffinate phase overhead for 66.26%) 1122kg/h
Condenser E-06 is condensed to temperature as quantizer V-04 is entered after 31 DEG C；Raffinate phase distillation column C-03 tower bottom distillates (have for waste water
Machine amount of substance content is 1.41%) 34833kg/h, discharges Jing after raffinate phase preheater E-05 heat exchange recovery waste heats.Quantizer V-
04 isolate it is light phase for extractant 136227kg/h, the light phase pump P-06 parts of light phase layered device send into extractant storage tank V-
02nd, another part is back to extraction phase distillation column C-02, and light phase capacity of returns with extraction phase overhead fraction amount mass ratio is
0.46, heavy phase 6858kg/h that quantizer V-04 is isolated is back to raffinate phase storage tank V-03.Process cycles extractant in process
Can be lossy, it is 75kg/h to supplement extraction dosage.Recovery rate is 99.79%.
Embodiment 2
Mass concentration is 50% aqueous acetic acid 60000kg/h and extractant（Extractant is isopropyl acetate, butanone and
The mixture of alkane, wherein isopropyl acetate mass fraction are 85.00%, and butanone mass fraction is 6.50%, hexane mass fraction
For 8.50%）85800kg/h carries out liquid-liquid extraction operation into extraction tower C-01, controls extraction tower C-01 operating pressures and is
0.30MPaG, temperature are 40 DEG C.Extraction phase 119798 at the top of extraction tower C-01 out enters extraction phase storage tank V-01, extraction phase
Storage tank V-01 upper aqueous phases 114985kg/h enters extraction phase one-level preheater E-01, and lower liquid 4813kg/h Jing pumps P-03 is returned
It flow to extraction tower C-01.Extraction tower C-01 bottoms raffinate phase 29170kg/h out enters raffinate phase storage tank V-03.Extraction phase
92330kg/h temperature Jing after two grades of preheater E-02 preheatings of extraction phase one-level preheater E-01 and extraction phase is 90 DEG C, wherein one
Level preheating is and raffinate phase distillation column C-03 overhead fraction heat exchanges that the two grades of preheater E-02 preheatings of extraction phase Jing extraction phases are laggard
Enter extraction phase distillation column C-02, control extraction phase distillation column C-02 0.06 ~ 0.09MPaG of operating pressure, extraction phase distillation column C-02
Bottom of towe arranges reboiler E-04, and tower top operation temperature is 70 DEG C, and bottom of towe operation temperature is 125 DEG C.Extraction phase distillation column C-02 towers
Bottom fraction is that acetic acid quality concentration is 99.80 % product acetic acid 29994kg/h, the distillation of overhead fraction 170355kg/h Jing extraction phases
Column overhead condenser E-03 is condensed to after 30 DEG C into quantizer V-04.Material 67692kg/h Jing in raffinate phase storage tank V-03
There is heat exchange, preheating with raffinate phase distillation column C-03 tower bottom distillates into raffinate phase preheater E-05 in raffinate phase feed pump P-04
Temperature is 85 DEG C and enters raffinate phase distillation column C-03 afterwards.Raffinate phase distillation column operating pressure 0.20MPaG；Tower top operation temperature
For 89 DEG C, bottom of towe operation temperature is 101 DEG C.Raffinate phase distillation column C-03 overhead fractions (Organic substance mass content is 66.26%)
1346kg/h enters the preheater E-01 heat exchanges of extraction phase one-level and raffinate phase overhead condenser E-06 is condensed to temperature
For quantizer V-04 is entered after 30 DEG C；Raffinate phase distillation column C-03 tower bottom distillates are waste water (Organic substance mass content is 1.41%)
30429kg/h, discharges Jing after raffinate phase preheater E-05 heat exchange recovery waste heats.It is light phase for extraction that quantizer V-04 is isolated
Agent 163472kg/h, the light phase pump P-06 parts of light phase separated device send into extractant storage tank V-02, another part and are back to extraction
Phase distillation column C-02 is taken, light phase capacity of returns is 0.46 with extraction phase overhead fraction amount mass ratio, and quantizer V-04 is separated
Heavy phase 36877kg/h for going out is back to raffinate phase storage tank V-03.Process cycles extractant in process can be lossy, supplements extractant
Measure as 90kg/h.Recovery rate is 99.78%.
The system embodiment of present invention recovery of acetic acid from aqueous acetic acid is as shown in Fig. 2 which includes extraction tower C-01, extraction
Phase distillation column C-02, raffinate phase distillation column C-03 and quantizer V-04 are taken, the extraction tower C-01 tops are distilled with extraction phase
Tower C-02 is connected by extraction phase pipeline, is connected with quantizer V-04 at the top of extraction phase distillation column C-02, the extraction tower C-01
Bottom is connected with raffinate phase distillation column C-03 by raffinate phase pipeline, with quantizer V-04 at the top of the raffinate phase distillation column C-03
Connection, is connected with light phase pipeline and heavy phase pipeline, is connected with and each leads on the light phase pipeline on the quantizer V-04
Two laterals of extraction phase distillation column C-02 and extraction tower C-01, the heavy phase pipeline are passed into raffinate phase distillation column C-03
In.The extraction phase pipeline is provided with extraction phase storage tank V-01 and extraction phase preheater, and extraction phase preheater includes that one-level is preheated
Device E-01 and two grades of preheater E-02, the raffinate phase distillation column C-03 tower tops are connected with the one-level preheater E-01.It is described
Raffinate phase pipeline is provided with raffinate phase storage tank V-03 and raffinate phase preheater E-05, the raffinate phase distillation column C-03 bottom of towe and extraction
Remaining phase preheater connects E-05.Extraction phase distillation column tower is provided with the top of the extraction phase distillation column C-02 and quantizer V-04 between
Overhead condenser E-03, is provided with raffinate phase overhead condenser E- and quantizer between at the top of the raffinate phase distillation column
06, the lateral for being passed into extraction tower connected on the light phase pipeline is provided with extractant storage tank V-02, the extraction phase
Distillation column C-02 bottom of towe is provided with reboiler E-04.
Claims (10)
1. a kind of method of the recovery of acetic acid from aqueous acetic acid, it is characterised in that comprise the steps：
（A）Liquid-liquid extraction：Dilute acetic acid aqueous solution and extractant enter extraction tower（C-01）Extracting operation is carried out, is extracted after extracting operation
Take tower（C-01）Bottom of towe is raffinate phase, extraction tower（C-01）Tower top is extraction phase；
（B）Extraction phase distills：Extraction phase distillation column is entered after extraction phase is preheated（C-02）, extraction phase distillation column（C-02）Bottom of towe
Fraction be product acetic acid, extraction phase distillation column（C-02）Quantizer is entered after overhead fraction condensation（V-04）；
（C）Raffinate phase distills：Raffinate phase distillation column is entered after raffinate phase is preheated（C-03）, raffinate phase distillation column（C-03）Tower top
Quantizer is entered after fraction condensation（V-04）, raffinate phase distillation column（C-03）Tower bottom distillate is waste water；
（D）Extractant is reclaimed：Quantizer（V-04）That what is isolated is light phase for extractant, light phase part return extraction tower（C-01）
Carry out Liquid-liquid Extraction Processes, another part and be back to extraction phase distillation column（C-02）Carry out extraction phase still-process, quantizer（V-
04）The heavy phase isolated is back to raffinate phase distillation column（C-03）Carry out raffinate phase still-process.
2. the method for the recovery of acetic acid from aqueous acetic acid according to claim 1, it is characterised in that：In step（A）In,
In the dilute acetic acid aqueous solution, acetic acid quality concentration is 10% ~ 80%, mixing of the extractant for isopropyl acetate, butanone and hexane
Thing, isopropyl acetate mass fraction are 60% ~ 100%, and butanone mass fraction is 0% ~ 25%, and hexane mass fraction is 0% ~ 15%；
Liquid-liquid extraction operating pressure is 0.1 ~ 1.0MPaG, and operation temperature is 30 ~ 50 DEG C.
3. the method for the recovery of acetic acid from aqueous acetic acid according to claim 1, it is characterised in that：In step（A）In,
Extraction tower（C-01）Top extraction phase out enters extraction phase storage tank（V-01）, extraction phase storage tank（V-01）Upper aqueous phase is entered
Extraction phase one-level preheater（E-01）, lower liquid be back to extraction tower（C-01）；In step（B）In, extraction phase preheating is adopted
Two-stage is preheated, and one-level preheating is and raffinate phase distillation column（C-03）Overhead fraction heat exchange, two-stage preheating after temperature of charge be 80 ~
95℃。
4. the method for the recovery of acetic acid from aqueous acetic acid according to claim 1, it is characterised in that：In step（B）In,
Extraction phase distillation column（C-02）0 ~ 0.1MPaG of operating pressure；Extraction phase distillation column（C-02）Tower top operation temperature is 65 ~ 100 DEG C,
Extraction phase distillation column（C-02）Bottom of towe operation temperature is 100 ~ 140 DEG C；Extraction phase distillation column（C-02）Overhead fraction is condensed
Temperature is 20 ~ 40 DEG C.
5. the method for the recovery of acetic acid from aqueous acetic acid according to claim 1, it is characterised in that：In step（C）In,
Raffinate phase preheating is raffinate phase and raffinate phase distillation column（C-03）Tower bottom distillate carries out heat exchange, and after raffinate phase preheating, temperature is 70
~100℃；Raffinate phase distillation column（C-03）0.05 ~ 0.50MPaG of operating pressure, raffinate phase distillation column（C-03）Tower top operation temperature
For 65 ~ 95 DEG C, raffinate phase distillation column（C-03）Bottom of towe operation temperature is 95 ~ 110 DEG C；Raffinate phase distillation column（C-03）Overhead fraction
Condensed temperature is 20 ~ 45 DEG C.
6. the method for the recovery of acetic acid from aqueous acetic acid according to claim 1, it is characterised in that：In step（D）In,
Light phase capacity of returns and extraction phase distillation column（C-02）Overhead fraction amount mass ratio is 0.40 ~ 0.70.
7. a kind of system of the recovery of acetic acid from aqueous acetic acid, it is characterised in that：Which includes extraction tower（C-01）, extraction phase steam
Evaporate tower（C-02）, raffinate phase distillation column（C-03）And quantizer（V-04）, the extraction tower（C-01）Steam with extraction phase on top
Evaporate tower（C-02）Connected by extraction phase pipeline, extraction phase distillation column（C-02）Top and quantizer（V-04）Connection, the extraction
Take tower（C-01）Bottom is by raffinate phase pipeline and raffinate phase distillation column（C-03）Connection, the raffinate phase distillation column（C-03）Top
Portion and quantizer（V-04）Connection, the quantizer（V-04）On be connected with light phase pipeline and heavy phase pipeline, the light phase pipeline
On be connected with and each lead into extraction phase distillation column（C-02）And extraction tower（C-01）Two laterals, the heavy phase pipeline
It is passed into raffinate phase distillation column（C-03）In.
8. the system of the recovery of acetic acid from aqueous acetic acid according to claim 7, it is characterised in that：The extraction phase pipe
Road is provided with extraction phase storage tank（V-01）With extraction phase preheater, extraction phase preheater includes one-level preheater（E-01）With two grades
Preheater（E-02）, the raffinate phase distillation column（C-03）Tower top and the one-level preheater（E-01）Connection.
9. the system of the recovery of acetic acid from aqueous acetic acid according to claim 7, it is characterised in that：The raffinate phase pipe
Road is provided with raffinate phase storage tank（V-03）With raffinate phase preheater（E-05）, the raffinate phase distillation column（C-03）Bottom of towe and raffinate
Phase preheater connects（E-05）.
10. the system of the recovery of acetic acid from aqueous acetic acid according to claim 7, it is characterised in that：The extraction phase
Distillation column（C-02）Top and quantizer（V-04）Between be provided with extraction phase distillation column column overhead condenser（E-03）, the raffinate
Raffinate phase overhead condenser is provided with the top of phase distillation column and quantizer between（E-06）, connect on the light phase pipeline
The lateral for being passed into extraction tower is provided with extractant storage tank（V-02）, the extraction phase distillation column（C-02）Bottom of towe is provided with
Reboiler（E-04）.
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| WO2020024886A1 (en) * | 2018-08-03 | 2020-02-06 | 天津大学 | Anti-corrosive process and device for methyl acetate hydrolysis and acetic acid refining in polyvinyl alcohol mother liquor recovery process |
| CN111348998A (en) * | 2020-04-17 | 2020-06-30 | 湖北三里枫香科技有限公司 | Energy-saving environment-friendly acetic acid production process |
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