CN106955500A - A kind of three tower is thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester - Google Patents
A kind of three tower is thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester Download PDFInfo
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- CN106955500A CN106955500A CN201710218232.8A CN201710218232A CN106955500A CN 106955500 A CN106955500 A CN 106955500A CN 201710218232 A CN201710218232 A CN 201710218232A CN 106955500 A CN106955500 A CN 106955500A
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- tower
- pressurizing
- acetic acid
- vacuum
- isopropyl acetate
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- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropyl acetate Chemical compound CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 31
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 87
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229940011051 isopropyl acetate Drugs 0.000 claims abstract description 29
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000047 product Substances 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 16
- 238000011084 recovery Methods 0.000 claims description 8
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 230000008676 import Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 238000009834 vaporization Methods 0.000 claims description 4
- 230000008016 vaporization Effects 0.000 claims description 4
- -1 isopropyl ester Chemical class 0.000 claims description 3
- 239000007792 gaseous phase Substances 0.000 claims description 2
- 238000009833 condensation Methods 0.000 abstract description 3
- 230000005494 condensation Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000976 ink Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 description 2
- QVVUTXIMBPAAKV-UHFFFAOYSA-N acetonitrile benzene methanol Chemical compound C1=CC=CC=C1.C(C)#N.CO QVVUTXIMBPAAKV-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- MTJGVAJYTOXFJH-UHFFFAOYSA-N 3-aminonaphthalene-1,5-disulfonic acid Chemical compound C1=CC=C(S(O)(=O)=O)C2=CC(N)=CC(S(O)(=O)=O)=C21 MTJGVAJYTOXFJH-UHFFFAOYSA-N 0.000 description 1
- XZTBFQNTALACFP-UHFFFAOYSA-N C(C)(C)O.C(C)(=O)O.C(C)(=O)OC(C)C Chemical compound C(C)(C)O.C(C)(=O)O.C(C)(=O)OC(C)C XZTBFQNTALACFP-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- IJMWOMHMDSDKGK-UHFFFAOYSA-N Isopropyl propionate Chemical compound CCC(=O)OC(C)C IJMWOMHMDSDKGK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 239000007798 antifreeze agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- 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
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to the method and device that a kind of three tower is thermally integrated variable-pressure rectification purifying acetic acid isopropyl ester, feed stream enters normal pressure extracting tower (T1), bottom of towe produces high-purity acetic acid, overhead stream enters pressurizing tower (T2) by pressurizeing, the isopropyl acetate product of high-purity is produced in pressurizing tower tower bottom, tower top produces isopropyl acetate with azeotropic thing steam and as vacuum tower (T3) tower base stream thermal source, realizes and is thermally integrated completely in heat exchanger (H3)；Enter vacuum tower (T3) after heat exchange condensation, high-purity isopropanol is produced in vacuum tower bottom of towe, overhead stream is recycled into pressurizing tower (T2) and is circulated utilization.The present invention solves complex system and separates and recovers the problem of isopropyl acetate, and obtains the isopropyl acetate of higher degree, using technique is thermally integrated, and energy consumption is reduced to greatest extent, and technique is simple, and device is reasonable.
Description
【Technical field】
Field is isolated and purified the invention belongs to chemical industry, being related to a kind of three tower, to be thermally integrated variable-pressure rectification purifying acetic acid different
The method and device of propyl ester.
【Background technology】
Isopropyl acetate is mainly used as the solvent of coating, printing-ink etc., is also industrially conventional dehydrating agent, medicine life
Is mainly used as Extraction solvent, paint solvent, solvent for printing inks, chemical reaction solvent of medicine etc. in production, is China
GB2760-86 is defined as the flavorant for allowing to use.The main solvent to prepare rum essence and fruit type spices.Second
Acid can be used as acidity regulator, acidulant, pickling agent, flavoring agent, spices etc., be also good antimicrobial.Isopropanol is made
It is that Organic Ingredients and solvent have extensive use, available for production coating, ink, extractant, aerosol agent etc., also acts as anti-
Freeze agent, cleaning agent, the additive of blended gasoline, the dispersant of pigment production, the fixative of printing and dyeing industry, glass and transparent plastic
Antifoggant etc..In the industrial production, acetic acid and isopropanol and concentrated sulfuric acid synthesis of acetic acid isopropyl ester are commonly used, the acetic acid of synthesis is different
Containing acetic acid and isopropanol impurity in propyl ester product, and acetic acid easily forms azeotropic mixture with isopropanol and is difficult to efficiently separate, therefore has
Imitate purifying acetic acid isopropyl ester and acetic acid is reclaimed with isopropanol and not only save energy and protect environment, while having very big to enterprise
Economic benefit.
Isopropyl acetate boiling point is 88.52 DEG C, and acetic acid boiling point is 118.01 DEG C, and isopropanol boiling point is 82.05 DEG C, under normal pressure
Isopropyl acetate easily forms minimum azeotropic mixture with isopropanol, so need to separate both mixtures using special extract rectification method,
Conventional special extract rectification method has variable-pressure rectification, extracting rectifying, film infiltration, rectifying coupling technique etc..Using traditional high-low pressure transformation
Rectifying, pressurizing tower condenser C1 thermic loads QC1 be far longer than vacuum tower needed for thermic load QR2, if therefore can using pressurizing tower it is cold
Condenser C1 thermic loads QC1 provides thermic load to vacuum tower, will greatly save energy ezpenditure.The present invention can effective purifying acetic acid isopropyl
Ester, and the problem that isopropyl acetate is separated with azeotropic system difficulty is handled, while having saved energy, realize Energy Efficient profit
With.
Patent (CN201510594602.9) discloses a kind of three towers variable-pressure rectification separating acetonitrile-Methanol-benzene ternary azeotrope
Method, be successfully separated multicomponent azeotropic mixture, but not using being thermally integrated.
Document (beautiful methanol-acetonitrile-benzene triplex mixture system separation process research [D] the Hebei University of Technology of ancestor,
2013.) five tower variable-pressure rectification separating acetonitriles-Methanol-benzene azeotropic mixture, but high energy consumption are reported, and separation process is complicated.
Document (Zhu Z, Xu D, Liu X, et al.Separation of acetonitrile/methanol/
benzene ternary azeotrope via triple column pressure-swing distillation[J]
.Separation&Purification Technology,2016,169:66-77.) report three tower variable-pressure rectifications separation second
The method of nitrile-Methanol-benzene ternary azeotrope, realizes efficiently separating for azeotropic mixture, does not use and is thermally integrated technique.
Document (Wu Y C, Huang H P, Chien I L.Investigation of the Energy-Saving
Design of an Industrial 1,4-Dioxane Dehydration Process with Light Feed
Impurity[J].Industrial&Engineering Chemistry Research,2014,53(40):15667-
15685.) three tower variable-pressure rectifications separation triethylamine, water, Isosorbide-5-Nitrae-dioxane are reported, Triethylamine gas is discharged using rectifying column,
Low high pressure double tower separation water and Isosorbide-5-Nitrae-dioxane are recycled, but use is not thermally integrated.
The present invention utilizes pressurizing tower (T2) overhead vapours using first atmospheric distillation, repressurization rectifying, last rectification under vacuum
The method that heat is provided to vacuum tower (T3) reboiler.Specifically, obtaining high-purity acetic acid product using atmospheric tower (T1), adding
Press in tower (T2), using isopropyl acetate and Isopropanol Solvent with pressure change, azeotropic constitutes shift this characteristic, second
Isopropyl propionate enters pressurizing tower (T2) rectifying, bottom of towe extraction isopropyl acetate product, from pressurizing tower with azeotropic thing
(T2) column overhead vapor is exchanged heat with vacuum tower (T3) tower base stream isopropanol, and gas is by heat exchange liquefaction, one completely
Partial reflux is into pressurizing tower (T2), and a part is entered in vacuum tower (T3) by pipeline 9, and the isopropanol liquid one of high-purity
By heat exchange, all vaporization enters vacuum tower (T3) for part, and a part is directly over pipeline 15 without heat exchange and produced, vacuum tower
(T3) overhead stream is after condenser C3 condensations, and a part of logistics is flowed back into tower, and a part is by pipeline 16 by high pressure
Pump P2 is recycled into pressurizing tower (T2) and carries out rectifying again.The present invention utilizes isopropyl acetate and normal propyl alcohol formation minimum azeotrope
Thing, and pressurizing tower overhead condenser thermic load is far longer than vacuum tower tower bottom reboiler thermic load, thus realize high vacuum tower it
Between be thermally integrated technique completely, reduce energy ezpenditure.
【The content of the invention】
[technical problem to be solved]
It is an object of the invention to provide a kind of method that three tower is thermally integrated variable-pressure rectification purifying acetic acid isopropyl ester.
It is a further object to provide be thermally integrated variable-pressure rectification purifying acetic acid isopropyl ester using the tower of described device three
Method and device be thermally integrated variable-pressure rectification purifying acetic acid isopropyl in three towers it is a further object to provide methods described
Purposes in ester.
[technical scheme]
The present invention is achieved through the following technical solutions.
1st, three towers are thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester, it is characterised in that for purifying acetic acid
The device of isopropyl ester mainly includes following part：
Atmospheric tower (T1), pressurizing tower (T2), vacuum tower (T3), condenser (C1), condenser (C3), reboiler (R1), again
Boil device (R2), heat exchanger (H3), force (forcing) pump (P1), force (forcing) pump (P2)；Wherein force (forcing) pump (P1) connects pressurizing tower (T2) charging aperture,
Reboiler (R1) is connected to atmospheric tower (T1) bottom of towe, and reboiler (R2) is connected to pressurizing tower (T2), condenser (C1), condenser
(C3) atmospheric tower (T1) and vacuum tower (T3) tower top are connected in turn, force (forcing) pump (P2) is connected with pressurizing tower (T2), pressurizing tower
(T2) gaseous phase outlet logistics is connected with the hot logistics import of heat exchanger (H3), the hot stream outlet force (forcing) pump (P3) of heat exchanger (H3)
Pressurizing tower (T2) tower top is connected to, vacuum tower (T3) bottom of towe is connected with the cold logistics import of heat exchanger (H3), heat exchanger (H3) cold thing
Flow export is connected with vacuum tower (T3)；
This method is mainly included the following steps that：
(1) crude product isopropyl acetate is entered in atmospheric tower (T1), the outlet of atmospheric tower (T1) bottom of towe distillates liquid phase acetic acid,
A portion is entered in reboiler (R1), and atmospheric tower (T1), another part logistics are entered after being boiled again through reboiler (R1)
Directly produced as acetic acid product, atmospheric tower (T1) overhead is entered in pressurizing tower (T2) by force (forcing) pump (P1)；
(2) in pressurizing tower (T2) tower top isopropyl acetate-IPA vapor as vacuum tower (T3) thermal source, and utilization should
Thermal source realizes and is thermally integrated that isopropyl acetate-IPA vapor from pressurizing tower (T2) tower top is with depressurizing in heat exchanger (H3)
Tower (T3) tower base stream isopropanol is exchanged heat, and isopropyl acetate-azeotropic thing gas liquefies completely by heat exchange, its
Middle a part of logistics is back in pressurizing tower (T2), and another part is entered in vacuum tower (T3), and vacuum tower (T3) bottoms
Flowing an isopropanol liquid part, all vaporization enters vacuum tower (T3) by heat exchange, and a part is without heat exchange directly from vacuum tower
(T3) bottom of towe is produced；
(3) vacuum tower (T3) is entered by condenser (C3) in vacuum tower (T3) overhead stream, another part is used as circulation
Logistics reenters pressurizing tower (T2) by pump (P2) and carries out rectifying again.
In accordance with another preferred embodiment of the present invention, it is characterised in that：It is characterized in that：Atmospheric tower (T1) theoretical tray
Number is 50~60 pieces, and flitch position is the 20th~30 piece, and pressurizing tower (T2) theoretical cam curve is 25~35 pieces, and charging Board position is
16th piece, recycle flows into flitch position for the 16th piece, and vacuum tower (T3) number of theoretical plate is 45~55 pieces, and charging Board position is the
31~38 pieces.In accordance with another preferred embodiment of the present invention, it is characterised in that：It is characterized in that：Atmospheric tower (T1) reflux ratio
For 0.4~0.6, pressurizing tower (T3) reflux ratio is that 1.6~1.9 vacuum towers (T3) reflux ratio is 1.6~1.9.
In accordance with another preferred embodiment of the present invention, it is characterised in that：It is characterized in that：Atmospheric tower (T1) tower top temperature
For 70.35~85.72 DEG C, 107.93~117.47 DEG C of atmospheric tower (T1) column bottom temperature, pressurizing tower (T2) column bottom temperature 152.42
~172.64 DEG C, vacuum tower (T3) tower top temperature is -10.41~-5.41 DEG C.
In accordance with another preferred embodiment of the present invention, it is characterised in that：It is characterized in that：The matter of crude product isopropyl acetate
It is 60%~75% to measure fraction.
In accordance with another preferred embodiment of the present invention, it is characterised in that：It is characterized in that：Isopropyl acetate after purification
Purity is more than 99.90%, and the rate of recovery is 99.90%~99.95%, and the purity of acetic acid is more than 99.90%, and the rate of recovery of acetic acid is
99.90%~99.98%, the purity of isopropanol is more than 99.90%, and the rate of recovery of isopropanol is 99.90%~99.97%.
Variable-pressure rectification is thermally integrated the method for purifying raw isopropyl acetate and is described in detail below in the present invention：
Isopropyl acetate-acetic acid-isopropanol mixture is entered in atmospheric tower (T1) by pipeline 1, in atmospheric tower, charging
Logistics enters tower bottom reboiler R1, and being passed through steam in reboiler is heated, and a part is produced by pipeline 5, it is a part of again
Return in tower, overhead stream enters and rectifying is carried out in pressurizing tower (T2), tower base stream vaporization is risen in pressurizing tower (T2), on
Tower top is raised to, overhead vapours is produced as vacuum tower (T3) thermal source by pipeline 6, realizes and be thermally integrated completely in heat exchanger H3, come
Self-pressurization column overhead steam is exchanged heat with the hot logistics isopropanol of vacuum tower bottom of towe, and gas is by heat exchange liquefaction completely, a part
It is back to by pipeline 11 in pressurizing tower (T2), a part is entered in vacuum tower (T3) by pipeline 12, on pressurizing tower (T2) is interior
The gas risen carries out multistage mass-and heat-transfer with the liquid declined, and another part logistics for dropping to bottom of towe is produced by pipeline 7, entered
Enter to the logistics in vacuum tower (T3), enter bottom of towe, by heat exchanger H3, a part is directly produced by pipeline 15, one
Lease making boils again to be condensed into vacuum tower (T3) tower top by condenser, and a condensed logistics part flows back into vacuum tower
(T3), a part is recycled into pressurizing tower (T2) by pump P2 by pipeline 16 and carries out rectifying again.
Atmospheric tower (T1) operating pressure that the present invention is used is 1atm (absolute pressure), and pressurizing tower (T2) operating pressure is 8atm
(absolute pressure), vacuum tower (T3) operating pressure is 0.01atm (absolute pressure)；Atmospheric tower (T1) theoretical cam curve is 50~55 pieces, flitch
Position is the 20th~30 piece, and pressurizing tower (T2) theoretical cam curve is 25~35 pieces, and charging Board position is the 16th piece, and recycle is flowed into
Flitch position is the 16th piece, and vacuum tower (T3) number of theoretical plate is 45~50 pieces, and charging Board position is the 31st~38 piece；Atmospheric tower
(T1) reflux ratio is 0.41~1.5, and pressurizing tower (T2) reflux ratio is 0.5~1.5, and vacuum tower (T3) reflux ratio is 2.85~3.8；
Atmospheric tower (T1) tower top temperature is 70.35~85.72 DEG C, atmospheric tower (T1) column bottom temperature 107.93~117.47, pressurizing tower
(T2) 152.42~172.64 DEG C of column bottom temperature, vacuum tower (T3) tower top temperature is -10.41~-5.41 DEG C.
Isopropyl acetate purity after present invention purification is more than 99.90%, and the rate of recovery is 99.90%~99.95%, acetic acid
Purity be more than 99.90%, the rate of recovery of acetic acid is 99.90%~99.98%, and the purity of isopropanol is more than 99.90%, isopropyl
The rate of recovery of alcohol is 99.90%~99.97%.
[beneficial effect]
The present invention compared with prior art, mainly there is following beneficial effect：
(1) isopropyl acetate product has successfully been purified, and has obtained two kinds of high purity product acetic acid and isopropanol.
(2) compared with traditional variable-pressure rectification technique, equipment investment expense of the invention is low.
(3) compared with traditional variable-pressure rectification technique, running cost of the invention is low, and heat utilization ratio is high.
(4) compared with extraction rectification technique, the present invention is not introduced into other components impurity, and product purity is high.
【Brief description of the drawings】
Accompanying drawing 1 is to be thermally integrated three tower variable-pressure rectification purifying acetic acid isopropyl ester structural representations.
In figure, T1 atmospheric towers；T2 pressurizing towers；T3 vacuum towers；C1, C3 condenser；R1, R3 reboiler；H3 heat exchangers；D2 is stored up
Flow container；P1, P2 force (forcing) pump；Numeral represents each logistics pipeline.
【Embodiment】
With reference to embodiment, the present invention is further illustrated, but the invention is not limited in embodiment.
Embodiment 1：
Feeding temperature is 25 DEG C, and flow is 1000kmol/h, and pressure is 1atm (absolute pressure), and isopropyl acetate is contained in charging
60%, containing acetic acid 5%, isopropanol 35%.Atmospheric tower number of theoretical plate 50, it is 20, pressurizing tower number of theoretical plate that delivered fresh, which flows into flitch,
For 25, it is 16 that delivered fresh, which flows into flitch, and it is 16 that recycle, which flows into flitch,；Vacuum tower number of theoretical plate is 45, and feedboard is 31.Normal pressure
Tower reflux ratio 0.41,70.35 DEG C of tower top temperature, 107.93 DEG C of column bottom temperature；Pressurizing tower operating pressure is 8atm (absolute pressure), backflow
Than for 0.5, tower top temperature is 135.75 DEG C, column bottom temperature is 152.42 DEG C；Vacuum tower operating pressure is 0.01atm (absolute pressure),
Reflux ratio is 2.85, and tower top temperature is -10.41 DEG C, and column bottom temperature is 47.58 DEG C.Isopropyl acetate product is obtained after separation pure
Spend for 99.95%, yield is 99.90%, acetic acid purity is 99.97%, and yield is 99.90%, isopropanol product purity
99.8%, yield 99.0%.
By the present invention process and device that are thermally integrated three tower variable-pressure rectification purifying acetic acid isopropyl esters that provide, using adding
Pressure column overhead distillate steam gives vacuum tower heat supply, compared with traditional variable-pressure rectification operation energy consumption, has saved pressurizing tower condensation
The cooling water amount of device and the steam consumption of vacuum tower reboiler, by separation 1000kmol/h Material calculations, reach same purity
And yield, cooling water amount saving 50%, steam consumption reduces 50%.The distillation system process operation parameter of table 1
Embodiment 2：
Feeding temperature is 25 DEG C, and flow is 1000kmol/h, and pressure is 1atm (absolute pressure), and isopropyl acetate is contained in charging
65%, containing acetic acid 10%, isopropanol 25%.Atmospheric tower number of theoretical plate 55, it is 23, pressurizing tower number of theoretical plate that delivered fresh, which flows into flitch,
For 30, it is 16 that delivered fresh, which flows into flitch, and it is 16 that recycle, which flows into flitch,；Vacuum tower number of theoretical plate is 48, and feedboard is 33.Normal pressure
Tower reflux ratio 0.44,79.75 DEG C of tower top temperature, 110.43 DEG C of column bottom temperature；Pressurizing tower operating pressure is 8atm (absolute pressure), backflow
Than for 0.8, tower top temperature is 140.46 DEG C, column bottom temperature is 160.34 DEG C；Vacuum tower operating pressure is 0.01atm (absolute pressure),
Reflux ratio is 3.05, and tower top temperature is -5.47 DEG C, and column bottom temperature is 52.58 DEG C.Isopropyl acetate product purity is obtained after separation
For 99.92%, yield is 99.90%, and acetic acid purity is 99.97%, and yield is 99.90%, isopropanol product purity
99.98%, yield 99.0%.
Embodiment 3：
Feeding temperature is 25 DEG C, and flow is 1000kmol/h, and pressure is 1atm (absolute pressure), and isopropyl acetate is contained in charging
70%, containing acetic acid 10%, isopropanol 20%.Atmospheric tower number of theoretical plate 60, it is 25, pressurizing tower number of theoretical plate that delivered fresh, which flows into flitch,
For 35, it is 16 that delivered fresh, which flows into flitch, and it is 16 that recycle, which flows into flitch,；Vacuum tower number of theoretical plate is 50, and feedboard is 38.Normal pressure
Tower reflux ratio 0.49,80.75 DEG C of tower top temperature, 115.53 DEG C of column bottom temperature；Pressurizing tower operating pressure is 8atm (absolute pressure), backflow
Than for 1, tower top temperature is 145.76 DEG C, column bottom temperature is 168.64 DEG C；Vacuum tower operating pressure is 0.01atm (absolute pressure), is returned
Stream is than being 3.3, and tower top temperature is -10.35 DEG C, and column bottom temperature is 54.6 DEG C.Isopropyl acetate product purity is obtained after separation is
99.94%, yield is 99.95%, and acetic acid purity is 99.95%, and yield is 99.90%, isopropanol product purity 99.97%,
Yield 99.3%.
Embodiment 4：
Feeding temperature is 25 DEG C, and flow is 1000kmol/h, and pressure is 1atm (absolute pressure), and isopropyl acetate is contained in charging
75%, containing acetic acid 15%, isopropanol 10%.Atmospheric tower number of theoretical plate 55, it is 23, pressurizing tower number of theoretical plate that delivered fresh, which flows into flitch,
For 30, it is 16 that delivered fresh, which flows into flitch, and it is 16 that recycle, which flows into flitch,；Vacuum tower number of theoretical plate is 55, and feedboard is 35.Normal pressure
Tower reflux ratio 0.5,85.72 DEG C of tower top temperature, 117.47 DEG C of column bottom temperature；Pressurizing tower operating pressure is 8atm (absolute pressure), backflow
Than for 1.5, tower top temperature is 125.76 DEG C, column bottom temperature is 172.64 DEG C；Vacuum tower operating pressure is 0.01atm (absolute pressure),
Reflux ratio is 3.8, and tower top temperature is -10.35 DEG C, and column bottom temperature is 57.87 DEG C.Isopropyl acetate product purity is obtained after separation
For 99.94%, yield is 99.95%, and acetic acid purity is 99.98%, and yield is 99.97%, isopropanol product purity
99.96%, yield 99.7%.
Claims (6)
1. a kind of three tower is thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester, it is characterised in that for purifying acetic acid
The device of isopropyl ester mainly includes following part：
Atmospheric tower (T1), pressurizing tower (T2), vacuum tower (T3), condenser (C1), condenser (C3), reboiler (R1), reboiler
(R2), heat exchanger (H3), force (forcing) pump (P1), force (forcing) pump (P2)；Wherein force (forcing) pump (P1) connection pressurizing tower (T2) charging aperture, then boil
Device (R1) is connected to atmospheric tower (T1) bottom of towe, and reboiler (R2) is connected to pressurizing tower (T2) bottom of towe, condenser (C1), condenser
(C3) atmospheric tower (T1) and vacuum tower (T3) tower top are connected in turn, force (forcing) pump (P2) is connected with pressurizing tower (T2), pressurizing tower
(T2) gaseous phase outlet logistics is connected with the hot logistics import of heat exchanger (H3), the pressurized pump of hot stream outlet of heat exchanger (H3)
(P3) pressurizing tower (T2) tower top is connected to, vacuum tower (T3) bottom of towe is connected with the cold logistics import of heat exchanger (H3), heat exchanger (H3)
Cold stream outlet is connected with vacuum tower (T3)；
This method is mainly included the following steps that：
(1) crude product isopropyl acetate is entered in atmospheric tower (T1), atmospheric tower (T1) bottom of towe distillate a portion enters
Into reboiler (R1), atmospheric tower (T1) is entered after being boiled again through reboiler (R1), another part logistics is straight as acetic acid product
Extraction is connect, atmospheric tower (T1) overhead is entered in pressurizing tower (T2) by force (forcing) pump (P1)；
(2) in pressurizing tower (T2) tower top isopropyl acetate-IPA vapor as vacuum tower (T3) thermal source, and the thermal source is utilized
Realize and be thermally integrated in heat exchanger (H3), isopropyl acetate-IPA vapor and vacuum tower from pressurizing tower (T2) tower top
(T3) tower base stream isopropanol is exchanged heat, and isopropyl acetate-azeotropic thing gas liquefies completely by heat exchange, wherein
A part of logistics is back in pressurizing tower (T2), and another part is entered in vacuum tower (T3), and vacuum tower (T3) tower base stream
By heat exchange, all vaporization enters vacuum tower (T3) to an isopropanol liquid part, and a part is without heat exchange directly from vacuum tower
(T3) bottom of towe is produced；
(3) vacuum tower (T3) is partly entered by condenser (C3) in vacuum tower (T3) overhead stream, another part is used as circulation
Logistics enters pressurizing tower (T2) by pump (P2) and reused.
2. a kind of three tower as claimed in claim 1 is thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester, it is special
Levy and be：Atmospheric tower (T1) theoretical cam curve is 50~60 pieces, and flitch position is the 20th~30 piece, pressurizing tower (T2) theoretical tray
Number is 25~35 pieces, and charging Board position is the 16th piece, and it is the 16th piece, vacuum tower (T3) number of theoretical plate that recycle, which flows into flitch position,
For 45~55 pieces, charging Board position is the 31st~38 piece.
3. a kind of three tower as claimed in claim 1 is thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester, it is special
Levy and be：Atmospheric tower (T1) reflux ratio is 0.41~1.5, and pressurizing tower (T2) reflux ratio is 0.5~1.5, vacuum tower (T3) backflow
Than for 2.85~3.8.
4. a kind of three tower as claimed in claim 1 is thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester, it is special
Levy and be：Atmospheric tower (T1) tower top temperature is 70.35~85.72 DEG C, 107.93~117.47 DEG C of atmospheric tower (T1) column bottom temperature,
152.42~172.64 DEG C of pressurizing tower (T2) column bottom temperature, vacuum tower (T3) tower top temperature is -10.41~-5.41 DEG C.
5. a kind of three tower as claimed in claim 1 is thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester, it is special
Levy and be：The mass fraction of isopropyl acetate is 60%~75% in crude product isopropyl acetate.
6. a kind of three tower as claimed in claim 1 is thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester, it is special
Levy and be：Isopropyl acetate purity after purification is more than 99.90%, and the rate of recovery is 99.90%~99.95%, the purity of acetic acid
More than 99.90%, the rate of recovery of acetic acid is 99.90%~99.98%, and the purity of isopropanol is more than 99.90%, time of isopropanol
Yield is 99.90%~99.97%.
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| CN108863793A (en) * | 2018-05-23 | 2018-11-23 | 惠州宇新化工有限责任公司 | A kind of preparation method of isopropyl acetate |
| CN111675602A (en) * | 2020-06-23 | 2020-09-18 | 山东中盛药化设备有限公司 | System and method for rectifying and purifying ethanol and butyraldehyde from butyraldehyde mother liquor |
| CN113214048A (en) * | 2021-05-08 | 2021-08-06 | 青岛科技大学 | Method for separating isobutanol, isobutyl acetate and ethanol by three-tower heat integration pressure swing rectification |
| CN114315581A (en) * | 2021-12-29 | 2022-04-12 | 扬州贝尔新环境科技有限公司 | Method for pressure swing separation of isopropyl acetate |
| CN115317946A (en) * | 2022-08-16 | 2022-11-11 | 浙江皇马科技股份有限公司 | Device and method for purifying ethylene glycol monopropyl ether by coupling rectification |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108863793A (en) * | 2018-05-23 | 2018-11-23 | 惠州宇新化工有限责任公司 | A kind of preparation method of isopropyl acetate |
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| CN111675602A (en) * | 2020-06-23 | 2020-09-18 | 山东中盛药化设备有限公司 | System and method for rectifying and purifying ethanol and butyraldehyde from butyraldehyde mother liquor |
| CN111675602B (en) * | 2020-06-23 | 2022-09-27 | 山东中盛药化设备有限公司 | System and method for rectifying and purifying ethanol and butyraldehyde from butyraldehyde mother liquor |
| CN113214048A (en) * | 2021-05-08 | 2021-08-06 | 青岛科技大学 | Method for separating isobutanol, isobutyl acetate and ethanol by three-tower heat integration pressure swing rectification |
| CN113214048B (en) * | 2021-05-08 | 2022-08-12 | 青岛科技大学 | Method for separating isobutanol, isobutyl acetate and ethanol by three-tower heat integration pressure swing rectification |
| CN114315581A (en) * | 2021-12-29 | 2022-04-12 | 扬州贝尔新环境科技有限公司 | Method for pressure swing separation of isopropyl acetate |
| CN115317946A (en) * | 2022-08-16 | 2022-11-11 | 浙江皇马科技股份有限公司 | Device and method for purifying ethylene glycol monopropyl ether by coupling rectification |
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