CN106905115A - A kind of method and device of aqueous acetone hydrogenation products separating isopropanol - Google Patents
A kind of method and device of aqueous acetone hydrogenation products separating isopropanol Download PDFInfo
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- CN106905115A CN106905115A CN201510980178.1A CN201510980178A CN106905115A CN 106905115 A CN106905115 A CN 106905115A CN 201510980178 A CN201510980178 A CN 201510980178A CN 106905115 A CN106905115 A CN 106905115A
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- tower
- rectification column
- azeotropy rectification
- isopropanol
- aqueous acetone
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 title claims abstract description 262
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 title claims abstract description 245
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 112
- 238000000034 method Methods 0.000 title claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 79
- 239000000463 material Substances 0.000 claims abstract description 48
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 21
- 239000002351 wastewater Substances 0.000 claims description 51
- 238000007599 discharging Methods 0.000 claims description 18
- 150000001335 aliphatic alkanes Chemical group 0.000 claims description 14
- 239000000470 constituent Substances 0.000 claims description 14
- 238000009835 boiling Methods 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 10
- 238000006297 dehydration reaction Methods 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 3
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 3
- -1 C 5 alkane Chemical class 0.000 claims description 2
- 239000000047 product Substances 0.000 description 72
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 12
- 239000003054 catalyst Substances 0.000 description 7
- 238000005265 energy consumption Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 239000012024 dehydrating agents Substances 0.000 description 5
- 150000001298 alcohols Chemical class 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- MWFMGBPGAXYFAR-UHFFFAOYSA-N 2-hydroxy-2-methylpropanenitrile Chemical compound CC(C)(O)C#N MWFMGBPGAXYFAR-UHFFFAOYSA-N 0.000 description 1
- TVEXGJYMHHTVKP-UHFFFAOYSA-N 6-oxabicyclo[3.2.1]oct-3-en-7-one Chemical compound C1C2C(=O)OC1C=CC2 TVEXGJYMHHTVKP-UHFFFAOYSA-N 0.000 description 1
- 229910017813 Cu—Cr Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910000564 Raney nickel Inorganic materials 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- XDTRNDKYILNOAP-UHFFFAOYSA-N phenol;propan-2-one Chemical compound CC(C)=O.OC1=CC=CC=C1 XDTRNDKYILNOAP-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The method and its device of a kind of aqueous acetone hydrogenation products separating isopropanol that the present invention is provided, methods described include：Step 1, first azeotropic distillation is carried out using the aqueous acetone hydrogenation products from hydrogenation reactor as feed material addition azeotropy rectification column, simultaneously toward addition entrainer step 2 in the azeotropy rectification column, the tower top azeotropic mixture of the azeotropy rectification column output is injected into gun barrel, the tower top azeotropic mixture is divided into oil reservoir and water layer using gun barrel, the water layer is located at gun barrel bottom, the oil reservoir is located at the knockout drum top, the oil reservoir of the gun barrel returns to the azeotropy rectification column as backflow material, the water layer of the gun barrel enters dehydrating tower；Step 3, the purity requirement of the isopropanol gone out according to azeotropy rectification column rectifying, using the azeotropy rectification column side line for being arranged at the azeotropy rectification column side, isopropanol qualified products is extracted out.
Description
Technical field
The invention belongs to technical field of petrochemical industry, it is related to a kind of suitable for aqueous acetone hydrogenation products separating isopropanol
New method.
Background technology
In recent years, the yield of acetone is continuously increased, but because the production method of methyl methacrylate has straight by C 4 fraction
The trend that oxidizing process replaces Acetone cyanohydrin method is connect, and acetone is constantly being reduced as solvent load, makes the range of application of acetone
Narrow, therefore acetone is changed into isopropanol fine chemicals and have great importance.Up to the present acetone hydrogenation prepares different
The catalyst of propyl alcohol has：Raney Ni catalyst, Ru/C catalyst, Ru/Al2O3Catalyst, Cu-Cr catalyst.Acetone is in the above
It is hydrogenated with the catalyst of type, typically using fixed bed reactors, acetone is with hydrogen in certain proportion in liquid phase or gas phase bar
Beds are entered under part, isopropanol is hydrogenated under appropriate temperature and pressure.
The purpose of the process for refining of isopropanol is to obtain high-purity isopropanol, is consequently belonging to separation engineering category.Isopropanol
Process units reactive moieties material out is complicated mixture, and isopropanol can produce azeotropic to constitute with water.Therefore it is different
The main process of propyl alcohol purification is first to remove light component impurity, secondly the weight in separating isopropanol and water, then separating isopropanol
Component.
Different according to the technique that isopropanol reaction process is used, corresponding FF is also different, but the subject matter for solving
Equally, i.e., weight component is separated by rectifying, azeotropic constitutes separating isopropanol and water obtains high-purity isopropanol and produces by destroying
Product.
It is raw material that acetone hydrogenation production isopropanol typically uses industrial grade acetone, and raw material only contains minor amount of water, but acetone hydrogenation
Process produces a small amount of water, and producing anhydrous isopropyl alcohol needs to remove this part water.Isopropanol dehydration is typically using energy and isopropanol
The entrainer for forming ternary azeotrope with water is carried out, and minimum boiling point azeotropic mixture is steamed from tower top.It is light in charging according to rectifying general knowledge
Concentration of component is low, and the reflux ratio of tower normal operating is big.In certain limit, tower capacity of returns maintains the model being basically unchanged to light impurity
Enclose.Isopropanol dehydration process, when water content increases to 2% (m/m) from 0.2%, tower capacity of returns is basically unchanged.In other words, enter
Water content increased 10 times in material, and rectifying and dewatering energy consumption is almost unchanged.And acetone is produced by third for phenol-acetone device
For ketone dehydration device, situation is varied considerably.Due under normal pressure acetone with shipwreck to separate, acetone dehydration using decompression grasp
Make, and need the number of plates very high.If the purity of acetone is reduced into 98% (m/m), third from 99.8% (m/m) of technical grade
Ketone is dehydrated difficulty and dehydration energy consumption and can significantly reduce.Raney's nickel catalyst is general to be preserved in water, can be in aqueous conditions
Under realize acetone hydrogenation produce isopropanol.Aqueous acetone hydrogenation can reduce the production cost of raw material acetone, and then reduce isopropyl
The cost of alcohol production process.
China Patent No. discloses the separation method that a kind of acetone hydrogenation produces isopropanol for the patent of CN103772145.
The method proposes three tower separation process：Acetone hydrogenation product is separated through azeotropy rectification column, and bottom of towe separates heavy constituent, and survey line is produced
Go out anhydrous isopropyl alcohol product, tower top steams azeotropic mixture.Overhead product extractant separates water with other components, and tower top is removed
Component beyond water, is recycled back into reactor, and the recovered column overhead removing water of materials at bottom of tower, bottom of towe reclaims extractant circulation.Should
The atmospheric boiling point of method azeotropy rectification column survey line anhydrous isopropyl alcohol is 82.4 DEG C, and water-azeotropic thing normal pressure azeotropic point is
80.4 DEG C, both clear separating difficulties are larger.
Aqueous acetone hydrogenation reaction product of the present invention feeds as azeotropy rectification column.Tower top steams acetone and is formed with dehydrating agent
Binary azeotrope and the ternary azeotrope that is formed of dehydrating agent and water and isopropanol, be generally divided into the liquid of weight two after azeotropic mixture cooling
Phase.When distillate is not stratified, suitable amount of water can be added in tower charging, be layered distillate.Light phase is used as reflux cycle
Return tower top.Heavy phase enters dehydrating tower, and control inlet amount makes layering tank liquid phase circle position constant.Dehydrating tower bottom of towe removes water, tower top material
Return to hydrogenation reactor circulation.When acetone hydrogenation product six oxygenate concentrations of carbon are not high, azeotrope column feed line and tower reactor it
Between correct position extraction meet the isopropanol of purity requirement.The present invention realizes that acetone adds by azeotrope column and dehydrating tower two-tower process
Hydrogen production is separated.With respect to three-column process flow, investment and energy consumption are reduced.
The content of the invention
The invention discloses a kind of method of aqueous acetone hydrogenation products separating isopropanol, methods described includes：Acetone adds
Hydrogen product is obtained the isopropanol that purity is up to more than 99.96% after azeotropy rectification column, dehydrating tower.Specifically include following steps：
Step 1, adds azeotropic distillation using the aqueous acetone hydrogenation products from hydrogenation reactor as feed material first
Tower carries out azeotropic distillation, while toward adding entrainer in the azeotropy rectification column；
Step 2, gun barrel is injected by the tower top azeotropic mixture of the azeotropy rectification column output, will using gun barrel
The tower top azeotropic mixture is divided into oil reservoir and water layer, and the oil reservoir of the gun barrel returns to the azeotropic as the first backflow material
Rectifying column, the water layer of the gun barrel enters dehydrating tower；
Step 3, the requirement of the isopropanol purity according to the azeotropy rectification column output, using being arranged at the azeotropic distillation
The azeotropy rectification column side line of tower side, isopropanol qualified products are extracted out.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, also includes：
Step 4, returns to the overhead product of dehydrating tower the hydrogenation reactor and recycles as the second backflow material, passes through
Feed material after hydrogenation reactor treatment as azeotropy rectification column adds the azeotropy rectification column；
Step 5, arranges outside a part of tower reactor waste water that the dehydrating tower is produced, and another part tower reactor waste water returns described common
Boiling rectifying column, returns to the tower reactor wastewater flow rate of the azeotropy rectification column, is hydrogenated with according to the aqueous acetone for entering the azeotropy rectification column
The water content of product is adjusted；
Step 6, stockline is gone out using the heavy constituent for being arranged at the azeotropy rectification column side, by the azeotropy rectification column output
Heavy constituent discharge.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, in step 5, returns to the tower of the azeotropy rectification column
Kettle wastewater flow rate, the water content that should meet the mix and convert thing produced after tower reactor wastewater flow rate and the feed material mix and convert for causing to return exists
1%~10%.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, according to the isopropanol of the azeotropy rectification column output
When purity reaches more than 99.96%, the isopropanol qualified products of the azeotropy rectification column are extracted out.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the isopropanol qualified products reach for purity
More than 99.96% isopropanol.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the acetone hydrogenation product aqueous 1%~10%；
Containing acetone 0.01%~5%.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the entrainer is alkane, and the alkane includes
Isopropyl ether, C 5 alkane, the alkane of carbon six, the alkane of carbon seven and hexamethylene.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, alkane of the preferred boiling point of entrainer less than 70 DEG C
Hydrocarbon.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the azeotropy rectification column is provided with a feeding line, institute
State the first half that feeding line is arranged at the azeotropy rectification column.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the feeding line of the azeotropy rectification column be arranged at away from
At the 1/3 of the azeotropic distillation top of tower.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the water layer is located at gun barrel bottom, institute
Oil reservoir is stated positioned at the knockout drum bottom.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the tower number of theoretical plate of the dehydrating tower for 15~
50, reflux ratio is 2：20.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, is provided with the middle part above position of the dehydrating tower
One water inlet, the bottom of the gun barrel is connected by a pipeline with the water inlet of the dehydrating tower.
The method of above-mentioned aqueous acetone hydrogenation products separating isopropanol, in step 2, using the gun barrel to institute
When stating tower top azeotropic mixture and carrying out water-oil separating, when the tower top azeotropic mixture profit is not stratified, injecting water into gun barrel makes institute
State tower top azeotropic mixture water-oil separating.
A kind of above-mentioned method suitable for aqueous acetone hydrogenation products separating isopropanol, the azeotropy rectification column is board-like
Tower or the packed tower with separating effect.
Present invention additionally comprises a kind of device of aqueous acetone hydrogenation products separating isopropanol, including：
The hydrogenation reaction of one azeotropy rectification column, the feeding line of the azeotropy rectification column and a generation aqueous acetone hydrogenation products
Device is connected, and one is provided with the top of the azeotropy rectification column and goes out stockline for the extraction of tower top azeotropic mixture, it is described go out stockline and the oil
Water separation tank is connected, and the side of the azeotropy rectification column is provided with the side line for extracting isopropanol qualified products out, the azeotropic distillation
The bottom of tower is provided with and for the heavy constituent that the heavy constituent of the azeotropy rectification column output is discharged to go out stockline；
One is used to the gun barrel that the tower top Azeotrope separation is water layer and oil reservoir, the gun barrel it is upper
Portion is connected with the azeotropy rectification column, and the bottom of the gun barrel is connected with the dehydrating tower, and the water layer is located at profit
Knockout drum bottom, the oil reservoir is located at the gun barrel bottom；
One dehydrating tower, the bottom with the gun barrel is connected, and the dehydrating tower is provided with a tower top and goes out stockline and a tower
Kettle waste water goes out stockline, and the tower top goes out stockline and is connected with the hydrogenation reactor, and the tower reactor waste water goes out stockline with the azeotropic
The feeding line connection of rectifying column.
The device of above-mentioned aqueous acetone hydrogenation products separating isopropanol, it is characterised in that the tower reactor waste water goes out stockline
Discharged branch line and the second tower reactor waste water discharging branch line including the first tower reactor waste water, the first tower reactor waste water discharging branch line with it is described
Azeotropy rectification column is connected, and a tower reactor waste water part for the dehydrating tower output enters institute through the first tower reactor waste water discharging branch line
Azeotropy rectification column is stated, another part tower reactor waste water outside the second tower reactor waste water discharging branch line through discharging.
The device of above-mentioned aqueous acetone hydrogenation products separating isopropanol, is provided with the middle part above position of the dehydrating tower
One water inlet, the bottom of the gun barrel is connected by a pipeline with the water inlet of the dehydrating tower.
The device of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the feeding line of the azeotropy rectification column is arranged at institute
State the first half of azeotropy rectification column.
The device of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the feeding line of the azeotropy rectification column be arranged at away from
At the 1/3 of the azeotropic distillation top of tower.
The device of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the acetone hydrogenation product aqueous 1%~10%；
It is 0.01%~5% containing amounts of acetone.
The device of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the tower number of theoretical plate of the dehydrating tower is
15~50, reflux ratio is 2：20.
The device of above-mentioned aqueous acetone hydrogenation products separating isopropanol, the azeotropy rectification column be plate column or with point
From the packed tower of effect.
The device and method of the aqueous acetone hydrogenation products separating isopropanol that the present invention is provided, just with two towers
The refined of isopropanol is realized, i.e., realizes that acetone hydrogenation product is separated by azeotrope column and dehydrating tower two-tower process, with respect to three tower streams
Journey, reduces investment and energy consumption, the separation costs that acetone hydrogenation method produces isopropanol is reduced, while can also process containing
The hydrogenation products of water acetone, reduce the cost of material of acetone in future.This method is prepared using azeotropic distillation and conventional distillation principle
High-purity isopropanol, it is simple that energy consumption consumes low, flow, it is easy to operates.
Brief description of the drawings
Fig. 1 is the structural representation of the aqueous acetone hydrogenation products separating isopropanol device of one embodiment of the invention.
Wherein, reference：
1st, hydrogenation reactor
2nd, azeotropy rectification column
21 feeding lines
3rd, stockline is gone out
4th, oil reservoir
5th, gun barrel
6th, water layer
7th, dehydrating tower
8th, tower top goes out stockline
9th, the first tower reactor waste water discharging branch line
10th, the second tower reactor waste water discharging branch line
11st, heavy constituent goes out stockline
12nd, side line
Specific embodiment
Structural principle of the invention and operation principle are described in detail below in conjunction with the accompanying drawings：
The device that a kind of acetone hydrogenation production isopropanol that the present invention is provided is separate, including azeotropy rectification column 2, water-oil separating
Tank 5, dehydrating tower 7, the feeding line 21 of azeotropy rectification column 2 are connected with the hydrogenation reactor 1 of a generation aqueous acetone hydrogenation products, contain
After water acetone hydrogenation product is through the rectifying of azeotropy rectification column 2, from the top extraction top azeotropic mixture of azeotropy rectification column 2, azeotropic distillation
The bottom extraction heavy constituent of tower 2, further, the feeding line 21 of azeotropy rectification column is arranged at away from azeotropic distillation top of tower 1/3.
When the purity of the isopropanol that azeotropy rectification column rectifying goes out reaches more than 99.6%, positioned at the side line 12 of the side of azeotropy rectification column
A part of isopropanol qualified products are extracted out, isopropanol qualified products are isopropanol of the purity up to more than 99.96%, acetone adds
Hydrogen product aqueous 1%~10%；Containing acetone 0.01%~5%.
The bottom of azeotropy rectification column 2 is provided with and for the heavy constituent that the heavy constituent of the output of azeotropy rectification column 2 is discharged to go out stockline 11；Altogether
The top of boiling rectifying column 2 is provided with one and goes out stockline 3, and the tower top azeotropic mixture of the top of azeotropy rectification column 2 extraction enters profit by going out stockline 3
Tower top Azeotrope separation is water layer 6 and oil reservoir 4 by knockout drum 5, gun barrel 5, and water layer 6 is located at gun barrel bottom, oil
Layer 4 is located at the top of gun barrel 5, and the top of gun barrel 5 is connected with azeotropy rectification column 2, the bottom of gun barrel 5 and
Dehydrating tower 7 is connected, and the bottom of gun barrel is connected by a pipeline with dehydrating tower 7, is set at the middle part above position of dehydrating tower 7
One water inlet, the water layer of gun barrel injects the water inlet of dehydrating tower 7 by a pipeline.
Dehydrating tower 7 is provided with a tower top and goes out the tower reactor waste water of stockline 8 and and goes out stockline, and tower top goes out stockline 8 and is back to acetone hydrogenation
Reactor 1, tower reactor waste water goes out stockline and boils rectifying column connection together.Tower reactor waste water goes out stockline includes the first tower reactor waste water discharging branch line
9 and the second tower reactor waste water discharging branch line 10, the feeding line of the first tower reactor waste water discharging branch line 10 and the azeotropy rectification column of dehydrating tower
21 connections, a tower reactor waste water part for dehydrating tower output enters azeotropy rectification column 2 through the first tower reactor waste water discharging branch line 9, another
Part tower reactor waste water is discharged through the second tower reactor waste water discharging branch line 10 is outer.
The invention also discloses a kind of method of aqueous acetone hydrogenation products separating isopropanol, acetone hydrogenation product is through azeotropic
The isopropanol that purity is up to more than 99.96% is obtained after rectifying column, dehydrating tower.Specifically include：
Step 1, adds azeotropic distillation using the aqueous acetone hydrogenation products from hydrogenation reactor as feed material first
Tower carries out azeotropic distillation, while forming binary azeotrope toward addition in azeotropy rectification column and acetone and forming three with water and isopropanol
The entrainer of first azeotropic mixture, entrainer promotion acetone is separated with isopropanol and water-azeotropic thing is separated with isopropanol；
Wherein acetone hydrogenation reactant aqueous 1%-10%, 0.01-5% containing acetone, the entrainer for being used is isopropyl ether, light dydrocarbon alkane
The alkane of hydrocarbon, the alkane of carbon six, the alkane of carbon seven and hexamethylene, preferably boiling point less than 70 DEG C, azeotropy rectification column is provided with a feeding line,
The feeding line of azeotropy rectification column is arranged at the first half of azeotropy rectification column, and away from azeotropic distillation top of tower 1/3 at.The present invention is adopted
Azeotropy rectification column is plate column or the packed tower with separating effect.
Step 2, gun barrel is injected by the tower top azeotropic mixture of azeotropy rectification column output, using gun barrel by tower top
Azeotropic mixture is divided into oil reservoir and water layer or the referred to as liquid phase of weight two, and light phase (oil phase) returns tower top as reflux cycle.Heavy phase (water
Layer) enter dehydrating tower, control inlet amount makes layering tank liquid phase circle position constant.Water layer is located at gun barrel bottom, and oil reservoir is located at and divides
From tank top, the oil reservoir of gun barrel returns to azeotropy rectification column as the first backflow material, and the water layer of gun barrel passes through
One pipeline is connected with dehydrating tower, and dehydrating tower middle part sets a water inlet above position, and the water layer of gun barrel is by the pipe
Road injects the water inlet of dehydrating tower.Further, in step 2, when carrying out water-oil separating to tower top azeotropic mixture using gun barrel,
When tower top azeotropic mixture profit is not stratified, water is added to make tower top azeotropic mixture water-oil separating.Place add water at azeotropy rectification column feeding line
Or profit water distributing can, the water of addition is from device is outer or tower reactor waste water from dehydrating tower.
Step 3, according to acetone hydrogenation product isopropanol product purity require, that is, when isopropanol purity requirement more than etc.
When 99.96%, using the azeotropy rectification column side line for being arranged at azeotropy rectification column side, a part of isopropanol qualified products are taken out
Go out, isopropanol qualified products are isopropanol of the purity up to more than 99.96%.
Step 4, hydrogenation reactor circulation profit is returned using the overhead product of dehydrating tower as acetone hydrogenation reaction mass component
With as azeotropy rectification column charging addition azeotropy rectification column after hydrogenated reactor for treatment；
Step 5, by the first outer row, another part tower reactor waste water is used as for a part of tower reactor waste water that dehydrating tower is produced
Two backflow materials point return to feed pipe by the first tower reactor waste water discharging branch line, return to the tower reactor wastewater flow rate of azeotropy rectification column, should
The water content of the mix and convert thing produced after the tower reactor wastewater flow rate and azeotropy rectification column feed material mix and convert for causing to return is met in 1-
10%.The overhead product of water in other acetone hydrogenation reactant from raw material acetone or from dehydrating tower.The present invention is used
Dehydrating tower tower number of theoretical plate be 15~50, reflux ratio is 2：20.
Step 6, stockline is gone out using the heavy constituent for being arranged at azeotropy rectification column side, by the heavy constituent of azeotropy rectification column output
Discharge.
It is further, the effect that the device and method that description using acetone hydrogenation production isopropanol separate are reached,
Especially exemplified by following examples.
Embodiment 1, the water content of acetone hydrogenation product is 2%, and content of acetone is 1%, 4- methyl anyl alcohols 0.04%, isopropyl
Alcohol 96.96%, acetone hydrogenation product injects azeotropy rectification column with the speed of 13 ton hours.Azeotropy rectification column totally 35 pieces of theoretical plates,
The feeding line of azeotropy rectification column is in the 8th piece of theoretical plate (from top to bottom), using n-hexane as dehydrating agent.Azeotropy rectification column
11.5 tons of the amount of the qualified isopropanol of side take-off, extraction position is in 33 theoretical plates, and the tower top from azeotropy rectification column is total to
Boiling material is cooled to 25 DEG C, and profit layering is carried out to tower top azeotropic material using gun barrel, and gun barrel upper strata is oil
Layer material, lower floor is water layer material, be back to the 1st theoretical plate of azeotropy rectification column after the preheating of oil reservoir material, and oil reservoir material is returned
The ton hour of flow velocity degree 49.The water layer material on gun barrel upper strata injects dehydration by a pipeline with the speed of 1.4 ton hours
Tower, the number of theoretical plate of dehydrating tower is 30 pieces, and the water inlet of dehydrating tower is located at the 20th theoretical plate, and the tower top material of dehydrating tower passes through tower
Ejection stockline rate of withdrawal is 1.13 ton hours, the tower top material aqueous 9.5% of dehydrating tower, isopropanol 62.2%, acetone
11.5%th, n-hexane 16.8%.The tower reactor waste water of dehydrating tower goes out stockline and discharges by tower reactor waste water, and the water concentration of tower reactor waste water is big
In 99.9%.Aforesaid operations, the precision of the isopropanol of extraction is 99.96%, and heat consumption is：Azeotropy rectification column heating load
8000 kilowatts, 800 kilowatts of dehydrating tower heating load.
Embodiment 2, acetone hydrogenation product includes：Aqueous 3.8%, acetone 1%, 4- methyl anyl alcohols 0.04%, isopropanol
95.15%.Acetone hydrogenation product injects azeotropy rectification column inlet amount with the speed of 13.12 ton hours.The azeotropy rectification column of use
35 pieces of theoretical plates, the feeding line of azeotropy rectification column is in the 8th piece, and it is dehydrating agent to use n-hexane, and the side line of azeotropy rectification column is adopted
11.5 tons of output, the side line of azeotropy rectification column is located at the 33rd piece of theoretical plate, will be cooled down from azeotropy rectification column tower top azeotropic material
To 25 DEG C, using gun barrel to tower top azeotropic material layering, the oil reservoir material on gun barrel upper strata, lower floor is water layer thing
Material, is back to the 1st piece of theoretical plate of azeotropy rectification column after the preheating of oil reservoir material, back-flow velocity is 56.1 ton hours.Water-oil separating
The water layer material of tank lower floor injects dehydrating tower by a pipeline with 1.84 ton hour speed.The water inlet position of dehydrating tower is located at
20th theoretical plate, dehydrating tower is provided with 30 pieces of theoretical plates, and the tower top material of dehydrating tower goes out stockline and produces by tower top, its rate of withdrawal
It is 1.48 ton hours, the tower top material aqueous 9.7% of dehydrating tower, isopropanol 64.08%, acetone 8.8%, n-hexane 17.4%.
Dehydrating tower bottom recovered water, water concentration is more than 99.9%.Operated more than, azeotropic distillation chats the isopropanol purity of lateral line withdrawal function
99.96%.9210 kilowatts of azeotropy rectification column heating load, 1060 kilowatts of dehydrating tower load.
Embodiment 3, acetone hydrogenation product includes aqueous 0.5%, acetone 1%, 4- methyl anyl alcohols 0.04%, isopropanol
98.46%, acetone hydrogenation product injects azeotropy rectification column with the speed of 12.8 ton hours, and the tower top material of azeotropy rectification column exists
It is not stratified in gun barrel, water is added the water inlet or gun barrel of azeotropy rectification column with 200 kgs/hour of flow
In so that tower top material layering, oil reservoir backflow, result and same embodiment 1 after operation balance.
Embodiment 4, acetone hydrogenation product includes aqueous 2%, acetone 1%, 4- methyl anyl alcohols 0.04%, isopropanol
96.96%, acetone hydrogenation product is injected into azeotropy rectification column with 13 ton hour inlet amounies.Azeotropy rectification column is provided with 35 pieces of theories
Plate, the feed entrance point of azeotropy rectification column is arranged at the 8th piece of theoretical plate, and it is dehydrating agent to use n-hexane.Azeotropy rectification column survey line is adopted
Go out the amount of isopropanol for 11.5 tons, extraction position is in the 33rd piece of theoretical plate, and the tower top material of azeotropy rectification column output is cooled down
To 25 DEG C, the azeotropic distillation column overhead azeotropic mixture material after cooling is layered using gun barrel, gun barrel upper strata is oil
Layer material, lower floor is water layer material, and the 1st piece of reason of azeotropy rectification column is back to after the oil reservoir material preheating on gun barrel upper strata
By plate, capacity of returns is 49 ton hours, and gun barrel lower floor is produced for water layer material, i.e. water layer material with 1.4 ton hour amounts
To dehydrating tower, dehydrating tower is provided with 30 pieces of theoretical plates, and the charging aperture of dehydrating tower is located at the 20th piece of theoretical plate, the overhead product of dehydrating tower
Produced quantity be 1.13 ton hours, overhead product aqueous 9.5%, isopropanol 62.2%, acetone 11.5%, n-hexane 16.8%.
Dehydrating tower bottom produces tower reactor waste water, and water concentration is more than 99.9%.Operate above, the isopropanol purity 99.96% of side take-off.Altogether
8000 kilowatts of boiling rectifying column heating load, 800 kilowatts of dehydrating tower load.
To sum up, the method and device of the aqueous acetone hydrogenation products separating isopropanol that the present invention is provided, just with two
Tower is to be capable of achieving refining for isopropanol, i.e., realize that acetone hydrogenation product is separated by azeotrope column and dehydrating tower two-tower process, relatively
Three-column process flow, reduces investment and energy consumption, the separation costs that acetone hydrogenation method produces isopropanol is reduced, while also may be used
The hydrogenation products of aqueous acetone are processed, the cost of material of acetone in future is reduced.This method is former using azeotropic distillation and conventional distillation
Reason prepares high-purity isopropanol, and it is simple that energy consumption consumes low, flow, it is easy to operates.
Claims (23)
1. a kind of method of aqueous acetone hydrogenation products separating isopropanol, it is characterised in that methods described includes：
Step 1, adds azeotropy rectification column to enter using the aqueous acetone hydrogenation products from hydrogenation reactor as feed material first
Row azeotropic distillation, while toward adding entrainer in the azeotropy rectification column；
Step 2, gun barrel is injected by the tower top azeotropic mixture of the azeotropy rectification column output, will be described using gun barrel
Tower top azeotropic mixture is divided into oil reservoir and water layer, and the oil reservoir of the gun barrel returns to the azeotropic distillation as the first backflow material
Tower, the water layer of the gun barrel enters dehydrating tower；
Step 3, the requirement of the isopropanol purity according to the azeotropy rectification column output, using being arranged at the azeotropy rectification column one
The azeotropy rectification column side line of side, isopropanol qualified products are extracted out.
2. the method for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 1, it is characterised in that also include：
Step 4, returns to the overhead product of dehydrating tower the hydrogenation reactor and recycles as the second backflow material, hydrogenated
After reactor for treatment the azeotropy rectification column is added as azeotropy rectification column feed material；
Step 5, arranges outside a part of tower reactor waste water that the dehydrating tower is produced, and another part tower reactor waste water returns to the azeotropic essence
Tower is evaporated, the tower reactor wastewater flow rate of the azeotropy rectification column is returned, according to the aqueous acetone hydrogenation products for entering the azeotropy rectification column
Water content adjust；
Step 6, stockline is gone out using the heavy constituent for being arranged at the azeotropy rectification column side, by the weight of the azeotropy rectification column output
Component is discharged.
3. the method for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 2, it is characterised in that in step 5, return
The tower reactor wastewater flow rate of the azeotropy rectification column is returned, should meet produced after causing the tower reactor wastewater flow rate for returning and the feed material mix and convert
The water content of raw mix and convert thing is 1%~10%.
4. the method for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 1, it is characterised in that according to described common
When the isopropanol purity for boiling rectifying column output reaches more than 99.96%, the isopropanol qualified products of the azeotropy rectification column are taken out
Go out.
5. the method for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 1, it is characterised in that：The isopropanol
Qualified products are isopropanol of the purity up to more than 99.96%.
6. the method for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 1, it is characterised in that the acetone adds
Hydrogen product aqueous 1%~10%；Containing acetone 0.01%~5%.
7. the method for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 1, it is characterised in that：The entrainer
It is alkane, the alkane includes isopropyl ether, C 5 alkane, the alkane of carbon six, the alkane of carbon seven and hexamethylene.
8. the method for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 7, it is characterised in that：The entrainer
It is preferred that alkane of the boiling point less than 70 DEG C.
9. the method for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 1, it is characterised in that the azeotropic essence
Evaporate tower and be provided with a feeding line, the feeding line is arranged at the first half of the azeotropy rectification column.
10. the method for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 9, it is characterised in that the azeotropic
The feeding line of rectifying column is arranged at away from the azeotropic distillation top of tower 1/3.
The method of 11. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 1, it is characterised in that the water layer
Positioned at gun barrel bottom, the oil reservoir is located at the knockout drum bottom.
The method of 12. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 1, it is characterised in that the dehydration
The tower number of theoretical plate of tower is 15~50, and reflux ratio is 2：20.
The method of 13. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 1, it is characterised in that the dehydration
It is provided with a water inlet at the middle part above position of tower, the bottom of the gun barrel is entered by a pipeline and the dehydrating tower
The mouth of a river connects.
The method of 14. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 1, it is characterised in that in step 2,
When carrying out water-oil separating to the tower top azeotropic mixture using the gun barrel, when the tower top azeotropic mixture profit is not stratified,
Injecting water into gun barrel makes the tower top azeotropic mixture water-oil separating.
A kind of 15. methods suitable for aqueous acetone hydrogenation products separating isopropanol as claimed in claim 1, its feature exists
In the azeotropy rectification column is plate column or the packed tower with separating effect.
A kind of 16. devices of aqueous acetone hydrogenation products separating isopropanol, it is characterised in that including：
The hydrogenation reactor of one azeotropy rectification column, the feeding line of the azeotropy rectification column and a generation aqueous acetone hydrogenation products connects
Connect, one be provided with the top of the azeotropy rectification column and go out stockline for the extraction of tower top azeotropic mixture, it is described go out stockline and the profit point
From tank connection, the side of the azeotropy rectification column is provided with the side line for extracting isopropanol qualified products out, the azeotropy rectification column
Bottom is provided with and for the heavy constituent that the heavy constituent of the azeotropy rectification column output is discharged to go out stockline；
One is used to the gun barrel that the tower top Azeotrope separation is water layer and oil reservoir, the top of the gun barrel with
The azeotropy rectification column connection, the bottom of the gun barrel is connected with the dehydrating tower, and the water layer is located at water-oil separating
Tank bottom, the oil reservoir is located at the gun barrel bottom；
One dehydrating tower, the bottom with the gun barrel is connected, and the dehydrating tower is provided with a tower top, and to go out stockline and a tower reactor useless
Water goes out stockline, and the tower top goes out stockline and is connected with the hydrogenation reactor, and the tower reactor waste water goes out stockline with the azeotropic distillation
The feeding line connection of tower.
The device of 17. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 16, it is characterised in that the tower reactor
Waste water goes out stockline includes the first tower reactor waste water discharging branch line and the second tower reactor waste water discharging branch line, the first tower reactor waste water discharging
Branch line is connected with the azeotropy rectification column, and a tower reactor waste water part for the dehydrating tower output discharges through the first tower reactor waste water
Branch line enters the azeotropy rectification column, and another part tower reactor waste water outside the second tower reactor waste water discharging branch line through discharging.
The device of 18. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 16, it is characterised in that the dehydration
It is provided with a water inlet at the middle part above position of tower, the bottom of the gun barrel is entered by a pipeline and the dehydrating tower
The mouth of a river connects.
The device of 19. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 16, it is characterised in that the azeotropic
The feeding line of rectifying column is arranged at the first half of the azeotropy rectification column.
The device of 20. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 19, it is characterised in that the azeotropic
The feeding line of rectifying column is arranged at away from the azeotropic distillation top of tower 1/3.
The device of 21. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 16, it is characterised in that the acetone
Hydrogenation products aqueous 1%~10%；It is 0.01%~5% containing amounts of acetone.
The device of 22. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 16, it is characterised in that the dehydration
The tower number of theoretical plate of tower is 15~50, and reflux ratio is 2：20.
The device of 23. aqueous acetone hydrogenation products separating isopropanols as claimed in claim 16, it is characterised in that the azeotropic
Rectifying column is plate column or the packed tower with separating effect.
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Cited By (1)
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| CN115259999A (en) * | 2022-07-25 | 2022-11-01 | 淮南中建材腾锋环保科技有限公司 | High-efficiency separation process and equipment for water-containing isopropanol |
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Application publication date: 20170630 |