CN109771980A - A kind of heterogeneous azeotropic rectification method separating 2 pentanone, 4- heptanone, water and carbon dioxide mixture - Google Patents
A kind of heterogeneous azeotropic rectification method separating 2 pentanone, 4- heptanone, water and carbon dioxide mixture Download PDFInfo
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Abstract
The present invention provides a kind of separation 2 pentanone 4- heptanone, the heterogeneous azeotropic rectification method of water and carbon dioxide mixture is by 2 pentanone to be separated, 4- heptanone, water and carbon dioxide raw material enter the left half side carry out gas-liquid separation of next door tower from the material inlet to be separated of next door tower, gas phase comes out from gaseous phase outlet enters condenser, condensate liquid is in the isolated carbon dioxide enriched vapour phase of vapour-liquid-liquid/gas separator, rich ketone phase and water-rich phase, it is half side that rich ketone mutually passes back into a next door tower left side, it is half side that water-rich phase passes back into the next door tower right side, extraction obtains carbon dioxide enriched gas and carries out speeding to put, the tower reactor that rich ketone mutually enters rectifying column obtains 4- heptanone product, the gas phase come out at the top of rectifying column is condensed using rectifying column condenser, a part flows back into rectifying column, another part obtains 2 pentanone product.The advantages of present invention has good separating effect, can significantly save equipment investment expense and installation space.
Description
Technical field
The present invention relates to mixed keton aqueous systems separation rectification process system, especially mixing acid cleavage 2 pentanone/
The downstream product separation field of 4- heptanone.
Background technique
Acetic acid is reacted with n-butyric acie can be obtained 2 pentanone/4- heptanone/water mixture, if the mixture does not add further
Work, it is difficult to meet marketing purity requirement.Therefore, it is badly in need of solving 2 pentanone/4- heptanone/water/carbon dioxide mixture
Separation and purification problem.
Although Luben WL (Luyben WL.Energy&Fuels, 2008,22,4249-4258) has studied heterogeneous total
The control of rectifying separation n-butanol-water system is boiled, but this research only limits binary system, separates mainly for n-butanol/water.
Since 2 pentanone, 4- heptanone form heterogeneous minimum boiling point azeotropic mixture with water respectively, component is difficult to realize with conventional distillation
High-purity separation, recent Xia etc. (Xia M.Ind.&Eng. Chem.Res., 2018,57,689-702) have studied for this mixing
Objects system proposes corresponding technological design and dynamic controls, but three rectifying columns of process requirement of paper proposition and one point
From device, equipment investment expense is larger, and equipment degree of integration is not high.
Summary of the invention
The object of the present invention is to provide a kind of good separating effect, can significantly save equipment investment expense and installation space and
Separate the heterogeneous azeotropic rectification method of 2 pentanone, 4- heptanone, water and carbon dioxide mixture.
The present invention provides a kind of for the non-equal of the reaction product 2 pentanone, 4- heptanone, water and carbon dioxide separation
Phase azeotropic distillation method is by a next door tower, a common rectifying tower and vapour-liquid-liquid/gas separator rectification process
With rectifier unit, it can be achieved that 2 pentanone/4- heptanone/water/carbon dioxide object system separation, obtains the purity that accords with the demands of the market
Product, while can substantially save equipment investment expense and installation space.
Method of the invention, including configure as follows and step:
(1) by 2 pentanone to be separated, 4- heptanone/, the material inlet to be separated of water and carbon dioxide raw material from next door tower
Half side (referred to as: on the left of next door) into a next door tower left side, reboiler boils offer reboiler again and boils offer heat again on the left of next door
Effect is lower to carry out gas-liquid separation, and gas phase comes out from the gaseous phase outlet of next door tower enters condenser, and the condensate liquid of acquisition enters vapour-
Liquid liquid separator is insulated, constant voltage operation, and it is flat that the residence time of experience 10- 30min carries out sufficient vapour-liquid-liquid
After weighing apparatus, isolated carbon dioxide enriched vapour phase, rich ketone phase and water-rich phase, rich ketone are mutually passed back on the left of next door, and water-rich phase passes back into
The next door tower right side is half side (referred to as: on the right side of next door), and extraction obtains carbon dioxide enriched gas and carries out speeding to put, and rich ketone mutually enters subsequent rectifying column
In 7；
This step operation condition:
Tower top temperature on the left of next door: 85-110 DEG C, preferably 90-100 DEG C
Column bottom temperature on the left of next door: 130-170 DEG C
Tower top operating pressure on the left of next door: 0.5-5bar
Tower top temperature on the right side of next door: 85-110 DEG C
Column bottom temperature on the right side of next door: 110-140 DEG C.
The operating pressure of tower top on the right side of next door: 0.5-5bar
The operation temperature of condenser: 40-60 DEG C
The operating pressure of condenser: 0.5-5bar
Vapour-liquid-liquid/gas separator operation temperature: adiabatic operation, 40-60 DEG C
Vapour-liquid-liquid/gas separator operating pressure: for 0.5-5bar
Reaction product mixed liquor charging as described above is not only limited to feed on the left of next door, can also feed vapour-
Liquid liquid separator charging, or can feed and be fed on the left of next door with vapour-liquid-liquid/gas separator simultaneously；
(2) the rich ketone that tower reactor obtains on the left of next door mutually enters rectifying column, is boiled again by rectifying tower reboiler, in rectifying tower
Kettle obtains 4- heptanone product, and from the gas phase of rectifying column top out using the condensation of rectifying column condenser, condensate liquid enters essence
Tower return tank is evaporated, a part flows back into rectifying column, and another part obtains 2 pentanone product；
This step operation condition:
The tower top temperature of rectifying column: 95-110 DEG C,
The column bottom temperature of rectifying column: 195-220 DEG C
The operating pressure of the tower top of rectifying column: 0.5-2bar
(3) reboiler boils again on the right side of the water-rich phase next door passed back on the right side of next door is provided under heat effect, to water-rich phase
It is separated again, obtained gas phase comes out from gaseous phase outlet enters condenser together with the gas phase come out on the left of next door.
On the left of next door as described above, on the right side of next door and rectifying column can be used packed tower, plate column or packed tower with it is board-like
The combining form of tower, selected filler can be Pall ring, Raschig ring, θ ring, structured packing etc., and all are known to those skilled in the art
Type, selected column plate can be all classes known to those skilled in the art such as sieve tray, bubble cap tray, float valve tray
Type；All three phase separators known to those skilled in the art can be used in the vapour-liquid-liquid/gas separator 4.
Specifically, what the next door left side of the next door tower, next door right side tower top steamed is rich in 2 pentanone/water/solution gas
Logistics be condensed by the condenser to 40-60 DEG C (preferably 48-53 DEG C), to use relatively inexpensive cooling water (32-42 DEG C)；
Condensed logistics is divided into carbon dioxide enriched vapour phase, rich ketone phase and water-rich phase, carbon dioxide enriched vapour in three phase separator and carries out
It speeds to put, rich ketone mutually squeezes into tower top on the left of next door, and water-rich phase squeezes into tower top on the right side of next door.By the implementation of rectifier unit, next door is left
Side tower bottom produces mixed keton, and the waste water of the tower bottom extraction trace of amount containing ketone on the right side of next door, wherein mixed keton enters rectifying column, realizes two
Class ketone is kept completely separate.
On the left of the next door of the next door tower and on the right side of next door, number of theoretical plate is suitable, is 15-40, on the left of next door 1 into
Flitch position is 5-15, controls next door column overhead pressure in 0.5-5bar, 85-110 DEG C of the operation temperature of tower top, tower reactor temperature
Degree is determined by tower top pressure and the number of plates, under the conditions of tower top pressure is respectively 0.5,1.1 and 5bar, passes through adjusting reboiler
Heating amount controls bottom temperature on the left of next door respectively in 130-135,135-140 and 160-170 DEG C；It is boiled again by adjusting
The heating amount of device controls bottom temperature respectively in 105-115,110-120 and 135-140 DEG C.Under above-mentioned process conditions,
Next door left side top and next door right hand top produce the azeotropic based on rich carbonated 2 pentanone/4- heptanone/water
Object enters condenser after merging at the top of partition, tower bottom produces mixed keton on the left of next door, and tower bottom produces ketone containing trace on the right side of next door
Waste water.
The rectifying column is common rectifying tower, and number of theoretical plate 25-45, charging Board position is 10-25, controls tower top
Pressure is between 0.5-5.0bar, and between 95-110 DEG C of operation temperature of tower top, bottom temperature is by tower top pressure and the number of plates
It determines, particularly, under the conditions of tower top pressure is respectively 0.5,1.1 and 5bar, by adjusting the heating amount of reboiler for tower reactor temperature
Degree is controlled respectively in 190-200,195-205 and 210-220 DEG C.Under above-mentioned process conditions, overhead extraction is commercially pure
2 pentanone, tower bottom obtain commercially pure 4- heptanone.
Vapour-liquid-the liquid/gas separator, temperature maintain between 40-60 DEG C, and temperature is controlled by condenser heat load,
Pressure maintains between 0.15-0.5bar, adiabatic operation.Under above-mentioned process conditions, vapour phase obtains carbon dioxide enriched, liquid phase
It is divided into rich ketone phase and water-rich phase, as its liquid-phase reflux, water-rich phase squeezes into the next door right side wherein rich ketone mutually squeezes into tower top on the left of next door
Side tower top is as its liquid-phase reflux.
For the better implementation present invention, a kind of next door tower is devised, it includes shell, lower head, upper cover, along shell
Axis direction has rectangular clapboard between shell, shell is divided on the left of next door and on the right side of next door, under rectangular clapboard bottom is through
End socket, go directly at the top of rectangular clapboard upper cover, or has segment space between upper cover, next door left upper portion have rich ketone mutually into
Mouthful, there is material inlet to be separated at middle part, and rich ketone phase reboiler import is arranged at lower part, and mixed keton is arranged at the lower head bottom on the left of next door
Outlet, next door right upper portion have water-rich phase import, and water-rich phase reboiler import, the lower head bottom on the right side of next door are arranged at lower part
There is water phase outlet, there is gaseous phase outlet at the top of upper cover.
The present invention have it is following innovative and the utility model has the advantages that
(1) compared with traditional azeotropic distillation, extraction and rectification separation method, this distillation system avoid introducing it is light/carry secretly again
Agent, but make full use of water to the entrainment effect of mixed keton and 2 pentanone/4- heptanone and water stratification principle, pass through separator
Split-phase makes concentration across rectifying boundary, reduces entrainer recovery tower quantity and reduces whole energy consumption, has simple process, equipment
The low feature of investment cost；
(2) it is compared with published correlative theses (Xia M.Ind.&Eng.Chem.Res., 2018,57,689-702),
By by original process lightness-removing column and dehydrating tower be integrated into a next door tower, reduce number of devices, thus reduce equipment throwing
Rate are used and installation space；
(3) technique disclosed through the invention, the 2 pentanone purity and the rate of recovery of acquisition respectively reach 99.5wt% and
99.9%, the 4- heptanone purity and the rate of recovery of acquisition are up to 99.5wt% and 99.9% respectively, while waste water purity reaches
99.9999wt% or more.
Detailed description of the invention
Fig. 1 be present system pressure in 1,5 and 10atm x-y scheme: (a) 2 pentanone/aqueous systems, (b) 4- heptanone/
Aqueous systems；
Fig. 2 is that present system pressure T-x-y in 1,5 and 10atm schemes: (a) 2 pentanone/aqueous systems and (b) 4- heptan
Ketone/aqueous systems；
Process flow chart Fig. 3 of the invention；
The structural schematic diagram of Fig. 4 next door tower of the present invention.
As shown, 1 is next door left side, 2 be condenser, and 3 be reboiler on the left of next door, and 4 be vapour-liquid-liquid/gas separator,
5 is on the right side of next door, 6 are reboiler on the right side of next door, and 7 be rectifying column, and 8 be rectifying column condenser, and 9 be rectifier column reflux tank, and 10 are
Rectifying tower reboiler, 11 be shell, and 12 be lower head, and 13 be upper cover, and 14 be rectangular clapboard, and 15 be rich ketone phase import, and 16 are
Material inlet to be separated, 17 export for rich ketone phase reboiler import, 18 for mixed keton, and 19 be water-rich phase import, and 20 be water-rich phase
Reboiler import, 21 export for water phase, and 22 be gaseous phase outlet.
The feasibility of separation method disclosed by the invention can be said by analysis vapor-liquid equilibrium x-y figure and T-x-y figure
It is bright.2 pentanone/water when system pressure is 1,5 and 10atm, 4-heptanone/water, two kinds of binary systems is set forth in Fig. 1 a, b
X-y figure, therefrom, it is evident that 2 pentanone/water, 4- heptanone/water have binary heterogeneous minimum boiling point at these pressures
Azeotropic mixture；Simultaneously as x-y line is remoter from diagonal line y=x, relative volatility is bigger, and separating difficulty is bigger, so pressure is got over
Height is bigger to separating difficulty, and the increase of separating difficulty is unobvious with pressure change when within 5atm.Therefore, the present invention uses
Tower top pressure be 0.5-5.0bar.2 pentanone/water, 4- when system pressure is 1,5 and 10atm is set forth in Fig. 2 a, b
The T-x-y of two kinds of binary systems of heptanone/water schemes.As shown, by taking system pressure is 5atm as an example, it is assumed that F is in azeotropic point for charging
Left side, then raw material can be in the low extraction B of tower after being passed through lightness-removing column12-purer pentanones are obtained, stripped overhead goes out nearly azeotropic mixture vapour
Body V1, this nearly azeotropic mixture be condensed to 40-60 DEG C after in two-phase section, this condensate liquid is divided by vapour-liquid-liquid/gas separator
For positioned at the rich ketone phase R of azeotropic point arranged on left and right sides1With water-rich phase R2, water-rich phase is located on the right side of azeotropic point, and it is de- to be squeezed into right side
After water tower, tower bottom produces B2In must can obtain the pure water of the trace containing ketone, stripped overhead goes out nearly azeotropic mixture steam V2It is condensed to
After 40-60 DEG C, this condensate liquid is in two-phase section, will can be from vapour phase in vapour-liquid-liquid/gas separator split-phase, a small amount of carbon dioxide
In speed to put.Also similar method can be used to analyze the separation of 4- heptanone/aqueous systems.Because of 2 pentanone/water, 4- heptanone/water
Scheme with similar xy, and shows similar distillation process with identical separation principle, while carbon dioxide is in system
Belong to readily removed light point, so 2 pentanone/4- heptanone/water/carbon dioxide system can be used this distillation system and realize
It is fully separating.
Specific embodiment
The present invention is further illustrated below with reference to example --- one kind is mixed for 2 pentanone/4- heptanone/water/carbon dioxide
Close the effect of the heterogeneous azeotropic rectification method of object separation.Obviously, illustrated embodiment is a part of the embodiment of the present invention, rather than
Whole embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work premise
Under every other embodiment obtained, belong to protection scope of the present invention.
Fig. 3 is 2 pentanone disclosed by the invention/4- heptanone/water/carbon dioxide separation distillation system process flow chart.
Controlled by the technological parameter to above-mentioned rectifier unit, using following rectification process can realize 2-pentanones/4- heptanone/
Water is kept completely separate.Raw material initially enters 1 on the left of the tower next door of next door, boils offer heating amount again by reboiler 3, obtains in its tower bottom
It, into the condenser 2 at top, is obtained after next door 1 overhead vapours of left side merges with 5 overhead vapours on the right side of next door to mixed keton
The condensate liquid obtained enters vapour-liquid-liquid/gas separator 4, is separated into carbon dioxide enriched vapour, water-rich phase and rich ketone phase logistics；Richness two
Carbonoxide vapour speeds to put, and rich ketone mutually enters 1 tower top on the left of next door, and, as its liquid-phase reflux, water-rich phase is entered 5 tower tops on the right side of next door
As its liquid-phase reflux；Ketone on the right side of next door in 5 pairs of water-rich phases does step stripping recycling, and tower bottom obtains seldom useless of amount containing ketone
Water, overhead vapor phase condense after merging with 1 overhead vapor phase on the left of next door, and condensate liquid enters separator 4 and completes closed loop, next door left side
The mixed keton of 1 bottom extraction enters rectifying column 7, obtains 2 pentanone product, overhead extraction 4- heptanone product in the column overhead.
Embodiment 1
A kind of next door tower, it includes shell 11, lower head 12, upper cover 13, along 11 axis direction of shell between shell 11
There is rectangular clapboard 14, shell 11 is divided into 5 on the right side of next door left side 1 and next door, go directly 14 bottom of rectangular clapboard lower head 12, square
Go directly upper cover 13 at the top of shape partition 14, or has segment space between upper cover 13, and rich ketone phase is arranged at 1 top on the left of next door
There is material inlet 16 to be separated at import 15, middle part, and rich ketone phase reboiler import 17, the lower head 12 in next door left side 1 are arranged at lower part
Bottom has mixed keton to export 18, and water-rich phase import 19 is arranged at 5 tops on the right side of next door, and water-rich phase reboiler import 20 is arranged at lower part,
5 12 bottom of lower head has water phase to export 21 on the right side of next door, there is gaseous phase outlet 22 at the top of upper cover 13.
A kind of heterogeneous azeotropic rectification method separating 2 pentanone 4- heptanone, water and carbon dioxide mixture, including such as
Lower step:
(1) the next door tower is to add a rectangular clapboard in shell axis direction in common rectifying tower interior parallel, by shell
It is divided into 5 on the right side of next door tower next door left side 1 and next door；Go directly shell lower head for partition bottom, and can go directly upper cover at the top of partition,
Can also at the top of it reserved part space；Partition and shell carry out welding or stamping connection；On the left of the tower bottom next door of next door 1 and every
5 are each configured with reboiler 3 and reboiler 6 on the left of wall, for providing tower two sides tower reactor reboiler heat；The configuration of next door top of tower
There are a condenser and vapour-liquid-liquid/gas separator；Enter condenser after merging from 5 overhead vapours on the right side of next door left side 1 and next door,
The condensate liquid of acquisition enters vapour-liquid-liquid/gas separator 4, is insulated, constant voltage operation, and the residence time of 30min is undergone to be filled
After the vapour-liquid divided-liquid balance, it is separated into carbon dioxide enriched vapour phase, rich ketone phase and water-rich phase；Rich ketone is mutually squeezed into 1 on the left of next door,
Water-rich phase is squeezed into 5 on the right side of next door；The charging of reaction product mixed liquor is not only limited to that vapour-can also be fed 1 on the left of charging next door
Liquid liquid separator 4, or next door left side 1 and vapour-liquid-liquid/gas separator 4 can be fed simultaneously；Pass through this next door tower and vapour-
Liquid liquid separator, 5 tower reactors of next door right side obtain the waste water of the trace of amount containing ketone, obtain in vapour-liquid-liquid/gas separator vapour phase extraction
Carbon dioxide enriched vapour is obtained, 1 tower reactor obtains the mixed keton of 2 pentanone and 4- heptanone on the left of next door, into subsequent rectifying column 7.
This step operation condition:
1 tower top temperature on the left of next door: 85 DEG C
1 column bottom temperature on the left of next door: 130.6 DEG C
The operating pressure of 1 tower top on the left of next door: 0.5bar
5 tower top temperatures on the right side of next door: 85 DEG C
5 column bottom temperatures on the right side of next door: 110.2 DEG C
The operating pressure of 5 tower tops on the right side of next door: 0.5bar
2 operation temperature of condenser: 40.2 DEG C
2 operating pressure of condenser: 0.5bar
4 operation temperature of vapour-liquid-liquid/gas separator: adiabatic operation, 40.2 DEG C
4 operating pressure of vapour-liquid-liquid/gas separator: 0.15bar
(2) mixed keton that 1 tower reactor obtains on the left of next door enters rectifying column 7, boiled again by 7 tower reactor reboiler 10 of rectifying column and
Rectifying column condenser 8 condenses, and obtains heavier 4- heptanone product in 7 tower reactor of rectifying column, obtains in 7 tower top of rectifying column lighter
2 pentanone product；
This step operation condition:
7 tower top temperature of rectifying column: 56 DEG C
7 column bottom temperature of rectifying column: 195.8 DEG C
The operating pressure of 7 tower top of rectifying column: 0.5bar
Specifically, what the next door left side 1 of the next door tower, 5 tower tops of next door right side steamed is rich in 2 pentanone/water/dissolution
The logistics of gas is condensed by condenser 2 to 40.2 DEG C, to use relatively inexpensive cooling water (32-42 DEG C)；Condensed logistics exists
It is divided into carbon dioxide enriched vapour, rich ketone phase and water-rich phase, carbon dioxide enriched vapour in three phase separator 4 to carry out speeding to put, rich ketone is mutually squeezed into
1 tower top on the left of next door, water-rich phase squeeze into 5 tower tops on the right side of next door.By the implementation of rectifier unit, the extraction of 1 tower bottom is mixed on the left of next door
Ketone is closed, the waste water of the 5 tower bottom extraction trace of amount containing ketone on the right side of next door, wherein mixed keton enters rectifying column 7, realizes the complete of two class ketone
It is fully separating.
5 on the right side of the next door left side 1 of the next door tower and next door, it is 20 that number of theoretical plate is suitable, feedboard on the left of next door
Position is 5, controls next door column overhead pressure in 0.5bar, 85 DEG C of the operation temperature of tower top, bottom temperature is by tower top pressure and tower
Plate number determines that the heating amount by adjusting reboiler 3 controls bottom temperature on the left of next door at 130-131 DEG C；By adjusting again
The heating amount for boiling device 6 controls bottom temperature at 110-111 DEG C.Under above-mentioned process conditions, on the left of next door 1 top and every
Azeotropic mixture on the right side of wall based on the rich carbonated 2 pentanone/4- heptanone/water of 5 tops extraction, merges at the top of partition
Enter condenser 2 afterwards, 1 tower bottom produces mixed keton on the left of next door, the waste water of 5 tower bottom extraction ketone containing trace on the right side of next door.
The rectifying column 7 is common rectifying tower, and number of theoretical plate 25, charging Board position is 13, and control tower top pressure exists
Between 0.5bar, 95 DEG C of the operation temperature of tower top, bottom temperature is determined by tower top pressure and the number of plates, by adjusting reboiler 10
Heating amount by bottom temperature control at 195-196 DEG C.Under above-mentioned process conditions, the commercially pure 2 pentanone of overhead extraction, tower
Bottom obtains commercially pure 4- heptanone.
Vapour-liquid-the liquid/gas separator 4, temperature maintain between 40.2 DEG C, and temperature is controlled by 2 thermic load of condenser,
Pressure maintains 0.15bar, adiabatic operation.Under above-mentioned process conditions, vapour phase obtains carbon dioxide enriched, and liquid phase is divided into rich ketone phase
And water-rich phase, wherein rich ketone mutually squeezes into 1 tower top on the left of next door, as its liquid-phase reflux, water-rich phase is squeezed into 5 tower tops on the right side of next door and is made
For its liquid-phase reflux.
1, next door right side 5 and rectifying column 7 are packed tower on the left of next door tower next door, using θ ring bulk loading filling material.
The present invention is made up of due to using above-mentioned rectificating method next door tower, rectifying column and vapour-liquid-liquid/gas separator
Heterogeneous azeotropic rectification system realize the separation of three components, can reach that conventional distillation cannot achieve is kept completely separate.
It is fed using the crude product in table 1 as distillation system, combined feed flow is 100000t/a, is calculated by simulation
The rectification process and rectifier unit of Application Example 1, three obtained product rectifying column separating resultings are listed in table 2, separator
Temperature is 40.2 DEG C, pressure 0.15bar, adiabatic operation, and vapour phase produces carbon dioxide, and rich ketone mutually squeezes into the 2nd plate of lightness-removing column work
For its liquid-phase reflux, water-rich phase squeezes into the 2nd plate of dehydrating tower as its liquid-phase reflux.
Slightly mixing ketone reaction products form table 1
| Crude reaction product | Acetic acid | 2 pentanone | 4- heptanone | Water | Carbon dioxide |
| Composition/mol% | ≤0.01 | 0.2 | 0.2 | 0.6 | ≤0.01 |
2 embodiment of table, 1 separating resulting
Embodiment 2
A kind of next door tower, it includes shell 11, lower head 12, upper cover 13, along 11 axis direction of shell between shell 11
There is rectangular clapboard 14, shell 11 is divided into 5 on the right side of next door left side 1 and next door, go directly 14 bottom of rectangular clapboard lower head 12, square
Go directly upper cover 13 at the top of shape partition 14, or has segment space between upper cover 13, and rich ketone phase is arranged at 1 top on the left of next door
Rich ketone phase reboiler import 17 arranged at import 15, lower part, and 1 12 bottom of lower head has mixed keton to export 18 on the left of next door, every
Water-rich phase import 19 is arranged at 5 tops on the right side of wall, and water-rich phase reboiler import 20,12 bottom of lower head on next door right side 5 are arranged at lower part
There is water phase to export 21, has gaseous phase outlet 22 at the top of upper cover 13, material inlet to be separated is arranged at vapour-liquid-liquid/gas separator top
16。
A kind of heterogeneous azeotropic rectification method separating 2 pentanone 4- heptanone, water and carbon dioxide mixture, including such as
Lower step:
(1) the next door tower is to add a rectangular clapboard in shell axis direction in common rectifying tower interior parallel, by shell
It is divided into 5 on the right side of next door tower next door left side 1 and next door；Go directly shell lower head for partition bottom, and can go directly upper cover at the top of partition,
Can also at the top of it reserved part space；Partition and shell carry out welding or stamping connection；On the left of the tower bottom next door of next door 1 and every
5 are each configured with reboiler 3 and reboiler 6 on the left of wall, for providing tower two sides tower reactor reboiler heat；The configuration of next door top of tower
There are a condenser and vapour-liquid-liquid/gas separator；Enter condenser after merging from 5 overhead vapours on the right side of next door left side 1 and next door,
The condensate liquid of acquisition enters vapour-liquid-liquid/gas separator 4, is insulated, constant voltage operation, and the residence time of 10min is undergone to be filled
After the vapour-liquid divided-liquid balance, it is separated into carbon dioxide enriched vapour phase, rich ketone phase and water-rich phase；Rich ketone is mutually squeezed into 1 on the left of next door,
Water-rich phase is squeezed into 5 on the right side of next door；The charging of reaction product mixed liquor is not only limited to that vapour-can also be fed 1 on the left of charging next door
Liquid liquid separator 4, or next door left side 1 and vapour-liquid-liquid/gas separator 4 can be fed simultaneously；Pass through this next door tower and vapour-
Liquid liquid separator, 5 tower reactors of next door right side obtain the waste water of the trace of amount containing ketone, obtain in vapour-liquid-liquid/gas separator vapour phase extraction
Carbon dioxide enriched vapour is obtained, 1 tower reactor obtains the mixed keton of 2 pentanone and 4- heptanone on the left of next door, into subsequent rectifying column 7.
This step operation condition:
1 tower top temperature on the left of next door: 90 DEG C
1 column bottom temperature on the left of next door: 138.1 DEG C
The operating pressure of 1 tower top on the left of next door: 1.1bar
5 tower top temperatures on the right side of next door: 90 DEG C
5 column bottom temperatures on the right side of next door: 116.4 DEG C
The operating pressure of 5 tower tops on the right side of next door: 1.1bar
2 operation temperature of condenser: 41 DEG C
2 operating pressure of condenser: 1.1bar
4 operation temperature of vapour-liquid-liquid/gas separator: adiabatic operation, 41 DEG C
4 operating pressure of vapour-liquid-liquid/gas separator: 0.3bar
(2) mixed keton that 1 tower reactor obtains on the left of next door enters rectifying column 7, boiled again by 7 tower reactor reboiler 10 of rectifying column and
Rectifying column condenser 8 condenses, and obtains heavier 4- heptanone product in 7 tower reactor of rectifying column, obtains in 7 tower top of rectifying column lighter
2 pentanone product；
This step operation condition:
7 tower top temperature of rectifying column: 100.1 DEG C
7 column bottom temperature of rectifying column: 201.2 DEG C
The operating pressure of 7 tower top of rectifying column: 1.1bar
Specifically, what the next door left side 1 of the next door tower, 5 tower tops of next door right side steamed is rich in 2 pentanone/water/dissolution
The logistics of gas is condensed by condenser 2 to 41 DEG C, to use relatively inexpensive cooling water (32-42 DEG C)；Condensed logistics is three
Be divided into carbon dioxide enriched vapour, rich ketone phase and water-rich phase, carbon dioxide enriched vapour in phase separator 4 to carry out speeding to put, rich ketone mutually squeeze into every
1 tower top on the left of wall, water-rich phase squeeze into 5 tower tops on the right side of next door.By the implementation of rectifier unit, the extraction of 1 tower bottom is mixed on the left of next door
Ketone, the waste water of the next door right side 5 tower bottom extraction trace of amount containing ketone, wherein mixed keton enters rectifying column 7, realizes dividing completely for two class ketone
From.
5 on the right side of the next door left side 1 of the next door tower and next door, it is 25 that number of theoretical plate is identical, feedboard on the left of next door
Position is 5, controls next door column overhead pressure in 1.1bar, 90 DEG C of the operation temperature of tower top, bottom temperature is by tower top pressure and tower
Plate number determines that the heating amount by adjusting reboiler 3 controls bottom temperature on the left of next door at 138-139 DEG C；It is de- by adjusting
The heating amount of water tower reboiler 6 controls bottom temperature at 116-117 DEG C.Under above-mentioned process conditions, 1 is pushed up on the left of next door
Azeotropic mixture on the right side of portion and next door based on the rich carbonated 2 pentanone/4- heptanone/water of 5 tops extraction, on partition top
Portion enters condenser 2 after merging, 1 tower bottom produces mixed keton on the left of next door, the waste water of 5 tower bottom extraction ketone containing trace on the right side of next door.
The rectifying column 7 is common rectifying tower, and number of theoretical plate 35, charging Board position is 17, and control tower top pressure exists
Between 1.1bar, 100.1 DEG C of the operation temperature of tower top, bottom temperature is determined by tower top pressure and the number of plates, is boiled again by adjusting
The heating amount of device 10 controls bottom temperature at 201-202 DEG C.Under above-mentioned process conditions, the commercially pure 2- penta of overhead extraction
Ketone, tower bottom obtain commercially pure 4- heptanone.
Vapour-liquid-the liquid/gas separator 4, temperature maintain between 41 DEG C, and temperature is controlled by 2 thermic load of condenser, pressure
Power maintains 0.3bar, adiabatic operation.Under above-mentioned process conditions, vapour phase obtain it is carbon dioxide enriched, liquid phase be divided into rich ketone phase and
Water-rich phase, wherein rich ketone mutually squeezes into 1 tower top on the left of next door, as its liquid-phase reflux, water-rich phase squeezes into 5 tower top conducts on the right side of next door
Its liquid-phase reflux.
Next door left side 1, next door right side 5 and the rectifying column 7 of next door as described above tower are plate column, using sieve-board type tower tray.
The present invention is made up of due to using above-mentioned rectificating method next door tower, rectifying column and vapour-liquid-liquid/gas separator
Heterogeneous azeotropic rectification system realize the separation of three components, can reach that conventional distillation cannot achieve is kept completely separate.
The charging as embodiment 2 is formed using what table 3 was listed, three product separating resultings are calculated by simulation and are listed in
In table 4, separator temperature is 41 DEG C, pressure 0.30bar, and adiabatic operation, vapour phase produces carbon dioxide, and rich ketone is mutually squeezed into de-
For light the 2nd plate of tower as its liquid-phase reflux, water-rich phase squeezes into the 2nd plate of dehydrating tower as its liquid-phase reflux.
Slightly mixing ketone reaction products form table 3
| Crude reaction product | Acetic acid | 2 pentanone | 4- heptanone | Water | Carbon dioxide |
| Composition/mol% | ≤0.01 | 0.15 | 0.15 | 0.69 | ≤0.01 |
4 embodiment of table, 2 separating resulting
Embodiment 3
A kind of next door tower, it includes shell 11, lower head 12, upper cover 13, along 11 axis direction of shell between shell 11
There is rectangular clapboard 14, shell 11 is divided into 5 on the right side of next door left side 1 and next door, go directly 14 bottom of rectangular clapboard lower head 12, square
Go directly upper cover 13 at the top of shape partition 14, or has segment space between upper cover 13, and rich ketone phase is arranged at 1 top on the left of next door
There is material inlet 16 to be separated at import 15, middle part, and rich ketone phase reboiler import 17, the lower head 12 in next door left side 1 are arranged at lower part
Bottom has mixed keton to export 18, and water-rich phase import 19 is arranged at 5 tops on the right side of next door, and water-rich phase reboiler import 20 is arranged at lower part,
5 12 bottom of lower head has water phase to export 21 on the right side of next door, there is gaseous phase outlet 22 at the top of upper cover 13.
A kind of heterogeneous azeotropic rectification method separating 2 pentanone 4- heptanone, water and carbon dioxide mixture, including such as
Lower step:
(1) the next door tower is to add a rectangular clapboard in shell axis direction in common rectifying tower interior parallel, by shell
It is divided into 5 on the right side of next door tower next door left side 1 and next door；Go directly shell lower head for partition bottom, and can go directly upper cover at the top of partition,
Can also at the top of it reserved part space；Partition and shell carry out welding or stamping connection；On the left of the tower bottom next door of next door 1 and every
5 are each configured with reboiler 3 and reboiler 6 on the left of wall, for providing tower two sides tower reactor reboiler heat；The configuration of next door top of tower
There are a condenser and vapour-liquid-liquid/gas separator；Enter condenser after merging from 5 overhead vapours on the right side of next door left side 1 and next door,
The condensate liquid of acquisition enters vapour-liquid-liquid/gas separator 4, is insulated, constant voltage operation, and the residence time of 20min is undergone to be filled
After the vapour-liquid divided-liquid balance, it is separated into carbon dioxide enriched vapour phase, rich ketone phase and water-rich phase；Rich ketone is mutually squeezed into 1 on the left of next door,
Water-rich phase is squeezed into 5 on the right side of next door；The charging of reaction product mixed liquor is not only limited to that vapour-can also be fed 1 on the left of charging next door
Liquid liquid separator 4, or next door left side 1 and vapour-liquid-liquid/gas separator 4 can be fed simultaneously；Pass through this next door tower and vapour-
Liquid liquid separator, 5 tower reactors of next door right side obtain the waste water of the trace of amount containing ketone, obtain in vapour-liquid-liquid/gas separator vapour phase extraction
Carbon dioxide enriched vapour is obtained, 1 tower reactor obtains the mixed keton of 2 pentanone and 4- heptanone on the left of next door, into subsequent rectifying column 7.
This step operation condition:
1 tower top temperature on the left of next door: 110 DEG C
1 column bottom temperature on the left of next door: 165.4 DEG C
The operating pressure of 1 tower top on the left of next door: 5bar
5 tower top temperatures on the right side of next door: 110 DEG C
5 column bottom temperatures on the right side of next door: 138.7 DEG C
The operating pressure of 5 tower tops on the right side of next door: 5bar
2 operation temperature of condenser: 60 DEG C
2 operating pressure of condenser: 5bar
4 operation temperature of vapour-liquid-liquid/gas separator: adiabatic operation, 60 DEG C
4 operating pressure of vapour-liquid-liquid/gas separator: 0.5bar
(2) mixed keton that 1 tower reactor obtains on the left of next door enters rectifying column 7, boiled again by 7 tower reactor reboiler 10 of rectifying column and
Rectifying column condenser 8 condenses, and obtains heavier 4- heptanone product in 7 tower reactor of rectifying column, obtains in 7 tower top of rectifying column lighter
2 pentanone product；
This step operation condition:
7 tower top temperature of rectifying column: 149.8 DEG C
7 column bottom temperature of rectifying column: 215.6 DEG C
The operating pressure of 7 tower top of rectifying column: 2bar
Specifically, what the next door left side 1 of the next door tower, 5 tower tops of next door right side steamed is rich in 2 pentanone/water/dissolution
The logistics of gas is condensed by condenser 2 to 60 DEG C, to use relatively inexpensive cooling water (32-42 DEG C)；Condensed logistics is three
Be divided into carbon dioxide enriched vapour, rich ketone phase and water-rich phase, carbon dioxide enriched vapour in phase separator 4 to carry out speeding to put, rich ketone mutually squeeze into every
1 tower top on the left of wall, water-rich phase squeeze into 5 tower tops on the right side of next door.By the implementation of rectifier unit, the extraction of 1 tower bottom is mixed on the left of next door
Ketone, the waste water of the next door right side 5 tower bottom extraction trace of amount containing ketone, wherein mixed keton enters rectifying column 7, realizes dividing completely for two class ketone
From.
5 on the right side of the next door left side 1 of the next door tower and next door, it is 40 that number of theoretical plate is suitable, and feedstock position is
Vapour-liquid-liquid/gas separator 4 controls next door column overhead pressure in 5bar, and 110 DEG C of the operation temperature of tower top, bottom temperature is by tower top
Pressure and the number of plates determine that the heating amount by adjusting reboiler 3 controls bottom temperature on the left of next door at 165-166 DEG C；It is logical
The heating amount for overregulating reboiler 6 controls bottom temperature at 138-139 DEG C.Under above-mentioned process conditions, 1 is pushed up on the left of next door
Azeotropic mixture on the right side of portion and next door based on the rich carbonated 2 pentanone/4- heptanone/water of 5 tops extraction, on partition top
Portion enters condenser 2 after merging, 1 tower bottom produces mixed keton on the left of next door, the waste water of 5 tower bottom extraction ketone containing trace on the right side of next door.
The rectifying column 7 is common rectifying tower, and number of theoretical plate 45, charging Board position is 25, and control tower top pressure exists
2bar, 149.8 DEG C of the operation temperature of tower top, bottom temperature is determined by tower top pressure and the number of plates, by adjusting reboiler 10
Heating amount controls bottom temperature at 215-216 DEG C.Under above-mentioned process conditions, the commercially pure 2 pentanone of overhead extraction, tower bottom
Obtain commercially pure 4- heptanone.
Vapour-liquid-the liquid/gas separator 4, temperature maintain between 60 DEG C, and temperature is controlled by 2 thermic load of condenser, pressure
Power maintains 0.5bar, adiabatic operation.Under above-mentioned process conditions, vapour phase obtain it is carbon dioxide enriched, liquid phase be divided into rich ketone phase and
Water-rich phase, wherein rich ketone mutually squeezes into 1 tower top on the left of next door, as its liquid-phase reflux, water-rich phase squeezes into 5 tower top conducts on the right side of next door
Its liquid-phase reflux.
1, next door right side 5 and rectifying column 7 are plate column on the left of the next door of the next door tower, using float-valve type tower tray.
The present invention is made up of due to using above-mentioned rectificating method next door tower, rectifying column and vapour-liquid-liquid/gas separator
Heterogeneous azeotropic rectification system realize the separation of three components, can reach that conventional distillation cannot achieve is kept completely separate.
The charging as embodiment 3 is formed using what table 5 was listed, three product separating resultings are calculated by simulation and are listed in
In table 6, separator temperature is 60 DEG C, pressure 0.50bar, and using adiabatic operation, vapour phase produces carbon dioxide, and rich ketone phase is beaten
Enter the 2nd plate of lightness-removing column as its liquid-phase reflux, water-rich phase squeezes into the 2nd plate of dehydrating tower as its liquid-phase reflux.
Slightly mixing ketone reaction products form table 5
| Crude reaction product | Acetic acid | 2 pentanone | 4- heptanone | Water | Carbon dioxide |
| Composition/mol% | ≤0.01 | 0.10 | 0.10 | 0.79 | ≤0.01 |
6 embodiment of table, 3 separating resulting
Claims (11)
1. a kind of heterogeneous azeotropic rectification method of separation 2 pentanone 4- heptanone, water and carbon dioxide mixture, feature exist
In including the following steps:
(1) by 2 pentanone to be separated, 4- heptanone, water and carbon dioxide raw material from the material inlet to be separated (16) of next door tower
Half side (1) into a next door tower left side, reboiler (3) boils again on the left of next door is provided under the action of reboiler (3) boil provide heat again
Gas-liquid separation is carried out, gas phase comes out from the gaseous phase outlet (22) of next door tower enters condenser (2), and the condensate liquid of acquisition enters vapour-
Liquid liquid separator (4), is insulated, constant voltage operation, and the residence time of 10-30min is undergone to carry out sufficient vapour-liquid-liquid
After balance, isolated carbon dioxide enriched vapour phase, rich ketone phase and water-rich phase, it is half side (1) that rich ketone mutually passes back into a next door tower left side, rich water
It is half side (5) mutually to pass back into the next door tower right side, extraction obtains carbon dioxide enriched gas and carries out speeding to put, and rich ketone mutually enters subsequent rectifying column (7)
In；
(2) the rich ketone that half side (1) tower reactor in a next door tower left side obtains mutually enters rectifying column (7), is boiled again by rectifying tower reboiler (10),
4- heptanone product is obtained in rectifying column (7) tower reactor, the gas phase come out from rectifying column (7) top is using rectifying column condenser (8)
Condensation, condensate liquid enters rectifier column reflux tank (9), and a part flows back into rectifying column (7), and another part obtains 2 pentanone production
Product；
(3) reboiler (6) on the right side of the water-rich phase next door on the next door tower right side half side (5) is passed back into boil again under offer heat effect, it is right
Water-rich phase is separated again, and obtained gas phase comes out and the gas phase from a next door tower left side half side (1) out from gaseous phase outlet (22)
Enter condenser (2) together.
2. the heterogeneous azeotropic of a kind of separation 2 pentanone 4- heptanone as described in claim 1, water and carbon dioxide mixture
Rectificating method, it is characterised in that the described reaction product mixed liquor charging be fed from a charging next door tower left side half side (1), or from into
Expect vapour-liquid-liquid/gas separator (4) charging, or feed simultaneously a next door tower left side half side (1) and vapour-liquid-liquid/gas separator (4) into
Material.
3. a kind of separation 2 pentanone 4- heptanone, water and carbon dioxide mixture is heterogeneous total as claimed in claim 1 or 2
Boil rectificating method, it is characterised in that step (1) operating condition are as follows:
The tower top temperature on a next door tower left side half side (1): 85-110 DEG C
The column bottom temperature on a next door tower left side half side (1): 130-170 DEG C
The tower top operating pressure on a next door tower left side half side (1): 0.5-5bar
The tower top temperature on the next door tower right side half side (5): 85-110 DEG C
The column bottom temperature on the next door tower right side half side (5): 110-140 DEG C
The operating pressure of the tower top on the next door tower right side half side (5): 0.5-5 bar
The operation temperature of condenser (2): 40-60 DEG C
The operating pressure of condenser (2): 0.5-5bar
The operation temperature of vapour-liquid-liquid/gas separator (4): adiabatic operation, 40-60 DEG C
The operating pressure of vapour-liquid-liquid/gas separator (4): for 0.5-5bar.
4. the heterogeneous azeotropic of a kind of separation 2 pentanone 4- heptanone as claimed in claim 3, water and carbon dioxide mixture
Rectificating method, it is characterised in that the tower top temperature of a next door tower left side half side (1): 90-100 DEG C.
5. a kind of separation 2 pentanone 4- heptanone, water and carbon dioxide mixture is heterogeneous total as claimed in claim 1 or 2
Boil rectificating method, it is characterised in that step (2) operating condition are as follows:
The tower top temperature of rectifying column (7): 95-110 DEG C,
The column bottom temperature of rectifying column (7): 195-220 DEG C
The operating pressure of the tower top of rectifying column (7): 0.5-2bar.
6. a kind of separation 2 pentanone 4- heptanone, water and carbon dioxide mixture is heterogeneous total as claimed in claim 1 or 2
Boil rectificating method, it is characterised in that a next door tower left side half side (1), the next door tower right side half side (5) and rectifying column (7) use filler
The combining form of tower, plate column or packed tower and plate column, selected filler can be Pall ring, Raschig ring, θ ring, regular fill out
Material, selected column plate is sieve tray, bubble cap tray, float valve tray.
7. a kind of separation 2 pentanone 4- heptanone, water and carbon dioxide mixture is heterogeneous total as claimed in claim 1 or 2
Boil rectificating method, it is characterised in that the richness that half side (5) tower top in a next door tower left side half side (1), the next door tower right side of the next door tower steams
It is condensed by condenser 2 to 40-60 DEG C containing 2 pentanone/water/solution gas logistics.
8. the heterogeneous azeotropic of a kind of separation 2 pentanone 4- heptanone as claimed in claim 7, water and carbon dioxide mixture
Rectificating method, it is characterised in that half side (5) tower top in a next door tower left side half side (1), the next door tower right side of the next door tower steamed is rich in
2 pentanone/water/solution gas logistics is condensed by condenser 2 to 48-53 DEG C.
9. a kind of separation 2 pentanone 4- heptanone, water and carbon dioxide mixture is heterogeneous total as claimed in claim 1 or 2
Boil rectificating method, it is characterised in that a next door tower left side half side (1) for the next door tower and the next door tower right side are half side (5), number of theoretical plate
It is identical, it is 15-40, it is 5-15 that a next door tower left side half side (1), which feeds Board position,.
10. a kind of separation 2 pentanone 4- heptanone, water and carbon dioxide mixture is heterogeneous as claimed in claim 1 or 2
Azeotropic distillation method, it is characterised in that the number of theoretical plate of the rectifying column (7) is 25-45, and charging Board position is 10-25, control
Tower top pressure processed is between 0.5-5.0 bar, between 95-110 DEG C of operation temperature of tower top.
11. a kind of next door tower, it includes shell (11), lower head (12), upper cover (13), along shell (11) axis direction in shell
(11) there are rectangular clapboard (14) between, shell (11) is divided on the right side of a next door tower left side half side (1) and next door (5), rectangular clapboard
(14) bottom is gone directly lower head (12), is gone directly upper cover (13) at the top of rectangular clapboard (14), or have portion between upper cover (13)
Divide space, rich ketone phase import (15) is arranged at half side (1) top in a next door tower left side, and middle part there are material inlet to be separated (16), and lower part has
Rich ketone phase reboiler import (17), lower head (12) bottom of a next door tower left side half side (1) have mixed keton export (18), every
There is water-rich phase import (19) (5) top on the right side of wall, water-rich phase reboiler import (20) is arranged at lower part, the lower envelope of (5) on the right side of next door
Head (12) bottom has water phase to export (21), has gaseous phase outlet (22) at the top of upper cover (13).
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