CN107304153A - It is a kind of to be hydrogenated with the device and method that iso-butane is prepared with isomerization - Google Patents
It is a kind of to be hydrogenated with the device and method that iso-butane is prepared with isomerization Download PDFInfo
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- CN107304153A CN107304153A CN201610258427.0A CN201610258427A CN107304153A CN 107304153 A CN107304153 A CN 107304153A CN 201610258427 A CN201610258427 A CN 201610258427A CN 107304153 A CN107304153 A CN 107304153A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/02—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation
- C07C5/03—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of non-aromatic carbon-to-carbon double bonds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/22—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by isomerisation
- C07C5/27—Rearrangement of carbon atoms in the hydrocarbon skeleton
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a kind of apparatus and method for being hydrogenated with and preparing iso-butane with isomerization.Described device includes：Pre- lightness-removing column, one-stage hydrogenation reactor, one-stage hydrogenation separator, one-stage hydrogenation circulating pump, one section of recirculation cooler, hydrogenation input and output material heat exchanger, second-stage hydrogenation reactor, secondary hydrogenation feed heater, secondary hydrogenation separator, lightness-removing column, iso-butane finishing column, isomerization input and output material heat exchanger, isomerization feed heater, isomerization reactor.Methods described includes：The raw material of carbon four enters described device via the feeding line of carbon four, iso-butane and normal butane is made after pre- de- light, hydrogenation, separation, iso-butane is made after isomerization reaction, separation in normal butane.The present invention can handle all rich in the lighter hydrocarbons of carbon four, while by waste heat recovery, improving the economic benefit of device.
Description
Technical field
The present invention relates to the lighter hydrocarbons field of carbon four, furtherly, it is related to a kind of hydrogenation and is prepared by isomerization
The device and method of iso-butane.
Background technology
With deepening continuously for petrochemical industry working depth, liquefied gas, associated gas, oil refining are filled
Put and ethylene unit by-product C4Reasonable utilize of each component is increasingly subject to pay attention in cut.C4In cut
The 1,3-butadiene contained can be separated with the method for extracting rectifying as production synthetic rubber, C4Evaporate
Isobutene in point generates MTBE by ether-based device and methanol reaction and can be by further accurate
Fractionation obtains the 1- butylene of high-purity, and the utilization of other components of carbon four is also less.Iso-butane can be produced
Methyl methacrylate, isobutene, isobutanol, expoxy propane etc..In recent years due to isobutene, different
The demand such as butanol and expoxy propane increases year by year so that the utilization of iso-butane increasingly causes people's
Pay attention to, and because the alkyl plant that domestic oil product upgrading drives is expanded on a large scale, it is different in refinery C four
Butane will switch to balance by surplus rapidly, even (be likely to) not enough.Meanwhile, with shale gas association
Amount of butane continue to increase, because its contain a large amount of normal butanes, by the normal butane caused in refinery C four more
Difficulty seeks one's fortune, and added value is by continuous decrease.
The wide material sources of refinery C four, are broadly divided into two types, a kind of is olefin-containing≤5wt% saturated carbon
Four, another is that carbon four is main after 40~50wt% of olefin(e) centent unsaturated carbon four, ethylene unit ether
It is alkane and monoolefine, 30~60wt% of olefin(e) centent.Currently, these C 4 mixtures overwhelming majority
Burnt up as liquefied gas as fuel, chemical utilization rate is relatively low, due to for the in great demand of iso-butane, and
Normal butane economic value is limited, and the yield for thereby how improving iso-butane is just most important.
Chinese patent literature CN102294203A discloses the carbon four in a kind of catalytic pyrolysis ethene
Secondary hydrogenation device and technique, by using two sections of selective hydrogenations, it is to avoid 1,3-butadiene depth adds
The problem of hydrogen causes reactor coking, reduction catalyst service life and plant running cycle, can be direct
Mixing carbon four is hydrogenated with, the utilization rate of raw material is improved.But for containing a small amount of or no diene
The C 4 mixture of hydrocarbon is without reference to specific separation method, also without reference to impurity such as organic sulfur nitrogen
Removal methods, more without reference to isomerization reaction etc..
Chinese patent literature CN102188985A disclose a kind of C-4-fraction selective hydrogenation catalyst and
Its preparation method, the catalyst can be by the alkynes selective hydrogenation in C-4-fraction, and butadiene is substantially not
Loss, catalyst has high activity, high selectivity and preparation method simple, is widely used.But should
Selective hydrogenation of the invention mainly to alkynes in C-4-fraction, without monoolefine in alkane, alkene mixture
Method of hydrotreating, and the simply preparation of catalyst, without reference to separation method, also without reference to organic
The removal methods of the impurity such as sulphur nitrogen, also without reference to isomerization reaction etc..
Chinese patent literature CN201410444683.X and CN1170632A disclose normal butane isomery
Change prepares catalyst and the application of iso-butane, but mainly catalyst system and process operation parameter, no
It is related to flow exploitation, is less related to the hydrogenation separation of olefin-containing material.
Chinese patent literature CN200680015930.8 discloses normal butane to the isomerization side of iso-butane
Method, but positive iso-butane mixture separated by permoselective membrane, and non-traditional ripe rectifying
Separation method, technique is using relatively difficult to achieve.
The content of the invention
Largely had more than needed for the normal butane that solves low value in the prior art, and the iso-butane of high added value is not
Sufficient the problems such as, the invention provides a kind of device and method for preparing iso-butane.By will hydrogenation, it is different
Structure chemical industry skill is combined, and the present invention can handle all rich in the lighter hydrocarbons of carbon four, including liquefied gas, oil
The carbon fourth class after field associated gas, refinery C four and ethylene unit ether, meanwhile, it is excellent by using heat-exchange network
Change technology, by waste heat recovery, improves the economic benefit of device.
An object of the present invention is to provide a kind of device for being hydrogenated with and iso-butane being prepared with isomerization, described
Device includes：Pre- lightness-removing column, one-stage hydrogenation reactor, one-stage hydrogenation separator, one-stage hydrogenation are followed
Ring pump, one section of recirculation cooler, hydrogenation input and output material heat exchanger, second-stage hydrogenation reactor, secondary hydrogenation
Feed heater, secondary hydrogenation separator, lightness-removing column, iso-butane finishing column, isomerization input and output material
Heat exchanger, isomerization feed heater and isomerization reactor；Wherein,
The feeding line of carbon four connects pre- lightness-removing column, pre- lightness-removing column bottom connection one-stage hydrogenation reactor, one
Two sections of connection adds after section hydrogenation separator, hydrogenation input and output material heat exchanger, secondary hydrogenation feed heater
Hydrogen reactor top；
One-stage hydrogenation separator bottom connects one-stage hydrogenation circulating pump, and pump discharge point two-way connects all the way
Connect after one section of recirculation cooler and to merge with the feeding line of carbon four, subsequently into one-stage hydrogenation reactor；Separately
Connection is hydrogenated with input and output material heat exchanger all the way；
Connection secondary hydrogenation separation dress after second-stage hydrogenation reactor bottom connection hydrogenation input and output material heat exchanger
Put, secondary hydrogenation separator is separated after being sequentially connected compressor suction tank, compressor with one-stage hydrogenation
Bottom of device pipeline merges, then connection hydrogenation input and output material heat exchanger；
With carbon after isomerization reaction after secondary hydrogenation separator bottom connection lightness-removing column input and output material heat exchanger
Four discharging pipelines merge connection lightness-removing column；
Lightness-removing column bottom connection lightness-removing column input and output material heat exchanger after connect iso-butane finishing column, iso-butane into
Product tower side line connects isomerization reaction after being sequentially connected isomerization input and output material heat exchanger, isomerization heater
Device entrance；
Lightness-removing column is connected after isomerization reactor outlet connection isomerization input and output material heat exchanger.
The one-stage hydrogenation reactor head is provided with fresh hydrogen feeding line.
The hydrogenation input and output material heat exchanger can be directly connected to by pipeline at the top of second-stage hydrogenation reactor.
The one-stage hydrogenation separator preferably includes one-stage hydrogenation hot knock-out pot, one-stage hydrogenation aftercooler
With the cold knockout drum of one-stage hydrogenation；
One-stage hydrogenation reactor bottom is connected at the top of one-stage hydrogenation hot knock-out pot, one-stage hydrogenation hot knock-out pot
It is sequentially connected at the top of one-stage hydrogenation aftercooler and the cold knockout drum of one-stage hydrogenation, the cold knockout drum of one-stage hydrogenation and connects
Connect compressor suction tank；The cold knockout drum bottom connection one-stage hydrogenation hot knock-out pot of one-stage hydrogenation；One section adds
Hydrogen hot knock-out pot bottom connects one-stage hydrogenation circulating pump.
The secondary hydrogenation separator is that secondary hydrogenation separator can in order to separate hydrogen and lighter hydrocarbons
Using one of following two compositions：
A) the secondary hydrogenation separator include secondary hydrogenation hot knock-out pot, secondary hydrogenation aftercooler and
The cold knockout drum of secondary hydrogenation；
Secondary hydrogenation thermal release is connected after second-stage hydrogenation reactor bottom connection hydrogenation input and output material heat exchanger
Secondary hydrogenation aftercooler and the cold knockout drum of secondary hydrogenation are sequentially connected at the top of tank, secondary hydrogenation hot knock-out pot,
Connection compressor suction tank at the top of the cold knockout drum of secondary hydrogenation；The cold knockout drum bottom connection two of secondary hydrogenation
Section hydrogenation hot knock-out pot；Secondary hydrogenation hot knock-out pot bottom connects lightness-removing column.
B) the secondary hydrogenation separator may also comprise secondary hydrogenation aftercooler and secondary hydrogenation separation
Tank；
It is sequentially connected after second-stage hydrogenation reactor bottom connection hydrogenation input and output material heat exchanger cold after secondary hydrogenation
Connection compressor suction tank, secondary hydrogenation at the top of device and secondary hydrogenation knockout drum, secondary hydrogenation knockout drum
Knockout drum bottom connects lightness-removing column.
According to two kinds of hydrogenation separators, can have after the hydrogenated input and output material heat exchanger heat exchange of reaction discharging
Two ways, one kind carries out gas-liquid separation to be introduced into secondary hydrogenation hot knock-out pot, and top gas phase passes through
Enter after the cooling of secondary hydrogenation aftercooler and connect at the top of the cold knockout drum of secondary hydrogenation, the cold knockout drum of secondary hydrogenation
Connect compressor suction tank, bottom connection secondary hydrogenation hot knock-out pot, secondary hydrogenation hot knock-out pot bottom liquid
Be connected lightness-removing column；Another way is first after the cooling of secondary hydrogenation aftercooler into secondary hydrogenation point
Pass through gas-liquid separation, top gas phase connection compressor suction tank, bottom liquid phases connection lightness-removing column from tank.
It is preferred to use first way.
Secondary hydrogenation feed heater described above can use common firing equipment in the prior art, such as：
Electric heater, steam heater or heating furnace.
Following technical scheme can specifically be used：
The device for preparing iso-butane includes：Pre- lightness-removing column, one-stage hydrogenation reactor, one-stage hydrogenation
Separator, one-stage hydrogenation circulating pump, one section of recirculation cooler, hydrogenation input and output material heat exchanger, two sections
Hydrogenation reactor, secondary hydrogenation feed heater, secondary hydrogenation separator, lightness-removing column, iso-butane
Finishing column, isomerization input and output material heat exchanger, isomerization feed heater and isomerization reactor；Wherein,
The feeding line of carbon four connects pre- lightness-removing column, pre- lightness-removing column bottom connection one-stage hydrogenation reactor, one
Two sections of connection adds after section hydrogenation separator, hydrogenation input and output material heat exchanger, secondary hydrogenation feed heater
Hydrogen reactor top；
One-stage hydrogenation separator bottom connects one-stage hydrogenation circulating pump, and pump discharge point two-way connects all the way
Connect after one section of recirculation cooler and to merge with the feeding line of carbon four, subsequently into one-stage hydrogenation reactor；Separately
Connection is hydrogenated with input and output material heat exchanger all the way；
Secondary hydrogenation thermal release is connected after second-stage hydrogenation reactor bottom connection hydrogenation input and output material heat exchanger
Tank；Secondary hydrogenation aftercooler and the cold knockout drum of secondary hydrogenation are sequentially connected at the top of secondary hydrogenation hot knock-out pot,
It is hydrogenated with the top of cold knockout drum and is sequentially connected after compressor suction tank, compressor and one-stage hydrogenation separator
Bottom line merges, then connection hydrogenation input and output material heat exchanger；The cold knockout drum bottom connection of secondary hydrogenation
Secondary hydrogenation hot knock-out pot；
With carbon after isomerization reaction after secondary hydrogenation hot knock-out pot bottom connection lightness-removing column input and output material heat exchanger
Four discharging pipelines merge connection lightness-removing column；
Lightness-removing column bottom connection lightness-removing column input and output material heat exchanger after connect iso-butane finishing column, iso-butane into
Product tower side line connects isomerization reaction after being sequentially connected isomerization input and output material heat exchanger, isomerization heater
Device entrance；
Lightness-removing column is connected after isomerization reactor outlet connection isomerization input and output material heat exchanger.
The second object of the present invention is to provide a kind of method that use described device prepares iso-butane, described
Method includes：
The raw material of carbon four enters described device via the feeding line of carbon four, after pre- de- light, hydrogenation, separation
Iso-butane and normal butane is made, iso-butane is made after isomerization reaction, separation in wherein normal butane.
Specifically it may include following steps：
(a) by the raw material of carbon four that out-of-bounds comes removed first through pre- lightness-removing column include carbon two, light group of carbon three
Point；Pre- lightness-removing column bottoms material enters one-stage hydrogenation reactor, by whole alkadienes and a small amount of monoolefine
It is hydrogenated with saturation；
(b) one-stage hydrogenation reactor bottom material enters one-stage hydrogenation separator, isolates hydrogen and enters
Enter compressor suction tank, one-stage hydrogenation separator bottoms material is divided to two after entering one-stage hydrogenation circulating pump
Stock, with pre- lightness-removing column bottoms material is mixed into one-stage hydrogenation anti-after one section of stock-traders' know-how recirculation cooler cooling
Device is answered, enters second-stage hydrogenation reactor by remaining monoene after another stock-traders' know-how hydrogenation input and output material heat exchanger heat exchange
Hydrocarbon hydrogenation saturation and imurity-removal, the impurity include micro organic sulfur nitrogen etc.；
(c) into secondary hydrogenation point after the hydrogenated input and output material heat exchanger of second-stage hydrogenation reactor bottom discharge
From device, the hydrogen isolated returns to second-stage hydrogenation reactor, secondary hydrogenation separator bottoms material
After being exchanged heat through lightness-removing column input and output material heat exchanger lightness-removing column is combined into carbon after isomerization reaction four；
(d) iso-butane finished product is entered after lightness-removing column bottoms material exchanges heat through lightness-removing column input and output material heat exchanger
Tower；Iso-butane product is obtained by top of tower by rectifying separation, tower reactor obtains light dydrocarbon heavy constituent, tower side
Mixture of the line extraction comprising normal butane and iso-butane；
(e) mixture comprising normal butane and iso-butane is through isomerization input and output material heat exchanger, isomery
Enter isomerization reactor after changing heater heat exchange, carry out isomerization reaction, normal butane is converted into different
Butane；
(f) isomerization reactor bottom discharge is separated after being exchanged heat through isomerization input and output material heat exchanger with hydrogenation
Bottom of device material is merged into lightness-removing column.
In step (a), the raw material of carbon four includes the light component of carbon two, carbon three through the removing of pre- lightness-removing column, in advance
Lightness-removing column bottoms material mixed with hydrogenation recycle stock, fresh hydrogen to enter after 30~160 DEG C one section plus
Hydrogen reactor.The hydrogenation recycle stock is to enter one of two strands separated after one-stage hydrogenation circulating pump.
Present invention additionally comprises fresh hydrogen is passed through into one-stage hydrogenation reactor, it is passed through each during fresh hydrogen
The mixture of material also needs to meet said temperature requirement.
In step (b), one-stage hydrogenation separator bottoms material enters after being heated to 160~300 DEG C
Second-stage hydrogenation reactor.When secondary hydrogenation reaction temperature rising is very high, then two sections are not needed to add during normal production
Hydrogen feed heater heats up, and can reach reaction temperature by input and output material heat exchange, two are needed when only driving
Section hydrogenation feed heater, now, the material of hydrogenated input and output material heat exchanger heat exchange can be straight by pipeline
Tap into second-stage hydrogenation reactor.When secondary hydrogenation reaction temperature rising is not high, then removes and pass through during normal production
Input and output material heat exchange is outer, in addition it is also necessary to which secondary hydrogenation feed heater is heated.
In step (c), when secondary hydrogenation separator includes secondary hydrogenation hot knock-out pot, secondary hydrogenation
When aftercooler and the cold knockout drum of secondary hydrogenation, the hydrogenated input and output material of second-stage hydrogenation reactor bottom discharge is changed
Hot device, which is cooled to after 50~100 DEG C, enters secondary hydrogenation hot knock-out pot, gas at the top of secondary hydrogenation hot knock-out pot
Enter the cold knockout drum of secondary hydrogenation after secondary hydrogenation aftercooler is cooled to 20~50 DEG C.
In step (c), when secondary hydrogenation separator includes secondary hydrogenation aftercooler and secondary hydrogenation point
During from tank, after the hydrogenated input and output material heat exchanger heat exchange of second-stage hydrogenation reactor bottoms material, then through two sections
Hydrogenation aftercooler, which is cooled to after 20~50 DEG C, enters secondary hydrogenation knockout drum.
Specifically, following technical scheme can be used：
(a) by the raw material of carbon four that out-of-bounds comes removed first through pre- lightness-removing column include carbon two, light group of carbon three
Point；Pre- lightness-removing column bottoms material is mixed with hydrogenation recycle stock, fresh hydrogen to entering after 30~160 DEG C
One-stage hydrogenation reactor, by whole alkadienes and a small amount of monoolefin hydrogenation saturation；
(b) one-stage hydrogenation reactor bottom material enters one-stage hydrogenation separator, isolates hydrogen and enters
Enter compressor suction tank, one-stage hydrogenation separator bottoms material is divided to two after entering one-stage hydrogenation circulating pump
Stock, with pre- lightness-removing column bottoms material is mixed into one-stage hydrogenation anti-after one section of stock-traders' know-how recirculation cooler cooling
Device, another stock-traders' know-how hydrogenation input and output material heat exchanger heat exchange are answered, then is warming up to through secondary hydrogenation feed heater
160~300 DEG C, second-stage hydrogenation reactor is finally entered by remaining monoolefin hydrogenation saturation and is had micro
Machine sulphur nitrogen is converted into H2S and NH3；
(c) second-stage hydrogenation reactor bottom discharge after hydrogenation charging heat exchange through with being cooled to 50~100 DEG C
After can have a two ways, one kind enter after being first cooled to 20~50 DEG C through secondary hydrogenation aftercooler two sections plus
Hydrogen knockout drum carries out gas-liquid separation, top gas phase connection compressor suction tank, bottom liquid phases connection dehydrogenation
Tower；Another way carries out gas-liquid separation to be introduced into secondary hydrogenation hot knock-out pot, and top gas phase passes through
Secondary hydrogenation aftercooler, which is cooled to after 20~50 DEG C, enters the cold knockout drum of secondary hydrogenation, cold point of secondary hydrogenation
Compressor suction tank, bottom connection secondary hydrogenation hot knock-out pot, secondary hydrogenation heat point are connected from tank top
Lightness-removing column is connected from pot bottom liquid phase；
Secondary hydrogenation knockout drum or the cold knockout drum top gas phase of secondary hydrogenation are returned mostly as circulating hydrogen
Hydrogenation reaction charging is returned, and non-hydrogen gas stable content in circulation hydrogen system is maintained by pipeline of releasing；
(d) fresh hydrogen is from being out-of-bounds divided to two strands, and one is directly mixed into one with pre- lightness-removing column substrate material
Section hydrogenation reactor, another stock is combined into compressor with compressor suction head space gas body, through compressor
Enter hydrogenation input and output material heat exchanger after supercharging together with one-stage hydrogenation separator bottoms material；
(e) with isomery after secondary hydrogenation hot knock-out pot bottoms material exchanges heat through lightness-removing column input and output material heat exchanger
Change carbon four after reaction and be mixed into lightness-removing column, separated by rectifying, top gaseous phase removing H2S, NH3
Deng fixed gas, liquid phase removing carbon two, the third light component of carbon, bottoms material enters iso-butane finishing column,
Iso-butane product is obtained at the top of iso-butane finishing column by rectifying separation, tower reactor obtains light dydrocarbon heavy constituent；
(f) by mixture of the iso-butane finishing column side take-off comprising normal butane and iso-butane with it is out-of-bounds new
The mixing of fresh hydrogen is heated to 100 by isomerization input and output material heat exchanger, isomerization feed heater~
Enter isomerization reactor after 250 DEG C, normal butane is converted into iso-butane herein；
(g) material enters de- light through isomerization input and output material heat exchanger heat exchange Posterior circle after isomerization reaction
Tower, is separated by rectifying, removed overhead H2、H2S, carbon two, the third light component of carbon, tower reactor are obtained just
Iso-butane mixture.
The present invention uses hydrogenation catalyst for nickel system or palladium series hydrocatalyst；Isomerization catalyst is
The catalyst that one or both of Pt, Pd, Ir are constituted.
The process conditions of each equipment of the present invention can use the process conditions generally used in the prior art,
In the present invention, preferably using following process conditions：
The operating condition of the pre- lightness-removing column includes：Pressure is 1~3MPaG (gauge pressure, as follows),
Tower top operation temperature is 20~90 DEG C, and the number of plates is 30~120, and reflux ratio is 1~15；
One-stage hydrogenation reactor is fixed bed reactors, and reactor inlet temperature is 30~120 DEG C, pressure
For 1.5~4.5MPaG, reaction temperature rising is 5~100 DEG C, and hydrogen/oil mol ratio is 0.05~10, liquid bulk
Product air speed is 0.5~10h-1；
Second-stage hydrogenation reactor is fixed bed reactors, and reactor inlet temperature is 160~300 DEG C, pressure
Power is 1.5~4.5MPaG, and reaction temperature rising is 5~100 DEG C, and hydrogen/oil mol ratio is 0.2~5, liquid bulk
Product air speed is 0.5~6h-1；
The operating condition of lightness-removing column includes：Pressure is 1~3MPaG, and tower top operation temperature is 30~90 DEG C,
The number of plates is 30~80, and reflux ratio is 1~100；
The operating condition of iso-butane finishing column includes：Pressure is 0.1~1MPaG, and tower top operation temperature is
20~70 DEG C, the number of plates is 80~150, and reflux ratio is 1~20；
Isomerization reactor is fixed bed reactors, and reactor inlet temperature is 100~250 DEG C, pressure
For 1.0~4.0MPaG, reaction temperature rising is 5~50 DEG C, and liquid volume air speed is 1~20h-1。
It is characteristic of the invention that：
1) unsaturated olefin (including alkadienes and monoolefine) is completely converted into saturated hydrocarbons by being hydrogenated with,
The impurity such as organic sulfur nitrogen in raw material is converted into H2S and NH3Removed, it is to avoid to the shadow of product
Ring；
2) by rationally setting heat exchange order, recover energy to the full extent, reduce system energy consumption, carry
The high economic benefit of device, passes through a series of heat exchange network optimizations, saves energy consumption more than 15%；
3) bottom temperature is made to be below 150 DEG C by suitable operating parameter, 45 DEG C or so of tower top temperature,
It can be exchanged heat using more cheap low-pressure steam and recirculated cooling water, the steaming high-grade without outside intervention
The chilled water of vapour and high-quality；
4) present invention can handle all rich in carbon four by the way that hydrogenation and isomerization process are combined
Lighter hydrocarbons be used to produce iso-butane, especially the C4 materials containing a small amount of alkadienes and can also handle；
5) present invention, can also by-product carbon two, the product of carbon three in addition to iso-butane is obtained.
Other features and advantages of the present invention will be described in detail in subsequent embodiment part.
Brief description of the drawings
It is of the invention by the way that exemplary embodiment of the invention is described in more detail with reference to accompanying drawing
Above-mentioned and other purposes, feature and advantage will be apparent, wherein, it is exemplary in the present invention
In embodiment, identical reference number typically represents same parts.
Fig. 1 is the schematic device for preparing iso-butane of the invention, wherein secondary hydrogenation separator bag
Include secondary hydrogenation hot knock-out pot, secondary hydrogenation aftercooler and the cold knockout drum of secondary hydrogenation.
Fig. 2 is the schematic device for preparing iso-butane of the invention, wherein secondary hydrogenation separator bag
Include secondary hydrogenation aftercooler and secondary hydrogenation knockout drum.
Description of reference numerals：
Pre- lightness-removing column 1, pre- condenser of light component removal column 2, pre- lightness-removing column reboiler 3, second-stage hydrogenation reactor
4th, hydrogenation input and output material heat exchanger 5, secondary hydrogenation feed heater 6, secondary hydrogenation aftercooler 7, two sections
It is hydrogenated with knockout drum 8, secondary hydrogenation hot knock-out pot 9, the cold knockout drum 10 of secondary hydrogenation, compressor suction tank
11st, compressor 12, lightness-removing column input and output material heat exchanger 13, lightness-removing column 14, condenser of light component removal column 15,
Lightness-removing column reboiler 16, iso-butane finishing column 17, iso-butane finishing column condenser 18, iso-butane finished product
Tower reboiler 19, isomerization input and output material heat exchanger 20, isomerization feed heater 21, isomerization reaction
Device 22, the raw material 23 of carbon four, pre- lightness-removing column fixed gas 24, pre- lightness-removing column top liquid phase 25, periodic off-gases 26,
Secondary hydrogenation hydrogen make-up 27, lightness-removing column top fixed gas 28, lightness-removing column top C3Liquid phase 29, iso-butane
Product 30, light dydrocarbon heavy constituent 31, isomerization hydrogen make-up 32, one-stage hydrogenation reactor 33, one section
Hydrogenation aftercooler 34, one-stage hydrogenation hot knock-out pot 35, the cold knockout drum 36 of one-stage hydrogenation, one-stage hydrogenation are followed
Ring pump 37, one section of recirculation cooler 38, one-stage hydrogenation hydrogen make-up 39.
Embodiment
The preferred embodiment of the present invention is more fully described below with reference to accompanying drawings.
Iso-butane is prepared using combination unit as shown in Figure 1.
The device includes：Pre- lightness-removing column 1, one-stage hydrogenation reactor 33, one-stage hydrogenation separator,
One-stage hydrogenation circulating pump 37, one section of recirculation cooler 38, second-stage hydrogenation reactor 4, hydrogenation input and output material
Heat exchanger 5, secondary hydrogenation feed heater 6, secondary hydrogenation separator, lightness-removing column 14, iso-butane
Finishing column 17, isomerization input and output material heat exchanger 20, isomerization feed heater 21 and isomerization reaction
Device 22；Wherein,
The feeding line of carbon four connects pre- lightness-removing column 1, and the pre- bottom of lightness-removing column 1 connects one-stage hydrogenation reactor
33rd, connect after one-stage hydrogenation separator, hydrogenation input and output material heat exchanger 5, secondary hydrogenation feed heater 6
Connect the top of second-stage hydrogenation reactor 4；
One-stage hydrogenation separator bottom connection one-stage hydrogenation circulating pump 37, pump discharge point two-way, all the way
Merge after one section of recirculation cooler 38 of connection with the feeding line of carbon four, subsequently into one-stage hydrogenation reactor
33；Another road connection hydrogenation input and output material heat exchanger 5；
Connection secondary hydrogenation heat point after the bottom of second-stage hydrogenation reactor 4 connection hydrogenation input and output material heat exchanger 5
From tank 9；The top of secondary hydrogenation hot knock-out pot 9 is sequentially connected secondary hydrogenation aftercooler 7 and secondary hydrogenation is cold
Knockout drum 10, the cold top of knockout drum 10 of secondary hydrogenation is sequentially connected compressor suction tank 11, compressor
Merge after 12 with one-stage hydrogenation separator bottom line, then connection hydrogenation input and output material heat exchanger 5；
The cold bottom of the knockout drum 10 connection secondary hydrogenation hot knock-out pot 9 of secondary hydrogenation；
With isomerization reaction after the bottom of secondary hydrogenation hot knock-out pot 9 connection lightness-removing column input and output material heat exchanger 13
The discharging of carbon four pipeline merges connection lightness-removing column 14 afterwards；
Connection iso-butane finishing column 17 after the bottom of lightness-removing column 14 connection lightness-removing column input and output material heat exchanger 13,
The side line of iso-butane finishing column 17 is sequentially connected isomerization input and output material heat exchanger 20, isomerization heater 21
The entrance of isomerization reactor 22 is connected afterwards；
Lightness-removing column 14 is connected after the outlet of isomerization reactor 22 connection isomerization input and output material heat exchanger 20；
The top of one-stage hydrogenation reactor 33 is provided with fresh hydrogen feeding line.
Preparing the method for iso-butane includes：
(a) by the raw material 23 of carbon four out-of-bounds come is removed including carbon two, carbon three through pre- lightness-removing column 1 first
Light component；The pre- bottoms material of lightness-removing column 1 and one-stage hydrogenation recycle stock, one-stage hydrogenation hydrogen make-up
39 are mixed to 45 DEG C into one-stage hydrogenation reactor 33, and whole alkadienes and a small amount of monoolefin hydrogenation are satisfied
With；
(b) bottoms material of one-stage hydrogenation reactor 33 enters one-stage hydrogenation separator, isolates hydrogen
Gas enters compressor suction tank 8, and one-stage hydrogenation separator bottoms material enters one-stage hydrogenation circulating pump
It is divided to two strands after 37, is mixed after one section of a stock-traders' know-how recirculation cooler 38 cooling with the pre- bottoms material of lightness-removing column 1
Enter one-stage hydrogenation reactor 33, another stock-traders' know-how hydrogenation input and output material heat exchanger 5 exchanges heat, then through secondary hydrogenation
Feed heater 6 is warming up to 240 DEG C, finally enters second-stage hydrogenation reactor 4 by olefins hydrogenation simultaneously
Micro organic sulfur nitrogen is converted into H2S and NH3；
(c) bottom discharge of second-stage hydrogenation reactor 4 through with hydrogenation charging heat exchange after be cooled to 80 DEG C it is laggard
Enter secondary hydrogenation hot knock-out pot 9 and carry out gas-liquid separation, top gas phase is cold by secondary hydrogenation aftercooler 7
But to entering the cold knockout drum 10 of secondary hydrogenation, the cold top of the knockout drum 10 connection pressure of secondary hydrogenation after 40 DEG C
Contracting machine suction tank 11, bottom connection secondary hydrogenation hot knock-out pot 9, the bottom of secondary hydrogenation hot knock-out pot 9
Liquid phase connects lightness-removing column 14；
The cold top gas phase of knockout drum 10 of secondary hydrogenation returns to hydrogenation reaction mostly as circulating hydrogen and entered
Material, and non-hydrogen gas stable content in the maintenance circulation hydrogen system of periodic off-gases 26 is discharged by pipeline of releasing；
(d) fresh hydrogen is from being out-of-bounds divided to two strands, and one is directly mixed into one with pre- lightness-removing column substrate material
Section hydrogenation reactor 33, another stock as secondary hydrogenation hydrogen make-up 27 from out-of-bounds with compressor suction tank
11 top gas bodies are combined into compressor 12, with one-stage hydrogenation separator bottom after being pressurized through compressor 12
Portion's material enters hydrogenation input and output material heat exchanger 5 together；
(e) after the bottoms material of secondary hydrogenation hot knock-out pot 9 exchanges heat through lightness-removing column input and output material heat exchanger 13
Lightness-removing column 14 is mixed into carbon after isomerization reaction four, is separated by rectifying, top gaseous phase removing H2S,
NH3Deng fixed gas, liquid phase removing carbon two, the third light component of carbon, bottoms material enters iso-butane finished product
Tower 17, obtains iso-butane product 30, tower reactor is obtained by rectifying separation by the top of iso-butane finishing column 17
To light dydrocarbon heavy constituent 31；
(f) by mixture of the side take-off of iso-butane finishing column 17 comprising normal butane and iso-butane and out-of-bounds
Fresh hydrogen is that the mixing of isomerization hydrogen make-up 32 is entered by isomerization input and output material heat exchanger 20, isomerization
Material heater 21 is heated to after 160 DEG C entering isomerization reactor 22, is herein converted into normal butane different
Butane；
(g) material enters de- through the heat exchange Posterior circle of isomerization input and output material heat exchanger 20 after isomerization reaction
Light tower 14, is separated, removed overhead H by rectifying2、H2S, carbon two, the third light component of carbon, tower reactor
Obtain positive iso-butane mixture.
Using following process conditions：
The operating condition of the pre- lightness-removing column includes：Pressure is 2MPaG, and tower top operation temperature is 55 DEG C,
The number of plates is 80, and reflux ratio is 10；
One-stage hydrogenation reactor is fixed bed reactors, and reactor inlet temperature is 45 DEG C, and pressure is
3.6MPaG, reaction temperature rising is 20 DEG C, and hydrogen/oil mol ratio is 0.1, and liquid volume air speed is 2.5h-1；
Second-stage hydrogenation reactor is fixed bed reactors, and reactor inlet temperature is 240 DEG C, and pressure is
3MPaG, reaction temperature rising is 25 DEG C, and hydrogen/oil mol ratio is 1.1, and liquid volume air speed is 2h-1；
The operating condition of lightness-removing column includes：Pressure is 1.8MPaG, and tower top operation temperature is 50 DEG C, tower
Plate number is 50, and reflux ratio is 50；
The operating condition of iso-butane finishing column includes：Pressure is 0.5MPaG, and tower top operation temperature is
50 DEG C, the number of plates is 130, and reflux ratio is 6；
Isomerization reactor is fixed bed reactors, and reactor inlet temperature is 160 DEG C, and pressure is
3.3MPaG, reaction temperature rising is 30 DEG C, and liquid volume air speed is 10h-1。
Using system as shown in Figure 1, the result of table 1 is obtained.
As a result show, using the system and method iso-butane of the present invention, iso-butane yield ＞ 97%.
Table 1
By said apparatus and process, energy consumption more than 15% is saved.
It is described above various embodiments of the present invention, described above is exemplary, and exhaustive
Property, and it is also not necessarily limited to disclosed each embodiment.In the model without departing from illustrated each embodiment
Enclose and spirit in the case of, many modifications and changes for those skilled in the art
It will be apparent from.
Claims (10)
1. a kind of be hydrogenated with the device that iso-butane is prepared with isomerization, it is characterised in that：
Described device includes：Pre- lightness-removing column, one-stage hydrogenation reactor, one-stage hydrogenation separator, one
Section hydrogenation circulating pump, one section of recirculation cooler, hydrogenation input and output material heat exchanger, second-stage hydrogenation reactor,
Secondary hydrogenation feed heater, secondary hydrogenation separator, lightness-removing column, iso-butane finishing column, isomery
Change input and output material heat exchanger, isomerization feed heater and isomerization reactor；Wherein,
The feeding line of carbon four connects pre- lightness-removing column, pre- lightness-removing column bottom connection one-stage hydrogenation reactor, one
Two sections of connection adds after section hydrogenation separator, hydrogenation input and output material heat exchanger, secondary hydrogenation feed heater
Hydrogen reactor top；
One-stage hydrogenation separator bottom connects one-stage hydrogenation circulating pump, and pump discharge point two-way connects all the way
Connect after one section of recirculation cooler and to merge with the feeding line of carbon four, subsequently into one-stage hydrogenation reactor；Separately
Connection is hydrogenated with input and output material heat exchanger all the way；
Connection secondary hydrogenation separation dress after second-stage hydrogenation reactor bottom connection hydrogenation input and output material heat exchanger
Put, secondary hydrogenation separator is separated after being sequentially connected compressor suction tank, compressor with one-stage hydrogenation
Bottom of device pipeline merges, then connection hydrogenation input and output material heat exchanger；
With carbon after isomerization reaction after secondary hydrogenation separator bottom connection lightness-removing column input and output material heat exchanger
Four discharging pipelines merge connection lightness-removing column；
Lightness-removing column bottom connection lightness-removing column input and output material heat exchanger after connect iso-butane finishing column, iso-butane into
Product tower side line connects isomerization reaction after being sequentially connected isomerization input and output material heat exchanger, isomerization heater
Device entrance；
Lightness-removing column is connected after isomerization reactor outlet connection isomerization input and output material heat exchanger.
2. hydrogenation as claimed in claim 1 and isomerization prepare the device of iso-butane, it is characterised in that：
The one-stage hydrogenation separator includes one-stage hydrogenation hot knock-out pot, one-stage hydrogenation aftercooler and one
The cold knockout drum of section hydrogenation；
One-stage hydrogenation reactor bottom is connected at the top of one-stage hydrogenation hot knock-out pot, one-stage hydrogenation hot knock-out pot
It is sequentially connected at the top of one-stage hydrogenation aftercooler and the cold knockout drum of one-stage hydrogenation, the cold knockout drum of one-stage hydrogenation and connects
Connect compressor suction tank；The cold knockout drum bottom connection one-stage hydrogenation hot knock-out pot of one-stage hydrogenation；One section adds
Hydrogen hot knock-out pot bottom connects one-stage hydrogenation circulating pump.
3. hydrogenation as claimed in claim 1 and isomerization prepare the device of iso-butane, it is characterised in that：
The secondary hydrogenation separator includes secondary hydrogenation hot knock-out pot, secondary hydrogenation aftercooler and two
The cold knockout drum of section hydrogenation；
Secondary hydrogenation thermal release is connected after second-stage hydrogenation reactor bottom connection hydrogenation input and output material heat exchanger
Secondary hydrogenation aftercooler and the cold knockout drum of secondary hydrogenation are sequentially connected at the top of tank, secondary hydrogenation hot knock-out pot,
Connection compressor suction tank at the top of the cold knockout drum of secondary hydrogenation；The cold knockout drum bottom connection two of secondary hydrogenation
Section hydrogenation hot knock-out pot；Secondary hydrogenation hot knock-out pot bottom connects lightness-removing column.
4. hydrogenation as claimed in claim 1 and isomerization prepare the device of iso-butane, it is characterised in that：
The secondary hydrogenation separator includes secondary hydrogenation aftercooler and secondary hydrogenation knockout drum；
It is sequentially connected after second-stage hydrogenation reactor bottom connection hydrogenation input and output material heat exchanger cold after secondary hydrogenation
Connection compressor suction tank, secondary hydrogenation at the top of device and secondary hydrogenation knockout drum, secondary hydrogenation knockout drum
Knockout drum bottom connects lightness-removing column.
5. a kind of method that device using as described in any one in claim 1-4 prepares iso-butane,
Characterized in that, methods described includes：
The raw material of carbon four enters described device via the feeding line of carbon four, after pre- de- light, hydrogenation, separation
Iso-butane and normal butane is made, iso-butane is made after isomerization reaction, separation in wherein normal butane.
6. the method as claimed in claim 5 for preparing iso-butane, it is characterised in that methods described bag
Include：
(a) by the raw material of carbon four that out-of-bounds comes removed first through pre- lightness-removing column include carbon two, light group of carbon three
Point；Pre- lightness-removing column bottoms material enters one-stage hydrogenation reactor, by whole alkadienes and a small amount of monoolefine
It is hydrogenated with saturation；
(b) one-stage hydrogenation reactor bottom material enters one-stage hydrogenation separator, isolates hydrogen and enters
Enter compressor suction tank, one-stage hydrogenation separator bottoms material is divided to two after entering one-stage hydrogenation circulating pump
Stock, with pre- lightness-removing column bottoms material is mixed into one-stage hydrogenation anti-after one section of stock-traders' know-how recirculation cooler cooling
Device is answered, enters second-stage hydrogenation reactor by remaining monoene after another stock-traders' know-how hydrogenation input and output material heat exchanger heat exchange
Hydrocarbon hydrogenation saturation and imurity-removal；
(c) into secondary hydrogenation point after the hydrogenated input and output material heat exchanger of second-stage hydrogenation reactor bottom discharge
From device, the hydrogen isolated returns to second-stage hydrogenation reactor, secondary hydrogenation separator bottoms material
After being exchanged heat through lightness-removing column input and output material heat exchanger lightness-removing column is combined into carbon after isomerization reaction four；
(d) iso-butane finished product is entered after lightness-removing column bottoms material exchanges heat through lightness-removing column input and output material heat exchanger
Tower；Iso-butane product is obtained by top of tower by rectifying separation, tower reactor obtains light dydrocarbon heavy constituent, tower side
Mixture of the line extraction comprising normal butane and iso-butane；
(e) mixture comprising normal butane and iso-butane is through isomerization input and output material heat exchanger, isomery
Enter isomerization reactor after changing heater heat exchange, carry out isomerization reaction, normal butane is converted into different
Butane；
(f) isomerization reactor bottom discharge is separated after being exchanged heat through isomerization input and output material heat exchanger with hydrogenation
Bottom of device material is merged into lightness-removing column.
7. the method as claimed in claim 6 for preparing iso-butane, it is characterised in that：
In step (a), the raw material of carbon four includes the light component of carbon two, carbon three through the removing of pre- lightness-removing column, in advance
Lightness-removing column bottoms material is mixed with hydrogenation recycle stock to entering one-stage hydrogenation reactor after 30~160 DEG C；
In step (b), one-stage hydrogenation separator bottoms material enters after being heated to 160~300 DEG C
Second-stage hydrogenation reactor.
8. the method as claimed in claim 6 for preparing iso-butane, it is characterised in that：
In step (c), when secondary hydrogenation separator includes secondary hydrogenation hot knock-out pot, secondary hydrogenation
When aftercooler and the cold knockout drum of secondary hydrogenation, the hydrogenated input and output material of second-stage hydrogenation reactor bottom discharge is changed
Hot device, which is cooled to after 50~100 DEG C, enters secondary hydrogenation hot knock-out pot, gas at the top of secondary hydrogenation hot knock-out pot
Enter the cold knockout drum of secondary hydrogenation after secondary hydrogenation aftercooler is cooled to 20~50 DEG C.
9. the method as claimed in claim 6 for preparing iso-butane, it is characterised in that：
In step (c), when secondary hydrogenation separator includes secondary hydrogenation aftercooler and secondary hydrogenation point
During from tank, after the hydrogenated input and output material heat exchanger heat exchange of second-stage hydrogenation reactor bottoms material, then through two sections
Hydrogenation aftercooler, which is cooled to after 20~50 DEG C, enters secondary hydrogenation knockout drum.
10. the method for preparing iso-butane as described in any one in claim 6-9, it is characterised in that：
The operating condition of pre- lightness-removing column includes：Pressure be 1~3MPaG, tower top operation temperature be 20~
90 DEG C, the number of plates is 30~120, and reflux ratio is 1~15；
One-stage hydrogenation reactor is fixed bed reactors, and reactor inlet temperature is 30~160 DEG C, pressure
For 1.5~4.5MPaG, reaction temperature rising is 5~100 DEG C, and hydrogen/oil mol ratio is 0.05~10, liquid bulk
Product air speed is 0.5~10h-1；
Second-stage hydrogenation reactor is fixed bed reactors, and reactor inlet temperature is 160~300 DEG C, pressure
Power is 1.5~4.5MPaG, and reaction temperature rising is 5~100 DEG C, and hydrogen/oil mol ratio is 0.2~5, liquid bulk
Product air speed is 0.5~6h-1；
The operating condition of lightness-removing column includes：Pressure is 1~3MPaG, and tower top operation temperature is 30~90 DEG C,
The number of plates is 30~80, and reflux ratio is 1~100；
The operating condition of iso-butane finishing column includes：Pressure is 0.1~1MPaG, and tower top operation temperature is
20~70 DEG C, the number of plates is 80~150, and reflux ratio is 1~20；
Isomerization reactor is fixed bed reactors, and reactor inlet temperature is 100~250 DEG C, pressure
For 1.0~4.0MPaG, reaction temperature rising is 5~50 DEG C, and liquid volume air speed is 1~20h-1。
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