CN107285978A - The preparation method of normal butane - Google Patents
The preparation method of normal butane Download PDFInfo
- Publication number
- CN107285978A CN107285978A CN201710531027.7A CN201710531027A CN107285978A CN 107285978 A CN107285978 A CN 107285978A CN 201710531027 A CN201710531027 A CN 201710531027A CN 107285978 A CN107285978 A CN 107285978A
- Authority
- CN
- China
- Prior art keywords
- butane
- normal butane
- removing column
- tower
- iso
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C07C5/2767—Changing the number of side-chains
- C07C5/277—Catalytic processes
- C07C5/2791—Catalytic processes with metals
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
- C07C7/14833—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound with metals or their inorganic compounds
- C07C7/14841—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound with metals or their inorganic compounds metals
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
- C07C7/163—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound by hydrogenation
Abstract
The invention discloses a kind of preparation method of normal butane, using butane as raw material, comprise the following steps：（1）Raw material is sent into lightness-removing column, removed after light component, feeding butane tower carries out isolated iso-butane；（2）The tower top of the butane tower is isolated into iso-butane and sends into positive structure reactor, thick normal butane and defective material are obtained in the bottom of positive structure reactor after catalytic reaction；（3）Thick normal butane is sent into weight-removing column, the heavy constituent of carbon four in thick normal butane is removed, the normal butane product that mass fraction is 97.5 ~ 99% is obtained in the tower top of the weight-removing column.Using positive structure catalyst, positive structureization reaction can be carried out at higher temperatures and pressures；Positive structureization reaction is carried out at higher temperatures, is conducive to improving the conversion ratio of iso-butane, is reduced the internal circulating load of iso-butane, reduces plant energy consumption.
Description
Technical field
The invention belongs to technical field of chemistry and chemical engineering, and in particular to a kind of method that normal butane is prepared by iso-butane, the party
The positive structure of iso-butane is turned to normal butane by method using positive structure catalyst.
Background technology
At present, the production method of normal butane is general using refinery's C-4-fraction as raw material, and normal butane is obtained using partition method.Just
The complex production process of butane, reaction temperature is unstable during reaction, it is impossible to obtain high-purity normal butane.
Such as Chinese patent literature（Application number 201010508814.8）It is prepared by the Methods For Purification for proposing a kind of use rectifying
The technology of normal butane, left reflux pump, left return tank, left condenser, raw material pump, debutanizing tower, butane reboiler, intermediate reflux
Pump, intermediate reflux tank, interconderser, left deisobutanizer, circulating pump, right deisobutanizer, iso-butane reboiler, normal butane
Tower, right condenser, right return tank, right reflux pump, normal butane reboiler are linked in sequence integrally and constituted by connecting pipeline.
And it is current, greater advance is obtained for the deep exploitation of raw material with carbon four, by extracting, etherificate, aromatisation etc.
After reason, the alkene in the component of carbon four is fully used substantially, and utilization rate is relatively low, is used generally as unskilled labor domestic fuel gas,
Cause the waste of the resource of carbon four.
The present invention provides a kind of method that normal butane is prepared by raw material of butane, raw material is obtained maximized profit
With cost-effective.
The content of the invention
The technical problem to be solved in the present invention be for the deficiencies in the prior art there is provided a kind of income it is high, turn
The preparation method for the normal butane that rate is high, utilization rate of raw materials is big.
In order to solve the above technical problems, the technical solution adopted by the present invention is：Using butane as raw material, including following step
Suddenly：
（1）Raw material is sent into lightness-removing column, removed after light component, feeding butane tower carries out isolated iso-butane；
（2）The tower top of the butane tower is isolated into iso-butane and sends into positive structure reactor, it is anti-in positive structureization after catalytic reaction
The bottom of device is answered to obtain thick normal butane and defective material；
（3）Thick normal butane is sent into weight-removing column, the heavy constituent of carbon four in thick normal butane is removed, is obtained in the tower top of the weight-removing column
Mass fraction is 97.5 ~ 99% normal butane product.
Further improve of the invention is that the preparation method of the normal butane is further comprising the steps of：
（4）By the step（2）In defective material feeding hydrogenation reactor, carry out hydrogenation reaction, make isobutene in defective material, third
Alkene, 1- butylene, 2- butylene hydrogenation, obtain including methane, ethane, propane, iso-butane, normal butane, the hydrogenation products of hydrogen；
（5）By hydrogenation products condensation separation, gaseous products are removed, the gaseous products are methane, ethane, propane and hydrogen, are obtained
To the positive structure product being made up of normal butane and iso-butane；
（6）By step（5）In the obtained positive structure product send into the lightness-removing column, and press the step successively（1）、（2）、
（3）Step process, obtains normal butane product.
It is used as the preferred scheme of the present invention, the step（1）Described in raw material be the material containing butane or to contain
The material of unsaturated carbon four.
The present invention, which is further improved, to be, the step（1）Described in lightness-removing column tower top use cryogenic condensation mode,
The temperature of condensation is 10 ~ 20 DEG C, and condensation operation is carried out using heat exchanger or segregation and fractionation system.In step（1）Middle butane
Or positive structure product enters lightness-removing column；Lightness-removing column bottom obtains the butane of propane content 0.2 ~ 0.4%, and butane content is
92~98wt%；Tower top obtains methane, ethane, propane and a small amount of iso-butane, content of the iso-butane in tower top discharging generally≤
18wt%；Lightness-removing column tower top pressure is 0.8 ~ 1.2MPaA, and tower top temperature is 50 ~ 60 DEG C, and full tower pressure drop is 20 ~ 50kPa, bottom of towe
Temperature is 70 ~ 85 DEG C, overhead reflux ratio >=3.2；Lightness-removing column top typically uses cryogenic condensation, cold to reclaim more iso-butanes
Solidifying temperature is 10 ~ 25 DEG C, and cryogenic condensation mode can directly be condensed using salt cooler.
The present invention, which is further improved, to be, the step（1）Described in butane tower be double tower.Butane tower can be using single
Tower is operated, when separation requirement is higher, it is necessary to which more theoretical tray, can change low by high tower, make double tower, is more beneficial for point
From.The iso-butane of butane tower top can send into positive structure reactor, can also be produced as product.Butane tower bottom reboiler plus
Thermal medium can be low-pressure steam, hot water, conduction oil or be dispatched by factory scenario.
The present invention, which is further improved, to be, the step（3）In obtain the heavy constituent of carbon four in the bottom of towe of the weight-removing column
Material；Wherein the mass fraction of normal butane is 10 ~ 15%.Weight-removing column tower top pressure be 0.4 ~ 0.8 MPa, tower top temperature be 40 ~
70 DEG C, full tower pressure drop is 20 ~ 60kPa, and column bottom temperature is 80 ~ 105 DEG C, overhead reflux ratio >=1.Weight-removing column bottom reboiler plus
Thermal medium can be low-pressure steam, hot water, conduction oil or be dispatched by factory scenario.
The present invention, which is further improved, to be, the step（2）In the positive structure reactor in catalyst include
Carrier, active constituent and auxiliary agent；The carrier is made up of refractory oxides or mixed oxide, and the carrier is zinc oxide, two
One or more mixing in silica, aluminum oxide, magnesia；The active constituent includes one or more VIII transition groups gold
Category mixing, constituent content is mass fraction 0.05 ~ 2.5%；The auxiliary agent is in tin oxide, zinc oxide, vanadium oxide, iron oxide
It is a kind of.The catalyst of positive structureization reaction used generally comprises carrier and active constituent；In addition, can also add in positive structure catalyst
Plus acidic component, such as chloride are to keep acid.One is also added into order to improve in the performance of catalyst, positive structure catalyst
A little auxiliary agents, such as Ce, Sn, Zn, V, La, Cr, Fe, Zr, Mn oxide；The geometry of catalyst for example can be spherical or
Cylinder（It is solid or hollow）.
The present invention, which is further improved, to be, the step（2）Described in positive structure reactor reaction temperature 400 ~ 550
DEG C, reaction pressure is 3 ~ 4.5MPa's.In step（2）In process portion, by step（1）It is anti-that obtained iso-butane sends into positive structureization
Device is answered, iso-butane reacts generation normal butane, but also generation isobutene, 1- butylene and 2- butylene under positive structure catalyst action,
Also form a small amount of methane, ethane, propane and propylene simultaneously.Also there is unconverted iso-butane and hydrogen in product gas mixture
Gas, it is also possible to there is CO, the CO brought into by hydrogen2, water and nitrogen.Positive structure reactor can use fixed bed, moving bed, stream
Change bed.Iso-butane can be contacted with the bed of catalyst granules in the way of up, descending or Radial Flow；Positive structure reactor can
Think separate unit, or many.Bed number in reactor is 1-2 layers.Catalytic inner temperature in positive structure reactor is led to
Often at 400 ~ 550 DEG C.Operating pressure is usually 3 ~ 4.5 MPa.Usual weight (hourly) space velocity (WHSV)（WHSV）For 0.5 ~ 5 h-1；Positive structureization reaction
Carried out generally under hydro condition, to reduce the coking rate of catalyst, while in balanced reactor catalyst bed
Temperature.Typically, total amount of the total amount of hydrogen based on butane is 1 ~ 3 mol/mol, can use pure hydrogen or containing≤20
The hydrogen mixed gas of mol% light paraffins.In a preferred embodiment of the invention, positive structure condition can make to include iso-butane
Material at least 40% the positive structure of iso-butane.
It is used as the preferred scheme of the present invention, the step（4）Described in hydrogenation reactor reaction temperature be 80 ~ 220
℃.Positive structure product is sent into hydrogenation reactor, alkene therein generates alkane on hydrogenation catalyst with hydrogen reaction；Almost
All alkene is converted into alkane, the conversion ratio of alkene>99%, there is methane in the product after hydrogenation, ethane, propane, different
Butane, normal butane and hydrogen, it is also possible to there is CO, CO2, water and nitrogen；Hydrogenation reactor can using fixed bed, moving bed,
Fluid bed；Material can be contacted with the bed of catalyst granules in the way of up, descending or Radial Flow；Hydrogenation reactor is usual
Only 1, the catalyst bed number of plies in reactor is 1-2 layers.In the preferred embodiment of the inventive method, in hydrogenation reactor
Preceding setting cooler, the temperature of hydrogenation reactor is entered with control material.
The present invention, which is further improved, to be, the step（5）Described in hydrogenation reaction product gas flow condensation temperature
For 10 ~ 30 DEG C；Condensing mode is using 2 ~ 4 grades of cooling down operations.In order to save energy expenditure, the condensation to hydrogenation reaction product air-flow
Generally using two-stage or multistage cooling, 2-4 grades of coolings are generally selected, the material after cooling can select to reclaim or do not reclaim this stock
The cold of logistics.Hydrogen in gaseous products can select to be directly used in positive structure reaction or hydrogenation reaction.
The present invention, which is further improved, to be, the step（5）It is middle that the gaseous products are entered into pressure-swing absorption apparatus, to reclaim
High-purity hydrogen.In step (5), the product gas flow of hydrogenation reaction is condensed, condensation temperature is 5 ~ 40 DEG C, most of positive fourth
The higher material of the boiling points such as alkane, iso-butane and propane is condensed into liquid, the relatively low material of boiling point such as most of hydrogen, methane, ethane
Still it is gas.Knockout drum is sent into condensed logistics, air-liquid two-phase is separated, liquid-phase product returns to feeding lightness-removing column, gas phase
Hydrogen purity is usually the % of molar fraction 70 ~ 90 in product, this strand of hydrogen can be at least partly used for positive structureization and react or add
Hydrogen reacts, or is transported to other application, such as producing electric energy in fuel cell.
The technical problem of the invention also to be solved, which is to provide one kind, can recycle raw material, cost-effective and section
The system and device that normal butane is prepared by the positive structure of iso-butane of energy.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：Including lightness-removing column, butane tower, weight-removing column
With positive structure reactor；Delivery outlet of the middle part of the lightness-removing column provided with charging input unit and its bottom is conveyed by butane tower
Pipe is connected with the charging aperture at the middle part of butane tower, and the top of the butane tower is exported provided with first gas；The first gas
Outlet is passed through mouth with the first gas of condensation current divider and the top of positive structure reactor successively by delivery pipe and is connected, described
Positive structure reactor bottom is exported provided with third gas, and the 3rd gas outlet is shunted with weight-removing column and condensation respectively through delivery pipe
Device is connected, and the top of the weight-removing column is exported provided with second gas and the weight-removing column bottom is provided with heavy constituent collector；Institute
State condensation current divider side be connected with hydrogenation reactor and it is described condense current divider top be passed through mouth provided with hydrogen, it is described
The bottom of hydrogenation reactor is provided with the 4th gas vent, and the 4th gas vent is by delivery pipe successively with cooler and separating
Tank is connected, and the bottom of the knockout drum is provided with the 5th gas vent and top is provided with the 6th gas vent, the 5th gas
Export and be connected by delivery pipe with the middle part of the lightness-removing column provided with charging input unit, the 6th gas vent passes through defeated
Pipe is sent to be connected with compressor.
Using above-mentioned technical proposal, set by such, the middle part of lightness-removing column is provided with charging input unit and its bottom
Delivery outlet be connected by butane tower delivery pipe with the charging aperture at the middle part of butane tower, raw material by charging input unit enter
After lightness-removing column, remove after light component, sent into by the delivery outlet of lightness-removing column bottom in butane tower, in butane tower after separation,
By the discharging opening of the bottom of butane tower by being passed through the first of the top of positive structure reactor after the condensed current divider of delivery pipe again
Gas is passed through mouth hence into positive structure reactor, after positive structure catalytic reaction, the through positive structure reactor bottom the 3rd
Thick normal butane feeding weight-removing column in the gas that gas vent is discharged and discharges positive structure reactor through delivery pipe carries out de- weight
After obtain normal butane, the remaining condensed current divider of gas component after send into hydrogenation reactor, the top of the condensation current divider
Mouth is passed through provided with hydrogen, the bottom of the hydrogenation reactor is provided with the 4th gas vent, and the 4th gas vent will be hydrogenated with anti-
Gas after answering send knockout drum after cooler, and the knockout drum will send into institute available for the raw material of recycling by delivery pipe
The middle part of lightness-removing column is stated provided with charging input unit and gaseous products are sent into compressor；Hydrogen can so be recycled and anti-
Remaining alkane or byproduct of reaction in answering, have saved raw material, have been both to save the energy, and reaction efficiency is high, and production is just
Butane purity is high, can produce the normal butane of purity >=97.5.In order to save energy expenditure, to the air-flow of hydrogenation reaction product
Cooling generally selects 2-4 grades of coolings generally using two-stage or multistage cooling, and the material after cooling can select to reclaim or do not return
Receive.
The present invention further improvement is that, the gas vent of the compressor with it is described condensation current divider hydrogen be passed through mouth
It is connected, and connection waste gas recovering device.
The present invention further improvement is that, positive the structure reactor and the hydrogenation reactor are fixed bed or movement
Bed or fluid bed.
The present invention further improvement is that, the quantity of the positive structure reactor is at least one；The positive structureization reaction
Bed number in device is 1-2 layers.
The present invention further improvement is that, the quantity of the hydrogenation reactor is the bed in one, the hydrogenation reactor
The number of plies is layer 2-3.
The present invention further improvement is that, the butane tower be Double-Tower Structure.
The present invention further improvement is that, in the charging input unit of the lightness-removing column be provided with low-temperature condenser.Be afraid of sample
Setting can reduce the consumption of cold, simplify operation equipment.The bottom of towe of lightness-removing column is provided with reboiler, and the heating medium of reboiler can
To be low-pressure steam or hot water or conduction oil.
The present invention further improvement is that, the inner upper end of the weight-removing column is provided with knockout drum, the gas-liquid separation
The top of the inner side of tank is provided with foam removal net.
Compared with prior art, the beneficial effect of the technical scheme is：The preparation method is simply controllable, and the process
High conversion rate, without accessory substance, yield is high, and economic benefit is more preferable；The preparation method is produced using butane as normal butane
Raw material, improve the economic value added of butane；The high usage of butane raw material, the iso-butane without by-product, work
Factory need not set iso-butane products pot and huge head tank group, and handling and traffic unit also can greatly reduce scale；Can
Produce the normal butane of purity >=97.5.
Brief description of the drawings
Technical scheme is further described below in conjunction with the accompanying drawings：
Fig. 1 is the structural representation of the system and device that normal butane is prepared by the positive structure of iso-butane of the present invention；
Wherein：1- feeds input unit；2- lightness-removing columns；3- butane towers；4- weight-removing columns；5- condenses current divider；501- hydrogen is passed through
Mouthful；The positive structure reactors of 6-；7- hydrogenation reactors；8- coolers；9- knockout drums；10- compressors；11- fresh hydrogen sources of the gas；12-
Waste gas recovering device；13- heavy constituent collectors.
Embodiment
Make further details of explanation to technical scheme with reference to specific embodiment, but not to present invention tool
There is restriction effect.
Embodiment 1：The preparation method of the normal butane, using butane as raw material, comprises the following steps：
（1）Raw material is sent into lightness-removing column 2, is removed after light component, is re-fed into butane tower 3 and carries out isolated iso-butane；
（2）The tower top of the butane tower 3 is isolated into iso-butane and sends into positive structure reactor 6, in positive structure after catalytic reaction
The bottom of reactor 6 obtains thick normal butane and defective material；
（3）Thick normal butane is sent into weight-removing column 4, the heavy constituent of carbon four in thick normal butane is removed, is obtained in the tower top of the weight-removing column 4
To the normal butane product that mass fraction is 97.5 ~ 99%；
（4）By the step（2）In defective material feeding hydrogenation reactor 7, carry out hydrogenation reaction, make isobutene in defective material, third
Alkene, 1- butylene, 2- butylene hydrogenation, obtain including methane, ethane, propane, iso-butane, normal butane, the hydrogenation products of hydrogen；
（5）By the condensed separation of product after hydrogenation reaction, gaseous products are removed, the gaseous products are methane, ethane, propane
And hydrogen, obtain the positive structure product being made up of normal butane and iso-butane；
（6）By step（5）In the obtained positive structure product send into the lightness-removing column 2, and press the step successively（1）、
（2）、（3）Step process, obtains normal butane product；
The step（1）Described in raw material be the material containing butane or the material containing unsaturated carbon four；The step
（1）Described in the tower top of lightness-removing column 2 use cryogenic condensation mode, the temperature of condensation is 10 DEG C, using heat exchanger or segregation and fractionation
System carries out condensation operation；The step（2）In the positive structure reactor 6 in catalyst include carrier, active constituent
And auxiliary agent；The carrier is made up of refractory oxides or mixed oxide, the carrier be zinc oxide, silica, aluminum oxide,
One or more mixing in magnesia；The active constituent is mixed comprising one or more VIII magnesium-yttrium-transition metals, and component contains
Measure as mass fraction 0.05%；The auxiliary agent is one kind in tin oxide, zinc oxide, vanadium oxide, iron oxide；The step（2）In
400 DEG C of the reaction temperature of the positive structure reactor 6, reaction pressure is 3MPa；The step（3）In in the weight-removing column 4
Bottom of towe obtains the material of the heavy constituent of carbon four；Wherein the mass fraction of normal butane is 10%；The tower top pressure of weight-removing column 4 is 0.4
MPa, tower top temperature is 40 DEG C, and full tower pressure drop is 20kPa, and column bottom temperature is 80 DEG C, overhead reflux ratio >=1；The step（4）In
The reaction temperature of the hydrogenation reactor 7 is 80 DEG C；The step（5）Described in hydrogenation reaction product gas flow condensation temperature
Spend for 10 DEG C；Condensing mode is using 2 ~ 4 grades of cooling down operations.
Embodiment 2：The preparation method of the normal butane, using butane as raw material, comprises the following steps：
（1）Raw material is sent into lightness-removing column 2, is removed after light component, is re-fed into butane tower 3 and carries out isolated iso-butane；
（2）The tower top of the butane tower 3 is isolated into iso-butane and sends into positive structure reactor 6, in positive structure after catalytic reaction
The bottom of reactor 6 obtains thick normal butane and defective material；
（3）Thick normal butane is sent into weight-removing column 4, the heavy constituent of carbon four in thick normal butane is removed, is obtained in the tower top of the weight-removing column 4
To the normal butane product that mass fraction is 97.5 ~ 99%.
（4）By the step（2）In defective material feeding hydrogenation reactor 7, carry out hydrogenation reaction, make the isobutyl in defective material
Alkene, propylene, 1- butylene, 2- butylene hydrogenation, obtain the hydrogenation comprising methane, ethane, propane, iso-butane, normal butane, hydrogen and produce
Thing；
（5）By hydrogenation products condensation separation, gaseous products are removed, the gaseous products are methane, ethane, propane and hydrogen, are obtained
To the positive structure product being made up of normal butane and iso-butane；
（6）By step（5）In the obtained positive structure product send into the lightness-removing column 2, and press the step successively（1）、
（2）、（3）Step process, obtains normal butane product；
The step（1）Described in raw material be the material containing butane or the material containing unsaturated carbon four；The step
（1）Described in the tower top of lightness-removing column 2 use cryogenic condensation mode, the temperature of condensation is 15 DEG C, using heat exchanger or segregation and fractionation
System carries out condensation operation；The step（2）In the positive structure reactor 6 in catalyst include carrier, active constituent
And auxiliary agent；The carrier is made up of refractory oxides or mixed oxide, the carrier be zinc oxide, silica, aluminum oxide,
One or more mixing in magnesia；The active constituent is mixed comprising one or more VIII magnesium-yttrium-transition metals, and component contains
Measure as mass fraction 1.25%；The auxiliary agent is one kind in tin oxide, zinc oxide, vanadium oxide, iron oxide；The step（2）In
480 DEG C of the reaction temperature of the positive structure reactor 6, reaction pressure is 4MPa；The step（3）In in the weight-removing column 4
Bottom of towe obtains the material of the heavy constituent of carbon four；Wherein the mass fraction of normal butane is 10 ~ 15%；The tower top pressure of weight-removing column 4 is 0.6
MPa, tower top temperature is 55 DEG C, and full tower pressure drop is 40kPa, and column bottom temperature is 95 DEG C, overhead reflux ratio >=1；The step（4）In
The reaction temperature of the hydrogenation reactor 7 is 150 DEG C；The step（5）Described in hydrogenation reaction product gas flow condensation temperature
Spend for 20 DEG C；Condensing mode is using 2 ~ 4 grades of cooling down operations.
Embodiment 3：The preparation method of the normal butane, using butane as raw material, comprises the following steps：
（1）Raw material is sent into lightness-removing column 2, is removed after light component, is re-fed into butane tower 3 and carries out isolated iso-butane；
（2）The tower top of the butane tower 3 is isolated into iso-butane and sends into positive structure reactor 6, in positive structure after catalytic reaction
The bottom of reactor 6 obtains thick normal butane and defective material；
（3）Thick normal butane is sent into weight-removing column 4, the heavy constituent of carbon four in thick normal butane is removed, is obtained in the tower top of the weight-removing column 4
To the normal butane product that mass fraction is 97.5 ~ 99%.
（4）By the step（2）In defective material feeding hydrogenation reactor 7, carry out hydrogenation reaction, make the isobutyl in defective material
Alkene, propylene, 1- butylene, 2- butylene hydrogenation, obtain the hydrogenation comprising methane, ethane, propane, iso-butane, normal butane, hydrogen and produce
Thing；
（5）By hydrogenation products condensation separation, gaseous products are removed, the gaseous products are methane, ethane, propane and hydrogen, are obtained
To the positive structure product being made up of normal butane and iso-butane；
（6）By step（5）In the obtained positive structure product send into the lightness-removing column 2, and press the step successively（1）、
（2）、（3）Step process, obtains normal butane product；
The step（1）Described in raw material be the material containing butane or the material containing unsaturated carbon four；The step
（1）Described in the tower top of lightness-removing column 2 use cryogenic condensation mode, the temperature of condensation is 20 DEG C, using heat exchanger or segregation and fractionation
System carries out condensation operation；The step（2）In the positive structure reactor in catalyst comprising carrier, active constituent and
Auxiliary agent；The carrier is made up of refractory oxides or mixed oxide, and the carrier is zinc oxide, silica, aluminum oxide, oxygen
Change one or more mixing in magnesium；The active constituent is mixed comprising one or more VIII magnesium-yttrium-transition metals, constituent content
For mass fraction 2.5%；The auxiliary agent is one kind in tin oxide, zinc oxide, vanadium oxide, iron oxide；The step（2）Middle institute
550 DEG C of the reaction temperature of positive structure reactor 6 is stated, reaction pressure is 4.5MPa；The step（3）In in the weight-removing column 4
Bottom of towe obtains the material of the heavy constituent of carbon four；Wherein the mass fraction of normal butane is 15%；The tower top pressure of weight-removing column 4 is 0.8
MPa, tower top temperature is 70 DEG C, and full tower pressure drop is 60kPa, and column bottom temperature is 105 DEG C, overhead reflux ratio >=1；The step（4）
Described in hydrogenation reactor 7 reaction temperature be 220 DEG C；The step（5）Described in hydrogenation reaction product gas flow condensation
Temperature is 30 DEG C；Condensing mode is using 2 ~ 4 grades of cooling down operations.
Embodiment 4：As shown in figure 1, the system and device of normal butane should be prepared by the positive structure of iso-butane, including lightness-removing column 2, fourth
Alkane tower 3, weight-removing column 4 and positive structure reactor 6；Output of the middle part of the lightness-removing column 2 provided with charging input unit 1 and its bottom
Mouth is connected by the delivery pipe of butane tower 3 with the charging aperture at the middle part of butane tower 3, and the top of the butane tower 3 is provided with the first gas
Body is exported；First gas outlet by delivery pipe successively with condensation current divider 5 and the top of positive structure reactor 6 first
Gas is passed through mouth and is connected, and the bottom of the positive structure reactor 6 is exported provided with third gas, and the 3rd gas outlet is through conveying
Pipe is connected with weight-removing column 4 and condensation current divider 5 respectively, and the top of the weight-removing column 4 is exported and described de- provided with second gas
The bottom of weight tower 4 is provided with heavy constituent collector 13；The side of the condensation current divider 5 is connected and described cold with hydrogenation reactor 7
The top of solidifying current divider 5 is passed through mouth 501 provided with hydrogen, and the bottom of the hydrogenation reactor 7 is provided with the 4th gas vent, and described the
Four gas vents are connected with cooler 8 and knockout drum 9 successively by delivery pipe, and the bottom of the knockout drum 9 is provided with the 5th gas
Body is exported and top is provided with the 6th gas vent, and the 5th gas vent is set by delivery pipe and the middle part of the lightness-removing column 2
There is charging input unit 1 to be connected, the 6th gas vent is connected by delivery pipe with compressor 10；The compressor 10
Gas vent be passed through mouth 501 with the hydrogen of the condensation current divider 5 and be connected, and connection waste gas recovering device 12；It is described just
Structure reactor 6 and the hydrogenation reactor 7 are fixed bed or moving bed or fluid bed；The number of the positive structure reactor 6
Measure as one；Bed number in the positive structure reactor 6 is 1-2 layers；The quantity of the hydrogenation reactor 7 is one, described
Bed number in hydrogenation reactor 7 is layer 2-3；The butane tower 3 is Double-Tower Structure；The charging input unit 1 of the lightness-removing column 2
In be provided with low-temperature condenser；The bottom of towe of lightness-removing column 2 is provided with reboiler, and the heating medium of reboiler can be low-pressure steam or hot water
Or conduction oil；The inner upper end of the weight-removing column 4 is provided with knockout drum, and the top of the inner side of the knockout drum is provided with
Foam removal net.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements done etc. should be included in the scope of the protection.
Claims (9)
1. a kind of preparation method of normal butane, using butane as raw material, comprises the following steps：
（1）Raw material is sent into lightness-removing column, removed after light component, feeding butane tower carries out isolated iso-butane；
（2）The tower top of the butane tower is isolated into iso-butane and sends into positive structure reactor, it is anti-in positive structureization after catalytic reaction
The bottom of device is answered to obtain thick normal butane and defective material；
（3）Thick normal butane is sent into weight-removing column, the heavy constituent of carbon four in thick normal butane is removed, is obtained in the tower top of the weight-removing column
Mass fraction is 97.5 ~ 99% normal butane product.
2. the preparation method of normal butane as claimed in claim 1, it is characterised in that the preparation method of the normal butane also include with
Lower step：
（4）By the step（2）In defective material feeding hydrogenation reactor, carry out hydrogenation reaction, make isobutene in defective material, third
Alkene, 1- butylene, 2- butylene hydrogenation, obtain including methane, ethane, propane, iso-butane, normal butane, the hydrogenation products of hydrogen；
（5）By hydrogenation products condensation separation, gaseous products are removed, the gaseous products are methane, ethane, propane and hydrogen, are obtained
To the positive structure product being made up of normal butane and iso-butane；
（6）By step（5）In the obtained positive structure product send into the dealkylation tower, and press the step successively（1）、（2）、
（3）Step process, obtains normal butane product.
3. the preparation method of normal butane as claimed in claim 1, it is characterised in that the step（1）Described in raw material be containing
There are the material of butane or the material containing unsaturated carbon four.
4. the preparation method of normal butane as claimed in claim 2, it is characterised in that the step（1）Described in lightness-removing column
Tower top uses cryogenic condensation mode, and the temperature of condensation is 10 ~ 20 DEG C, and condensation behaviour is carried out using heat exchanger or segregation and fractionation system
Make.
5. the preparation method of normal butane as claimed in claim 4, it is characterised in that the step（2）In the positive structure
Catalyst in reactor includes carrier, active constituent and auxiliary agent；The carrier is made up of refractory oxides or mixed oxide,
The carrier is one or more mixing in zinc oxide, silica, aluminum oxide, magnesia；The active constituent includes one
Plant or the mixing of several VIII magnesium-yttrium-transition metals, constituent content is mass fraction 0.05 ~ 2.5%；The auxiliary agent is tin oxide, oxidation
One kind in zinc, vanadium oxide, iron oxide.
6. the preparation method of normal butane as claimed in claim 5, it is characterised in that the step（2）Described in positive structureization it is anti-
400 ~ 550 DEG C of the reaction temperature of device is answered, reaction pressure is 3 ~ 4.5MPa.
7. the preparation method of normal butane as claimed in claim 6, it is characterised in that the step（3）In in the weight-removing column
Bottom of towe obtain the material of the heavy constituent of carbon four；Wherein the mass fraction of normal butane is 10 ~ 15%.
8. the preparation method of normal butane as claimed in claim 7, it is characterised in that the step（4）Described in hydrogenation reaction
The reaction temperature of device is 80 ~ 220 DEG C.
9. the preparation method of normal butane as claimed in claim 8, it is characterised in that the step（5）Described in hydrogenation reaction
Product gas flow condensation temperature be 10 ~ 30 DEG C；Condensing mode is using 2 ~ 4 grades of cooling down operations.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710531027.7A CN107285978A (en) | 2017-07-03 | 2017-07-03 | The preparation method of normal butane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710531027.7A CN107285978A (en) | 2017-07-03 | 2017-07-03 | The preparation method of normal butane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107285978A true CN107285978A (en) | 2017-10-24 |
Family
ID=60099539
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710531027.7A Pending CN107285978A (en) | 2017-07-03 | 2017-07-03 | The preparation method of normal butane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107285978A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830861A (en) * | 2019-11-25 | 2021-05-25 | 中国石油化工股份有限公司 | Device and method for producing n-butane |
| CN115505420A (en) * | 2021-06-23 | 2022-12-23 | 中国石化工程建设有限公司 | Light naphtha normalization method |
| CN115505419A (en) * | 2021-06-23 | 2022-12-23 | 中国石化工程建设有限公司 | Light naphtha positive structuring method |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101143812A (en) * | 2007-09-25 | 2008-03-19 | 张文慧 | Technique for producing formate |
| CN101219945A (en) * | 2007-12-20 | 2008-07-16 | 林德增 | Technique for producing sodium formate with semiwater gas |
| CN201445894U (en) * | 2009-07-31 | 2010-05-05 | 山东联合化工股份有限公司 | Device capable of pressure swing absorption, decarbonization, pressure release and recovery |
| CN102317242A (en) * | 2009-01-13 | 2012-01-11 | 塞彭公司 | Process for obtaining high-purity 1-butene from c4 hydrocarbon mixtures |
| CN102992933A (en) * | 2012-10-13 | 2013-03-27 | 东华工程科技股份有限公司 | Separation method for mixed C4 |
| CN103073376A (en) * | 2013-02-22 | 2013-05-01 | 南京炼油厂有限责任公司 | Separation process of mixed pentane |
| CN104892339A (en) * | 2015-06-05 | 2015-09-09 | 常州瑞华化工工程技术有限公司 | Method for preparing n-butane by using iso-butane |
-
2017
- 2017-07-03 CN CN201710531027.7A patent/CN107285978A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101143812A (en) * | 2007-09-25 | 2008-03-19 | 张文慧 | Technique for producing formate |
| CN101219945A (en) * | 2007-12-20 | 2008-07-16 | 林德增 | Technique for producing sodium formate with semiwater gas |
| CN102317242A (en) * | 2009-01-13 | 2012-01-11 | 塞彭公司 | Process for obtaining high-purity 1-butene from c4 hydrocarbon mixtures |
| CN201445894U (en) * | 2009-07-31 | 2010-05-05 | 山东联合化工股份有限公司 | Device capable of pressure swing absorption, decarbonization, pressure release and recovery |
| CN102992933A (en) * | 2012-10-13 | 2013-03-27 | 东华工程科技股份有限公司 | Separation method for mixed C4 |
| CN103073376A (en) * | 2013-02-22 | 2013-05-01 | 南京炼油厂有限责任公司 | Separation process of mixed pentane |
| CN104892339A (en) * | 2015-06-05 | 2015-09-09 | 常州瑞华化工工程技术有限公司 | Method for preparing n-butane by using iso-butane |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830861A (en) * | 2019-11-25 | 2021-05-25 | 中国石油化工股份有限公司 | Device and method for producing n-butane |
| CN112830861B (en) * | 2019-11-25 | 2023-03-28 | 中国石油化工股份有限公司 | Device and method for producing n-butane |
| CN115505420A (en) * | 2021-06-23 | 2022-12-23 | 中国石化工程建设有限公司 | Light naphtha normalization method |
| CN115505419A (en) * | 2021-06-23 | 2022-12-23 | 中国石化工程建设有限公司 | Light naphtha positive structuring method |
| CN115505419B (en) * | 2021-06-23 | 2023-11-03 | 中国石化工程建设有限公司 | Light naphtha orthographic structuring method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101348412B (en) | Energy-saving method for phenyl ethylene rectification | |
| CN101475429B (en) | Method for comprehensive utilization of cracking C4 | |
| CN102040445B (en) | Technology device and method for preparing propylene by dehydrogenating propane or propane-enriched low carbon hydrocarbon | |
| CN103965002B (en) | The oxidative dehydrogenation processes of lower carbon number hydrocarbons | |
| CN102060664B (en) | High-efficiency and energy-saving reaction process for preparing ethylene glycol through hydrogenation of oxalate | |
| CN101115700B (en) | Process for production of aromatic compound and process for production of hydrogenated aromatic compound | |
| CN101306973B (en) | Process for recovering ethylene in process of ethylene preparation by ethanol dehydration | |
| CN1830934A (en) | Method for producing dimethyl ether using methanol as raw material | |
| CN102267850A (en) | Method for separating light olefins gas | |
| CN101429089A (en) | Bulkhead type rectification column for separating materials containing ethylbenzene and vinyl benzene | |
| CN107285978A (en) | The preparation method of normal butane | |
| CN103086828B (en) | The method of volume increase divinyl | |
| CN101747128B (en) | Separation method for preparing low-carbon olefin by conversion of methanol | |
| CN101429088A (en) | Distillation method for separating ethylbenzene and vinyl benzene-containing flow | |
| CN101092325B (en) | Method for preparing propylene by catalytic cracking olefin of containing carbon | |
| CN107285977A (en) | A kind of system and device that normal butane is prepared by the positive structure of iso-butane | |
| CN101085711B (en) | Method for synthesizing ethyl benzene and diethyl benzene | |
| CN107089644A (en) | A kind of carbon dioxide discharge-reduction and the apparatus and method of comprehensive utilization | |
| CN104892339B (en) | A kind of method that normal butane is prepared by iso-butane | |
| CN107673952A (en) | The method that 1,2 propane diols and normal propyl alcohol are prepared using biological glycerol | |
| CN103420752B (en) | Separation refinement method for ethylene preparation through biomass ethanol dehydration | |
| CN101633597A (en) | Method for saving energy in rectification of styrene | |
| CN103772102B (en) | The separation and refining method of producing ethylene from dehydration of ethanol | |
| CN105585421B (en) | The method that ester high selectivity prepares alcohol | |
| CN105523887B (en) | The highly selective method for preparing alcohol of ester |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171024 |