CN109438167A - A kind of cyclohexene production energy-saving system and production method - Google Patents
A kind of cyclohexene production energy-saving system and production method Download PDFInfo
- Publication number
- CN109438167A CN109438167A CN201811610923.3A CN201811610923A CN109438167A CN 109438167 A CN109438167 A CN 109438167A CN 201811610923 A CN201811610923 A CN 201811610923A CN 109438167 A CN109438167 A CN 109438167A
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- China
- Prior art keywords
- benzene
- tower
- cyclohexene
- rectifying column
- extractant
- Prior art date
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- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 title claims abstract description 177
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 46
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 611
- 238000006243 chemical reaction Methods 0.000 claims abstract description 106
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims abstract description 68
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000011084 recovery Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims description 53
- 229910052739 hydrogen Inorganic materials 0.000 claims description 53
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 238000010992 reflux Methods 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000009834 vaporization Methods 0.000 claims description 11
- 230000008016 vaporization Effects 0.000 claims description 11
- 238000000605 extraction Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 238000010926 purge Methods 0.000 claims description 8
- 239000007790 solid phase Substances 0.000 claims description 8
- 238000007670 refining Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 8
- 239000006227 byproduct Substances 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 description 11
- 238000003860 storage Methods 0.000 description 11
- 230000001351 cycling effect Effects 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- -1 hexamethylene Alkene Chemical class 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002510 pyrogen Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- C07C5/02—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation
- C07C5/10—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of aromatic six-membered rings
- C07C5/11—Partial hydrogenation
-
- 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
- C07C5/10—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of aromatic six-membered rings
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/10—Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids
-
- 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
-
- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
-
- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of cyclohexene production energy-saving system and production methods, belong to cyclohexene production technical field.The present invention is with benzene raw materials hydrogenation catalyst, separating-purifying is carried out to reaction product by system for separating and purifying, cyclohexene is made, the present invention passes through setting heat recovery system simultaneously, by the recovered utilization of the heat of reaction material liquid during separating-purifying, energy saving colleague also improves production efficiency, in addition, participating in raw material of the invention: benzene and extractant are all recycled again, it is all back in feed system after separating-purifying and utilizes again, saved resource.Simultaneously as entire production process is all generated without by-product, obtained product hexamethylene and cyclohexene will all be used as products application, very environmentally protective.
Description
Technical field
The present invention relates to cyclohexene preparation technical fields, and in particular to a kind of cyclohexene production energy-saving system and producer
Method.
Background technique
Adipic acid, caprolactam production route based on cyclohexene hydration method are the mainstream works in current industrialized production
Skill.Wherein, the production of cyclohexene mostly uses the partial hydrogenation of benzene, under the effect of the catalyst, in the liquid-solid four phase system of solution-air-
Reaction generates cyclohexene, hexamethylene and water.
Traditional partial hydrogenation of benzene generates cyclohexene and does not utilize to reaction heat, is only carried out by recirculated cooling water cold
But, the waste of the energy is caused, production cost is increased.
Summary of the invention
The object of the present invention is to provide a kind of cyclohexene production energy-saving system and production methods, to solve existing ring
The high problem of the wasting of resources of hexene production technology, production cost.
The technical scheme to solve the above technical problems is that
A kind of cyclohexene production energy-saving system characterized by comprising feed system, reaction system, system for separating and purifying
And heat recovery system；Wherein:
Feed system include connect respectively with reaction system plus benzene device, hydrogenation plant and nitrogen purging device and with
System for separating and purifying connection adds extractant device；
Reaction system include with plus benzene device, hydrogenation plant and the nitrogen purging device reaction kettle and and reaction kettle that connect
The liquid-phase outlet of the subsider of connection, subsider is connect with system for separating and purifying；
System for separating and purifying includes benzene knockout tower, benzene rectifying column, hexamethylene knockout tower and cyclohexene rectifying column；Benzene knockout tower
Entrance respectively with the liquid-phase outlet of subsider and extractant device is added connect, the tower bottom of benzene knockout tower exports and tower top outlet
It is connect respectively with the tower bottom entrance of the entrance of benzene rectifying column and hexamethylene knockout tower；The tower top outlet and tower bottom of benzene rectifying column export
Respectively with add benzene device and add extractant device connect；The tower bottom outlet of hexamethylene knockout tower is connect with cyclohexene rectifying column；Ring
The tower bottom outlet of hexene rectifying column is connect with extractant device is added；
Heat recovery system includes that First Heat Exchanger, the second heat exchanger, third heat exchanger, the first reboiler and second boil again
Device；First Heat Exchanger is connect with the entrance of the outlet and reaction kettle that add benzene device respectively, and First Heat Exchanger is also changed with second respectively
Hot device is connected with the entrance of benzene rectifying column；First reboiler is connect with the outlet of the tower bottom of benzene knockout tower and the second heat exchanger respectively,
And the tower bottom of the first reboiler and benzene rectifying column, which exports, to be connected；Second heat exchanger, third heat exchanger and the second reboiler are successively
It is connected in the tower bottom outlet of hexamethylene knockout tower；Third heat exchanger exports with the tower bottom of cyclohexene rectifying column respectively and adds extraction
The entrance of agent device connects；The outlet of second reboiler is connect with hexamethylene knockout tower and cyclohexene rectifying column respectively.
Further, in preferred embodiments of the present invention, the solid-phase outlet of above-mentioned subsider passes through pipeline and reaction kettle
Connection.
Further, in preferred embodiments of the present invention, above-mentioned cyclohexene production energy-saving system further includes extractant storage
Deposit tank, the entrance of extractant holding vessel is connect with the first reboiler and third heat exchanger respectively, the outlet of extractant holding vessel with
The entrance of extractant device is added to connect.
Further, in preferred embodiments of the present invention, above-mentioned plus benzene device include benzene holding vessel and respectively with benzene
The refining benzene pipeline and recycle benzene pipeline of the entrance connection of holding vessel, recycle benzene pipeline are connect with the tower top outlet of benzene rectifying column.
Further, in preferred embodiments of the present invention, above-mentioned hydrogenation plant includes that hydrogen inlet manifold road and hydrogen follow
Endless tube road, hydrogen inlet manifold road and hydrogen circulating line are connected by the entrance of booster pump and reaction kettle, hydrogen circulating line with
The hydrogen outlet of reaction kettle connects.
A method of utilizing above-mentioned cyclohexene production energy-saving system production cyclohexene, comprising:
(1) raw material benzene hydrogenation and catalyst are reacted in a kettle, the mixed liquor after reaction is settled through subsider；
(2) obtained supernatant will be delivered to separating-purifying in benzene knockout tower after sedimentation, by what is obtained through benzene knockout tower
Overhead distillate is sent into hexamethylene knockout tower, by the tower reactor mixed liquor obtained through benzene knockout tower be delivered in the first reboiler with
After the tower reactor feed liquid heat exchange of benzene rectifying column, benzene rectifying column is entered to after the second heat exchanger and First Heat Exchanger heat exchange by pipeline
In；Wherein, the heat that the tower reactor mixed liquor of benzene knockout tower enters First Heat Exchanger is used to preheat benzene feedstock, benzene knockout tower
Tower reactor mixed liquor include benzene and extractant, the overhead distillate of benzene knockout tower includes hexamethylene and cyclohexene；
(3) benzene obtained after benzene rectifying column separating-purifying is exported from tower top, and is back to and is added in benzene device by pipeline,
The tower reactor feed liquid of benzene rectifying column exports after the heat exchange of the first reboiler from tower bottom, and the part of vaporization is back to benzin by pipeline and evaporates
In tower, unboiled part is back to by pipeline plus extractant device；Wherein, the tower reactor feed liquid of benzene rectifying column includes benzene and extraction
Take agent；
(4) overhead distillate from benzene knockout tower is through hexamethylene knockout tower separating-purifying, and obtained hexamethylene is from tower top
Output, while the tower reactor mixed liquor of hexamethylene knockout tower being delivered in the second heat exchanger and is mixed with the tower reactor from benzene knockout tower
After liquid heat, exchanges heat again with the tower reactor feed liquid from cyclohexene rectifying column into third heat exchanger, enters back into the second reboiler,
The part vaporized in second reboiler is back in hexamethylene knockout tower by pipeline, and unboiled part enters to cyclohexene essence
It evaporates in tower；
(5) after cyclohexene rectifying column separating-purifying, obtained cyclohexene is defeated from tower top for part unboiled in step (4)
Out, remaining extractant, which exports to be back to by pipeline after the heat exchange of third heat exchanger from tower bottom, adds extractant device.
Further, in preferred embodiments of the present invention, it is 4- that the reaction condition in reaction kettle, which includes: in Hydrogen Vapor Pressure,
7MPa, reaction temperature are to react 10-50min at 140-180 DEG C, are continually fed into hydrogen during the reaction and keep pressure permanent
Fixed, the mass ratio of benzene feedstock and catalyst is (10-30): 1.
Present invention Hydrogen Vapor Pressure in control reaction process is 4-7MPa, can combine hydrogen activity and to cyclohexene
Selectivity.Because will lead to that hydrogenation activity is excessively low when Hydrogen Vapor Pressure is lower than 4MPa, so that the conversion ratio of benzene reduces, it is unfavorable
It is improved in production efficiency；When Hydrogen Vapor Pressure is higher than 7MPa, hydrogenation activity is too high, so that cyclohexene selectively reduces, it is easily generated
Excessive hexamethylene is unfavorable for the production of primary target product cyclohexene.In addition, in conjunction with suitable 140-180 DEG C of reaction temperature
Degree, can both guarantee that benzene can be converted sufficiently in this temperature range, improve productivity, and can lead to avoid because temperature is excessively high
Cyclohexene is caused selectively to reduce.
Further, in preferred embodiments of the present invention, the reaction condition of benzene knockout tower includes: that bottom temperature is 120-
140 DEG C, tower top temperature is 80-100 DEG C, full tower pressure drop 0.01-0.04MPa, tower top molar reflux ratio >=1.5；Benzene rectifying column
Reaction condition includes: that bottom temperature is 75-85 DEG C, and tower top temperature is 42-48 DEG C, full tower vacuum degree >=0.03MPa, and reflux ratio >=
0.8。
Further, in preferred embodiments of the present invention, the reaction condition of hexamethylene knockout tower includes: that bottom temperature is
90-110 DEG C, tower top temperature is 85-95 DEG C, full tower pressure drop 0.01-0.04MPa, overhead reflux ratio >=3.0；Cyclohexene rectifying column
Reaction condition include: bottom temperature be 130~150 DEG C, tower top temperature be 42-50 DEG C, full tower vacuum degree >=0.03MPa, tower
Push up molar reflux ratio >=0.8.
The tower reactor temperature that the present invention passes through control benzene knockout tower, benzene rectifying column, hexamethylene knockout tower and cyclohexene rectifying column
Degree, tower top temperature, full tower pressure drop and the control of molar reflux ratio, can be in the evaporation rate for meeting kettle material and cooling speed
While rate, tower top material and the mass fraction of kettle material product can be equally set to reach the set goal, to maintain tower
It operates normally.In addition, in benzene rectifying column and cyclohexene rectifying column when separating-purifying, the full tower vacuum degree of present invention control >=
The boiling point of tower top material can be maintained 42 DEG C or more under conditions of absolute pressure is higher than 0.03MPa by 0.03MPa, thus
More cheap heat source (cooling medium) cooling material can be used, and then reach energy saving purpose.
The invention has the following advantages:
The present invention is carried out separating-purifying to reaction product by system for separating and purifying and hexamethylene is made with benzene raw materials hydrogenation catalyst
Alkene, while the present invention is saved the recovered utilization of the heat of reaction material liquid during separating-purifying by setting heat recovery system
Production efficiency is also improved while the energy, in addition, participating in raw material of the invention: benzene and extractant are all recycled again,
It is all back in feed system after separating-purifying and utilizes again, saved resource.Simultaneously as entire production process does not all have
There is by-product generation, obtained product hexamethylene and cyclohexene will all be used as products application, very environmentally protective.The present invention is whole
High-purity hexamethylene is obtained during a positive production, can also be used as the production system of hexamethylene.
The present invention carries out sedimentation separation to the product after reaction by subsider, and the solid phase after sedimentation is catalyst, passes through
Pipeline is set in solid-phase outlet, catalyst can be back in reaction kettle again and carry out catalysis reaction, avoid the wasting of resources.
The present invention recycles the extractant after entire separating-purifying process by the first reboiler and third heat exchanger,
Then concentrate be stored in extractant holding vessel, by pipeline be back to plus extractant device in participate in system for separating and purifying again
In, so that resource circulation utilization.
Pipeline is arranged by the hydrogen outlet at the top of reaction kettle in the present invention, can return to the complete hydrogen of unreacted
It is utilized into hydrogenation plant, avoids the wasting of resources.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of production system of the present invention.
In figure: 10- reaction kettle；21- benzene knockout tower；22- benzene rectifying column；23- hexamethylene knockout tower；24- cyclohexene rectifying
Tower；31- First Heat Exchanger；The first reboiler of 32-；The second heat exchanger of 33-；34- third heat exchanger；The second reboiler of 35-；41-
Benzene holding vessel；42- subsider；43- extractant holding vessel；44- adds extractant device；50- circulating pump；60- booster pump.
Specific embodiment
Principles and features of the present invention are described below in conjunction with drawings and examples, example is served only for explaining this
Invention, is not intended to limit the scope of the present invention.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Embodiment 1
Please refer to Fig. 1, cyclohexene production energy-saving system of the invention comprising: feed system, reaction system, separation mention
Pure lines system and heat recovery system.
Feed system include connect respectively with reaction system plus benzene device, hydrogenation plant and nitrogen purging device and with
System for separating and purifying connection adds extractant device 44.Add the outlet of benzene device, hydrogenation plant and nitrogen purging device respectively with
The entrance of the reaction kettle 10 of reaction system connects.
The benzene in benzene device is added to be delivered in reaction kettle 10 by circulating pump 50.Benzene in benzene device is added to derive from two parts:
Recycle benzene in additional refining benzene and production system.Add benzene device include benzene holding vessel 41 and respectively with benzene holding vessel 41
The refining benzene pipeline and recycle benzene pipeline of entrance connection.The tower top outlet of the benzene rectifying column 22 of recycle benzene pipeline and system for separating and purifying
Connection.
After hydrogen in hydrogenation plant is pressurized by booster pump 60, it is delivered in reaction kettle 10, is inputted into reaction kettle 10
The hydrogen of pressure needed for reacting.Hydrogen source in hydrogenation plant is in two parts: reaction kettle in added hydrogen and production system
The remaining hydrogen that unreacted is completed in 10.Hydrogenation plant includes hydrogen inlet manifold road and hydrogen circulating line.Hydrogen inlet manifold road
It is connect by booster pump 60 with the entrance of reaction kettle 10 with hydrogen circulating line.Hydrogen inlet manifold road is connect with hydrogen container.Hydrogen
Circulating line is connect with the hydrogen outlet of reaction kettle 10.
Nitrogen purging device is blown into reaction kettle 10 after being pressurized by booster pump 60, for excluding reaction kettle 10 before the reaction
Interior air.Add the extractant in extractant device 44 to be delivered in separation proposition system by circulating pump 50, is used for benzene, hexamethylene
The separating-purifying of alkane, cyclohexene.Adding the extractant in extractant device 44 includes two parts: the additional extractant from storage tank with
And the extractant after production system separating-purifying.
Reaction system include with plus the reaction kettle 10 that connect of benzene device, hydrogenation plant and nitrogen purging device and with react
The subsider 42 that kettle 10 connects.The liquid-phase outlet of subsider 42 is connect with system for separating and purifying, makes the supernatant obtained after sedimentation
It enters to and carries out separating-purifying in separation system.The solid-phase outlet of subsider 42 is connect by pipeline with reaction kettle 10, will be settled
Catalyst afterwards, which is back in reaction kettle 10, continues to participate in catalysis reaction.Catalyst is taken out by circulating pump 50 from 42 bottom of subsider
It is back in reaction kettle 10 out.
System for separating and purifying includes benzene knockout tower 21, benzene rectifying column 22, hexamethylene knockout tower 23 and cyclohexene rectifying column 24.
The entrance of benzene knockout tower 21 respectively with the liquid-phase outlet of subsider 42 and add extractant device 44 connect.Conveying is heavy
The pipeline of drop 42 supernatant of slot is connected to the lower section of benzene knockout tower 21.The pipeline of conveying extractant is connected to the upper of benzene knockout tower 21
Section.The tower bottom of benzene knockout tower 21 exports and the tower top outlet tower bottom with the entrance of benzene rectifying column 22 and hexamethylene knockout tower 23 respectively
Entrance connection.The mixed liquor of the hexamethylene and cyclohexene that distillate at the top of benzene knockout tower 21 is pumped to hexamethylene by circulating pump 50
The lower section of knockout tower 23, further separating-purifying.The mixed liquor warp of the benzene and extractant that go out from 21 bottom column stilling of benzene knockout tower
The first reboiler 32, the second heat exchanger 33 and the First Heat Exchanger 31 of heat recovery system are delivered in benzene rectifying column 22 after exchanging heat,
Further separating-purifying.Benzene rectifying column 22 tower top outlet and tower bottom outlet respectively with add benzene device and plus extractant device 44 company
It connects.The benzene distillated at the top of stupid rectifying column, to adding in benzene device, is recycled by pipeline.It is evaporated from 22 bottom of benzene rectifying column
Through pipeline into the first reboiler 32, the part of vaporization is back in benzene rectifying column 22 separation again and mentions extractant out
Pure, unboiled part is back to by pipeline to be added in extractant device 44.The tower bottom of hexamethylene knockout tower 23 exports and hexamethylene
Alkene rectifying column 24 connects.The tower bottom outlet of cyclohexene rectifying column 24 is connect with extractant device 44 is added.
Heat recovery system includes First Heat Exchanger 31, the second heat exchanger 33, third heat exchanger 34, the first reboiler 32 and
Two reboilers 35.First Heat Exchanger 31 is connect with the entrance for the outlet and reaction kettle 10 for adding benzene device respectively, is come from for preheating
Described plus benzene device benzene feedstock.First Heat Exchanger 31 is also connect with the entrance of the second heat exchanger 33 and benzene rectifying column 22 respectively,
For carrying out heat exchange, pre- pyrogen in the raw material in First Heat Exchanger 31 after boiling the tower reactor mixed liquor heating of benzene knockout tower 21 again
Expect benzene.First reboiler 32 is connect with the outlet of the tower bottom of benzene knockout tower 21 and the second heat exchanger 33 respectively, and the first reboiler
32 export with the tower bottom of benzene rectifying column 22 and connect, for by the benzene from the benzene knockout tower 21 and extractant and the stupid rectifying
After the tower reactor mixed liquor of tower exchanges heat in first reboiler 32, through second heat exchanger 33 and the First Heat Exchanger 31
It is back to after heat exchange in the benzene rectifying column 22.Second heat exchanger 33, third heat exchanger 34 and the second reboiler 35 are sequentially connected in series
In the tower bottom outlet of hexamethylene knockout tower 23, for the tower reactor mixed liquor of the hexamethylene knockout tower 23 to be changed through described second
Enter second reboiler 35 after hot device 33 and the third heat exchanger 34 heat exchange, under the action of low-pressure steam, a part
The tower reactor mixed liquor of vaporization is back to the hexamethylene knockout tower 23, and the unboiled tower reactor mixed liquor of another part enters to described
Cyclohexene rectifying column 24.Third heat exchanger 34 exports with the tower bottom of cyclohexene rectifying column 24 respectively and adds entering for extractant device 44
Mouth connection, for the extractant of cyclohexene rectifying column 24 distillated to be back to described plus extractant device 44 after exchanging heat.The
The outlet of two reboilers 35 is connect with hexamethylene knockout tower 23 and cyclohexene rectifying column 24 respectively, for coming from hexamethylene knockout tower
After 23 tower reactor mixed liquor heat exchange, a part vaporization is back in hexamethylene knockout tower 23, and another part is unboiled to enter to ring
In hexene rectifying column 24.
Cyclohexene production energy-saving system further includes extractant holding vessel 43, and the entrance of extractant holding vessel 43 is respectively with first
Reboiler 32 and third heat exchanger 34 connect, and the outlet of extractant holding vessel 43 is connect with the entrance of extractant device 44 is added.
Embodiment 2
The production method of the cyclohexene of the present embodiment includes:
First by the Ru-Zn catalyst handled well according to the mass ratio of benzene feedstock and catalyst be 10:1 ratio be added to
In reaction kettle 10, with the air in nitrogen replacement reaction kettle 10, continuous 3 times.Additional refining benzene with come from 22 tower top of benzene rectifying column
Recycle benzene mixing after enter benzene storage tank, mixed raw material entered in First Heat Exchanger 31 by benzene delivery pump, the benzene after heat exchange
Pass through pipeline to reaction kettle 10.Hydrogen by booster pump 60 by pipeline to reaction kettle 10, during this, use hydrogen
Nitrogen in replacement reaction kettle 10, continuous 3 times.Being passed through hydrogen again after displacement reaches the Hydrogen Vapor Pressure in reaction kettle 10
Then reaction kettle 10 is heated to 140 DEG C by 4.0MPa, stir 10min at this temperature, in reaction process, is continually fed into hydrogen,
Keep constant 10 internal pressure power of reaction kettle.After completion of the reaction time, hydrogen valve is closed, stops stirring, stop heating.
Solution after reaction passes through pipeline to gravitation settler 42 by the overflow weir built in reaction kettle 10, and solid phase is urged
Catalyst is recycled to reaction kettle 10 by pipeline after separation, by circulating pump 50 by agent.Supernatant after separation is through gravity
Overflow weir in subsider 42 enters lower region in benzene knockout tower 21.
After additional extractant is mixed with the cycling extraction agent for carrying out self-circulating pump 50, through extractant storage tank, extractant conveying
Pump is delivered to the middle and upper part point of benzene knockout tower 21, controls the bottom temperature of benzene knockout tower 21 for 120 DEG C, 80 DEG C of tower top temperature, entirely
Tower pressure drop temperature 0.01MPa, tower top molar reflux ratio >=1.5.The benzene distillated from tower reactor enters first with extractant mixed liquor and boils again
After 32 tube side of device, with the heat exchange of the feed liquid of 22 tower reactor of benzene rectifying column, 33 tube side of the second heat exchanger is entered by pipeline, finally by the
After the heat exchange of one heat exchanger 31, through pipeline into benzene rectifying column 22.21 tower top of benzene knockout tower distillates cyclohexene and hexamethylene
Mixed liquor, the middle and lower part of hexamethylene knockout tower 23 is delivered to through circulating pump 50, and extractant is delivered to hexamethylene point through circulating pump 50
Middle and upper part from tower 23.
The bottom temperature for controlling benzene rectifying column 22 is 75 DEG C, and tower top temperature is 42 DEG C, full tower vacuum degree >=0.03MPa, is returned
Flow ratio >=0.8.22 tower reactor solution of benzene rectifying column enters 32 shell side of the first reboiler at this time, returns to benzin after part solution vaporization and evaporates
Tower 22, unboiled part is by pipeline into extractant holding vessel 43.22 overhead distillate of benzene rectifying column is benzene, is passed through
Pipeline is into benzene storage tank.
The bottom temperature for controlling hexamethylene knockout tower 23 is 90 DEG C, and tower top temperature is 85 DEG C, full tower pressure drop 0.01MPa, tower
Push up reflux ratio >=3.0.23 tower top of hexamethylene knockout tower distillates high-purity hexamethylene, and mass fraction > 99.5% passes through pipeline
System out.After the tower reactor mixed liquor of hexamethylene knockout tower 23 is introduced into the heat exchange of 33 shell side of the second heat exchanger, through third heat exchanger 34
After tube side and the heat exchange of 24 tower reactor distillate of cyclohexene rectifying column, into 35 shell side of the second reboiler, tube side is passed through low-pressure steam, makes
It is back in hexamethylene knockout tower 23 after the vaporization of distillate part, unboiled solution enters cyclohexene rectifying column 24 through pipeline.
The bottom temperature for controlling cyclohexene rectifying column 24 is 130 DEG C, and tower top temperature is 42 DEG C, full tower vacuum degree >=
0.03MPa, tower top molar reflux ratio >=0.8.At this point, 24 overhead distillate of cyclohexene rectifying column is high-purity cyclohexene, quality
Score >=98.0% goes out system by pipeline.24 tower reactor distillate of cyclohexene rectifying column is extractant, through third heat exchanger
After 34 heat exchange, into extractant holding vessel 43.The cycling extraction agent of benzene rectifying column 22 and 24 tower reactor of cyclohexene rectifying column, which passes through, to follow
Ring pump 50 is delivered to add and be recycled in extractant device 44.
Embodiment 3
The production method of the cyclohexene of the present embodiment includes:
First by the Ru-Zn catalyst handled well according to the mass ratio of benzene feedstock and catalyst be 30:1 ratio be added to
In reaction kettle 10, with the air in nitrogen replacement reaction kettle 10, continuous 5 times.Additional refining benzene with come from 22 tower top of benzene rectifying column
Recycle benzene mixing after enter benzene storage tank, mixed raw material entered in First Heat Exchanger 31 by benzene delivery pump, the benzene after heat exchange
Pass through pipeline to reaction kettle 10.Hydrogen by booster pump 60 by pipeline to reaction kettle 10, during this, use hydrogen
Nitrogen in replacement reaction kettle 10, continuous 5 times.Being passed through hydrogen again after displacement reaches the Hydrogen Vapor Pressure in reaction kettle 10
Then reaction kettle 10 is heated to 180 DEG C by 7.0MPa, stir 50min at this temperature, in reaction process, is continually fed into hydrogen,
Keep constant 10 internal pressure power of reaction kettle.After completion of the reaction time, hydrogen valve is closed, stops stirring, stop heating.
Solution after reaction passes through pipeline to gravitation settler 42 by the overflow weir built in reaction kettle 10, and solid phase is urged
Catalyst is recycled to reaction kettle 10 by pipeline after separation, by circulating pump 50 by agent.Supernatant after separation is through gravity
Overflow weir in subsider 42 enters lower region in benzene knockout tower 21.
After additional extractant is mixed with the cycling extraction agent for carrying out self-circulating pump 50, through extractant storage tank, extractant conveying
Pump is delivered to the middle and upper part point of benzene knockout tower 21, controls the bottom temperature of benzene knockout tower 21 for 140 DEG C, 100 DEG C of tower top temperature, entirely
Tower pressure drop temperature 0.04MPa, tower top molar reflux ratio >=1.5.The benzene distillated from tower reactor enters first with extractant mixed liquor and boils again
After 32 tube side of device, with the heat exchange of the feed liquid of 22 tower reactor of benzene rectifying column, 33 tube side of the second heat exchanger is entered by pipeline, finally by the
After the heat exchange of one heat exchanger 31, through pipeline into benzene rectifying column 22.21 tower top of benzene knockout tower distillates cyclohexene and hexamethylene
Mixed liquor, the middle and lower part of hexamethylene knockout tower 23 is delivered to through circulating pump 50, and extractant is delivered to hexamethylene point through circulating pump 50
Middle and upper part from tower 23.
The bottom temperature for controlling benzene rectifying column 22 is 85 DEG C, and tower top temperature is 48 DEG C, full tower vacuum degree >=0.03MPa, is returned
Flow ratio >=0.8.22 tower reactor solution of benzene rectifying column enters 32 shell side of the first reboiler at this time, returns to benzin after part solution vaporization and evaporates
Tower 22, unboiled part is by pipeline into extractant holding vessel 43.22 overhead distillate of benzene rectifying column is benzene, is passed through
Pipeline is into benzene storage tank.
The bottom temperature for controlling hexamethylene knockout tower 23 is 110 DEG C, and tower top temperature is 95 DEG C, full tower pressure drop 0.04MPa, tower
Push up reflux ratio >=3.0.23 tower top of hexamethylene knockout tower distillates high-purity hexamethylene, and mass fraction > 99.5% passes through pipeline
System out.After the tower reactor mixed liquor of hexamethylene knockout tower 23 is introduced into the heat exchange of 33 shell side of the second heat exchanger, through third heat exchanger 34
After tube side and the heat exchange of 24 tower reactor distillate of cyclohexene rectifying column, into 35 shell side of the second reboiler, tube side is passed through low-pressure steam, makes
It is back in hexamethylene knockout tower 23 after the vaporization of distillate part, unboiled solution enters cyclohexene rectifying column 24 through pipeline.
The bottom temperature for controlling cyclohexene rectifying column 24 is 150 DEG C, and tower top temperature is 50 DEG C, full tower vacuum degree >=
0.03MPa, tower top molar reflux ratio >=0.8.At this point, 24 overhead distillate of cyclohexene rectifying column is high-purity cyclohexene, quality
Score >=98.0% goes out system by pipeline.24 tower reactor distillate of cyclohexene rectifying column is extractant, through third heat exchanger
After 34 heat exchange, into extractant holding vessel 43.The cycling extraction agent of benzene rectifying column 22 and 24 tower reactor of cyclohexene rectifying column, which passes through, to follow
Ring pump 50 is delivered to add and be recycled in extractant device 44.
Embodiment 4
The production method of the cyclohexene of the present embodiment includes:
First by the Ru-Zn catalyst handled well according to the mass ratio of benzene feedstock and catalyst be 20:1 ratio be added to
In reaction kettle 10, with the air in nitrogen replacement reaction kettle 10, continuous 4 times.Additional refining benzene with come from 22 tower top of benzene rectifying column
Recycle benzene mixing after enter benzene storage tank, mixed raw material entered in First Heat Exchanger 31 by benzene delivery pump, the benzene after heat exchange
Pass through pipeline to reaction kettle 10.Hydrogen by booster pump 60 by pipeline to reaction kettle 10, during this, use hydrogen
Nitrogen in replacement reaction kettle 10, it is 3-5 times continuous.Being passed through hydrogen again after displacement reaches the Hydrogen Vapor Pressure in reaction kettle 10
Then reaction kettle 10 is heated to 150 DEG C by 5MPa, stir 30min at this temperature, in reaction process, is continually fed into hydrogen, is made
10 internal pressure power of reaction kettle is kept constant.After completion of the reaction time, hydrogen valve is closed, stops stirring, stop heating.
Solution after reaction passes through pipeline to gravitation settler 42 by the overflow weir built in reaction kettle 10, and solid phase is urged
Catalyst is recycled to reaction kettle 10 by pipeline after separation, by circulating pump 50 by agent.Supernatant after separation is through gravity
Overflow weir in subsider 42 enters lower region in benzene knockout tower 21.
After additional extractant is mixed with the cycling extraction agent for carrying out self-circulating pump 50, through extractant storage tank, extractant conveying
Pump is delivered to the middle and upper part point of benzene knockout tower 21, controls the bottom temperature of benzene knockout tower 21 for 130 DEG C, 90 DEG C of tower top temperature, entirely
Tower pressure drop temperature 0.02MPa, tower top molar reflux ratio >=1.5.The benzene distillated from tower reactor enters first with extractant mixed liquor and boils again
After 32 tube side of device, with the heat exchange of the feed liquid of 22 tower reactor of benzene rectifying column, 33 tube side of the second heat exchanger is entered by pipeline, finally by the
After the heat exchange of one heat exchanger 31, through pipeline into benzene rectifying column 22.21 tower top of benzene knockout tower distillates cyclohexene and hexamethylene
Mixed liquor, the middle and lower part of hexamethylene knockout tower 23 is delivered to through circulating pump 50, and extractant is delivered to hexamethylene point through circulating pump 50
Middle and upper part from tower 23.
The bottom temperature for controlling benzene rectifying column 22 is 80 DEG C, and tower top temperature is 45 DEG C, full tower vacuum degree >=0.03MPa, is returned
Flow ratio >=0.8.22 tower reactor solution of benzene rectifying column enters 32 shell side of the first reboiler at this time, returns to benzin after part solution vaporization and evaporates
Tower 22, unboiled part is by pipeline into extractant holding vessel 43.22 overhead distillate of benzene rectifying column is benzene, is passed through
Pipeline is into benzene storage tank.
The bottom temperature for controlling hexamethylene knockout tower 23 is 100 DEG C, and tower top temperature is 90 DEG C, full tower pressure drop 0.02MPa, tower
Push up reflux ratio >=3.0.23 tower top of hexamethylene knockout tower distillates high-purity hexamethylene, and mass fraction > 99.5% passes through pipeline
System out.After the tower reactor mixed liquor of hexamethylene knockout tower 23 is introduced into the heat exchange of 33 shell side of the second heat exchanger, through third heat exchanger 34
After tube side and the heat exchange of 24 tower reactor distillate of cyclohexene rectifying column, into 35 shell side of the second reboiler, tube side is passed through low-pressure steam, makes
It is back in hexamethylene knockout tower 23 after the vaporization of distillate part, unboiled solution enters 140 DEG C through pipeline, and tower top temperature is
45 DEG C, full tower vacuum degree >=0.03MPa, tower top molar reflux ratio >=0.8.At this point, 24 overhead distillate of cyclohexene rectifying column is
High-purity cyclohexene, mass fraction >=98.0% go out system by pipeline.24 tower reactor distillate of cyclohexene rectifying column is extraction
Agent is taken, after the heat exchange of third heat exchanger 34, into extractant holding vessel 43.Benzene rectifying column 22 and 24 tower reactor of cyclohexene rectifying column
Cycling extraction agent is delivered to add in extractant device 44 by circulating pump 50 and is recycled.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of cyclohexene production energy-saving system characterized by comprising feed system, reaction system, system for separating and purifying and
Heat recovery system；Wherein:
The feed system include connect respectively with the reaction system plus benzene device, hydrogenation plant and nitrogen purging device with
And what is connect with the system for separating and purifying adds extractant device (44)；
The reaction system include the reaction kettle (10) being connect with described plus benzene device, hydrogenation plant and nitrogen purging device and
The subsider (42) connecting with the reaction kettle (10), the liquid-phase outlet and the system for separating and purifying of the subsider (42) connect
It connects；
The system for separating and purifying includes benzene knockout tower (21), benzene rectifying column (22), hexamethylene knockout tower (23) and cyclohexene essence
Evaporate tower (24)；The entrance of the benzene knockout tower (21) respectively with the liquid-phase outlet of the subsider (42) and described plus extractant
Device (44) connection, the tower bottom outlet of the benzene knockout tower (21) and the tower top outlet entrance with the benzene rectifying column (22) respectively
It is connected with the tower bottom entrance of the hexamethylene knockout tower (23)；The tower top outlet and tower bottom of the benzene rectifying column (22) export difference
It is connect with described plus benzene device and described plus extractant device (44)；The hexamethylene knockout tower (23) tower bottom outlet with it is described
Cyclohexene rectifying column (24) connection；Tower bottom outlet and described plus extractant device (44) of the cyclohexene rectifying column (24) connect
It connects；
The heat recovery system includes First Heat Exchanger (31), the second heat exchanger (33), third heat exchanger (34), the first reboiler
(32) and the second reboiler (35)；The First Heat Exchanger (31) respectively with the outlet of described plus benzene device and the reaction kettle
(10) entrance connection, the First Heat Exchanger (31) also respectively with second heat exchanger (33) and the benzene rectifying column (22)
Entrance connection；First reboiler (32) exports respectively with the tower bottom of the benzene knockout tower (21) and second heat exchanger
(33) it connects, and the tower bottom of first reboiler (32) and the benzene rectifying column (22) is exported and connected；Second heat exchange
Device (33), the third heat exchanger (34) and second reboiler (35) are sequentially connected in series in the hexamethylene knockout tower (23)
In tower bottom outlet；The third heat exchanger (34) exports respectively with the tower bottom of the cyclohexene rectifying column (24) and described plus extraction
The entrance of agent device (44) connects；The outlet of second reboiler (35) respectively with the hexamethylene knockout tower (23) and described
Cyclohexene rectifying column (24) connection.
2. cyclohexene production energy-saving system according to claim 1, which is characterized in that the solid phase of the subsider (42) goes out
Mouth is connect by pipeline with the reaction kettle (10).
3. cyclohexene production energy-saving system according to claim 1, which is characterized in that the cyclohexene production energy-saving system
Further include extractant holding vessel (43), the entrance of the extractant holding vessel (43) respectively with first reboiler (32) and institute
Third heat exchanger (34) connection is stated, the outlet of the extractant holding vessel (43) and described plus extractant device (44) entrances connect
It connects.
4. cyclohexene production energy-saving system according to claim 1-3, which is characterized in that described plus benzene device packet
The refining benzene pipeline and recycle benzene pipeline for including benzene holding vessel (41) and being connect respectively with the entrance of the benzene holding vessel (41), it is described
Recycle benzene pipeline is connect with the tower top outlet of the benzene rectifying column (22).
5. cyclohexene production energy-saving system according to claim 4, which is characterized in that the hydrogenation plant includes that hydrogen is defeated
Enter pipeline and hydrogen circulating line, the hydrogen inlet manifold road and hydrogen circulating line pass through booster pump (60) and the reaction kettle
(10) entrance connection, the hydrogen circulating line are connect with the hydrogen outlet of the reaction kettle (10).
6. a kind of method using the described in any item cyclohexene production energy-saving system production cyclohexene of claim 1-5, special
Sign is, comprising:
(1) reaction in reaction kettle (10) by raw material benzene hydrogenation and catalyst, the mixed liquor after reaction are settled through subsider (42)；
(2) obtained supernatant will be delivered to separating-purifying in benzene knockout tower (21) after sedimentation, will be obtained through benzene knockout tower (21)
To overhead distillate send into hexamethylene knockout tower (23), the tower reactor mixed liquor obtained through benzene knockout tower (21) is delivered to
In one reboiler (32) and after the heat exchange of the tower reactor feed liquid of benzene rectifying column (22), changed by pipeline through the second heat exchanger (33) and first
It is entered in benzene rectifying column (22) after hot device (31) heat exchange；Wherein, the tower reactor mixed liquor of benzene knockout tower (21) enters the first heat exchange
For the heat of device (31) for preheating to benzene feedstock, the tower reactor mixed liquor of benzene knockout tower (21) includes benzene and extractant, benzene point
Overhead distillate from tower (21) includes hexamethylene and cyclohexene；
(3) benzene obtained after benzene rectifying column (22) separating-purifying is exported from tower top, and is back to and is added in benzene device by pipeline,
The tower reactor feed liquid of benzene rectifying column (22) exports after the first reboiler (32) heat exchange from tower bottom, and the part of vaporization is returned by pipeline
Into benzene rectifying column (22), unboiled part is back to by pipeline plus extractant device (44)；Wherein, benzene rectifying column (22)
Tower reactor feed liquid include benzene and extractant；
(4) from benzene knockout tower (21) overhead distillate through hexamethylene knockout tower (23) separating-purifying, obtained hexamethylene from
Tower top output, while the tower reactor mixed liquor of hexamethylene knockout tower (23) being delivered in second heat exchanger (33) and coming from benzene
After the tower reactor mixed liquor heat of knockout tower (21), into third heat exchanger (34) again with the tower reactor material that comes from cyclohexene rectifying column (24)
Liquid exchanges heat, and enters back into the second reboiler (35), and the part vaporized in the second reboiler (35) is back to hexamethylene by pipeline
In alkane knockout tower (23), unboiled part is entered in cyclohexene rectifying column (24)；
(5) after cyclohexene rectifying column (24) separating-purifying, obtained cyclohexene is defeated from tower top for part unboiled in step (4)
Out, remaining extractant, which exports to be back to by pipeline after third heat exchanger (34) heat exchange from tower bottom, adds extractant device (44).
7. according to the method described in claim 6, it is characterized in that, the reaction condition in reaction kettle (10) includes: in hydrogen pressure
Power is 4-7MPa, reaction temperature reacts 10-50min at being 140-180 DEG C, is continually fed into hydrogen during the reaction and keeps
Pressure is constant, and the mass ratio of benzene feedstock and catalyst is (10-30): 1.
8. according to the method described in claim 6, it is characterized in that, the reaction condition of benzene knockout tower (21) includes: bottom temperature
It is 120-140 DEG C, tower top temperature is 80-100 DEG C, full tower pressure drop 0.01-0.04MPa, tower top molar reflux ratio >=1.5；Benzin
It is 75-85 DEG C that the reaction condition for evaporating tower (22), which includes: bottom temperature, and tower top temperature is 42-48 DEG C, full tower vacuum degree >=
0.03MPa, reflux ratio >=0.8.
9. according to the method described in claim 6, it is characterized in that, the reaction condition of hexamethylene knockout tower (23) includes: tower reactor
Temperature is 90-110 DEG C, and tower top temperature is 85-95 DEG C, full tower pressure drop 0.01-0.04MPa, overhead reflux ratio >=3.0；Cyclohexene
The reaction condition of rectifying column (24) includes: that bottom temperature is 130-150 DEG C, and tower top temperature is 42-50 DEG C, and full tower vacuum degree >=
0.03MPa, tower top molar reflux ratio >=0.8.
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