CN117085605A - Hydroisomerization reaction device and method for preparing hanging tetrahydrodicyclopentadiene - Google Patents

Hydroisomerization reaction device and method for preparing hanging tetrahydrodicyclopentadiene Download PDF

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CN117085605A
CN117085605A CN202210515392.XA CN202210515392A CN117085605A CN 117085605 A CN117085605 A CN 117085605A CN 202210515392 A CN202210515392 A CN 202210515392A CN 117085605 A CN117085605 A CN 117085605A
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inlet
liquid phase
gas phase
reaction
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丁辉
黄声骏
张大治
邹明明
焦雨桐
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • 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
    • C07C5/13—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation with simultaneous isomerisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00004—Scale aspects
    • B01J2219/00006—Large-scale industrial plants

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The application discloses a hydroisomerization reaction device and a method for preparing hanging tetrahydrodicyclopentadiene, wherein the hydroisomerization reaction device is a circulating reaction device and comprises a reaction unit and a separation unit which are connected in sequence; the reaction unit comprises a reactor; the separation unit comprises a gas phase separation device, a rectifying tower I, a rectifying tower II and a crystallization device which are connected in sequence. The process flow adopts the cyclic operation of raw material preheating, reaction, gas phase separation, fractional condensation rectification, full condensation rectification, crystallization separation and multistage compression recovery, and the method can be used for producing the hanging type tetrahydrodicyclopentadiene, has continuous process and simple flow, saves material consumption and energy consumption of the process through hydrogen multistage compression and mother liquor circulation, and is suitable for industrialized large-scale continuous operation.

Description

Hydroisomerization reaction device and method for preparing hanging tetrahydrodicyclopentadiene
Technical Field
The application relates to a hydroisomerization reaction device and a method for preparing hanging tetrahydrodicyclopentadiene, and belongs to the technical field of chemical industry.
Background
The hanging tetrahydrodicyclopentadiene is a high-energy density fuel with excellent performance, has higher volume heat value, can provide more pushing energy under the same volume, obviously improves the range and speed of an aircraft, can obviously reduce the volume of a fuel tank while guaranteeing the flight performance, is widely applied to the aerospace field, and is one of the basic guarantee fuels of a novel ultra-high-speed aircraft.
Chinese patent CN110923023 discloses a high-density fuel laboratory synthesis method, chinese patent CN109651045 discloses a refining method for obtaining tetrahydrodicyclopentadiene by crystallization, washing and extraction. Chinese patent CN111217663 discloses a process for preparing tetrahydrodicyclopentadiene. Chinese patent CN111662148 discloses a process for preparing bridge tetrahydrodicyclopentadiene.
In the prior art, the research on the continuous synthesis method of the hanging tetrahydrodicyclopentadiene is basically limited to a conceptual stage, and a detailed continuous full-flow design is not seen.
Disclosure of Invention
The application provides a synthesis method of multi-carbon-number hydrocarbon, which is a production process of hanging-type tetrahydrodicyclopentadiene, wherein the method generates the hanging-type tetrahydrodicyclopentadiene through the hydroisomerization of bridge-type tetrahydrodicyclopentadiene, and the qualified product is obtained through separation, and the process flow adopts the cyclic operation of raw material preheating, reaction, gas phase separation, fractional condensation rectification, full condensation rectification, crystallization separation and multistage compression recovery, and the process is continuous, the flow is simple, and the material consumption and the energy consumption of the process are saved through the multistage compression of hydrogen and the cyclic use of mother liquor, thereby being suitable for industrial large-scale continuous operation.
In one aspect, the application provides a hydroisomerization reaction device, which is a circulating reaction device and comprises a reaction unit and a separation unit which are sequentially connected;
the reaction unit comprises a reactor, wherein the reactor comprises a raw material inlet I, a raw material inlet II and an outlet I;
the separation unit comprises a gas phase separation device, a rectifying tower I, a rectifying tower II and a crystallization device which are connected in sequence;
the gas phase separation device is provided with an inlet I, a gas phase outlet I and a liquid phase outlet I, and the inlet I and the outlet I are connected through a pipeline;
the rectifying tower I is provided with a liquid phase inlet I-1, a liquid phase inlet I-2, a gas phase outlet II and a liquid phase outlet II, and the top of the rectifying tower I is provided with a product outlet; the liquid phase inlet I-1 is connected with the liquid phase outlet I through a pipeline;
the rectifying tower II is provided with a liquid phase inlet II, an outlet III is arranged at the top, and an outlet II is arranged at the bottom; the liquid phase inlet II is connected with the liquid phase outlet II through a pipeline;
the top of the crystallization device is provided with an inlet II and a liquid phase outlet IV, and the bottom of the crystallization device is provided with a crystallization outlet; the inlet II is connected with the outlet III through a pipeline, and the liquid phase outlet IV is connected with the liquid phase inlet I-2 through a pipeline;
the outlet II is connected with the raw material inlet I through a pipeline;
the gas phase outlet I and the gas phase outlet II are respectively connected with the raw material inlet II through pipelines.
Optionally, a preheater I is further arranged on the connecting pipeline of the outlet II and the raw material inlet I;
the connecting pipelines of the gas phase outlet I and the raw material inlet II are also provided with a preheater II;
and a preheater II is also arranged on the connecting pipeline of the gas phase outlet II and the raw material inlet II.
Optionally, the connecting pipelines of the gas phase outlet I and the raw material inlet II are also provided with a supercharging device I;
the connecting pipelines of the gas phase outlet II and the raw material inlet II are also provided with a supercharging device II;
and the connecting pipelines of the outlet II and the raw material inlet I are also provided with a supercharging device III.
Optionally, the separation unit further comprises condensing means;
the outlet I, the condensing device and the inlet I are connected through pipelines in sequence.
Optionally, the reflux ratio of the rectifying tower I is 1-100;
optionally, the reflux ratio of the rectifying tower I is independently selected from any value of 1, 20, 40, 60, 80 and 100 or any value between any two points.
Optionally, the theoretical plates of the rectifying tower I are 10-80;
optionally, the theoretical plate number of the rectifying tower I is independently selected from any value of 10, 30, 50 and 80 or any value between any two points.
Optionally, the reflux ratio of the rectifying tower II is 1-150;
optionally, the reflux ratio of the rectifying tower II is independently selected from any value of 1, 30, 60, 95, 120 and 150 or any value between any two points;
optionally, the theoretical plates of the rectifying tower II are 10-80;
optionally, the theoretical plate number of the rectifying tower II is independently selected from any value of 10, 30, 50 and 80 or any value between any two points.
In another aspect of the present application, there is provided a method for preparing a pendant-type tetrahydrodicyclopentadiene, comprising: introducing a raw material containing bridge-type tetrahydrodicyclopentadiene and hydrogen into a reaction device containing a catalyst to perform hydroisomerization reaction to obtain a product containing the pendent tetrahydrodicyclopentadiene and adamantane; wherein the reaction device is selected from the hydroisomerization reaction device.
Optionally, the method comprises the following steps:
(1) Introducing a raw material containing bridge-type tetrahydrodicyclopentadiene and hydrogen into a reactor containing a catalyst to carry out hydroisomerization reaction to obtain a hydroisomerization reaction product;
(2) The hydroisomerization reaction product is introduced into a gas phase separation device through an inlet I to realize separation of a gas phase I and a liquid phase I, wherein the gas phase I comprises unreacted hydrogen, and is introduced into a reactor through a gas phase outlet I and a raw material inlet II to perform hydroisomerization reaction with bridge tetrahydrodicyclopentadiene;
(3) The liquid phase I is introduced into the rectifying tower I through a liquid phase outlet I and a liquid phase inlet I-1, and is rectified and separated to obtain a gas phase II, a product containing hanging tetrahydrodicyclopentadiene and a liquid phase II;
wherein the gas phase II comprises unreacted hydrogen, and the unreacted hydrogen is introduced into the reactor through a gas phase outlet II and a raw material inlet II to carry out hydroisomerization reaction with bridge-type tetrahydrodicyclopentadiene;
the product containing the hanging tetrahydrodicyclopentadiene is discharged from a product outlet;
(4) The liquid phase I I is introduced into the rectifying tower II through a liquid phase outlet II and a liquid phase inlet II, and is rectified and separated to obtain an alkane mixture and a liquid phase III, wherein the liquid phase III comprises unreacted bridge-type tetrahydrodicyclopentadiene, and is introduced into a reactor through an outlet II and a raw material inlet I to undergo hydroisomerization reaction with hydrogen;
(5) Introducing the alkane mixture into a crystallization device through an outlet III and an inlet II to obtain adamantane and crystallization mother liquor; the adamantane is discharged from the crystallization outlet; the crystallization mother liquor is provided with a liquid phase outlet IV and a liquid phase inlet I-2, and is fed into a rectifying tower I for rectifying and separating.
Optionally, in the hydroisomerization reaction, the molar ratio of bridge tetrahydrodicyclopentadiene to hydrogen is 1:2 to 10;
optionally, the molar ratio of the bridge tetrahydrodicyclopentadiene to the hydrogen is independently selected from any value of 1:2, 1:4, 1:6, 1:8, 1:10 or any value between any two points;
optionally, the reaction temperature of the hydroisomerization reaction is 80-200 ℃, and the reaction pressure is 1.5-5.0 MPaG;
optionally, the reaction temperature of the hydroisomerization reaction is independently selected from any value of 80 ℃, 100 ℃, 130 ℃, 150 ℃, 180 ℃ and 200 ℃ or any value between any two points;
optionally, the reaction pressure is independently selected from any value of 1.5MPaG, 1.8MPaG, 2MPaG, 2.3MPaG, 3MPaG, 3.5MPaG, 4MPaG, 4.5MPaG, 5MPaG or any value between any two points of the above;
optionally, the temperature of the gas phase separation device is 0-100 ℃; the separation pressure is 0.1-15 MPa;
optionally, the temperature of the gas phase separation device is independently selected from any value of 0 ℃, 20 ℃, 40 ℃, 60 ℃, 72 ℃, 80 ℃ and 100 ℃ or any value between any two points;
optionally, the separation pressure is independently selected from any value of 0.1MPa, 2.2MPa, 4MPa, 6MPa, 8MPa, 10MPa, 12MPa and 15MPa or any value between any two points;
optionally, the temperature of the top of the rectifying tower I is 0-80 ℃; the pressure at the top of the tower is 1-400 kPa;
optionally, the top temperature of the rectifying tower I is independently selected from any value of 0 ℃, 20 ℃, 42 ℃, 60 ℃ and 80 ℃ or any value between any two points;
optionally, the top pressure of the rectifying tower I is independently selected from any value of 1kPa, 8kPa, 50kPa, 100kPa, 150kPa, 200kPa, 250kPa, 300kPa, 350kPa and 400kPa or any value between any two points;
optionally, the temperature of the top of the rectifying tower II is 150-300 ℃; the pressure at the top of the tower is 1-400 kPa.
Optionally, the top temperature of the rectifying tower II is independently selected from any value of 150 ℃, 189 ℃, 210 ℃, 240 ℃, 270 ℃ and 300 ℃ or any value between any two points;
optionally, the top pressure of the rectifying tower II is independently selected from any value of 1kPa, 5kPa, 50kPa, 100kPa, 150kPa, 200kPa, 250kPa, 300kPa, 350kPa and 400kPa or any value between any two points;
optionally, the bridge tetrahydrodicyclopentadiene is heated by a preheater I and then enters the reactor through a source flow inlet I;
after being heated by the preheater II, the hydrogen enters the reactor through the raw material inlet II;
optionally, in step (2), the gas phase I enters the reactor via a gas phase outlet I, a pressurizing device I, a preheater II, a feedstock inlet II;
optionally, in step (3), the gas phase II enters the reactor via a gas phase outlet II, a pressurizing device II, a preheater II, a feedstock inlet II;
optionally, in the step (2), the hydroisomerization reaction product enters the gas phase separation device through the condensing device and the inlet I;
optionally, in step (4), the liquid phase III enters the reactor via outlet II, supercharging device III, preheater I, feed inlet I.
As a specific embodiment, the device comprises the following components: raw material preheater 1 (preheater I), hydrogen preheater 2 (preheater II), reactor 3, condenser 4 (condensing unit), gas-liquid separation tank 5 (gas phase separation unit), 1# hydrogen compressor 6 (pressurizing unit I), product column 7 (rectifying column I), 2# hydrogen compressor 8 (pressurizing unit II), light component removal column 9 (rectifying column II), circulating pump 10 (pressurizing unit III), and crystallization unit 11.
The method for using the device comprises the following steps:
s001, mixing fresh bridge tetrahydrodicyclopentadiene with circulating bridge tetrahydrodicyclopentadiene, and heating to the reaction temperature in a raw material preheater 1;
s002, mixing fresh hydrogen and circulating hydrogen, heating to a reaction temperature in a hydrogen preheater 2, sending the mixture and bridge-type tetrahydrodicyclopentadiene into a reactor 3, and carrying out catalytic reaction to obtain a hydroisomerization reaction product;
s003, condensing a hydroisomerization reaction product in a condenser 4, changing the hydroisomerization reaction product into gas-liquid two phases at low temperature, realizing gas-liquid separation in a gas-liquid separation tank 5, pressurizing the separated unreacted hydrogen by a No. 1 hydrogen compressor 6, and mixing the unreacted hydrogen with fresh hydrogen;
the liquid phase separated by the S004 gas-liquid separation tank 5 is sent to a product tower 7, unreacted hydrogen and hanging type tetrahydrodicyclopentadiene products with the purity reaching the standard are separated from the top of the tower through rectification, the hydrogen is mixed with fresh hydrogen after being pressurized by a No. 2 hydrogen compressor 8, and distillate at the bottom of the product tower 7 is sent to a light component removal tower 9 for rectification separation;
s005 light component removing tower 9 adopts full condensation rectification separation, unreacted bridge type tetrahydrodicyclopentadiene is obtained at the bottom of the tower and is mixed with fresh raw materials after being pressurized by a circulating pump 10, alkane mixture obtained at the top of the tower is sent to a crystallization device 11, adamantane crystals and crystallization mother liquor are obtained through crystallization, adamantane crystals are sent out as byproducts, and the crystallization mother liquor is sent to a product tower 7 to separate tetrahydrodicyclopentadiene mixture.
Wherein, the hydroisomerization reaction product at the outlet of the reactor 3 is cooled and flash-distilled to separate out unreacted hydrogen, and the unreacted hydrogen is pressurized by a No. 1 hydrogen compressor 6 and recycled; the top of the product tower 7 adopts a dephlegmator to separate non-condensable hydrogen, and the non-condensable hydrogen is circularly used after being pressurized by a No. 2 hydrogen compressor 8; the light component removal tower 9 adopts full condensation rectification, unreacted bridge-type tetrahydrodicyclopentadiene separated from the tower bottom is pressurized by the circulating pump 10 and recycled; purifying adamantane by-products by adopting crystallization operation on the mixture separated from the top of the light component removing tower 9; the mother liquor obtained by the crystallization device 11 is sent to a product tower for separation, and the product yield is improved.
The application has the beneficial effects that:
the method can be used for producing the hanging tetrahydrodicyclopentadiene, has continuous process and simple flow, saves process material consumption and energy consumption through hydrogen multistage compression and mother liquor circulation, and is suitable for industrial large-scale continuous operation.
Drawings
FIG. 1 is a schematic view of a hydroisomerization reaction apparatus in an embodiment of the present application.
Wherein:
1. a raw material preheater; 2. a hydrogen preheater; 3. a reactor; 4. a condenser; 5. a gas-liquid separation tank; 6. a 1# hydrogen compressor; 7. a product tower; 8. a 2# hydrogen compressor; 9. a light component removing tower; 10. a circulation pump; 11. and a crystallization device.
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
The starting materials and catalysts in the examples of the present application were purchased commercially, unless otherwise specified.
Example 1
The hydroisomerization reaction device diagram shown in fig. 1 comprises a raw material preheater 1, a hydrogen preheater 2, a reactor 3, a condenser 4, a gas-liquid separation tank 5, a No. 1 hydrogen compressor 6, a product tower 7, a No. 2 hydrogen compressor 8, a light component removal tower 9, a circulating pump 10 and a crystallization device 11.
The reactor 3, the condenser 4 and the gas-liquid separation tank 5 are connected in sequence; the inlet I and the inlet II of the reactor are respectively provided with a raw material preheater 1 and a hydrogen preheater 2, the top outlet of the gas-liquid separation tank 5 is connected with the inlet II of the reactor through a 1# hydrogen compressor 6 and a hydrogen preheater 2, and the bottom outlet of the gas-liquid separation tank 5 is connected with the tower side wall inlet I of the product tower 7 through a pipeline; the outlet of the tower top of the product tower 7 is connected with an inlet II pipeline of the reactor through a No. 2 hydrogen compressor 8 and a hydrogen preheater 2; the bottom outlet of the product tower 7 is connected with a side wall inlet pipeline of the light component removing tower 9; the top outlet of the light component removing tower 9 is connected with the top inlet pipeline of the crystallization device 11; the bottom outlet of the light component removal tower 9 is connected with the inlet I of the reactor through a circulating pump 10 and a raw material preheater 1; the upper end of the crystallization device 11 is also provided with a crystallization mother liquor outlet which is connected with a side wall inlet II pipeline of the product tower 7; the bottom of the crystallization device 11 is provided with a crystallization product outlet; the upper end of the product tower 7 is also provided with a product outlet.
Example 2
By adopting the hydroisomerization reaction device described in example 1, fresh bridge tetrahydrodicyclopentadiene and circulating bridge tetrahydrodicyclopentadiene are mixed and then heated to 130 ℃ in a raw material preheater 1, meanwhile, fresh hydrogen and circulating hydrogen are mixed and then heated to 130 ℃ in a hydrogen preheater 2, and the fresh hydrogen and the bridge tetrahydrodicyclopentadiene are fed into a reactor 3 containing a supported Ni catalyst together (wherein the molar ratio of the bridge tetrahydrodicyclopentadiene to the hydrogen is 1:4), and a hydroisomerization reaction product is obtained through catalytic reaction under the pressure of 2.3 MPaG. Condensing the hydroisomerization reaction product to 72 ℃ in a condenser 4, changing the product into gas-liquid two-phase at low temperature, realizing gas-liquid separation in a gas-liquid separation tank 5 under 2.2MPa, pressurizing the separated unreacted hydrogen by a No. 1 hydrogen compressor 6, mixing with fresh hydrogen, sending the liquid phase separated by the gas-liquid separation tank 5 to a product tower 7, separating the unreacted hydrogen and a hanging tetrahydrodicyclopentadiene product with the purity of 98.8%wt at the top of the tower by rectification, pressurizing the hydrogen by a No. 2 hydrogen compressor 8, mixing with the fresh hydrogen, and sending the distillate at the bottom of the product tower 7 to a light component removal tower 9 for rectification separation. The pressure of the product column 7 is 8kPa, the temperature of the top of the column is 42 ℃, the theoretical plate number is 50, and the reflux ratio is 40. Unreacted bridge tetrahydrodicyclopentadiene is obtained at the bottom of the light component removing tower 9, pressurized by a circulating pump 10 and mixed with fresh raw materials, and alkane mixture is obtained at the top of the tower and sent to a crystallization device 11. The pressure of the light component removal column 9 is 5kPa, the temperature of the top of the column is 189 ℃, the theoretical plate number is 50, and the reflux ratio is 95. The crystallization product of the crystallization device 11 is by-product adamantane crystals and crystallization mother liquor, the adamantane crystals are sent out as by-products, and the crystallization mother liquor is sent to the product tower 7 to separate the tetrahydrodicyclopentadiene mixture.
While the application has been described in terms of preferred embodiments, it will be understood by those skilled in the art that various changes and modifications can be made without departing from the scope of the application, and it is intended that the application is not limited to the specific embodiments disclosed.

Claims (10)

1. A hydroisomerization reaction device is characterized in that,
the reaction device is a circulating reaction device and comprises a reaction unit and a separation unit which are connected in sequence;
the reaction unit comprises a reactor, wherein the reactor comprises a raw material inlet I, a raw material inlet II and an outlet I;
the separation unit comprises a gas phase separation device, a rectifying tower I, a rectifying tower II and a crystallization device which are connected in sequence;
the gas phase separation device is provided with an inlet I, a gas phase outlet I and a liquid phase outlet I, and the inlet I and the outlet I are connected through a pipeline;
the rectifying tower I is provided with a liquid phase inlet I-1, a liquid phase inlet I-2, a gas phase outlet II and a liquid phase outlet II, and the top of the rectifying tower I is provided with a product outlet; the liquid phase inlet I-1 is connected with the liquid phase outlet I through a pipeline;
the rectifying tower II is provided with a liquid phase inlet II, an outlet III is arranged at the top, and an outlet II is arranged at the bottom; the liquid phase inlet II is connected with the liquid phase outlet II through a pipeline;
the top of the crystallization device is provided with an inlet II and a liquid phase outlet IV, and the bottom of the crystallization device is provided with a crystallization outlet; the inlet II is connected with the outlet III through a pipeline, and the liquid phase outlet IV is connected with the liquid phase inlet I-2 through a pipeline;
the outlet II is connected with the raw material inlet I through a pipeline;
the gas phase outlet I and the gas phase outlet II are respectively connected with the raw material inlet II through pipelines.
2. A reaction device according to claim 1, wherein,
the connecting pipelines of the outlet II and the raw material inlet I are also provided with a preheater I;
the connecting pipelines of the gas phase outlet I and the raw material inlet II are also provided with a preheater II;
and a preheater II is also arranged on the connecting pipeline of the gas phase outlet II and the raw material inlet II.
3. A reaction device according to claim 1, wherein,
the connecting pipelines of the gas phase outlet I and the raw material inlet II are also provided with a supercharging device I;
the connecting pipelines of the gas phase outlet II and the raw material inlet II are also provided with a supercharging device II;
and the connecting pipelines of the outlet II and the raw material inlet I are also provided with a supercharging device III.
4. A reaction device according to claim 1, wherein,
the separation unit further comprises condensing means;
the outlet I, the condensing device and the inlet I are connected through pipelines in sequence.
5. A reaction device according to claim 1, wherein,
the reflux ratio of the rectifying tower I is 1-100;
the theoretical plate number of the rectifying tower I is 10-80.
6. A reaction device according to claim 1, wherein,
the reflux ratio of the rectifying tower II is 1-150;
the theoretical plate number of the rectifying tower II is 10-80.
7. A process for preparing a pendant-type tetrahydrodicyclopentadiene, comprising:
introducing a raw material containing bridge-type tetrahydrodicyclopentadiene and hydrogen into a reaction device containing a catalyst to perform hydroisomerization reaction to obtain a product containing the pendent tetrahydrodicyclopentadiene and adamantane;
wherein the reaction device is selected from the hydroisomerization reaction device according to any one of claims 1 to 6.
8. The method according to claim 7, comprising the steps of:
(1) Introducing a raw material containing bridge-type tetrahydrodicyclopentadiene and hydrogen into a reactor containing a catalyst to carry out hydroisomerization reaction to obtain a hydroisomerization reaction product;
(2) The hydroisomerization reaction product is introduced into a gas phase separation device through an inlet I to realize separation of a gas phase I and a liquid phase I, wherein the gas phase I comprises unreacted hydrogen, and is introduced into a reactor through a gas phase outlet I and a raw material inlet II to perform hydroisomerization reaction with bridge tetrahydrodicyclopentadiene;
(3) The liquid phase I is introduced into the rectifying tower I through a liquid phase outlet I and a liquid phase inlet I-1, and is rectified and separated to obtain a gas phase II, a product containing hanging tetrahydrodicyclopentadiene and a liquid phase II;
wherein the gas phase II comprises unreacted hydrogen, and the unreacted hydrogen is introduced into the reactor through a gas phase outlet II and a raw material inlet II to carry out hydroisomerization reaction with bridge-type tetrahydrodicyclopentadiene;
the product containing the hanging tetrahydrodicyclopentadiene is discharged from a product outlet;
(4) The liquid phase II is introduced into the rectifying tower II through a liquid phase outlet II and a liquid phase inlet II, and alkane mixture and liquid phase III are obtained through rectification separation, wherein the liquid phase III comprises unreacted bridge-type tetrahydrodicyclopentadiene, and is introduced into a reactor through an outlet II and a raw material inlet I to carry out hydroisomerization reaction with hydrogen;
(5) Introducing the alkane mixture into a crystallization device through an outlet III and an inlet II to obtain adamantane and crystallization mother liquor; the adamantane is discharged from the crystallization outlet; the crystallization mother liquor is provided with a liquid phase outlet IV and a liquid phase inlet I-2, and is fed into a rectifying tower I for rectifying and separating.
9. The method of claim 8, wherein the step of determining the position of the first electrode is performed,
in the hydroisomerization reaction, the molar ratio of bridge tetrahydrodicyclopentadiene to hydrogen is 1:2 to 10;
preferably, the reaction temperature of the hydroisomerization reaction is 80-200 ℃, and the reaction pressure is 1.5-5.0 MPaG;
preferably, the temperature of the gas phase separation device is 0-100 ℃; the separation pressure is 0.1-15 MPa;
preferably, the temperature of the top of the rectifying tower I is 0-80 ℃; the pressure at the top of the tower is 1-400 kPa;
preferably, the temperature of the top of the rectifying tower II is 150-300 ℃; the pressure at the top of the tower is 1-400 kPa.
10. The method of claim 8, wherein the step of determining the position of the first electrode is performed,
the bridge tetrahydrodicyclopentadiene is heated by a preheater I and then enters the reactor through a source fluid inlet I;
after being heated by the preheater II, the hydrogen enters the reactor through the raw material inlet II;
preferably, in step (2), the gas phase I enters the reactor via a gas phase outlet I, a pressurizing device I, a preheater II, a feed inlet II;
preferably, in step (3), the gas phase II enters the reactor via a gas phase outlet II, a pressurizing device II, a preheater II, a feed inlet II;
preferably, in the step (2), the hydroisomerization reaction product enters the gas phase separation device through the condensing device and the inlet I;
preferably, in step (4), the liquid phase III enters the reactor via outlet II, supercharging device III, preheater I, feed inlet I.
CN202210515392.XA 2022-05-12 2022-05-12 Hydroisomerization reaction device and method for preparing hanging tetrahydrodicyclopentadiene Pending CN117085605A (en)

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