CN116474659B - A loop reactor suitable for gas-liquid-solid three-phase reaction and a gas-liquid-solid three-phase reaction method - Google Patents
A loop reactor suitable for gas-liquid-solid three-phase reaction and a gas-liquid-solid three-phase reaction method Download PDFInfo
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- CN116474659B CN116474659B CN202310643308.7A CN202310643308A CN116474659B CN 116474659 B CN116474659 B CN 116474659B CN 202310643308 A CN202310643308 A CN 202310643308A CN 116474659 B CN116474659 B CN 116474659B
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/005—Separating solid material from the gas/liquid stream
- B01J8/0065—Separating solid material from the gas/liquid stream by impingement against stationary members
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/005—Separating solid material from the gas/liquid stream
- B01J8/007—Separating solid material from the gas/liquid stream by sedimentation
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/085—Feeding reactive fluids
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/087—Heating or cooling the reactor
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Abstract
本发明涉及一种适用于气液固三相反应的回路反应器及气液固三相反应方法，该回路反应器包括反应釜、换热器、循环泵和文丘里气液喷射器，所述的反应釜的下部和上部分别设置有气液进口和加料口，位于气液进口和加料口之间设置有液相出口和气相出口且气相出口位于液相出口的上方，在反应釜内部正对液相出口处设置有折形挡板，折形挡板设置有连通反应釜内部和液相出口的通道；反应釜、换热器、循环泵和文丘里气液喷射器连接构成循环回路。本发明设置折形挡板能够避免多数固体催化剂进入液相出口，中环形流道的设置进一步阻挡固体催化剂随从液相分离流出，进而避免固体催化剂进入循环泵，保证固体催化剂的反应活性。
The present invention relates to a loop reactor suitable for gas-liquid-solid three-phase reaction and a gas-liquid-solid three-phase reaction method, the loop reactor comprises a reactor, a heat exchanger, a circulation pump and a venturi gas-liquid ejector, the lower part and the upper part of the reactor are respectively provided with a gas-liquid inlet and a feeding port, a liquid phase outlet and a gas phase outlet are provided between the gas-liquid inlet and the feeding port, and the gas phase outlet is located above the liquid phase outlet, a folding baffle is provided inside the reactor directly opposite to the liquid phase outlet, and the folding baffle is provided with a channel connecting the inside of the reactor and the liquid phase outlet; the reactor, the heat exchanger, the circulation pump and the venturi gas-liquid ejector are connected to form a circulation loop. The folding baffle provided in the present invention can prevent most solid catalysts from entering the liquid phase outlet, and the setting of the middle annular flow channel further blocks the solid catalyst from flowing out with the liquid phase separation, thereby preventing the solid catalyst from entering the circulation pump, and ensuring the reaction activity of the solid catalyst.
Description
Technical Field
The invention relates to the field of chemical production of gas-liquid-solid multiphase reactions, in particular to a loop reactor suitable for gas-liquid-solid three-phase reactions and a gas-liquid-solid three-phase reaction method.
Background
The gas-liquid-solid three-phase reaction is a common reaction in the chemical industry field, and is more in variety, most of the solid is a catalyst in most cases, and the gas and the liquid are reactants and products. The traditional loop reactor has the advantages of good mass transfer effect, large heat exchange area outside the reactor, good device tightness and the like, and is widely applied to gas-liquid two-phase reactions.
There are also many patent documents on loop reactors, for example, CN109810024a discloses a jet loop reactor for preparing glutarimate, which comprises a jet mixer, a liquid phase feed pipe, a gas phase feed pipe, a circulating pump, a gas-liquid separator, a shell-and-tube heat exchanger, a receiver, and a sampling pipe, and a method for using the same. CN218924706U discloses a phosgenation loop reactor, which comprises a material storage tank, wherein the inlet of the material storage tank is provided with a throat pipe, phosgene and substrate are conveyed into the material storage tank through the throat pipe, the bottom of the material storage tank is provided with a material outlet, the material outlet is connected with a heat exchanger through a circulating pump, and the heat exchanger is also connected with the inlet of the material storage tank, so that a loop is formed between the material storage tank and the heat exchanger. CN114011336a discloses a continuous production equipment and a production method of biodiesel, the continuous production equipment adopts a jet loop reactor and a filter core pipe, the filter core pipe consists of an inner pipe and an outer pipe of a tubular filter core, the bottom of a reaction kettle is communicated with a heat exchanger through a circulating pump, the heat exchanger is sequentially communicated with an inner pipe of the filter core pipe and a feed pipe and a venturi injector arranged at the top end of the reaction kettle, the venturi injector comprises an inlet section, a nozzle, a mixing section and a diffusion section which are sequentially communicated, tapered annular air chambers are arranged at the peripheries of the inlet section and the nozzle, the air chambers are communicated with the mixing section, the air chambers are communicated with an air inlet arranged at the upper part of the reaction kettle through a gas circulating pipe, a feed inlet is arranged on the feed pipe, and a discharge outlet is arranged on the outer pipe of the filter core pipe.
However, in the existing loop reactor, the dispersion effect of the solid catalyst in the reaction kettle is poor, and the solid catalyst is easy to break or deactivate under the high shearing effect of the circulating pump, so that the application of the gas-liquid-solid three-phase reaction in the traditional loop reactor is limited.
Disclosure of Invention
Aiming at the defects and shortcomings existing in the prior art, the invention provides the loop reactor suitable for the gas-liquid-solid three-phase reaction, which can uniformly disperse the gas-liquid-solid three phases, prevent the catalyst from entering a circulating pump and ensure the reaction activity of the catalyst.
The technical scheme of the invention is as follows:
the loop reactor suitable for the gas-liquid-solid three-phase reaction comprises a reaction kettle, a heat exchanger, a circulating pump and a Venturi gas-liquid injector, wherein a gas-liquid inlet and a charging port are respectively arranged at the lower part and the upper part of the reaction kettle, a liquid phase outlet and a gas phase outlet are arranged between the gas-liquid inlet and the charging port and above the liquid phase outlet, a folded baffle is arranged at the position, opposite to the liquid phase outlet, inside the reaction kettle, and a channel for communicating the inside of the reaction kettle with the liquid phase outlet is arranged on the folded baffle;
The gas-liquid inlet of the reaction kettle is connected with the gas-liquid outlet of the Venturi gas-liquid injector, the liquid-phase outlet of the reaction kettle is connected with the liquid-phase inlet of the Venturi gas-liquid injector through a heat exchanger and a circulating pump, and the gas-phase outlet of the reaction kettle is connected with the gas-phase inlet of the Venturi gas-liquid injector.
According to the invention, preferably, an annular flow passage is arranged at the liquid phase outlet of the reaction kettle, the side wall of the annular flow passage is provided with a pore canal and is communicated with the reaction kettle, and a filter screen is arranged in the pore canal;
Preferably, the shape of the pore canal is a sector;
preferably, the maximum pore diameter of the filter screen is smaller than the average particle diameter of the solid catalyst;
Preferably, the bottom of the annular flow passage is provided with a discharge hole.
According to the invention, preferably, the folded baffle plate is provided with a notch in the direction of the gas-liquid inlet, the notch forms a channel for communicating the inside of the reaction kettle with the liquid phase outlet, and further preferably, the folded baffle plate is uniformly provided with holes, and the holes and the notch jointly form a channel for communicating the inside of the reaction kettle with the liquid phase outlet.
According to the invention, preferably, a porous baffle is arranged in the reaction kettle between the liquid phase outlet and the gas phase outlet. A porous baffle is provided for separation of the gas phase from the liquid phase.
According to the invention, preferably, the upper part of the reaction kettle is also provided with an auxiliary function port. The auxiliary function port can be used for measuring parameters such as temperature, pressure and the like, and also can be used for observation and the like.
According to the invention, preferably, a check valve is arranged between the gas-liquid inlet of the reaction kettle and the gas-liquid outlet of the Venturi gas-liquid injector, and further preferably, an evacuation valve is arranged between the check valve and the gas-liquid inlet of the reaction kettle.
According to the invention, preferably, the gas phase outlet is also connected with a gas inlet, and the gas phase and the gas raw material separated from the reaction kettle are introduced into the gas phase inlet of the Venturi gas-liquid injector through a pipeline.
According to the invention, preferably, the reaction kettle is of a cylindrical structure, a catalyst suspension area, a sedimentation area and a gas phase area are sequentially arranged between a gas inlet and a feed inlet, and the area between the folded baffle and a liquid phase outlet is a solid phase separation area;
Preferably, the diameter of the catalyst suspension zone is smaller than the diameter of the sedimentation zone, i.e. the catalyst suspension zone comprises a reducing zone and a small diameter zone, and the sedimentation zone is a large diameter zone.
The invention also provides a method for carrying out gas-liquid-solid three-phase reaction by using the loop reactor, which comprises the following steps:
The solid catalyst and the liquid raw material are added into a reaction kettle through a feed port, the gas raw material enters a gas phase inlet of a Venturi gas-liquid ejector through a gas inlet, a liquid phase enters a heat exchanger from a liquid phase outlet and is pumped into a liquid phase inlet of the Venturi gas-liquid ejector through a circulating pump after heat exchange, the Venturi gas-liquid ejector mixes the gas phase and the liquid phase and then enters the reaction kettle through the gas-liquid inlet, the gas-liquid-solid three-phase reaction is carried out on the solid catalyst in the reaction kettle, and unreacted gas phase enters the Venturi gas-liquid ejector through the gas phase outlet to carry out circulating loop reaction.
The invention is provided with the folded baffle plate at the position, which is opposite to the liquid phase outlet, inside the reaction kettle, and the folded baffle plate can prevent most solid catalysts from entering the solid phase separation zone. The arrangement of the annular flow channel further prevents the solid catalyst from flowing out along with the liquid phase separation, so that the solid catalyst is prevented from entering the circulating pump, and the reaction activity of the solid catalyst is ensured. The porous baffle is used for separating the gas phase from the liquid phase, and prevents the liquid phase from entering the gas phase outlet. The reaction kettle, the heat exchanger, the circulating pump and the Venturi gas-liquid injector are connected to form a circulating loop, which is very beneficial to the gas-liquid-solid three-phase circulation loop reaction.
The beneficial effects of the invention are as follows:
1. the invention is provided with the folded baffle plate at the position, which is opposite to the liquid phase outlet, inside the reaction kettle, and the folded baffle plate can prevent most solid catalysts from entering the solid phase separation zone.
2. The annular flow channel is further arranged to prevent the solid catalyst from flowing out along with the liquid phase separation, so that the solid catalyst is prevented from entering the circulating pump, and the reaction activity of the solid catalyst is ensured.
3. The diameter of the catalyst suspension area of the reaction kettle is smaller than that of the sedimentation area, namely the diameter of the reaction kettle is increased from bottom to top. The gas-liquid-solid three-phase catalyst can be uniformly dispersed in the catalyst suspension area, and the sedimentation area is more favorable for sedimentation of the solid catalyst, and has a certain effect on preventing the solid catalyst from entering the liquid phase outlet.
4. The invention connects the reaction kettle, the heat exchanger, the circulating pump and the Venturi gas-liquid injector to form a circulating loop, which is very beneficial to the gas-liquid-solid three-phase reaction.
Drawings
FIG. 1 is a schematic diagram of the main structure of a loop reactor according to the present invention.
FIG. 2 is a schematic diagram of the main structure of a reaction vessel in a loop reactor according to the present invention.
FIG. 3 is a schematic diagram of the main structure of the annular flow channel in the reaction kettle structure of the invention.
FIG. 4 is a schematic diagram of the interface of the venturi gas-liquid ejector in the loop reactor of the present invention.
The device comprises a 1-reaction kettle, a 2-heat exchanger, a 3-circulating pump, a 4-Venturi gas-liquid injector, a 5-check valve, a 6-evacuation valve, a 7-gas inlet, a 10-auxiliary function port, a 11-charging port, a 12-porous baffle, a 13-folded baffle, a 14-annular runner, a 15-liquid phase outlet, a 16-filter screen, a 17-discharge port, a 18-gas-liquid inlet, a 19-gas phase outlet, an I-catalyst suspension zone, a II-sedimentation zone, a III-solid phase separation zone, an IV-gas phase zone, a 41-gas-liquid outlet, a 42-gas phase inlet and a 43-liquid phase inlet.
Detailed Description
The invention will now be further illustrated by, but is not limited to, the following specific examples in connection with the accompanying drawings.
Example 1
As shown in fig. 1-4, a loop reactor suitable for gas-liquid-solid three-phase reaction comprises a reaction kettle 1, a heat exchanger 2, a circulating pump 3 and a venturi gas-liquid injector 4, wherein a gas-liquid inlet 18 and a charging port 11 are respectively arranged at the lower part and the upper part of the reaction kettle 1, a liquid phase outlet 15 and a gas phase outlet 19 are arranged between the gas-liquid inlet 18 and the charging port 11, the gas phase outlet is positioned above the liquid phase outlet 15, a folded baffle 13 is arranged in the reaction kettle 1 and opposite to the liquid phase outlet 15, and a channel for communicating the interior of the reaction kettle 1 and the liquid phase outlet 15 is arranged on the folded baffle 13;
The gas-liquid inlet 18 of the reaction kettle 1 is connected with the gas-liquid outlet 41 of the Venturi gas-liquid injector 4, the liquid phase outlet 15 of the reaction kettle 1 is connected with the liquid phase inlet 43 of the Venturi gas-liquid injector 4 through the heat exchanger 2 and the circulating pump 3, and the gas phase outlet 19 of the reaction kettle 1 is connected with the gas phase inlet 42 of the Venturi gas-liquid injector 4.
The folded baffle 13 in the embodiment is provided with a notch in the direction of the gas-liquid inlet 18, and the notch forms a channel for communicating the inside of the reaction kettle 1 with the liquid phase outlet 15;
The gas phase outlet 19 is also connected with the gas inlet 7, and the gas phase and the gas raw material separated from the reaction kettle 1 enter the gas phase inlet 42 of the Venturi gas-liquid injector 4 through a pipeline;
The reaction kettle 1 is of a cylindrical structure, a catalyst suspension area I, a sedimentation area II and a gas phase area IV are sequentially arranged between a gas inlet 18 and a feed inlet 11, a solid phase separation area III is arranged between the folded baffle 13 and a liquid phase outlet 15, the catalyst suspension area I, the sedimentation area II and the solid phase separation area III are main places for gas-liquid-solid three-phase reaction, the diameter of the catalyst suspension area I is smaller than that of the sedimentation area II, namely the catalyst suspension area I comprises a reducing area and a small-diameter area, and the sedimentation area is a large-diameter area.
Example 2
As described in example 1, the difference is that:
The folded baffle 13 is uniformly provided with pore passages, and the pore passages and the gaps form a channel which is communicated with the inside of the reaction kettle 1 and the liquid phase outlet 15.
Example 3
As described in example 1 or 2, except that:
An annular flow channel 14 is arranged at a liquid phase outlet 15 of the reaction kettle 1, a pore canal is arranged on the side wall of the annular flow channel 14 and is communicated with the reaction kettle 1, and a filter screen 16 is arranged in the pore canal;
Preferably, the pore channel is fan-shaped, and the maximum pore diameter of the filter screen 16 is smaller than the average particle diameter of the solid catalyst.
Example 4
As described in example 3, the difference is that:
the bottom of the annular flow passage 14 is provided with a discharge outlet 17.
Example 5
As described in examples 1 or 2 or 3 or 4, except that:
A porous baffle 12 is arranged in the reaction kettle 1 and positioned between the liquid phase outlet 15 and the gas phase outlet 19. A porous barrier 12 is provided for separation of the gas phase from the liquid phase.
Example 6
As described in examples 1 or 2 or 3 or 4 or 5, except that:
the upper part of the reaction kettle 1 is also provided with an auxiliary function port 10. The auxiliary function port 10 may be used for a measurement port for parameters such as temperature and pressure, or for observation.
Example 7
As described in examples 1 or 2 or 3 or 4 or 5, except that:
A check valve 5 is also arranged between the gas-liquid inlet 18 of the reaction kettle 1 and the gas-liquid outlet 41 of the venturi gas-liquid injector 4, and an evacuation valve 6 is preferably arranged between the check valve 5 and the gas-liquid inlet 18 of the reaction kettle 1.
Example 8
A method for performing a gas-liquid-solid three-phase reaction using any one of the loop reactors of examples 1-7, comprising the steps of:
The solid catalyst is added into the reaction kettle 1 through a feed port 11, the gas raw material enters a gas phase inlet 42 of the Venturi gas-liquid ejector 4 through a gas inlet 7, the liquid raw material enters a liquid phase inlet 43 of the Venturi gas-liquid ejector 4, the Venturi gas-liquid ejector 4 mixes the gas phase and the liquid phase and then enters the reaction kettle 1 through a gas-liquid inlet 18, the gas-liquid-solid three-phase reaction is carried out on the solid catalyst in the reaction kettle 1, the liquid phase enters the heat exchanger 2 from a liquid phase outlet 15 for heat exchange, and then is pumped into the Venturi gas-liquid ejector 4 through a circulating pump 3 for carrying out circulating loop reaction, and the gas phase enters the Venturi gas-liquid ejector 4 through a gas phase outlet 19 for carrying out circulating loop reaction.
The invention is provided with the folded baffle 13 in the reaction kettle 1 opposite to the liquid phase outlet 15, and the folded baffle 13 can prevent most solid catalysts from entering the solid phase separation zone III. The annular flow channel 14 further prevents the solid catalyst from flowing out along with the liquid phase separation, so that the solid catalyst is prevented from entering the circulating pump 3, and the reaction activity of the solid catalyst is ensured. The porous barrier 12 serves to separate the gas phase from the liquid phase, avoiding entry of the liquid phase into the gas phase outlet 19. The reaction kettle 1, the heat exchanger 2, the circulating pump 3 and the Venturi gas-liquid injector 4 are connected to form a circulating loop, which is very beneficial to the gas-liquid-solid three-phase circulation loop reaction.
Claims (11)
1. The loop reactor is characterized by comprising a reaction kettle, a heat exchanger, a circulating pump and a Venturi gas-liquid injector, wherein a gas-liquid inlet and a charging port are respectively arranged at the lower part and the upper part of the reaction kettle, a liquid phase outlet and a gas phase outlet are arranged between the gas-liquid inlet and the charging port and above the liquid phase outlet, a folded baffle is arranged in the reaction kettle and opposite to the liquid phase outlet, and a channel for communicating the reaction kettle with the liquid phase outlet is arranged on the folded baffle;
The gas-liquid inlet of the reaction kettle is connected with the gas-liquid outlet of the Venturi gas-liquid injector, the liquid-phase outlet of the reaction kettle is connected with the liquid-phase inlet of the Venturi gas-liquid injector through a heat exchanger and a circulating pump, and the gas-phase outlet of the reaction kettle is connected with the gas-phase inlet of the Venturi gas-liquid injector;
The reactor is of a cylindrical structure, a catalyst suspension area, a sedimentation area and a gas phase area are sequentially arranged between a gas-liquid inlet and a charging hole, a solid-phase separation area is arranged in the area between the folded baffle and the liquid-phase outlet, and the diameter of the catalyst suspension area is smaller than that of the sedimentation area.
2. The loop reactor for gas-liquid-solid three-phase reactions according to claim 1 wherein said tunnel is fan-shaped.
3. The loop reactor for gas-liquid-solid three-phase reactions according to claim 1 wherein the maximum pore size of said screen is less than the average particle size of the solid catalyst.
4. The loop reactor for gas-liquid-solid three-phase reaction according to claim 1, wherein the bottom of the annular flow channel is provided with a discharge port.
5. The loop reactor for gas-liquid-solid three-phase reaction according to claim 1, wherein the folded baffle plate is provided with a notch in the direction of the gas-liquid inlet.
6. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 1, wherein the folded baffle plates are uniformly provided with pore channels.
7. The loop reactor for gas-liquid-solid three-phase reaction according to claim 1, wherein the upper part of the reaction kettle is further provided with an auxiliary function port.
8. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 1, wherein a check valve is further arranged between the gas-liquid inlet of the reaction kettle and the gas-liquid outlet of the venturi gas-liquid injector.
9. The loop reactor for gas-liquid-solid three-phase reactions according to claim 8 wherein an evacuation valve is provided between the check valve and the gas-liquid inlet of the reaction vessel.
10. The loop reactor for gas-liquid-solid three-phase reactions according to claim 1 wherein said gas phase outlet is further connected to a gas inlet.
11. A method of gas-liquid-solid three-phase reaction comprising the use of the loop reactor of any one of claims 1-10, comprising the steps of:
The solid catalyst is added into the reaction kettle through a feed port, the gas raw material is introduced into a gas phase inlet of a Venturi gas-liquid ejector through a gas inlet, the liquid raw material is introduced into a liquid phase inlet of the Venturi gas-liquid ejector, the Venturi gas-liquid ejector mixes the gas phase and the liquid phase and then enters the reaction kettle through the gas-liquid inlet, the gas-liquid-solid three-phase reaction is carried out on the solid catalyst in the reaction kettle, the liquid phase enters a heat exchanger from a liquid phase outlet, the heat exchange is carried out, the liquid phase is pumped into the Venturi gas-liquid ejector through a circulating pump for carrying out the circulating loop reaction, and the gas phase enters the Venturi gas-liquid ejector through a gas phase outlet for carrying out the circulating loop reaction.
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| CN202310643308.7A CN116474659B (en) | 2023-06-01 | 2023-06-01 | A loop reactor suitable for gas-liquid-solid three-phase reaction and a gas-liquid-solid three-phase reaction method |
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| CN202310643308.7A CN116474659B (en) | 2023-06-01 | 2023-06-01 | A loop reactor suitable for gas-liquid-solid three-phase reaction and a gas-liquid-solid three-phase reaction method |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101074194A (en) * | 2007-06-25 | 2007-11-21 | 沈建冲 | Carboxide synthesis and synthesizer |
| CN101804317A (en) * | 2010-04-02 | 2010-08-18 | 南京大学 | Multiphase catalysis tower type collision current reactor |
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- 2023-06-01 CN CN202310643308.7A patent/CN116474659B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101074194A (en) * | 2007-06-25 | 2007-11-21 | 沈建冲 | Carboxide synthesis and synthesizer |
| CN101804317A (en) * | 2010-04-02 | 2010-08-18 | 南京大学 | Multiphase catalysis tower type collision current reactor |
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