A loop reactor suitable for gas-liquid-solid three-phase reaction and a gas-liquid-solid three-phase reaction method

By setting a folded baffle and annular flow channel in the loop reactor, the problem of poor dispersion effect of solid catalysts in the reactor and easy deactivation is solved, achieving uniform dispersion of gas-liquid solid three-phase reactions and effective protection of the catalyst.

CN116474659BActive Publication Date: 2025-06-06WEIHAI XINYUAN CHEM MASCH CO LTD +2
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Patent Information

Application Number
CN202310643308.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-01
Publication Date
2025-06-06
Estimated Expiration
2043-06-01

AI Technical Summary

Technical Problem

In existing loop reactors, solid catalysts have poor dispersion effects in the reactor and are easily broken or inactivated under the high shear effect of the circulation pump, limiting the application of gas-liquid solid three-phase reactions.

Method used

A circuit reactor including a reactor, a heat exchanger, a circulation pump and a Venturi gas-liquid injector was designed. By setting a folded baffle and an annular flow channel in the reactor, the solid catalyst is prevented from entering the solid phase separation zone and the circulation pump, and the reactivity of the catalyst is ensured.

Benefits of technology

The uniform dispersion of gas, liquid and solid phases is achieved, and the deactivation and breakage of the catalyst is avoided, and the reaction efficiency and product quality are improved.

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Abstract

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.
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Description

Technical Field

[0001] The invention relates to the field of chemical production of gas-liquid-solid multiphase reaction, and in particular to a loop reactor suitable for gas-liquid-solid three-phase reaction and a gas-liquid-solid three-phase reaction method. Background Art

[0002] Gas-liquid-solid three-phase reaction is a common reaction in the chemical industry. There are many types. In most cases, solids are catalysts, and gases and liquids are reactants and products. Traditional loop reactors have the advantages of good mass transfer effect, large heat exchange area outside the kettle, and good sealing of the device. They are widely used in gas-liquid two-phase reactions.

[0003] There are also many patent documents reporting on loop reactors, for example: CN109810024A discloses a jet loop reactor for preparing pentamethylene diisocyanate and a method of using the same, the jet loop reactor comprising a jet mixer, a liquid phase feed pipe, a gas phase feed pipe, a circulation pump, a gas-liquid separator, a shell-and-tube heat exchanger, a receiver, and a sampling tube. CN218924706U discloses a phosgenation loop reactor, comprising a material storage tank, a throat is provided at the inlet of the material storage tank, phosgene and substrate are both transported to the material storage tank through the throat, a material outlet is provided at the bottom of the material storage tank, the material outlet is connected to the heat exchanger via a circulation pump, and the heat exchanger is also connected to 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 device and a production method for biodiesel, the continuous production device adopts a jet loop reactor and a filter tube; the filter tube is composed of an inner tube and an outer tube of a tubular filter; the bottom of the reactor is connected to a heat exchanger through a circulation pump; the heat exchanger is connected to a venturi injector arranged at the top of the reactor through the inner tube of the filter tube and a feed pipe in sequence; the venturi injector includes an inlet section, a nozzle, a mixing section and a diffusion section which are connected in sequence, and a tapered annular air chamber is provided on the periphery of the inlet section and the nozzle, the air chamber is connected to the mixing section, and the air chamber is connected to an air inlet arranged on the upper part of the reactor through a gas circulation pipe; a feed port is provided on the feed pipe; and a discharge port is provided on the outer tube of the filter tube.

[0004] However, in existing loop reactors, the solid catalyst has a poor dispersion effect in the reactor and is easily broken or deactivated under the high shear effect of the circulation pump, which limits the application of gas-liquid-solid three-phase reaction in traditional loop reactors. Summary of the invention

[0005] In view of the shortcomings and defects in the prior art, the present invention provides a loop reactor suitable for gas-liquid-solid three-phase reaction, which can disperse the gas-liquid-solid three-phase evenly and prevent the catalyst from entering the circulation pump, thereby ensuring the reaction activity of the catalyst.

[0006] The technical solution of the present invention is as follows:

[0007] A loop reactor suitable for gas-liquid-solid three-phase reaction, comprising a reactor, a heat exchanger, a circulation pump and a venturi gas-liquid ejector, wherein 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 folded baffle is provided inside the reactor directly opposite to the liquid phase outlet, and the folded baffle is provided with a channel connecting the inside of the reactor and the liquid phase outlet;

[0008] The gas-liquid inlet of the reactor is connected to the gas-liquid outlet of the venturi gas-liquid ejector, the liquid phase outlet of the reactor is connected to the liquid phase inlet of the venturi gas-liquid ejector through a heat exchanger and a circulation pump, and the gas phase outlet of the reactor is connected to the gas phase inlet of the venturi gas-liquid ejector.

[0009] According to the present invention, preferably, an annular flow channel is provided at the liquid phase outlet of the reactor, a hole is provided on the side wall of the annular flow channel and is connected to the reactor, and a filter is provided in the hole;

[0010] Preferably, the shape of the hole is fan-shaped;

[0011] Preferably, the maximum pore size of the filter is smaller than the average particle size of the solid catalyst;

[0012] Preferably, a discharge port is provided at the bottom of the annular flow channel.

[0013] According to the present invention, preferably, the folded baffle is provided with a notch in the gas-liquid inlet direction, and the notch constitutes a channel connecting the interior of the reactor and the liquid phase outlet; further preferably, holes are evenly arranged on the folded baffle, and the holes and the notch together constitute a channel connecting the interior of the reactor and the liquid phase outlet.

[0014] According to the present invention, preferably, a porous baffle is provided between the liquid phase outlet and the gas phase outlet in the reactor. The porous baffle is provided for separation of the gas phase and the liquid phase.

[0015] According to the present invention, preferably, the upper part of the reactor is also provided with an auxiliary function port, which can be used for measuring parameters such as temperature and pressure, and can also be used for observation.

[0016] According to the present invention, preferably, a check valve is further provided between the gas-liquid inlet of the reactor and the gas-liquid outlet of the venturi gas-liquid injector; further preferably, a drain valve is provided between the check valve and the gas-liquid inlet of the reactor.

[0017] According to the present invention, preferably, the gas phase outlet is also connected to the gas inlet, and the gas phase and gas raw materials separated by the reactor enter the gas phase inlet of the venturi gas-liquid injector through a pipeline.

[0018] According to the present invention, preferably, the reactor is a cylindrical structure, and the catalyst suspension zone, the sedimentation zone, and the gas phase zone are arranged in sequence from the gas-liquid inlet to the feed port, and the area between the folded baffle and the liquid phase outlet is the solid phase separation zone; the catalyst suspension zone, the sedimentation zone, and the solid phase separation zone are the main places for the gas-liquid-solid three-phase reaction;

[0019] Preferably, the diameter of the catalyst suspension zone is smaller than the diameter of the sedimentation zone; that is, the catalyst suspension zone includes a variable diameter zone and a small diameter zone, and the sedimentation zone is a large diameter zone.

[0020] The present invention also provides a method for performing a gas-liquid-solid three-phase reaction using the above loop reactor, comprising the following steps:

[0021] The solid catalyst and liquid raw material are added into the reactor through the feed port, the gas raw material enters the gas phase inlet of the venturi gas-liquid injector through the gas inlet, the liquid phase enters the heat exchanger from the liquid phase outlet for heat exchange and is pumped into the liquid phase inlet of the venturi gas-liquid injector through a circulation pump, the venturi gas-liquid injector mixes the gas and liquid phases and then enters the reactor through the gas-liquid inlet to carry out a gas-liquid-solid three-phase reaction with the solid catalyst in the reactor, and the unreacted gas phase enters the venturi gas-liquid injector through the gas phase outlet for a circulation loop reaction.

[0022] The present invention is provided with a folded baffle plate inside the reactor directly opposite to the liquid phase outlet, and the folded baffle plate can prevent most solid catalysts from entering the solid phase separation zone. The setting of the 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, thereby ensuring the reaction activity of the solid catalyst. The porous baffle plate is used to separate the gas phase from the liquid phase, and prevents the liquid phase from entering the gas phase outlet. The reactor, the heat exchanger, the circulation pump and the venturi gas-liquid ejector are connected to form a circulation loop, which is very conducive to the gas-liquid-solid three-phase circulation loop reaction.

[0023] The beneficial effects of the present invention are as follows:

[0024] 1. The present invention provides a folded baffle plate inside the reactor directly opposite to the liquid phase outlet, and the folded baffle plate can prevent most solid catalysts from entering the solid phase separation zone.

[0025] 2. The setting of the annular flow channel in the present invention further blocks the solid catalyst from flowing out of the liquid phase separation, thereby preventing the solid catalyst from entering the circulation pump, thereby ensuring the reaction activity of the solid catalyst.

[0026] 3. The diameter of the catalyst suspension zone of the reactor of the present invention is smaller than that of the sedimentation zone, that is, the diameter of the reactor increases from bottom to top. This not only allows the three phases of gas, liquid and solid to be evenly dispersed in the catalyst suspension zone, but also facilitates the sedimentation of the solid catalyst in the sedimentation zone, and has a certain effect on preventing the solid catalyst from entering the liquid phase outlet.

[0027] 4. The present invention connects the reaction kettle, the heat exchanger, the circulation pump and the Venturi gas-liquid ejector to form a circulation loop, which is very conducive to the gas-liquid-solid three-phase reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a schematic diagram of the main structure of the loop reactor of the present invention.

[0029] Figure 2 It is a schematic diagram of the main structure of the reactor in the loop reactor of the present invention.

[0030] Figure 3 It is a schematic diagram of the main structure of the annular flow channel in the reactor structure of the present invention.

[0031] Figure 4 It is a schematic diagram of the interface of the Venturi gas-liquid ejector in the loop reactor of the present invention.

[0032] Wherein: 1-reactor, 2-heat exchanger, 3-circulation pump, 4-Venturi gas-liquid ejector, 5-check valve, 6-drain valve, 7-gas inlet, 10-auxiliary function port, 11-feeding port, 12-porous baffle, 13-folded baffle, 14-annular flow channel, 15-liquid phase outlet, 16-filter, 17-discharge port, 18-gas-liquid inlet, 19-gas phase outlet, I-catalyst suspension zone, II-sedimentation zone, III-solid phase separation zone, IV-gas phase zone, 41-gas-liquid outlet, 42-gas phase inlet, 43-liquid phase inlet. DETAILED DESCRIPTION

[0033] The present invention will be further described below through specific embodiments in conjunction with the accompanying drawings, but is not limited thereto.

[0034] Example 1

[0035] like Figure 1-4 As shown, a loop reactor suitable for gas-liquid-solid three-phase reaction comprises a reactor 1, a heat exchanger 2, a circulation pump 3 and a venturi gas-liquid ejector 4, wherein a gas-liquid inlet 18 and a feeding port 11 are respectively arranged at the lower part and the upper part of the reactor 1, a liquid phase outlet 15 and a gas phase outlet 19 are arranged between the gas-liquid inlet 18 and the feeding port 11, and the gas phase outlet is located above the liquid phase outlet 15, and a folded baffle 13 is arranged inside the reactor 1 directly opposite to the liquid phase outlet 15, and the folded baffle 13 is provided with a channel connecting the inside of the reactor 1 and the liquid phase outlet 15;

[0036] The gas-liquid inlet 18 of the reactor 1 is connected to the gas-liquid outlet 41 of the Venturi gas-liquid ejector 4, the liquid phase outlet 15 of the reactor 1 is connected to the liquid phase inlet 43 of the Venturi gas-liquid ejector 4 through the heat exchanger 2 and the circulation pump 3, and the gas phase outlet 19 of the reactor 1 is connected to the gas phase inlet 42 of the Venturi gas-liquid ejector 4.

[0037] The folded baffle 13 described in this embodiment is provided with a notch in the direction of the gas-liquid inlet 18, and the notch constitutes a channel connecting the interior of the reactor 1 and the liquid phase outlet 15;

[0038] The gas phase outlet 19 is also connected to the gas inlet 7, and the gas phase and gas raw materials separated by the reactor 1 enter the gas phase inlet 42 of the venturi gas-liquid injector 4 through the pipeline;

[0039] The reactor 1 is a cylindrical structure, and the catalyst suspension zone I, the sedimentation zone II, and the gas phase zone IV are arranged in sequence from the gas-liquid inlet 18 to the feed port 11. The area between the folded baffle 13 and the liquid phase outlet 15 is the solid phase separation zone III; the catalyst suspension zone I, the sedimentation zone II and the solid phase separation zone III are the main places for the gas-liquid-solid three-phase reaction; the diameter of the catalyst suspension zone I is smaller than the diameter of the sedimentation zone II; that is, the catalyst suspension zone I includes a variable diameter zone and a small diameter zone, and the sedimentation zone is a large diameter zone.

[0040] Example 2

[0041] As described in Example 1, except that:

[0042] The folded baffle 13 is evenly provided with holes, and the holes and the notches together form a channel connecting the interior of the reactor 1 and the liquid phase outlet 15 .

[0043] Example 3

[0044] As described in Example 1 or 2, except that:

[0045] An annular flow channel 14 is provided at the liquid phase outlet 15 of the reactor 1, and a hole is provided on the side wall of the annular flow channel 14 and is connected to the reactor 1, and a filter screen 16 is provided in the hole;

[0046] Preferably, the shape of the pores is fan-shaped, and the maximum pore size of the filter screen 16 is smaller than the average particle size of the solid catalyst.

[0047] Example 4

[0048] As described in Example 3, except that:

[0049] A discharge port 17 is provided at the bottom of the annular flow channel 14 .

[0050] Example 5

[0051] As described in Example 1 or 2 or 3 or 4, except that:

[0052] A porous baffle 12 is provided in the reactor 1 between the liquid phase outlet 15 and the gas phase outlet 19. The porous baffle 12 is provided for separation of the gas phase and the liquid phase.

[0053] Example 6

[0054] As described in Example 1 or 2 or 3 or 4 or 5, except that:

[0055] The upper part of the reactor 1 is also provided with an auxiliary function port 10. The auxiliary function port 10 can be used for measuring parameters such as temperature and pressure, and can also be used for observation.

[0056] Example 7

[0057] As described in Example 1 or 2 or 3 or 4 or 5, except that:

[0058] A check valve 5 is further provided between the gas-liquid inlet 18 of the reactor 1 and the gas-liquid outlet 41 of the venturi gas-liquid ejector 4 ; preferably, an exhaust valve 6 is provided between the check valve 5 and the gas-liquid inlet 18 of the reactor 1 .

[0059] Example 8

[0060] The method for performing a gas-liquid-solid three-phase reaction using any one of the loop reactors of Examples 1-7 comprises the following steps:

[0061] The solid catalyst is added to the reactor 1 through the feed port 11, the gas raw material enters the gas phase inlet 42 of the Venturi gas-liquid injector 4 through the gas inlet 7, and the liquid raw material enters the liquid phase inlet 43 of the Venturi gas-liquid injector 4. The Venturi gas-liquid injector 4 mixes the gas and liquid phases and enters the reactor 1 through the gas-liquid inlet 18 to perform a gas-liquid-solid three-phase reaction with the solid catalyst in the reactor 1. The liquid phase enters the heat exchanger 2 from the liquid phase outlet 15 for heat exchange and is pumped into the Venturi gas-liquid injector 4 through the circulation pump 3 for a circulation loop reaction. The gas phase enters the Venturi gas-liquid injector 4 through the gas phase outlet 19 for a circulation loop reaction.

[0062] The present invention is provided with a folded baffle 13 at the liquid phase outlet 15 inside the reactor 1, and the folded baffle 13 can prevent most solid catalysts from entering the solid phase separation zone III. The setting of the annular flow channel 14 further blocks the solid catalyst from flowing out with the liquid phase separation, thereby preventing the solid catalyst from entering the circulation pump 3, thereby ensuring the reaction activity of the solid catalyst. The porous baffle 12 is used to separate the gas phase from the liquid phase, and prevent the liquid phase from entering the gas phase outlet 19. The reactor 1, the heat exchanger 2, the circulation pump 3 and the venturi gas-liquid ejector 4 are connected to form a circulation loop, which is very conducive to the gas-liquid-solid three-phase circulation loop reaction.

Claims

1. A loop reactor suitable for gas-liquid-solid three-phase reaction, It is characterized in that The invention comprises a reactor, a heat exchanger, a circulation pump and a venturi gas-liquid ejector, wherein 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, and a folded baffle is provided inside the reactor directly opposite to the liquid phase outlet, and the folded baffle is provided with a channel connecting the inside of the reactor and the liquid phase outlet; The gas-liquid inlet of the reactor is connected to the gas-liquid outlet of the venturi gas-liquid ejector, the liquid phase outlet of the reactor is connected to the liquid phase inlet of the venturi gas-liquid ejector through a heat exchanger and a circulation pump, and the gas phase outlet of the reactor is connected to the gas phase inlet of the venturi gas-liquid ejector; An annular flow channel is arranged at the liquid phase outlet of the reactor, a hole is arranged on the side wall of the annular flow channel and is connected to the reactor, and a filter is arranged in the hole; a porous baffle is arranged between the liquid phase outlet and the gas phase outlet in the reactor; the reactor is a cylindrical structure, and the catalyst suspension zone, the sedimentation zone, and the gas phase zone are arranged from the gas-liquid inlet to the feeding port in sequence, the area between the folded baffle and the liquid phase outlet is the solid phase separation zone, and the diameter of the catalyst suspension zone is smaller than the diameter of the sedimentation zone.

2. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 1, It is characterized in that The shape of the hole is fan-shaped.

3. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 1, It is characterized in that The maximum pore size of the filter is smaller than the average particle size of the solid catalyst.

4. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 1, It is characterized in that A discharge port is arranged at the bottom of the annular flow channel.

5. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 1, It is characterized in that The folded baffle 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, It is characterized in that The folding baffle is evenly provided with holes.

7. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 1, It is characterized in that The upper part of the reaction kettle is also provided with an auxiliary function port.

8. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 1, It is characterized in that A check valve is also provided between the gas-liquid inlet of the reactor and the gas-liquid outlet of the venturi gas-liquid ejector.

9. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 8, It is characterized in that An exhaust valve is arranged between the check valve and the gas-liquid inlet of the reactor.

10. The loop reactor suitable for gas-liquid-solid three-phase reaction according to claim 1, It is characterized in that The gas phase outlet is also connected to the gas inlet.

11. A method for gas-liquid-solid three-phase reaction, comprising using the loop reactor according to any one of claims 1 to 10, comprising the following steps: The solid catalyst is added to the reactor through the feed port, the gas raw material enters the gas phase inlet of the Venturi gas-liquid injector through the gas inlet, and the liquid raw material enters the liquid phase inlet of the Venturi gas-liquid injector. The Venturi gas-liquid injector mixes the gas and liquid phases and then enters the reactor through the gas-liquid inlet to perform a gas-liquid-solid three-phase reaction with the solid catalyst in the reactor. The liquid phase enters the heat exchanger from the liquid phase outlet for heat exchange and is pumped into the Venturi gas-liquid injector through a circulation pump for a circulation loop reaction. The gas phase enters the Venturi gas-liquid injector through the gas phase outlet for a circulation loop reaction.

Citation Information

Patent Citations

  • Spraying loop reactor for preparing pentyl diisocyanate and application method thereof

    CN109810024A

  • Continuous production equipment of biodiesel and production method thereof

    CN114011336A

  • Phosgenation loop reactor

    CN218924706U

  • Carboxide synthesis and synthesizer

    CN101074194A

  • Multiphase catalysis tower type collision current reactor

    CN101804317A