CN111686648A - Fixed bed hydrogenation micro-interface reaction system - Google Patents

Abstract

The invention provides a fixed-bed hydrogenation micro-interface reaction system. The system comprises: a fixed-bed reactor and a micro-interface generator; wherein, the micro-interface generator is connected with the fixed-bed reactor, and during the hydrogenation reaction process, the pressure energy of hydrogen and/or the liquid in the reaction process are converted into The kinetic energy of the hydrogen gas is converted into the surface energy of the hydrogen bubbles, so that the hydrogen bubbles are broken into microbubbles, and the microbubbles are mixed with the liquid to form a gas-liquid emulsion, and the gas-liquid emulsion enters the fixed-bed reactor for subsequent reactions. The fixed-bed hydrogenation micro-interface reaction system of the present invention has the advantages of low energy consumption, low operating pressure, large gas-liquid mass transfer phase interface area, fast apparent reaction speed, and high gas utilization rate.

Description

A fixed-bed hydrogenation micro-interface reaction system

technical field

The invention relates to the technical field of fixed-bed reaction systems, in particular to a fixed-bed hydrogenation micro-interface reaction system.

Background technique

At present, gas-liquid, gas-liquid-solid and other gas-liquid reaction processes exist widely in energy, petrochemical, fine chemical and other fields. Such as oxidation, hydrogenation, chlorination and other gas-liquid heterogeneous reactions, the macroscopic reaction rate is generally controlled by the mass transfer process. The volumetric mass transfer coefficient of the gas-liquid reaction is mainly affected by the mass transfer coefficient and the gas-liquid interface area. Previous studies have shown that the phase boundary area has a great influence on the volumetric mass transfer coefficient and is easy to control. Therefore, increasing the phase interface area is regarded as an effective way to increase the gas-liquid macroscopic reaction rate.

A fixed bed reactor is a commonly used form of chemical reactor, which means that a granular solid catalyst or solid reactant is filled in the reactor to form a stacked bed with a certain height, and the gas or liquid material flows through the static fixed bed through the particle gap. At the same time, a heterogeneous reaction process is realized. The characteristics of this type of reactor are that the solid particles filled in the equipment are fixed, which is different from the moving bed and fluidized bed in which the solid material moves in the equipment, also known as the packed bed reactor. Fixed bed reactors are widely used in gas-solid and liquid-solid reaction processes.

However, the problems existing in the hydrogenation of hydrogen and the reaction liquid in the fixed bed reaction system are: high operating pressure, small gas-liquid mass transfer phase interface area, slow apparent reaction speed, low gas utilization rate, large investment, high consumption Low, difficult to operate and other issues.

SUMMARY OF THE INVENTION

In view of this, the present invention proposes a fixed-bed hydrogenation micro-interface reaction system, which aims to solve the existing problem of insufficient reaction due to the small contact area between the hydrogen and the liquid, resulting in high energy consumption.

In one aspect, the present invention provides a fixed-bed hydrogenation micro-interface reaction system, comprising: a fixed-bed reactor, a micro-interface generator, and a gas-liquid separation tank; wherein,

The micro-interface generator is connected to the fixed-bed reactor, and in the hydrogenation reaction process, the pressure energy of hydrogen and/or the kinetic energy of the liquid in the reaction process are converted into the surface energy of hydrogen bubbles, so that the hydrogen bubbles are broken into microscopic particles. bubbles, and the microbubbles are mixed with the liquid in the reaction process to form a gas-liquid emulsion, and then the gas-liquid emulsion enters the fixed-bed reactor for subsequent reactions;

The fixed-bed reactor is used as a reaction place for hydrogenation reaction, so as to form a stable gas-liquid enhanced fixed-bed reaction system when the gas-liquid emulsion enters it;

The fixed-bed reactor is used as a reaction place for hydrogenation reaction, so as to form a stable gas-liquid enhanced fixed-bed reaction system when the gas-liquid emulsion enters it;

The gas-liquid separation tank is connected with the fixed-bed reactor, and is used for gas-liquid separation of the reaction-completed mixture in the fixed-bed reactor.

Further, in the above-mentioned fixed-bed hydrogenation micro-interface reaction system, the micro-interface generator is selected from one or more of pneumatic micro-interface generators, hydraulic micro-interface generators and gas-liquid linkage micro-interface generators.

Further, in the above-mentioned fixed-bed hydrogenation micro-interface reaction system, the micro-interface generator is arranged on the upper part of the fixed-bed reactor.

Further, in the above-mentioned fixed-bed hydrogenation micro-interface reaction system, the micro-interface generator is arranged at the lower part of the fixed-bed reactor.

Further, in the above-mentioned fixed-bed hydrogenation micro-interface reaction system, the fixed-bed reactor includes: a reaction tank and a catalyst bed; wherein,

The reaction tank is a tank for providing a reaction space for the gas-liquid emulsion, and the reaction tank is provided with an outlet for outputting the reacted mixture;

The catalyst bed is fixed inside the reaction tank, and a catalyst for improving the reaction efficiency of the gas-liquid emulsion is arranged in the bed.

Further, the above-mentioned fixed-bed hydrogenation micro-interface reaction system also includes: a raw material tank, a power mechanism and a feed preheater; wherein,

The raw material tank is connected with the power mechanism for storing hydrogen and reaction liquid;

The other end of the power mechanism is connected with the feed preheater to provide power for transporting hydrogen and reaction liquid;

The other end of the feed preheater is connected to the micro-interface reactor for preheating the hydrogen gas and the reaction liquid to reach a specified temperature.

Further, in the above-mentioned fixed-bed hydrogenation micro-interface reaction system, the raw material tank includes: a liquid raw material tank and a gas raw material buffer tank; wherein,

the liquid raw material tank is connected with the feeding pump for storing the liquid raw material;

The gas raw material buffer tank is connected to the compressor for storing hydrogen.

Further, in the above-mentioned fixed-bed hydrogenation micro-interface reaction system, the power mechanism includes: a feed pump and a compressor; wherein,

The feed pump is connected with the liquid feed preheater to provide power for conveying liquid raw materials;

The compressor is connected to the gas feed preheater for powering the delivery of hydrogen.

Further, in the above-mentioned fixed bed hydrogenation micro-interface reaction system, the feed preheater includes: a liquid feed preheater and a gas feed preheater; wherein,

The liquid feed preheater is connected with the micro-interface generator, and is used to preheat the liquid raw material to make it reach a specified temperature, and send it into the micro-interface generator;

The gas feed preheater is connected to the micro-interface generator for preheating the hydrogen gas to reach a specified temperature and feeding it into the micro-interface generator.

Further, in the above-mentioned fixed-bed hydrogenation micro-interface reaction system, when the number of the fixed-bed reactors is greater than one, the highest part of the connecting pieces connected to each other is higher than the preceding fixed-bed reactors in order from back to front. The highest point of the bed reactor.

Compared with the prior art, the beneficial effect of the present invention is that, in the fixed-bed hydrogenation micro-interface reaction system provided by the present invention, by adding a micro-interface generator to the fixed-bed reaction system, the hydrogen gas is broken into a diameter of 1 μm. The gas with ≤d<1mm forms a micro-bubble system. The micro-bubble has the advantages of rigidity, good independence, and is not easy to coalesce, so that in the gas-liquid reaction process, the gas-liquid reaction is strengthened, and the mass transfer efficiency is improved. Emulsion of a large number of microbubbles, thereby forming a higher phase boundary area in the reactor.

Further, by providing a micro-interface generator, the fixed-bed hydrogenation micro-interface reaction system of the present invention has the advantages of high gas utilization rate, high desulfurization rate, low investment, low energy consumption and flexible process in engineering.

Description of drawings

Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are for the purpose of illustrating preferred embodiments only and are not to be considered limiting of the invention. Also, the same components are denoted by the same reference numerals throughout the drawings. In the attached image:

Fig. 1 is the structural representation of the upward type fixed bed hydrogenation micro-interface reaction system provided by the embodiment of the present invention;

2 is a schematic structural diagram of an upward-type multi-stage fixed-bed hydrogenation micro-interface reaction system provided by an embodiment of the present invention;

3 is a schematic structural diagram of a descending fixed-bed hydrogenation micro-interface reaction system provided in an embodiment of the present invention;

4 is a schematic structural diagram of a descending multi-stage fixed-bed hydrogenation micro-interface reaction system provided in an embodiment of the present invention.

Detailed ways

In order to make the purpose and advantages of the present invention clearer, the present invention will be further described below with reference to the embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention.

It should be noted that, in the description of the present invention, the terms “upper”, “lower”, “left”, “right”, “inner”, “outer” and other terms indicated in the direction or the positional relationship are based on the drawings. The direction or positional relationship shown is only for the convenience of description, rather than indicating or implying that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present invention.

In addition, it should also be noted that, in the description of the present invention, unless otherwise expressly specified and limited, the terms "installed", "connected" and "connected" should be understood in a broad sense, for example, it may be a fixed connection or a It is a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, or it can be the internal communication between two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.

Referring to FIG. 1 , an upward-type fixed-bed hydrogenation micro-interface reaction system is provided in an embodiment of the present invention. In this system, a micro-interfacial generator (Micro Interfacial Generator, MIG for short) is arranged at the lower part of the fixed-bed reactor, and is used In the process, the hydrogen is broken into microbubbles by the micro-interface generator, and the gas-liquid emulsion formed by mixing the formed microbubbles with the liquid enters the fixed-bed reactor through the lower inlet of the fixed-bed reactor for subsequent reaction, and the mixture after the reaction is completed. It is discharged through the upper outlet of the fixed-bed reactor to form an upward fixed-bed hydrogenation micro-interface reaction system, which includes: a fixed-bed reactor 4, a micro-interface generator, a gas-liquid separation tank 5, a raw material tank, a power mechanism and an inlet Feed preheater; wherein, the raw material tank is connected with the power mechanism to store hydrogen and reaction liquid, and the other end of the power mechanism is connected with the feed preheater to provide power for transporting hydrogen and reaction liquid, and the feed preheater is another One end is connected with the micro-interface reactor to preheat the hydrogen and the reaction liquid to reach the specified temperature. The micro-interface generator is arranged at the lower part of the fixed bed reactor 4 to break the hydrogen into micro-bubbles and separate the gas and liquid. The tank 5 is connected with the micro-interface generator to separate and discharge the reaction products; before the reaction starts, hydrogen and liquid are sent out through the raw material tank, and are sent to the feed preheater by the power provided by the power mechanism. The heater enters into the micro-interface generator after preheating; the micro-interface generator is arranged in the lower part of the fixed bed reactor 4, and in the hydrogenation reaction process, the pressure energy of hydrogen and/or the kinetic energy of the liquid in the reaction process are converted into The surface energy of the hydrogen bubbles breaks the hydrogen into microbubbles, and the microbubbles are mixed with the liquid in the reaction process to form a gas-liquid emulsion, and then the gas-liquid emulsion enters the fixed-bed reactor through the lower inlet of the fixed-bed reactor 4 After the reaction is completed, the product is introduced into the gas-liquid separation tank 5 through the outlet of the upper part of the fixed-bed reactor 4, and then separated through the gas-liquid separation tank 5, and finally discharged.

It can be understood that the specific position of the micro-interface generator is not limited in this embodiment, and it only needs to be arranged at the lower part of the fixed-bed reactor 4 .

Continuing to refer to FIG. 1, the raw material tank includes: a liquid raw material tank 9 and a gas raw material buffer tank 12, wherein the liquid raw material tank 9 and the gas raw material buffer tank 12 are used to store liquid raw materials and gas raw materials respectively; the power mechanism includes: feeding The pump 10 and the compressor 13, wherein the feed pump 10 and the compressor 13 are used to provide power for conveying the liquid raw material and the gaseous raw material respectively; the feed preheater includes: a liquid raw material preheater 11 and a gas raw material preheater 14 , wherein, the liquid raw material preheater 11 and the gas raw material preheater 14 are used to preheat the liquid raw material and the gas raw material respectively; the micro interface generator is provided with a catalyst bed for promoting the reaction of gas-liquid emulsion, including: The liquid-linked micro-interface generator 3 and the pneumatic micro-interface generator 15 are provided. The interface generator 15 is provided with a pneumatic micro-interface generator liquid phase inlet 16 and a pneumatic micro-interface generator gas phase inlet 17; the gas-liquid separation tank 5 is provided with a liquid phase outlet 7 and a gas phase outlet 6; The liquid in 9 is sent to the liquid raw material preheater 11 by the feed pump 10 to provide power for preheating. The inlet 1 enters the gas-liquid linkage type micro-interface generator 3, the other way enters the pneumatic micro-interface generator 15 through the pneumatic micro-interface generator liquid phase inlet 16 of the pneumatic micro-interface generator 15, and the hydrogen in the gas raw material buffer tank 12 passes through The compressor 13 provides power to enter the gas raw material preheater 14 for preheating. After the preheating is completed, the hydrogen gas enters the gas-liquid linkage micro-interface generator 3 through the gas-liquid linkage micro-interface generator gas phase inlet 2 all the way, and the other way passes through the gas-liquid linkage type micro-interface generator. The gas-phase inlet 17 of the pneumatic micro-interface generator enters the pneumatic micro-interface generator 15, and the hydrogen entering the micro-interface generator is broken into micro-bubbles and mixed with the liquid to form a gas-liquid emulsion, and the formed gas-liquid emulsion reacts through the fixed bed The inlet of the lower part of the reactor 4 enters the interior of the fixed-bed reactor 4, and the reaction is fully and completely under the catalytic action of the catalyst. Separation of the gas-liquid separation tank 5, unreacted gas raw materials and other gases generated by the reaction are extracted from the gas-phase outlet 6 of the gas-liquid separation tank 5, and the liquid-phase reaction product is extracted from the liquid-phase outlet 7 of the gas-liquid separation tank 5 , collected separately for subsequent processing.

It can be understood that the number of the fixed-bed reactors 4 is not limited in this example, and only needs to be configured according to the needs of the reaction system; at the same time, the specific positions of the gas-phase outlet 6 and the liquid-phase outlet 7 of the gas-liquid separation tank 5 are not affected. It is limited as long as both of them can discharge gas and liquid. Of course, the present invention is applicable to the catalyst systems already mentioned, but also to other hydrogenation catalyst systems not mentioned. Only when different catalysts are used, the operating temperature will be appropriately adjusted according to the activation temperature of the catalyst, without affecting the reactor of the present invention, which can greatly (or multiply) reduce the operating pressure and increase the space velocity under different catalyst systems. (processing capacity) outstanding advantages.

Please refer to Fig. 2. The difference between this system and the upward fixed bed hydrogenation micro-interface reaction system shown in Fig. 1 is that the system has multiple catalyst beds, and each catalyst bed is provided with a corresponding micro-interface Generators 3, each of the micro-interface generators 3 is connected with the gas raw material preheater 14, and the system can make the reaction more sufficient and more thorough due to more catalyst beds.

Referring to FIG. 3 , a descending fixed-bed hydrogenation micro-interface reaction system is provided in an embodiment of the present invention. In the system, a micro-interfacial generator (Micro Interfacial Generator, MIG for short) is arranged on the upper part of the fixed-bed reactor. During the process, the hydrogen is broken into micro-bubbles by the micro-interface generator, and the gas-liquid emulsion formed by mixing the formed micro-bubbles with the liquid enters the fixed-bed reactor through the upper inlet of the fixed-bed reactor for subsequent reactions. It is discharged through the outlet of the lower part of the fixed bed reactor to form a downward fixed bed hydrogenation micro-interface reaction system. In particular, in this system, in order to ensure that the reactants can fill the fixed-bed reactor 4 during the reaction, the highest point of the outlet connecting pipe should be higher than the fixed-bed reactor 4 . The system includes: a fixed bed reactor 4, a micro-interface generator, a gas-liquid separation tank 5, a raw material tank, a power mechanism and a feed preheater; wherein, the raw material tank is connected with the power mechanism to store hydrogen and reaction liquid, The other end of the power mechanism is connected with the feed preheater to provide power for transporting hydrogen and reaction liquid, and the other end of the feed preheater is connected with the micro-interface reactor to preheat the hydrogen and the reaction liquid to reach the At a specified temperature, the micro-interface generator is arranged on the upper part of the fixed-bed reactor 4 to break the hydrogen into micro-bubbles, and the gas-liquid separation tank 5 is connected with the micro-interface generator to separate and discharge the reaction products; before the reaction starts, The hydrogen and liquid are sent out through the raw material tank, and are transmitted to the feed preheater through the power provided by the power mechanism, and then enter the micro-interface generator after being preheated by the feed pre-heater; the micro-interface generator is arranged in the fixed bed In the upper part of the reactor 4, in the hydrogenation reaction process, the pressure energy of hydrogen and/or the kinetic energy of the liquid in the reaction process are converted into the surface energy of hydrogen gas bubbles, so that the hydrogen gas is broken into microbubbles, and the microbubbles are combined with the reaction process. The liquid is mixed to form a gas-liquid emulsion, and then the gas-liquid emulsion is entered into the fixed-bed reactor 4 through the upper inlet of the fixed-bed reactor 4 to carry out the subsequent reaction, and the product after the reaction is completed passes through the fixed-bed reactor 4. The outlet at the bottom Introduced into the gas-liquid separation tank 5, and then separated by the gas-liquid separation tank 5, and finally discharged.

It can be understood that the specific position of the micro-interface generator is not limited in this embodiment, and it only needs to be arranged at the lower part of the fixed-bed reactor 4 .

Continuing to refer to FIG. 3, the raw material tank includes: a liquid raw material tank 9 and a gas raw material buffer tank 12, wherein the liquid raw material tank 9 and the gas raw material buffer tank 12 are used to store liquid raw materials and gas raw materials respectively; the power mechanism includes: feeding A pump 10 and a compressor 13, wherein the feed pump 10 and the compressor 13 are used to provide power for conveying liquid raw materials and gaseous raw materials respectively; the feed preheater includes: a liquid raw material preheater 11 and a gas raw material preheater 14 , wherein the liquid raw material preheater 11 and the gas raw material preheater 14 are used to preheat the liquid raw material and the gas raw material respectively; the micro interface generator is internally provided with a catalyst bed for promoting the gas-liquid emulsion reaction, which includes: Gas-liquid linkage micro-interface generator 3 and pneumatic micro-interface generator 15, gas-liquid linkage micro-interface generator 3 is provided with gas-liquid linkage type micro-interface generator liquid phase inlet 1 and gas-liquid linkage type micro-interface generator gas phase inlet 2, pneumatic The gas-liquid separation tank 5 is provided with a liquid-phase outlet 7 and a gas-phase outlet 6; before the reaction starts, the liquid raw materials are The liquid in the tank 9 is sent to the liquid raw material preheater 11 by the feed pump 10 for preheating, and the preheated liquid passes through the gas-liquid linkage micro-interface generator liquid of the gas-liquid linkage micro-interface generator 3 all the way. The phase inlet 1 enters the gas-liquid linkage micro-interface generator 3, and the other way enters the pneumatic micro-interface generator 15 through the pneumatic micro-interface generator liquid phase inlet 16 of the pneumatic micro-interface generator 15. The hydrogen in the gas raw material buffer tank 12 The compressor 13 provides power and enters the gas raw material preheater 14 for preheating. After the preheating is completed, the hydrogen gas enters the gas-liquid linkage micro-interface generator 3 through the gas-liquid linkage micro-interface generator gas inlet 2 all the way. Entering the dynamic micro-interface generator 15 through the gas-phase inlet 17 of the pneumatic micro-interface generator, the hydrogen gas entering the micro-interface generator is broken into micro-bubbles and mixed with the liquid to form a gas-liquid emulsion, and the formed gas-liquid emulsion passes through the fixed bed The inlet of the upper part of the reactor 4 enters the interior of the fixed-bed reactor 4, and the reaction is fully and completely under the catalytic action of the catalyst, and the product after the reaction is completed is transferred to the inside of the gas-liquid separation tank 5 through the outlet at the bottom of the fixed-bed reactor 4, Through the separation of the gas-liquid separation tank 5, the unreacted gas raw materials and other gases generated by the reaction are extracted from the gas-liquid separation tank 5 from the gas-phase outlet 6, and the liquid-phase reaction product is extracted from the liquid-phase outlet 7 of the gas-liquid separation tank 5. They are collected separately for subsequent processing.

It can be understood that the number of the fixed bed reactors 4 is not limited in this example, and it only needs to be configured according to the needs of the reaction system. It should be particularly noted that, in order to ensure that the reactants are filled with the fixed bed reactor 4, the highest point of the outlet connecting pipe should be higher than its top. The specific positions of the gas-phase outlet 6 and the liquid-phase outlet 7 of the gas-liquid separation tank 5 are also not limited, as long as both can discharge gas and liquid. Of course, the present invention is applicable to the catalyst systems already mentioned, but also to other hydrogenation catalyst systems not mentioned. Only when different catalysts are used, the operating temperature will be appropriately adjusted according to the activation temperature of the catalyst, without affecting the reactor of the present invention, which can greatly (or multiply) reduce the operating pressure and increase the space velocity under different catalyst systems. (processing capacity) outstanding advantages.

Please refer to Fig. 4. The difference between this system and the downward fixed-bed hydrogenation micro-interface reaction system shown in Fig. 3 is that the system has multiple catalyst beds, and each catalyst bed is provided with a corresponding micro-interface Generators 3, each of the micro-interface generators 3 is connected with the gas raw material preheater 14, and the system can make the reaction more sufficient and more thorough due to more catalyst beds.

Example 1

Fresh hydrogen and gasoline enter the gas-liquid linkage micro-interface generator 3 through the gas-phase inlet 2 of the gas-liquid linkage type micro-interface generator and the liquid phase inlet 1 of the gas-liquid linkage type micro-interface generator respectively at a standard volume ratio of 0.25:1. All the way into the pneumatic micro-interface generator 15 through the gas phase inlet 17 of the pneumatic micro-interface generator and the liquid phase inlet 16 of the pneumatic micro-interface generator respectively at a standard volume ratio of 800:1. Under the action of the gas-liquid linkage micro-interface generator 3 and the pneumatic micro-interface generator 15, the hydrogen is broken into microbubbles with an average diameter of 1μm≤d<1mm, and the gas and liquid are violently mixed to form a gas-liquid emulsion, which enters the fixed bed for reaction The bottom end of the vessel 4 flows from bottom to top, passes through a section of catalyst bed 8, and performs hydrodesulfurization reaction under the action of the catalyst. The reaction product enters the gas-liquid separation tank 5 from the top of the fixed-bed reactor 4, and the unreacted H of the fixed-bed reactor 4 and the H2S generated by the reaction are extracted from the gas-phase outlet 6 of the gas-liquid separation tank. The liquid phase oil is extracted from the liquid phase outlet 7 of the gas-liquid separation tank, and collected separately for subsequent processing.

The reaction pressure in the fixed bed reactor 4 was 3 MPa, and the reaction temperature was 220°C. A molybdenum-nickel catalyst is used in the fixed-bed reactor 4, and the space velocity is controlled to be 0.3h ^-1 . The sulfur content in the raw gasoline is 120 ppm, which is reduced to 20 ppm after being processed by this hydrodesulfurization reaction process.

Embodiment 2

Fresh hydrogen and kerosene enter the gas-liquid linkage micro-interface generator 3 through the gas-phase inlet 2 of the gas-liquid linkage type micro-interface generator and the liquid phase inlet 1 of the gas-liquid linkage type micro-interface generator respectively at a standard volume ratio of 0.3:1. All the way into the pneumatic micro-interface generator 15 through the gas phase inlet 17 of the pneumatic micro-interface generator and the liquid phase inlet 16 of the pneumatic micro-interface generator respectively at a standard volume ratio of 900:1. Under the action of the gas-liquid linkage micro-interface generator 3 and the pneumatic micro-interface generator 15, the hydrogen is broken into micro-bubbles with an average diameter of 1μm≤d<1mm, and the gas and liquid are vigorously mixed to form a gas-liquid emulsion, which enters the fixed bed reactor 4. The top, flowing from top to bottom, passes through a section of catalyst bed 8, and performs hydrodesulfurization reaction under the action of catalyst. The reaction product enters the gas-liquid separation tank 5 from the bottom end of the fixed-bed reactor _{4, and the gases such as the unreacted H of the fixed-bed reactor 4 and the H 2 S} generated by the reaction are extracted from the gas-phase outlet 6 of the gas-liquid separation tank. The liquid-phase oil product after hydrodesulfurization is extracted from the liquid-phase outlet 7 of the gas-liquid separation tank, and collected separately for subsequent processing.

The reaction pressure in the fixed bed reactor 4 was 3 MPa, and the reaction temperature was 250°C. A molybdenum-nickel catalyst is used in the fixed-bed reactor 4, and the space velocity is controlled to be 1.2h ^-1 . The sulfur content in the raw kerosene is 150 ppm, which is reduced to 50 ppm after being processed by this hydrodesulfurization reaction process.

Embodiment 3

Fresh hydrogen and diesel fuel enter the gas-liquid linkage micro-interface generator 3 through the gas-phase inlet 2 of the gas-liquid linkage micro-interface generator and the liquid-phase inlet 1 of the gas-liquid linkage micro-interface generator respectively at a standard volume ratio of 0.2:1. All the way into the pneumatic micro-interface generator 15 through the gas phase inlet 17 of the pneumatic micro-interface generator and the liquid phase inlet 16 of the pneumatic micro-interface generator at a standard volume ratio of 1000:1 respectively. Under the action of the gas-liquid linkage micro-interface generator 3 and the pneumatic micro-interface generator 15, the hydrogen is broken into micro-bubbles with an average diameter of 1μm≤d<1mm, and the gas and liquid are vigorously mixed to form a gas-liquid emulsion, which enters the fixed bed reactor 4. The bottom end flows from bottom to top, passes through a section of catalyst bed 8, and performs hydrodesulfurization reaction under the action of the catalyst. The reaction product enters the gas-liquid separation tank 5 from the top of the fixed-bed reactor 4, and the gases such as the unreacted H of the fixed _- bed reactor ₄ and the H2S generated by the reaction are extracted from the gas-phase outlet 6 of the gas-liquid separation tank. The liquid-phase oil product after hydrodesulfurization is extracted from the liquid-phase outlet 7 of the gas-liquid separation tank, and collected separately for subsequent treatment.

The reaction pressure in the fixed bed reactor 4 is 6MPa, and the reaction temperature is 300°C. The FZC-302 type catalyst is used in the fixed bed reactor 4, and the space velocity is controlled to be 3.0h ^-1 . The sulfur content in the raw kerosene is 220 ppm, which is reduced to 50 ppm after being processed by this hydrodesulfurization reaction process.

It will be appreciated that the present invention is applicable to the catalyst systems already mentioned, as well as to other hydrogenation catalyst systems not mentioned. Only when different catalysts are used, the operating temperature will be appropriately adjusted according to the activation temperature of the catalyst, without affecting the reactor of the present invention, which can greatly (or multiply) reduce the operating pressure and increase the space velocity under different catalyst systems. (processing capacity) outstanding advantages.

In addition, the micro-interface generator can also be used in other multi-phase reaction technical fields to form gas-liquid-solid micro-mixed flow, gas-liquid-solid micro-nano flow, gas-liquid-solid emulsion flow, gas-liquid-solid microstructure flow, multi-phase micro-mixed flow , multi-phase micro-nano flow, multi-phase emulsification flow, multi-phase micro-structure flow, micro-bubble, micro gas-liquid flow, gas-liquid micro-nano emulsion flow, ultra-micro flow, ultra-micro fluidization, micro-dispersed flow, micro-turbulent flow, micro- Bubble flow, micro-nano bubble flow, etc., are multiphase fluids formed by micro-scale particles, or multi-phase fluids formed by micro-nano-scale particles (referred to as micro-interface fluids), which can also be applied to such as micro-bubble mass transfer, micro-bubble Transfer, microbubble reaction, microbubble absorption, microbubble oxygenation, microbubble contact, micromixing, microbubble, microbubble, microfluidization, microbubble fermentation, microbubble bubbling and other reactions, as well as microbubble biochemical reactions In reactors such as reactors and microbubble bioreactors, the mass transfer area of the phase boundary between the gas phase and/or liquid phase and the liquid phase and/or solid phase in the reaction process is effectively increased.

Obviously, the beneficial effect of the present invention is that, in the fixed-bed hydrogenation micro-interface reaction system provided by the present invention, by adding a micro-interface generator to the fixed-bed reaction system, the hydrogen gas is broken into particles with a diameter of 1 μm≦d<1 mm. gas to form a micro-bubble system. The micro-bubbles have the advantages of rigidity, good independence, and not easy to coalesce. In the process of gas-liquid reaction, the gas-liquid reaction is strengthened, and the mass transfer efficiency is improved, so an emulsification containing a large number of micro-bubbles is obtained. liquid, thereby forming a higher phase boundary area in the reactor. Further, by providing a micro-interface generator, the fixed-bed hydrogenation micro-interface reaction system of the present invention has the advantages of high gas utilization rate, high desulfurization rate, low investment, low energy consumption and flexible process in engineering.

So far, the technical solutions of the present invention have been described with reference to the preferred embodiments shown in the accompanying drawings, however, those skilled in the art can easily understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention; for those skilled in the art, the present invention may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims (10)

1. A fixed bed hydrogenation micro-interface reaction system is characterized by comprising: the system comprises a fixed bed reactor, a micro-interface generator and a gas-liquid separation tank; the micro-interface generator is connected with the fixed bed reactor, the pressure energy of hydrogen and/or the kinetic energy of liquid in the reaction process are converted into the surface energy of hydrogen bubbles in the hydrogenation reaction process, the hydrogen bubbles are crushed into micro-bubbles, the micro-bubbles and the liquid are mixed to form a gas-liquid emulsion, and the gas-liquid emulsion enters the fixed bed reactor to perform subsequent reaction; the fixed bed reactor is used as a reaction site of hydrogenation reaction to form a stable gas-liquid reinforced fixed bed reaction system when the gas-liquid emulsion enters the fixed bed reactor; the gas-liquid separation tank is connected with the fixed bed reactor and is used for carrying out gas-liquid separation on the mixture after the reaction in the fixed bed reactor.

2. The fixed bed hydrogenation micro-interface reaction system of claim 1, wherein the micro-interface generator is selected from one or more of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator.

3. The fixed bed hydrogenation micro-interfacial reaction system of claim 1, wherein the micro-interfacial generator is disposed in an upper portion of the fixed bed reactor.

4. The fixed bed hydrogenation micro-interfacial reaction system of claim 1, wherein the micro-interfacial generator is disposed in a lower portion of the fixed bed reactor.

5. The fixed bed hydrogenation micro-interfacial reaction system of claim 1, wherein the fixed bed reactor comprises: a reaction tank and a catalyst bed layer; the reaction tank is a tank body and is used for providing a reaction space for the gas-liquid emulsion, and a mixture outlet used for outputting the reacted mixture is formed in the reaction tank; the catalyst bed is fixed inside the reaction tank, and a catalyst for improving the reaction efficiency of the gas-liquid emulsion is arranged in the catalyst bed.

6. The fixed bed hydrogenation micro-interfacial reaction system of claim 1, further comprising: the device comprises a raw material tank, a power mechanism and a feeding preheater; the raw material tank is connected with the power mechanism and used for storing hydrogen and reaction liquid; the other end of the power mechanism is connected with the feeding preheater and used for providing power for conveying hydrogen and reaction liquid; the other end of the feed preheater is connected with the micro-interface reactor and is used for preheating the hydrogen and the reaction liquid so as to enable the hydrogen and the reaction liquid to reach the specified temperature.

7. The fixed bed hydrogenation micro-interface reaction system of claim 6, wherein the feed tank comprises a liquid feed tank and a gas feed surge tank; wherein the liquid raw material tank is connected with the feeding pump and used for storing the liquid raw material; the gas raw material buffer tank is connected with the compressor and used for storing hydrogen.

8. The fixed bed hydrogenation micro-interface reaction system as claimed in claim 6, wherein the power mechanism comprises: a feed pump and compressor; wherein the feed pump is connected with the liquid feed preheater and used for providing power for conveying liquid raw materials; the compressor is connected with the gas feed preheater and is used for providing power for conveying hydrogen.

9. The fixed bed hydrogenation micro-interfacial reaction system of claim 6, wherein the feed preheater comprises: a liquid feed preheater and a gas feed preheater; the liquid feed preheater is connected with the micro-interface generator and is used for preheating the liquid raw material to a specified temperature and sending the liquid raw material into the micro-interface generator; the gas feed preheater is connected to the micro-interface generator for preheating the hydrogen gas to a specified temperature and feeding it into the micro-interface generator.

10. The fixed bed hydrogenation micro-interface reaction system as claimed in claim 3, wherein the highest of the connecting pipes of the fixed bed reactor is higher than the fixed bed reactor.

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