CN117358440A - Three-phase separator capable of regulating short-circuit flow, ebullated bed hydrogenation reactor and method - Google Patents

Abstract

The invention belongs to the technical field of biomass energy equipment, and particularly discloses a three-phase separator capable of regulating and controlling short-circuit flow, a fluidized bed hydrogenation reactor and a fluidized bed hydrogenation method, which aim at solving the technical problem of how to reduce the adverse effect of the short-circuit flow on an axial liquid inlet type cyclone or a reactor and/or a method using the axial liquid inlet type cyclone. The three-phase separator forms an assembly with an annular overflow structure in the annular overflow pipe and the light liquid guide pipe, so that in the use process, or in the working process of the reactor and/or the method using the three-phase separator, partial fluid separated from the main flow can be drained, the partial fluid is prevented from entering the light liquid guide pipe along the outer wall of the light liquid guide pipe by bypassing the bottom of the side wall of the light liquid guide pipe, and short-circuit flow is formed by escaping from the upper end of the light liquid guide pipe, the regulation and control of the short-circuit flow are realized, the adverse effect of the short-circuit flow can be effectively reduced, the separation precision and efficiency are ensured, and the escaping or the escaping loss of catalyst micro powder is reduced.

Description

Three-phase separator capable of regulating short-circuit flow, ebullated bed hydrogenation reactor and method

Technical Field

The invention belongs to the technical field of biomass energy equipment, and particularly relates to a three-phase separator capable of regulating and controlling short-circuit flow, a fluidized bed hydrogenation reactor and a fluidized bed hydrogenation method.

Background

The ebullated bed hydrogenation reactor is a device for realizing the mixing, mass transfer and heat transfer between solid particles and gas phase and liquid phase, and is a common reactor in industry. Since the development of the reactor, the reactor is mainly used for processing high sulfur, high nitrogen, high metal (nickel and vanadium), poor heavy residual oil with high asphaltene content, coal tar or biomass oil produced by coal pyrolysis, and the like which are difficult to process in the traditional technology, and is widely applied to petrochemical industry and new energy manufacturing industry. The advantages of ebullated bed hydrogenation reactors can be summarized as follows: (1) the adaptability of the raw materials is strong; (2) the reaction rate is high; (3) the operation condition is flexible; (4) the catalyst can be replaced on line, and the product quality is relatively stable; (5) the internal temperature difference is small, so that local overheating is avoided, and the bed pressure is reduced; (6) the device has long running time.

Review the recent decades of commercial development history of ebullated bed hydrogenation reactors, and can be categorized into two major categories, the expanded bed regime and the full mixed flow ebullated bed regime, depending on the state of catalyst fluidization within the reactor. The ebullated bed hydrogenation reactor in the expanded bed state is mainly based on foreign H-Oil and LC-Fining technologies and derivative technologies thereof; the gas-liquid-solid mixed flow boiling bed type hydrogenation reactor is represented by domestic petrochemical 'STRONG' technology. The functional requirements for the separators arranged in ebullated bed hydrogenation reactors are also quite different, due to the different fluidization conditions of the catalysts inside the two types of reactors. For the ebullated bed hydrogenation reactor in the expanded bed state, after the internal catalyst bed layer is expanded to a certain height, the upper part of the reactor is a sedimentation zone of catalyst particles, and a gas-liquid two-phase product without solid particles is obtained, so that the requirement on a separator arranged in the reactor is to perform gas-liquid two-phase separation; for a gas-liquid-solid total mixed flow ebullated bed type hydrogenation reactor, the space from the distribution plate to the height of the material surface of the reactor is a gas-liquid-solid three-phase mixture, so that the gas-liquid-solid three-phase separation is required for the separator arranged in the reactor.

In the case of ebullated bed hydrogenation reactors in the expanded bed state, for example: U.S. patent application US20170081599A1 discloses a ebullated bed hydrogenation reactor that can control the reaction rate by a circulation channel in the center of the reactor and a circulation cup at the top to keep the heat released by the reaction at a safe level; also for example: chinese patent No. CN103102930B discloses a ebullated bed hydrogenation reactor, which can effectively improve the mass transfer efficiency of gas-liquid two phases through a circulation cup at the upper part and a circulation pipeline at the lower part in the reactor cylinder; similarly, in order to improve the mass transfer efficiency of the gas-liquid two phases, chinese patent No. CN103100356B discloses a ebullated bed hydrogenation reactor, in which a rotatable centrifugal impeller is disposed in a circulation line at the lower part of the reactor cylinder. In summary, it can be found that the ebullated bed hydrogenation reactor in the expanded bed state actively controls the flow of the gas-liquid two phases entering the reactor, indirectly controls the expansion height of the catalyst bed, realizes the separation of the gas-liquid two phases and the catalyst particles in the settling zone at the upper part of the bed, and adopts a circulating cup and a circulating channel at the upper part of the reactor cylinder body, thereby realizing the separation of the gas-liquid two phase products, and further meeting the production requirements. However, such reactors suffer from the following disadvantages: (1) low reactor space utilization. The sedimentation area of catalyst particles is needed to be reserved in the expanded bed state, so that the effective utilization space in the reactor is less; and (2) the mass transfer resistance of the catalyst is large, and the conversion rate is low. The separation of the catalyst particles in the expanded bed state is completely settled by the gravity of the catalyst, so that the granularity of the catalyst filler is larger, the mass transfer process of the catalyst is influenced, and the conversion rate is low; (3) Catalyst particles are easy to coke, and the operation period of the reactor is short. Because the gas phase and the liquid phase are separated by the circulating cup at the upper part of the reactor in the state of the expanded bed, the separation strength is smaller, the separation time is longer, and the liquid phase product is easy to coke with the fine particle catalyst in the sedimentation zone. Therefore, under the conditions of increasingly complicating and inferior oil products, the reactor in the gas-liquid-solid fully mixed flow state is the development direction of the fluidized bed hydrogenation reactor in the future.

In the aspect of the fluidized bed hydrogenation reactor in a gas-liquid-solid fully mixed flow state, the technology of petroleum and chemical industry and the derivative technology thereof are represented in China, and the fluidized bed hydrogenation reactor is mainly characterized in that a three-phase separator with a three-layer or multi-layer concentric sleeve structure is arranged at the top of the reactor, and three-phase separation is mainly realized by baffling sedimentation, for example: the Chinese patent application CN1448212A only depends on the gravity action of the catalyst particles and cannot be disturbed by external fluid, and has certain limitation on the fluidization operation. Then, in order to optimize gravity sedimentation conditions, a Z-shaped baffle structure is arranged between an inner support cylinder and an outer support cylinder on the basis of CN1448212A in the Chinese patent application CN 108114510A; the Chinese patent application CN101721960A is characterized in that the concentric inner cylinder and the outer cylinder are designed into a structure with an inverted cone at the upper part and a positive cone at the lower part; in addition, on the basis of CN1448212A, a diamond-shaped diversion cone is arranged below the three-phase separator in the Chinese patent application CN 101721961A. Said invented patent application optimizes the separation condition to different extent, but its substantial separation principle still depends on baffling sedimentation, and separation efficiency and accuracy are limited by operation condition of reactor.

In order to solve the problems, researchers at the university of eastern China have conducted extensive and intensive studies, and then introduced the reinforced separation methods such as cyclone separation and guide vane separation into the design of the ebullated bed hydrogenation reactor in a fully mixed flow state. For example: the invention patent CN113083169B discloses a fluidized bed hydrogenation reactor and a use method thereof, wherein the fluidized bed hydrogenation reactor strengthens gas-liquid-solid three-phase separation in a gas-liquid-solid three-phase cyclone separator and internal components thereof which are arranged in the upper space of the reactor by cyclone separation, sieve mesh separation and guide vane separation methods; for another example: the invention discloses a fluidized bed hydrogenation reactor and a use method thereof, wherein a baffle plate arranged in the upper space of the reactor and a gas-liquid-solid three-phase cyclone separator connected with the baffle plate are utilized to strengthen the gas-liquid-solid three-phase separation by cyclone separation, baffle separation and guide vane separation methods; also for example: the invention discloses a fluidized bed hydrogenation reactor and a use method thereof, wherein a gas-liquid-solid three-phase cyclone separator and internal components thereof arranged in the upper space of the reactor are utilized to strengthen the gas-liquid-solid three-phase separation by cyclone separation and guide vane separation methods. Said invention mainly uses cyclone separation mode to intensify gas-liquid-solid three-phase separation in the reactor, and compared with baffle sedimentation method it has the advantages of large operation elasticity and high separation strength; however, because the upper end of the overflow pipe is of an opening structure, and the overflow pipe is sleeved on the periphery of the liquid-falling type liquid-phase product eduction pipe, the upper end of the liquid-falling type liquid-phase product eduction pipe is lower than the upper end of the overflow pipe, and therefore, the phenomenon of short-circuit flow can be inevitably generated in the operation process of the three-phase cyclone separator. The short-circuit flow is formed by that after fluid enters the three-phase cyclone separator along the axial inlet due to the viscous action of the wall surface boundary layer, the speed of the boundary layer fluid is low due to the viscous force of the wall surface, and the generated centrifugal force is insufficient, so that part of the fluid escapes without participating in separation, namely, part of the fluid separated from the main flow directly escapes along the outer wall of the liquid-falling type liquid-phase product eduction tube, bypasses the bottom of the liquid-falling type liquid-phase product eduction tube and is formed by the upper end of the overflow tube, and is opposite to the fluid entering the three-phase cyclone separator along the axial direction. The existence of short-circuit flow can cause problems such as reduction of separation precision and separation efficiency, escape or running loss of catalyst micro powder and the like.

In the research of improving short-circuit flow in a three-phase cyclone separator, researchers mainly reduce the influence of the short-circuit flow on separation efficiency by changing a motion path. For example: chinese patent No. CN211937451U discloses a cyclone with a short-circuit flow suppressing structure, which is provided with a short-circuit flow suppressing component below a top cap of a cylinder at an upper end of the cylinder, and improves classification efficiency by changing an internal short-circuit flow path of the cyclone through the suppressing component. Similarly, chinese patent No. CN106475238B discloses a cyclone separator for suppressing top short-circuit flow, which is provided with a protrusion structure on the top plate of the barrel section to limit the flow rate of the top plate short-circuit flow, thereby improving the separation efficiency. The above patents are all solutions proposed by changing the short-circuit flow motion path to reduce the adverse effect, and are all solutions proposed by the cyclone structure based on the tangential inlet, but the axial liquid inlet type cyclone is different from the tangential liquid inlet type cyclone short-circuit flow forming mechanism, so that no related prior art is proposed at present.

In view of the foregoing, in order to reduce the adverse effects of short-circuit flow on the separation strength and separation efficiency of the ebullated bed hydrogenation reactor in the gas-liquid-solid fully mixed flow state during the operation of the three-phase cyclone separator, and reduce the escape or run-out behavior of the catalyst fines, there is a strong need in the art to develop a three-phase separator and ebullated bed hydrogenation reactor and method that overcome the above-mentioned technical drawbacks.

Disclosure of Invention

The invention provides a three-phase separator capable of regulating and controlling short-circuit flow, a fluidized bed hydrogenation reactor and a fluidized bed hydrogenation method, and aims to solve the technical problem of how to reduce the adverse effect of the short-circuit flow on an axial liquid inlet type cyclone or a reactor and/or a method using the axial liquid inlet type cyclone.

The technical scheme adopted for solving the technical problems is as follows: the three-phase separator capable of regulating short-circuit flow comprises a separator main body, an annular gap overflow pipe, a rotational flow guide blade, a light liquid guide pipe, a liquid-solid mixed phase product eduction pipe and a liquid phase product eduction pipe;

the separator body comprises a straight barrel section;

the annular gap overflow pipe and the straight barrel section are coaxially arranged, the lower end of the annular gap overflow pipe extends into the inner cavity of the straight barrel section, and the upper end of the annular gap overflow pipe is higher than the upper end of the straight barrel section;

the swirl guide vane is arranged in an annular gap channel between the straight cylinder section and the annular gap overflow pipe;

the light liquid guide pipe and the annular gap overflow pipe are coaxially arranged;

the liquid-solid mixed phase product eduction tube is arranged on a tube section of the annular gap overflow tube outside the straight tube section and is communicated with the inner cavity of the annular gap overflow tube through a liquid-solid inlet of the liquid-solid mixed phase product eduction tube;

the lower end of the light liquid guide pipe extends into the inner cavity of the annular gap overflow pipe, and the upper end of the light liquid guide pipe is higher than the upper end of the annular gap overflow pipe; a closed structure is arranged between the light liquid guide pipe and the upper end of the annular gap overflow pipe;

The liquid-phase product eduction tube is arranged on the tube section of the light liquid guide tube outside the annular overflow tube and is communicated with the inner cavity of the light liquid guide tube through the liquid-phase inlet of the liquid-phase product eduction tube.

Further, the three-phase separator also comprises a non-return cone;

the separator body further comprises a cone section and a underflow pipe;

the straight cylinder section, the conical cylinder section and the underflow pipe are sequentially and coaxially connected together from top to bottom;

the non-return cone is arranged at the bottom flow port at the lower end of the bottom flow pipe.

Further, the inner diameter Da of the annular gap overflow pipe is 75-95% of the inner diameter D of the straight cylinder section, and the height of the annular gap overflow pipe is 50-130% of the height of the light liquid guide pipe;

the inclination angle theta of the cyclone guide vane is 45-65 degrees;

the inner diameter Do of the light liquid guide pipe is 70-90% of the inner diameter Da of the annular gap overflow pipe, and the height of the light liquid guide pipe is 100-150% of the height of the straight cylinder section;

the included angle alpha between the bus of the cone section and the axis of the cone section is 10-25 degrees.

Further, the lower end of the light liquid guide pipe is higher than the lower end of the straight cylinder section;

the axis of the liquid-solid mixed phase product eduction tube is mutually perpendicular to the axis of the annular gap overflow tube;

the axis of the liquid phase product eduction tube is mutually perpendicular to the axis of the light liquid flow guide tube.

The invention also provides a fluidized bed hydrogenation reactor, which comprises a pressure-bearing shell and a gas-liquid-solid three-phase separator arranged at the upper part of the inner cavity of the pressure-bearing shell;

the top of the pressure-bearing shell is provided with a gas phase outlet, and the bottom of the pressure-bearing shell is provided with a gas-liquid mixed phase inlet;

the gas-liquid-solid three-phase separator is the three-phase separator capable of regulating and controlling short-circuit flow;

the liquid-solid mixed phase product eduction tube and the liquid phase product eduction tube are penetrated out from the side wall of the pressure-bearing shell.

Further, the height difference between the liquid-solid mixed phase product eduction tube and the liquid phase product eduction tube is h1, and h1 is 40-90% of the inner diameter Dn of the pressure-bearing shell;

the inner diameter of the liquid-solid mixed phase product leading-out pipe is equal to the inner diameter of the liquid phase product leading-out pipe.

Further, the inner diameter D of the straight cylinder section is 50-90% of the inner diameter Dn of the pressure-bearing shell, and the height of the straight cylinder section is 3-10% of the tangential height of the pressure-bearing shell;

the height difference between the upper end of the straight cylinder section and the upper end of the light liquid guide pipe is h2, and h2 is 60-100% of the inner diameter Dn of the pressure-bearing shell;

the height difference between the upper end of the light liquid guide pipe and the upper end of the annular gap overflow pipe is h3, and h3 is 10-60% of the inner diameter Dn of the pressure-bearing shell;

The height difference between the upper end of the light liquid guide pipe and the axis of the liquid product eduction pipe is h4, and h4 is 5-20% of the inner diameter Dn of the pressure-bearing shell.

The invention also provides a fluidized bed hydrogenation reaction method, which adopts the fluidized bed hydrogenation reactor to carry out reaction, and comprises the following steps:

step one, cyclone degassing: loading the gas-liquid-solid three-phase mixture into a fluidized bed hydrogenation reactor for reaction, and under the fluidization effect of the fluidized bed hydrogenation reactor, breaking the large bubbles under the inertia effect and continuing to move upwards to be discharged from a gas phase outlet; the residual gas phase, liquid phase and catalyst particles enter a gas-liquid-solid three-phase separator from the upper end of an annular gap channel between a straight cylinder section and an annular gap overflow pipe, a centrifugal force field is formed by the drainage effect of a rotational flow guide blade, small bubbles move towards the center of a light liquid guide pipe under the effect of the centrifugal force field and continue to upwards along the light liquid guide pipe, enter the inner cavity top space of a pressure-bearing shell from the upper end of the light liquid guide pipe, and are discharged from a gas phase outlet; part of liquid phase close to the center of the light liquid guide pipe moves upwards along the light liquid guide pipe under the action of internal rotational flow, and is finally discharged from the liquid phase product eduction pipe as liquid phase product;

Step two, primary rotational flow solid removal: the catalyst particles with large particle size in the first step are thrown to the side wall of the gas-liquid-solid three-phase separator under the action of a centrifugal force field, move downwards along the cone section and the underflow pipe, and finally return to the inner cavity of the pressure-bearing shell from the underflow port at the lower end of the underflow pipe to continue to react; catalyst particles or powder with smaller particle size and partial liquid phase substances move upwards through an annular space between the annular space overflow pipe and the light liquid flow guide pipe under the action of the swirling flow field, and are finally discharged from the liquid-solid mixed phase product eduction pipe as liquid-solid mixed phase products.

Further, the method also comprises the step three:

step three, secondary rotational flow solid removal: and (3) continuously moving the liquid-solid mixed phase product out of the ebullated bed hydrogenation reactor along a liquid-solid mixed phase product outlet pipe and a liquid-solid mixed phase product circulating pipe connected to a liquid-solid outlet of the liquid-solid mixed phase product outlet pipe, further removing solids in a secondary cyclone connected to the lower end of the liquid-solid mixed phase product circulating pipe, and further removing solids to obtain a clean liquid phase product which enters the bottom of an inner cavity of the pressure-bearing shell along a cyclone guide pipe connected to the secondary cyclone and enters the upper part of the inner cavity of the pressure-bearing shell under the action of a gas-liquid distributor to continuously participate in reaction.

Further, the particle size range of the catalyst particles is 0.04-0.1 mm;

the particle size range of the large-particle-size catalyst particles is 0.07-0.1 mm;

the smaller particle size catalyst particles or powders have a particle size of less than 0.07mm;

at least two ebullated bed hydrogenation reactors are connected in series in a grading way;

the liquid phase outlet of the liquid phase product eduction tube of the ebullated bed hydrogenation reactor is connected with the gas-liquid mixed phase inlet of the ebullated bed hydrogenation reactor at the next stage through a pipeline;

the liquid level difference h5 between any two adjacent two-stage ebullated-bed hydrogenation reactors is greater than the on-way drag loss +0.5m.

The beneficial effects of the invention are as follows:

(1) According to the three-phase separator provided by the invention, the lower end of the light liquid guide pipe extends into the inner cavity of the annular overflow pipe, the upper end of the light liquid guide pipe is higher than the upper end of the annular overflow pipe, and a closed structure is arranged between the light liquid guide pipe and the upper end of the annular overflow pipe, so that the annular overflow pipe and the light liquid guide pipe form a component with an annular overflow structure in the three-phase separator; in the using process of the three-phase separator or the reactor and/or the method using the three-phase separator, small bubbles can move towards the center of the light liquid guide pipe under the action of a centrifugal force field, continuously upwards move along the light liquid guide pipe, are discharged from the upper end of the light liquid guide pipe, and are finally discharged from the gas phase outlet; meanwhile, catalyst particles or powder with smaller particle sizes and partial liquid phase substances can move upwards through an annular space between the annular space overflow pipe and the light liquid flow guide pipe under the action of the swirling flow field, and are finally discharged through a liquid-solid mixed phase product eduction pipe; in addition, the liquid-phase product eduction tube is arranged on the tube section of the light liquid guide tube outside the annular overflow tube, and is communicated with the inner cavity of the light liquid guide tube through the liquid-phase inlet of the liquid-phase product eduction tube, so that part of light liquid near the center of the light liquid guide tube moves upwards along the light liquid guide tube under the action of internal rotational flow, and is finally discharged from the liquid-phase product eduction tube; therefore, the three-phase separator or the reactor and/or the method using the three-phase separator can drain partial fluid separated from the main flow, prevent the partial fluid from entering the light liquid guide pipe along the outer wall of the light liquid guide pipe by bypassing the bottom of the side wall of the light liquid guide pipe, and form a short-circuit flow by escaping from the upper end of the light liquid guide pipe, thereby realizing the regulation and control of the short-circuit flow, effectively reducing the adverse effect of the short-circuit flow, ensuring the separation precision and efficiency and reducing the escape or the running loss of the catalyst micro powder.

(2) The annular overflow pipe and the light liquid guide pipe form an assembly with an annular overflow structure in the three-phase separator, the internal flow field distribution of the three-phase separator can be improved, the range of a zero-axis speed envelope surface is enlarged, most of catalyst particles move downwards without escaping, and meanwhile, the intensity of turbulent flow in the three-phase separator is increased, so that the separation precision and the separation efficiency of the three-phase separator are further improved, and the separation effect is enhanced.

(3) According to the fluidized bed hydrogenation reaction method provided by the invention, the liquid-solid mixed phase product flowing into the annular space between the annular space overflow pipe and the light liquid guide pipe can be discharged out of the fluidized bed hydrogenation reactor through the liquid-solid mixed phase product eduction pipe, and is conveyed into an external secondary cyclone through the liquid-solid mixed phase product circulating pipe to further remove solids, so that the catalyst micro powder in the fluidized bed hydrogenation reaction method can be removed, the catalyst micro powder is prevented from being coked and adhered to the flowing wall surface of the fluidized bed hydrogenation reaction method, the wall surface corrosion and the catalyst deactivation are caused, and the removal and regeneration of the catalyst micro powder are realized.

(4) The particle size range of the catalyst particles which can be added in the ebullated bed hydrogenation reactor and the method is between 0.04 and 0.1mm, and compared with the existing ebullated bed hydrogenation reactor, the particle size of the catalyst which can be added is smaller, the specific surface area is larger, and the reaction rate is higher; in addition, the fluidized bed hydrogenation reaction method further removes solids through the secondary cyclone, so that the coking phenomenon of the catalyst micropowder can be avoided, and the clean liquid phase substance obtained after the further removal of solids can continuously participate in the reaction.

Drawings

FIG. 1 is a schematic three-dimensional schematic of a three-phase separator of the present invention with controllable short-circuit flow;

FIG. 2 is a schematic diagram of a three-phase separator with controllable short-circuit flow in partial cutaway according to the present invention;

FIG. 3 is a schematic view of a boiling bed hydrogenation reactor in partial cutaway configuration according to the present invention;

FIG. 4 is a schematic diagram of the operation state of the present invention for regulating short-circuit flow;

FIG. 5 is a schematic diagram of the structure of two ebullated bed hydrogenation reactors used in series in a cold die experiment in example 1 of the present invention;

FIG. 6 is a schematic diagram of the structure of the two ebullated bed hydrogenation reactors used in series in the embodiment 2 of the present invention applied to hydrodeoxygenation of 50 ten thousand tons/year of straw pyrolysis liquid;

marked in the figure as: straight section 1, annular gap overflow pipe 2, cyclone guide vane 3, light liquid guide pipe 4, liquid-solid mixed phase product guide pipe 5, liquid phase product guide pipe 6, conical section 7, underflow pipe 8, non-return cone 9, connecting bracket 10, closed structure 11, gas phase outlet 21, gas-liquid-solid three-phase separator 22, pressure-bearing shell 23, gas-liquid distributor 24, gas-liquid mixed phase inlet 25, secondary cyclone 26, liquid-solid mixed phase product circulation pipe 27, cyclone guide pipe 28, air compressor 41, first ebullated bed hydrogenation reactor 42-1, second ebullated bed hydrogenation reactor 42-2, liquid phase product feed pipe 43, circulation tank 44, water pump 45, first secondary cyclone 46, first booster pump 47, second secondary cyclone 48, second booster pump 49, heating furnace 51, third ebullated bed hydrogenation reactor 52-1, fourth ebullated bed hydrogenation reactor 52-2, separator 53, air cooler 54, third secondary cyclone 55, third booster pump 56, fourth secondary cyclone 57, and cushion feeder 58.

Detailed Description

The invention is further described below with reference to the drawings and examples.

First, it should be noted that the term "about" as used herein means ±10%; the terms "comprising," "including," "having," and variations thereof mean "including but not limited to"; the terms "upper," "lower," "top," "bottom," "inner," "outer," and the like are used for convenience of description only and are not to be construed as limiting the invention, as the means or elements referred to must have, be constructed or operated in a particular orientation; the term "plurality" when referring to a number, generally refers to a number of three or more, for example: "plurality" generally refers to three or more; the term "light liquid" or "liquid product" refers to liquid phase materials that carry less to the catalyst, such as: the amount of catalyst carried out for 0.04mm is 0.9 [ mu ] g/g or less, the amount of catalyst carried out for 0.08mm is 0.4 [ mu ] g/g or less, and the amount of catalyst carried out for 0.1mm is 0; the terms "large bubbles" and "small bubbles" are two relative concepts, "large bubbles" generally mean bubbles that are able to collapse under the influence of inertia, typically over 5mm in diameter, before a gas-liquid-solid three-phase mixture enters a gas-liquid-solid three-phase separator; "small bubbles" refers to other bubbles of the gas-liquid-solid three-phase mixture that are not "large bubbles"; the term "catalyst micropowder" refers to a powder having a smaller particle diameter, which is formed by the action of cyclone shearing or collision with a wall surface during the reaction, and the particle diameter of the catalyst micropowder is usually 30 μm or less; the expression "consisting essentially of or consisting of … …" is to be interpreted as also containing structural elements not mentioned in this sentence; the term "and/or" is merely an association relationship describing an associated object, meaning that three relationships may exist, for example: a and/or B may represent: a exists alone, A and B exist together, and B exists alone. Furthermore, the terms "first," "second," "third," "fourth," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.

The word "optionally" as used herein means "provided in some embodiments and not provided in other embodiments. Any particular embodiment of the invention may include a plurality of "optional" features unless such features conflict. All percentages and parts herein indicating the amount of a substance are by weight unless otherwise indicated.

Referring to fig. 1 and 2, the three-phase separator capable of regulating short-circuit flow comprises a separator main body, an annular gap overflow pipe 2, a rotational flow guide blade 3, a light liquid guide pipe 4, a liquid-solid mixed phase product eduction pipe 5, a liquid phase product eduction pipe 6 and a non-return cone 9;

the three-phase separator is usually arranged at the upper part of the inner cavity of the pressure-bearing shell 23 of the ebullated bed hydrogenation reactor for use;

the separator body is a body part of the three-phase separator and generally comprises a straight cylinder section 1, a cone cylinder section 7 and an underflow pipe 8 which are coaxially connected together in sequence from top to bottom;

the annular gap overflow pipe 2 is coaxially arranged with the straight barrel section 1, the lower end of the annular gap overflow pipe extends into the inner cavity of the straight barrel section 1, and the upper end of the annular gap overflow pipe is higher than the upper end of the straight barrel section 1;

the swirl guide vanes 3 are arranged in an annular gap channel between the straight cylinder section 1 and the annular gap overflow pipe 2; the swirl guide vanes 3 are mainly used for spirally guiding a gas-liquid-solid three-phase mixture entering from the upper end of the annular gap channel, providing required centrifugal force for phase separation, and realizing acceleration and rotation movement of fluid and catalyst particles; the swirl guide vanes 3 are generally arranged on the inner wall surface of the straight barrel section 1 and/or the outer wall surface of the annular gap overflow pipe 2 at a certain inclined angle, and the swirl guide vanes 3 are generally arranged in two or more blocks and distributed in an annular array in the annular gap channel around the axis of the straight barrel section 1; the structure of the swirl guide vane 3 can be various, and is preferably a spiral vane so as to realize better swirl guide effect;

The liquid-solid mixed phase product eduction tube 5 is arranged on the tube section of the annular gap overflow tube 2 outside the straight tube section 1 and is communicated with the inner cavity of the annular gap overflow tube 2 through a liquid-solid inlet thereof; the liquid-solid mixed phase product eduction tube 5 is used for guiding and discharging the liquid-solid mixed phase product outwards;

the non-return cone 9 is arranged at a bottom flow port at the lower end of the bottom flow pipe 8, and a gap for discharging large-particle-diameter catalyst particles, liquid phase and other substances is reserved between the non-return cone and the bottom flow port; the non-return cone 9 is mainly used for preventing gas-liquid-solid three-phase mixture and substances such as large-particle-size catalyst particles and liquid phase discharged from a bottom flow port at the lower end of the bottom flow pipe 8 from entering the three-phase separator from the bottom flow port at the lower end of the bottom flow pipe 8; the non-return cone 9 is generally arranged at the bottom flow port through a connecting bracket 10, and the structure of the non-return cone can be various, and is preferably a spindle-shaped structure; the non-return cone 9 is more preferably a spindle-shaped structure with an upper cone angle of 15-150 ° and a lower cone angle greater than the upper cone angle;

the light liquid guide pipe 4 and the annular gap overflow pipe 2 are coaxially arranged, the lower end of the light liquid guide pipe extends into the inner cavity of the annular gap overflow pipe 2, and the upper end of the light liquid guide pipe is higher than the upper end of the annular gap overflow pipe 2; a closed structure 11 is arranged between the light liquid guide pipe 4 and the upper end of the annular gap overflow pipe 2; the sealing structure 11 may be a structure part integrated with the annular space overflow pipe 2 and/or the light liquid guide pipe 4, or may be a sealing member arranged between the annular space overflow pipe 2 and the light liquid guide pipe 4; so, can make annular space overflow pipe 2 and light liquid honeycomb duct 4 form the assembly with annular space overflow structure in the three-phase separator, and this annular space overflow structure has annular space that the upper end is closed and communicates with liquid-solid mixed phase product eduction tube 5, and discharge the small bubble and guide the vertical overflow channel of the light liquid outside; so that the three-phase separator can make small bubbles move towards the center of the light liquid guide pipe 4 under the action of a centrifugal force field and continuously upwards along the light liquid guide pipe 4 in the use process or in the working process of a reactor and/or a method using the three-phase separator, and the small bubbles are discharged from the upper end of the light liquid guide pipe 4 and can be finally discharged from the gas phase outlet 21; meanwhile, catalyst particles or powder with smaller particle sizes and partial liquid phase substances can move upwards through an annular space between the annular space overflow pipe 2 and the light liquid flow guide pipe 4 under the action of the swirling flow field, and are finally discharged through the liquid-solid mixed phase product outlet pipe 5; therefore, the formed annular overflow structure can drain part of fluid separated from the main flow, prevent the part of fluid from entering the light liquid guide pipe 4 along the outer wall of the light liquid guide pipe 4 by bypassing the bottom of the side wall of the light liquid guide pipe 4, and escape from the upper end of the light liquid guide pipe 4 to form a short-circuit flow, so that the effective regulation and control of the short-circuit flow are realized;

The liquid-phase product eduction tube 6 is arranged on a tube section of the light liquid guide tube 4 outside the annular gap overflow tube 2 and is communicated with the inner cavity of the light liquid guide tube 4 through a liquid-phase inlet thereof; the liquid product eduction tube 6 is mainly used for educing and discharging the light liquid overflowed by the light liquid flow guide tube 4; in the working process, the liquid phase product eduction tube 6, the light liquid guide tube 4 and the annular overflow tube 2 together enable part of liquid phase (light liquid) close to the center of the light liquid guide tube 4 to move upwards along the light liquid guide tube 4 under the action of internal rotational flow, and finally, the liquid phase product eduction tube 6 is discharged.

Referring to fig. 4, the process of regulating the short-circuit flow by the three-phase separator or the reactor and/or the method using the three-phase separator is as follows: the gas-liquid-solid three-phase mixture moves upwards along the axial direction of the reactor, the gas phase mainly composed of large bubbles continues to move upwards under the action of inertia through a channel between the three-phase separator and the wall of the reactor, and when the fluidization liquid level exceeds the straight barrel section 1 of the three-phase separator, the rest gas phase, liquid phase and catalyst particles enter the three-phase separator through an annular gap channel between the straight barrel section 1 of the three-phase separator and an annular gap overflow pipe 2, as shown by an arrow at A in fig. 4; the gas-liquid-solid three phases form a centrifugal force field through the drainage effect of the cyclone guide vane 3, the fluid flow velocity near the wall surface is reduced due to the viscous force of the annular gap channel wall surface, the received centrifugal force is reduced, and the fluid can form short-circuit flow in the past; because the lower end of the light liquid guide pipe 4 extends into the inner cavity of the annular gap overflow pipe 2, the upper end of the light liquid guide pipe is higher than the upper end of the annular gap overflow pipe 2, and a closed structure 11 is arranged between the light liquid guide pipe 4 and the upper end of the annular gap overflow pipe 2, an annular gap overflow structure capable of regulating and controlling short-circuit flow is formed, and the short-circuit flow can be led out of the reactor from the liquid-solid mixed phase product eduction pipe 5 through the annular gap overflow structure, as shown by an arrow at B in fig. 4; the mixture, which consists mainly of large particle size catalyst, continues to rotate down the cone section 7 and the underflow pipe 8 to effect separation, as indicated by the arrow at C in fig. 4.

In a preferred embodiment of the invention, as shown in connection with fig. 2 and 4, the inner diameter Da of the annular overflow pipe 2 is optionally 75-95% of the inner diameter D of the straight section 1; therefore, the gas-liquid-solid three-phase mixture entering the three-phase separator can be ensured to generate enough centrifugal force under the flow guiding action of the rotational flow guide vanes 3 in the annular space channel, and meanwhile, the flow guiding quantity during annular space overflow is ensured; the inner diameter Da of the annular overflow pipe 2 is preferably 85% of the inner diameter D of the straight section 1. Optionally, the height of the annular gap overflow pipe 2 is 50-130% of the height of the light liquid guide pipe 4, so that the short-circuit flow in the three-phase separator is guided by an annular gap overflow structure formed by the annular gap overflow pipe 2 and the light liquid guide pipe 4; the height of the annular overflow pipe 2 is preferably set to 80% of the height of the light liquid guide pipe 4, and the short-circuit flow rate can be set to 0.

Considering that the inclination angle theta of the swirl guide vanes 3 is a main influencing factor for generating centrifugal force, the tangential velocity of the fluid is determined; the inclination angle of the swirl guide vane 3 is represented by an included angle between a tangent line of the ventral surface of the swirl guide vane 3 and the axis of the straight barrel section 1; the inclination angle is smaller than 45 degrees, so that the axial speed of the fluid is increased, the tangential speed is reduced, and the basic centrifugal force condition required by the separation of the catalyst particles can not be met; the inclination angle is larger than 65 degrees, so that the axial speed of the fluid is reduced, the tangential speed is increased, the separation condition of catalyst particles is achieved, but the integral pressure drop of the reactor is increased, and the energy consumption is increased; therefore, the swirl guide vanes 3 are preferably provided at an inclination angle of 45 to 65 °. The inclination angle θ of the swirl vane 3 is more preferably 50 °, 55 °, 60 °.

On the basis of the above, the swirl guide vanes 3 are preferably arranged at an inclination angle of 55 °; thus, the separation efficiency of the three-phase separator can be more than 99.2%, the amount of the catalyst with the particle size of 0.04mm is less than or equal to 0.9 mug/g, the amount of the catalyst with the particle size of 0.08mm is less than or equal to 0.4 mug/g, and the amount of the catalyst with the particle size of 0.1mm is 0; the pressure drop was 70kPa.

Considering that the gas content and the catalyst particle ratio are about 30-40% and the liquid phase ratio is about 60-70% at the lower part of the inner cavity of the straight barrel section 1 in the working process, the gas phase ratio is reduced in the upward fluidization process, the catalyst particles are collected, the liquid phase ratio is increased, and the liquid velocity in the light liquid guide pipe 4 is required to be reduced in order to prevent the liquid phase from flowing upward at the same speed to carry catalyst particles and escaping, so that the inner diameter Do of the light liquid guide pipe 4 is limited to be 70-90% of the inner diameter Da of the annular overflow pipe 2 and is larger than the highest ratio of the liquid phase, so that the purpose of reducing the real liquid velocity of the liquid phase is achieved, and the probability of the liquid phase carrying catalyst particles or micro powder is effectively reduced.

In addition to the above, the inner diameter Do of the light liquid guide pipe 4 is preferably set to 85% of the inner diameter Da of the annular overflow pipe 2; thus, the true liquid velocity in the light liquid guide pipe 4 can be reduced from 6.9mm/s to 5.2mm/s or less, resulting in 0.04mm of catalyst being carried over in an amount of 0.9 μg/g or less, resulting in 0.08mm of catalyst being carried over in an amount of 0.4 μg/g or less, resulting in 0.1mm of catalyst being carried over in an amount of 0.

Referring again to fig. 2, in a preferred embodiment of the present invention, optionally, the height of the light liquid guide pipe 4 is 100-150% of the height of the straight section 1; therefore, the light liquid guide pipe 4 is ensured to have enough insertion depth, the separation efficiency is improved, the probability of liquid phase entraining catalyst particles or micro powder is reduced, and good flow field adjustment and short-circuit flow drainage effects are achieved; the height of the light liquid guide pipe 4 is preferably 120% of the height of the straight cylinder section 1, and the flow field adjustment and the short-circuit flow drainage function are optimal.

Referring again to fig. 2, in a preferred embodiment of the invention, alternatively the angle α of the generatrix of the cone section 7 to its axis is between 10 and 25 °; in this way, it is ensured that the denser catalyst particles impinge on the outer conical surface and return along the impingement path, and that about 60% of the catalyst returns directly to the lower reaction bed in the reactor. The angle α is preferably 10 ° at which the three-phase separator has the highest separation efficiency for the catalyst particles.

Referring again to fig. 2, in some preferred embodiments of the present invention, the light liquid guide pipe 4 may be configured to have a lower end higher than the liquid-solid inlet of the liquid-solid mixed phase product lead-out pipe 5, may be configured to have a lower end lower than the liquid-solid inlet of the liquid-solid mixed phase product lead-out pipe 5 and higher than the lower end of the annular overflow pipe 2, may have a lower end equal to the lower end of the annular overflow pipe 2, and may be configured to have a lower end lower than the lower end of the annular overflow pipe 2 and higher than the lower end of the straight section 1; therefore, the adjusting effect on the flow field and the drainage effect on the short-circuit flow can be effectively improved. It is further preferable to make the lower end of the light liquid guide pipe 4 lower than the liquid-solid inlet of the liquid-solid mixed phase product outlet pipe 5 so as to promote the utility of the above-mentioned regulation and drainage.

Referring again to fig. 1 and 2, in a preferred embodiment of the present invention, optionally, the axis of the liquid-solid mixed phase product outlet pipe 5 is perpendicular to the axis of the annular space overflow pipe 2, so that the liquid-solid mixed phase product in the annular space between the annular space overflow pipe 2 and the light liquid guide pipe 4 is smoothly discharged outwards, and the amount of catalyst particles or micro powder carried out is reduced; simultaneously, the axis of the liquid-phase product eduction tube 6 is mutually perpendicular to the axis of the light liquid guide tube 4, so that the light liquid guide tube 4 is beneficial to smoothly and outwards guiding and discharging the liquid-phase product, and the amount of catalyst particles or micro powder carried out is reduced.

As shown in fig. 3, the present invention further provides a ebullated bed hydrogenation reactor, which comprises a pressure-bearing shell 23 and a gas-liquid-solid three-phase separator 22 disposed at the upper part of the inner cavity of the pressure-bearing shell 23; the pressure-bearing shell 23 is a main body part of the ebullated bed hydrogenation reactor and is mainly used for the installation and arrangement of other parts and the reaction of materials; the top of the pressure-bearing shell 23 is provided with a gas phase outlet 21, and the bottom of the pressure-bearing shell is provided with a gas-liquid mixed phase inlet 25; the gas-liquid-solid three-phase separator 22 is the three-phase separator capable of regulating short-circuit flow, and the gas-liquid-solid three-phase separator 22 is generally coaxially arranged with the pressure-bearing shell 23; both the liquid-solid mixed phase product eduction tube 5 and the liquid phase product eduction tube 6 penetrate out from the side wall of the pressure-bearing shell 23.

According to the fluidized bed hydrogenation reactor, the three-phase separator is arranged, partial fluid separated from the main flow can be drained, the partial fluid is prevented from entering the light liquid guide pipe 4 along the outer wall of the light liquid guide pipe 4 and bypassing the bottom of the side wall of the light liquid guide pipe, and short-circuit flow is formed by escaping from the upper end of the light liquid guide pipe 4, so that the regulation and control of the short-circuit flow are realized, the adverse effect of the short-circuit flow can be effectively reduced, the separation precision and efficiency are ensured, and the escaping or the escaping loss of catalyst micro powder is reduced.

In a preferred embodiment of the present invention, as shown in fig. 2 and 3, alternatively, the height difference between the liquid-solid mixed phase product eduction tube 5 and the liquid phase product eduction tube 6 is h1, h1 being 40 to 90% of the inner diameter Dn of the pressure-bearing housing 23; the inner diameter of the liquid-solid mixed phase product eduction tube 5 is equal to the inner diameter of the liquid phase product eduction tube 6. In this way, the fluidization velocity required in the ebullated bed hydrogenation reactor can be reduced, and the energy consumption can be reduced. Preferably, h1 is 40%, 50% or 60% of the inner diameter Dn of the pressure-bearing shell 23, and most preferably 40%, at which time the fluidization velocity required in the ebullated bed hydrogenation reactor is minimized and the energy consumption is minimized. The difference in height between the liquid-solid phase product outlet pipe 5 and the liquid phase product outlet pipe 6 is typically characterized by the height distance between the axes of the two, and may also be characterized by the height distance between the lower or upper edges of the two.

Referring again to fig. 2 and 3, in a preferred embodiment of the invention, the inner diameter D of the straight barrel section 1 is optionally 50-90% of the inner diameter Dn of the pressure housing 23; thus, the channel between the gas-liquid-solid three-phase separator 22 and the wall of the ebullated bed hydrogenation reactor has better acceleration effect on the upward movement of the gas-liquid-solid three-phase mixture and the separation promotion effect of the gas phase; the inner diameter D of the straight tube segment 1 is preferably set to 80% of the inner diameter Dn of the pressure-bearing housing 23, and in this case, the acceleration of the upward movement of the gas-liquid-solid three-phase mixture and the separation acceleration of the gas phase are preferably optimized. Alternatively, the height of the straight cylinder section 1 is 3-10% of the tangential height of the pressure-bearing shell 23; therefore, the gas-liquid two-phase carried part catalyst with smaller density can move upwards, so that the gas phase is ensured to have sufficient separation space, and the energy consumption is reduced. The height of the straight section 1 is preferably 6% of the tangential height of the pressure housing 23 to optimize the above effect. The tangential height of the pressure-bearing housing 23 is: the distance between the tangent line at the top end of the pressure-bearing shell 23 and the tangent line at the bottom end thereof; colloquially the maximum height of the pressure bearing housing 23.

Referring again to fig. 2 and 3, in a preferred embodiment of the present invention, optionally, the height difference between the upper end of the straight tube section 1 and the upper end of the light liquid guiding tube 4 is h2, h2 being 60-100% of the inner diameter Dn of the pressure-bearing housing 23; thus, the liquid-phase product eduction tube 6 and the light liquid flow guide tube 4 are convenient to install, the probability of entraining catalyst particles or micro powder by the liquid-phase product is reduced, and the effect of preventing the gas-liquid-solid three-phase mixture from flowing back into the gas-liquid-solid three-phase separator 22 from the annular overflow tube 2 is also achieved. Preferably, h2 is 70%, 80% or 90% of the inner diameter Dn of the pressure-bearing housing 23; it is further preferable that h2 is 100% of the inner diameter Dn of the pressure-bearing housing 23 so as to optimize the above effect.

Referring again to fig. 2 and 3, in a preferred embodiment of the present invention, optionally, the height difference between the upper end of the light liquid guiding pipe 4 and the upper end of the annular overflow pipe 2 is h3, h3 being 10-60% of the inner diameter Dn of the pressure-bearing housing 23; thus, the short-circuit flow in the gas-liquid-solid three-phase separator 22 can be effectively guided by the annular gap overflow structure. Preferably, h3 is 20% of the inner diameter Dn of the pressure-bearing shell 23, and at this time, the short-circuit flow in the gas-liquid-solid three-phase separator 22 is guided by the annular overflow structure, and the short-circuit flow is 0.

Referring again to fig. 2 and 3, in a preferred embodiment of the present invention, optionally, the height difference between the upper end of the light liquid guide pipe 4 and the axis of the liquid product outlet pipe 6 is h4, where h4 is 5-20% of the inner diameter Dn of the pressure-bearing housing 23; thus, the upward movement and separation of partial gas phase mixed in the liquid phase product are facilitated, and the amount of catalyst particles and catalyst micropowder carried in the liquid phase product is reduced. Preferably, h4 is 8%, 10% and 15% of the inner diameter Dn of the pressure-bearing housing 23; it is further preferable that h4 is 10% of the inner diameter Dn of the pressure-bearing housing 23 so as to optimize the above effect.

The thickness calculation method of the side wall of each part of the ebullated bed hydrogenation reactor can follow the current national standard: pressure vessel part 1: the thickness calculation method of the pressure container of the general requirement (GB/T150.1-2011) is used for determination.

The invention also provides a boiling bed hydrogenation reaction method, which is combined with the figures 3 and 4 to carry out reaction by adopting the boiling bed hydrogenation reactor, and comprises the following steps:

step one, cyclone degassing: loading the gas-liquid-solid three-phase mixture into a fluidized bed hydrogenation reactor for reaction, after reaching the fluidized liquid level of the fluidized bed hydrogenation reactor, under the fluidization action of the fluidized bed hydrogenation reactor, enabling the gas-liquid-solid three-phase mixture to flow to the upper part of the fluidized bed hydrogenation reactor and pass through a channel between a gas-liquid-solid three-phase separator 22 and a pressure-bearing shell 23, and before the gas-liquid-solid three-phase mixture enters the gas-liquid-solid three-phase separator 22, breaking large bubbles under the action of inertia and continuing to move upwards to be discharged from a gas phase outlet 21; the rest gas phase, liquid phase and catalyst particles enter a gas-liquid-solid three-phase separator 22 from the upper end of an annular gap channel between a straight cylinder section 1 and an annular gap overflow pipe 2, a centrifugal force field is formed through the drainage effect of a rotational flow guide blade 3, and the gas phase mainly composed of small bubbles moves towards the center of a light liquid guide pipe 4 under the effect of the centrifugal force field due to the large density difference of the gas phase and the liquid phase, and continues to upwards along the light liquid guide pipe 4 after the gas phase has small density, enters the inner cavity top space of a pressure-bearing shell 23 from the upper end of the light liquid guide pipe 4 and is discharged from a gas phase outlet 21; part of liquid phase close to the center of the light liquid guide pipe 4 moves upwards along the light liquid guide pipe 4 under the driving action of the internal rotational flow of the gas phase, and finally is discharged out of the ebullated bed hydrogenation reactor as liquid phase product through a liquid phase product eduction pipe 6;

Step two, primary rotational flow solid removal: the catalyst particles with large particle size in the first step are thrown to the side wall of the gas-liquid-solid three-phase separator 22 under the action of the centrifugal force field, move downwards along the cone section 7 and the underflow pipe 8, and finally return to the inner cavity of the pressure-bearing shell 23 from the underflow port at the lower end of the underflow pipe 8 for continuous reaction; catalyst particles or powder with smaller particle size and partial liquid phase substances move upwards from an annular space between the annular space overflow pipe 2 and the light liquid flow guide pipe 4 under the action of the swirling flow field, and finally are discharged out of the ebullated bed hydrogenation reactor as liquid-solid mixed phase products through the liquid-solid mixed phase product outlet pipe 5, so that the short-circuit flow regulation and control are realized.

The fluidized bed hydrogenation reaction method can drain partial fluid separated from the main flow, prevent the partial fluid from entering the light liquid guide pipe 4 along the outer wall of the light liquid guide pipe 4 by bypassing the bottom of the side wall of the light liquid guide pipe, and escape from the upper end of the light liquid guide pipe 4 to form short-circuit flow, thereby realizing the regulation and control of the short-circuit flow, effectively reducing the adverse effect of the short-circuit flow, ensuring the separation precision and efficiency, and reducing the escape or the running loss of the catalyst micro powder. In addition, the boiling bed hydrogenation reaction method can also improve the internal flow field distribution of the gas-liquid-solid three-phase separator 22, enlarge the range of the zero axial velocity envelope surface, ensure that most catalyst particles move downwards without escaping, and increase the intensity of turbulent flow in the three-phase separator at the same time, thereby improving the separation precision and efficiency and realizing the strengthening of the separation effect.

Optionally, the method further comprises a step three;

step three, secondary rotational flow solid removal: the liquid-solid mixed phase product in the second step is discharged out of the fluidized bed hydrogenation reactor, then continuously moves along the liquid-solid mixed phase product eduction tube 5 and the liquid-solid mixed phase product circulating tube 27 connected to the liquid-solid outlet of the liquid-solid mixed phase product eduction tube 5, enters the secondary cyclone 26 connected to the lower end of the liquid-solid mixed phase product circulating tube 27 for further solid removal, and the clean liquid phase product obtained after further solid removal enters the bottom of the inner cavity of the pressure-bearing shell 23 along the cyclone guide tube 28 connected to the secondary cyclone 26, and enters the upper part of the inner cavity of the pressure-bearing shell 23 under the action of the gas-liquid distributor 24 to continuously participate in the reaction.

The boiling bed hydrogenation reaction method is a solution provided by the inventor aiming at the problems of catalyst escape, running loss, low separation efficiency and the like caused by short-circuit flow in the reinforced separation process of a three-phase cyclone separator in a boiling bed hydrogenation reactor in the prior art, and mainly adopts an annular gap overflow pipe 2, a light liquid guide pipe 4, a liquid-solid mixed phase product circulation pipe 27 and a secondary cyclone 26 to carry out the deep separation of gas, liquid and solid phases and the recycling of liquid phase products.

In addition, the liquid-solid mixed phase product is conveyed into an external secondary cyclone 26 through a liquid-solid mixed phase product circulating pipe 27 to further remove solid, so that catalyst micro powder in the liquid-solid mixed phase product is removed, the catalyst micro powder is prevented from being coked and adhered to the flowing wall surface, the wall surface corrosion and the catalyst deactivation are caused, and the removal and the regeneration of the catalyst micro powder are realized.

In addition, the clean liquid phase product obtained after further solid removal enters the ebullated bed hydrogenation reactor along the cyclone conduit 28 connected to the secondary cyclone 26, and enters the upper part of the inner cavity of the pressure-bearing shell 23 under the action of the gas-liquid distributor 24 to continuously participate in the reaction, thereby realizing the same-level recycling of the liquid phase product, improving the separation efficiency and the utilization rate of resources.

Specifically, the particle size range of the catalyst particles is 0.04-0.1 mm; the particle size range of the large-particle-size catalyst particles is 0.07-0.1 mm; smaller particle size catalyst particles or powders having a particle size of less than 0.07mm. The particle size range of the catalyst particles which can be added in the ebullated bed hydrogenation reactor and the method provided by the invention is between 0.04 and 0.1mm, and compared with the existing ebullated bed hydrogenation reactor, the catalyst particle size which can be added is smaller, the specific surface area is larger, and the reaction rate is higher.

Optionally, in order to further improve the separation effect, as shown in fig. 5 or fig. 6, at least two ebullated bed hydrogenation reactors are used in the ebullated bed hydrogenation reaction method and are connected in series in a grading manner; the liquid phase outlet of the liquid phase product eduction tube 6 of the ebullated bed hydrogenation reactor is connected with the gas-liquid mixed phase inlet 25 of the ebullated bed hydrogenation reactor of the next stage through a pipeline; the liquid level difference h5 between any two adjacent boiling bed hydrogenation reactors is larger than the on-way resistance loss which is the sum of the loss of a pipeline connecting the two boiling bed hydrogenation reactors and the loss of mechanical energy for lifting the liquid level needed by the next boiling bed hydrogenation reactor.

Example 1

The three-phase separator provided by the invention is applied to a 5000L/h ebullated bed hydrogenation reactor cold mould experiment.

1) The experimental equipment comprises the following components and process flows:

as shown in fig. 5, the equipment used in the present experiment includes an air compressor 41, a first ebullated bed hydrogenation reactor 42-1, a second ebullated bed hydrogenation reactor 42-2, a liquid product delivery pipe 43, a circulation tank 44, a water pump 45, a first secondary cyclone 46, a first booster pump 47, a second secondary cyclone 48, and a second booster pump 49;

The air outlet of the air compressor 41 and the water outlet of the water pump 45 are respectively connected with the gas-liquid mixed phase inlet 25 of the first ebullated bed hydrogenation reactor 42-1 through pipelines;

the liquid-solid mixed phase product eduction tube 5 of the first ebullated bed hydrogenation reactor 42-1 is connected with the lateral tangential feed inlet of the first secondary cyclone 46 through the liquid-solid mixed phase product circulating tube 27 thereof, and the top center discharge port of the first secondary cyclone 46 is communicated with the bottom of the inner cavity of the first ebullated bed hydrogenation reactor 42-1 or the gas-liquid mixed phase inlet 25 through the first booster pump 47; the liquid-phase product outlet pipe 6 of the first ebullated-bed hydrogenation reactor 42-1 is communicated with the gas-liquid mixed phase inlet 25 of the second ebullated-bed hydrogenation reactor 42-2 through the liquid-phase product outlet pipe 43;

the liquid-solid mixed phase product eduction tube 5 of the second ebullated bed hydrogenation reactor 42-2 is connected with the side tangential feed inlet of the second secondary cyclone 48 through the liquid-solid mixed phase product circulating tube 27 thereof, and the top center discharge port of the second secondary cyclone 48 is communicated with the bottom of the inner cavity of the second ebullated bed hydrogenation reactor 42-2 or the gas-liquid mixed phase inlet 25 through the second booster pump 49; the liquid-phase product eduction tube 6 of the second ebullated-bed hydrogenation reactor 42-2 is connected with the liquid inlet of the circulation tank 44 through a pipeline;

The liquid outlet of the circulating tank 44 is connected with the water inlet of the water pump 45 through a pipeline;

wherein, the first ebullated bed hydrogenation reactor 42-1 and the second ebullated bed hydrogenation reactor 42-2 are both provided with the three-phase separator provided by the present invention.

Referring to fig. 5, the process flow of this experiment is: after the water is pressurized by the water pump 45, the water and the air compressed by the air compressor 41 are fed into the first ebullated bed hydrogenation reactor 42-1 through the gas-liquid mixed phase inlet 25 at the bottom; the catalyst particles in the first ebullated bed hydrogenation reactor 42-1 reach a fluidized state under the force of air and water; separating the gas-liquid-solid three-phase mixture in the first ebullated bed hydrogenation reactor 42-1 through a three-phase separator, discharging the obtained gas phase (and air) from the gas phase outlet 21 of the first ebullated bed hydrogenation reactor 42-1, discharging the obtained liquid-solid mixed phase product from the liquid-solid mixed phase product eduction tube 5, removing solids through the first secondary cyclone 46, pressurizing by the first booster pump 47, entering the first-stage reactor to participate in the reaction again, discharging the obtained liquid phase product from the liquid phase product eduction tube 43, continuously reacting through the second ebullated bed hydrogenation reactor 42-2 connected in series to jointly realize the deep purification and high-efficiency reaction of the liquid phase product, discharging the gas phase (and air) obtained by the second ebullated bed hydrogenation reactor 42-2, and delivering the obtained liquid phase product into the circulation tank 44 for recycling; where h5 represents the liquid level difference between the first ebullated-bed hydrogenation reactor 42-1 and the second ebullated-bed hydrogenation reactor 42-2.

2) Major structural dimensions of ebullated bed hydrogenation reactor

The main structural dimensions of the ebullated bed hydrogenation reactor are shown in Table 1 below, and the first ebullated bed hydrogenation reactor 42-1 and the second ebullated bed hydrogenation reactor 42-2 are identical in size and structure.

Table 1:5000L/h ebullated bed hydrogenation reactor cold mould device structural dimension

3) Effect of the invention

The test procedure of the 5000L/h ebullated bed hydrogenation reactor cold mold apparatus was conducted using water and air, and the test results are shown in Table 2 below.

Table 2:5000L/h ebullated bed hydrogenation reactor cold die device test results

From the test results, the catalyst achieves uniform fluidization, no faults occur in continuous operation for 80 hours, the catalyst carrying-out amount of 0.04mm is controlled to be less than or equal to 0.9 mug/g, the catalyst carrying-out amount of 0.08mm is controlled to be less than or equal to 0.4 mug/g, and the catalyst carrying-out amount of 0.1mm is controlled to be 0; in addition, in the operation process of filling catalysts with different particle sizes into the fluidized bed hydrogenation reactor, no short-circuit flow appears at the bottom of the light liquid guide pipe 4, and the short-circuit flow rate is zero, which indicates that the structural design of the invention realizes the effective regulation and control of the short-circuit flow in the fluidized bed hydrogenation reactor.

Example 2

The ebullated bed hydrogenation reactor provided by the invention is applied to a 50 ten thousand tons/year straw pyrolysis liquid hydrodeoxygenation process.

1) The equipment comprises the following components and the process flow:

as shown in FIG. 6, the apparatus used in this example comprises a heating furnace 51, a third ebullated bed hydrogenation reactor 52-1, a fourth ebullated bed hydrogenation reactor 52-2, a separator 53, an air cooler 54, a third secondary cyclone 55, a third booster pump 56, a fourth secondary cyclone 57, a fourth booster pump 58, and a cyclone cushion feeder 59;

the gas outlet of the heating furnace 51 is connected with the gas-liquid mixed phase inlets 25 of the third ebullated bed hydrogenation reactor 52-1 and the fourth ebullated bed hydrogenation reactor 52-2 respectively through pipelines;

the liquid-solid mixed phase product eduction tube 5 of the third ebullated bed hydrogenation reactor 52-1 is connected with the lateral tangential feed inlet of the third secondary cyclone 55 through the liquid-solid mixed phase product circulating tube 27 thereof, and the top center discharge port of the third secondary cyclone 55 is communicated with the bottom of the inner cavity of the third ebullated bed hydrogenation reactor 52-1 or the gas-liquid mixed phase inlet 25 through the third booster pump 56; the gas phase outlet 21 of the third ebullated bed hydrogenation reactor 52-1 is connected to the gas inlet of the separator 53 through the air cooler 54; the liquid-phase product eduction tube 6 of the third ebullated bed hydrogenation reactor 52-1 is communicated with the gas-liquid mixed phase inlet 25 of the fourth ebullated bed hydrogenation reactor 52-2 through a pipeline;

The liquid-solid mixed phase product eduction tube 5 of the fourth ebullated bed hydrogenation reactor 52-2 is connected with the side tangential feed inlet of the fourth secondary cyclone 57 through the liquid-solid mixed phase product circulating tube 27 thereof, and the top center discharge port of the fourth secondary cyclone 57 is communicated with the bottom of the inner cavity of the fourth ebullated bed hydrogenation reactor 52-2 or the gas-liquid mixed phase inlet 25 through the fourth booster pump 58; the gas phase outlet 21 of the fourth ebullated bed hydrogenation reactor 52-2 is connected to the gas inlet of the separator 53 through the air cooler 54; the liquid-phase product eduction tube 6 of the fourth ebullated-bed hydrogenation reactor 52-2 is communicated with the liquid inlet of the separator 53 through a pipeline;

the cyclone cushion feeder 59 is arranged at the lower part of the third ebullated bed hydrogenation reactor 52-1 and is positioned at the upper side of the gas-liquid distributor 24 of the third ebullated bed hydrogenation reactor 52-1;

wherein, the third ebullated bed hydrogenation reactor 52-1 and the fourth ebullated bed hydrogenation reactor 52-2 are both ebullated bed hydrogenation reactors provided by the present invention.

Referring to fig. 6, the process flow of this embodiment is as follows: the straw pyrolysis liquid and the hydrogen supply agent enter the third ebullated bed hydrogenation reactor 52-1 from the cyclone cushion feeder 59, and the mass ratio of the straw pyrolysis liquid to the hydrogen supply agent is 7:1. The hydrogen enters from the gas-liquid mixed phase inlet 25 at the bottom of the third ebullated bed hydrogenation reactor 52-1 after being heated by the heating furnace 51, and is mixed with the straw pyrolysis liquid to reach a fluidization state under the action of the gas-liquid distributor 24; separating the gas-liquid-solid three-phase mixture in the third fluidized bed hydrogenation reactor 52-1 through a three-phase separator, discharging the obtained hydrogen from a gas phase outlet 21 of the third fluidized bed hydrogenation reactor 52-1, cooling by an air cooler 54, purifying by a subsequent process, discharging the obtained liquid-solid mixed phase product from a liquid-solid mixed phase product eduction tube 5, removing solids by a third secondary cyclone 55, pressurizing by a third booster pump 56, entering the present-stage reactor to participate in the reaction again, and discharging the catalyst micro powder obtained by separating by the third secondary cyclone 55 from a bottom flow port; the obtained liquid phase product is discharged from a liquid phase product outlet pipe 6 of a third ebullated bed hydrogenation reactor 52-1, and then continuously reacts through a fourth ebullated bed hydrogenation reactor 52-2 which is connected in series in two stages, so that the deep purification and the high-efficiency reaction of the liquid phase product are realized together, and the liquid phase product obtained by the fourth ebullated bed hydrogenation reactor 52-2 is discharged from the liquid phase product outlet pipe 6 and then enters a separator 53 for separation; where h5 represents the liquid level difference between the third ebullated bed hydrogenation reactor 52-1 and the fourth ebullated bed hydrogenation reactor 52-2.

2) Major structural dimensions of ebullated bed hydrogenation reactor

The main structural dimensions of the ebullated bed hydrogenation reactor are shown in Table 3 below, and the dimensions of the third ebullated bed hydrogenation reactor 52-1 and the fourth ebullated bed hydrogenation reactor 52-2 are identical.

Table 3:50 ten thousand tons/year straw pyrolysis liquid hydrodeoxygenation ebullated bed hydrogenation reactor device structural dimension

3) Effect of the invention

The test process of the 50 ten thousand ton/year ebullated bed hydrogenation cold die device was carried out by using the straw pyrolysis liquid, and the test results are shown in the following table 4.

Table 4:50 ten thousand tons/year straw pyrolysis liquid hydrodeoxygenation test result

Project	Operating condition one	Operating condition two	Operating condition III
				Liquid phase	Straw pyrolysis liquid	Straw pyrolysis liquid	Straw pyrolysis liquid
Reaction temperature (DEG C)	400	400	400
				Pressure MPa	14	14	14
Hydrogen to oil ratio v/v	700	500	500
				Catalyst particle size μm	10	80	100
Catalyst loading m 3	3.6	3.6	3.6
				Ten thousand t/a of circulating oil	175	175	175
Catalyst carry-over amount. Mu.g/g	1.2	0.4	0.07
				Short circuit flow rate%	0	0	0

；

From the test results, the inside of the reactor reaches a full mixed flow state, the catalyst is fluidized uniformly, the continuous operation is carried out for 1000 hours without faults, the catalyst carrying-out amount of 0.01mm is controlled to be less than or equal to 1.2 mug/g, the catalyst carrying-out amount of 0.08mm is controlled to be less than or equal to 0.4 mug/g, and the catalyst carrying-out amount of 0.1mm is controlled to be less than or equal to 0.07 mug/g; in addition, in the operation process of filling catalysts with different particle sizes into the fluidized bed hydrogenation reactor, no short-circuit flow appears at the bottom of the light liquid guide pipe 4, and the short-circuit flow rate is zero, which indicates that the structural design of the invention realizes the effective regulation and control of the short-circuit flow in the fluidized bed hydrogenation reactor.

Comparative example

Listed in this comparative example are the ebullated bed hydrogenation reactor disclosed in chinese patent CN113244860B and the present invention provides some of the conditions and results of ebullated bed hydrogenation reactor in apathy experiments.

(1) The treated materials are water, air and alumina carrier particles.

(2) Other interference factors do not exist in the experimental process, and the air tightness of the device and the running condition of the detection table are checked before the experiment.

(3) The process environment conditions were consistent as set forth in table 5 below.

Table 5: comparison of experimental parameters

As can be seen from the comparison, the ebullated bed hydrogenation reactor provided by the invention is superior to the Chinese patent CN113244860B in terms of throughput, operating pressure, minimum catalyst particle size, continuous operation time, catalyst carry-over amount and short-circuit flow rate, in particular to the aspects of minimum catalyst particle size and short-circuit flow regulation; the minimum catalyst particle diameter which can be filled in the reactor can reach 40 mu m, no catalyst particles are carried out, short-circuit flow is eliminated, and the separation precision and the reaction rate are ensured.

The description of the various embodiments of the present invention has been presented for purposes of illustration only and is not intended to be exhaustive or limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein was chosen to best explain the principles of the embodiments, the practical application, or the technological advancement, or to enable others skilled in the art to understand the embodiments disclosed herein, as compared to commercially available technology.

Various embodiments of the invention may be presented herein in a range format. It should be understood that the description of the range format is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the invention. Accordingly, the description of a range should be considered to specifically disclose all possible sub-ranges and individual values within the range. For example, descriptions such as ranges from 1 to 6 should be considered to specifically disclose subranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as individual values within the range, e.g., 1, 2, 3, 4, 5, 6, independent of the width of the range.

It is appreciated that certain features of the invention, which are, for clarity, described in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features of the invention which are, for brevity, described in the context of a single embodiment, may also be provided separately or in any suitable subcombination or in any other described embodiment of the invention where appropriate. Certain features described in the context of various embodiments are not to be considered essential features of those embodiments unless the embodiments are not functional without those features.

All publications, patents, and patent applications mentioned herein are incorporated herein by reference in their entirety to the same extent as if each individual publication, patent, or patent application was specifically and individually indicated to be incorporated herein by reference. Furthermore, citation or identification of any reference herein shall not be construed as an admission that such reference is available as prior art to the present invention. To the extent that section titles are used, section titles should not be construed as necessarily limiting.

Claims (10)

1. The three-phase separator capable of regulating short-circuit flow comprises a separator main body, an annular gap overflow pipe (2), a rotational flow guide blade (3), a light liquid guide pipe (4), a liquid-solid mixed phase product eduction pipe (5) and a liquid phase product eduction pipe (6);

the separator body comprises a straight section (1);

the annular gap overflow pipe (2) and the straight barrel section (1) are coaxially arranged, the lower end of the annular gap overflow pipe extends into the inner cavity of the straight barrel section (1), and the upper end of the annular gap overflow pipe is higher than the upper end of the straight barrel section (1);

the swirl guide vane (3) is arranged in an annular gap channel between the straight cylinder section (1) and the annular gap overflow pipe (2);

the light liquid guide pipe (4) and the annular gap overflow pipe (2) are coaxially arranged;

the liquid-solid mixed phase product eduction tube (5) is arranged on a tube section of the annular gap overflow tube (2) outside the straight tube section (1) and is communicated with the inner cavity of the annular gap overflow tube (2) through a liquid-solid inlet of the liquid-solid mixed phase product eduction tube;

The method is characterized in that: the lower end of the light liquid guide pipe (4) extends into the inner cavity of the annular gap overflow pipe (2), and the upper end of the light liquid guide pipe is higher than the upper end of the annular gap overflow pipe (2); a closed structure (11) is arranged between the light liquid guide pipe (4) and the upper end of the annular gap overflow pipe (2);

the liquid-phase product eduction tube (6) is arranged on a tube section of the light liquid guide tube (4) outside the annular gap overflow tube (2) and is communicated with the inner cavity of the light liquid guide tube (4) through a liquid-phase inlet thereof.

2. The three-phase separator with controllable short-circuit flow according to claim 1, characterized in that: also comprises a non-return cone (9);

the separator body further comprises a cone section (7) and an underflow pipe (8);

the straight cylinder section (1), the cone cylinder section (7) and the underflow pipe (8) are sequentially and coaxially connected together from top to bottom;

the non-return cone (9) is arranged at a bottom flow port at the lower end of the bottom flow pipe (8).

3. The three-phase separator with controllable short-circuit flow according to claim 2, characterized in that: the inner diameter Da of the annular gap overflow pipe (2) is 75-95% of the inner diameter D of the straight section (1), and the height of the annular gap overflow pipe (2) is 50-130% of the height of the light liquid guide pipe (4);

the inclination angle theta of the cyclone guide vane (3) is 45-65 degrees;

the inner diameter Do of the light liquid guide pipe (4) is 70-90% of the inner diameter Da of the annular gap overflow pipe (2), and the height of the light liquid guide pipe (4) is 100-150% of the height of the straight cylinder section (1);

The included angle alpha between the bus of the cone section (7) and the axis of the cone section is 10-25 degrees.

4. A three-phase separator with controllable short-circuit flow according to any one of claims 1 to 3, characterized in that: the lower end of the light liquid guide pipe (4) is higher than the lower end of the straight cylinder section (1);

the axis of the liquid-solid mixed phase product eduction tube (5) is mutually perpendicular to the axis of the annular gap overflow tube (2);

the axis of the liquid-phase product eduction tube (6) is mutually perpendicular to the axis of the light liquid guide tube (4).

5. The fluidized bed hydrogenation reactor comprises a pressure-bearing shell (23) and a gas-liquid-solid three-phase separator (22) arranged at the upper part of the inner cavity of the pressure-bearing shell (23);

the top of the pressure-bearing shell (23) is provided with a gas phase outlet (21), and the bottom of the pressure-bearing shell is provided with a gas-liquid mixed phase inlet (25);

the method is characterized in that: the gas-liquid-solid three-phase separator (22) is a three-phase separator with adjustable short-circuit flow according to any one of claims 1 to 4;

the liquid-solid mixed phase product eduction tube (5) and the liquid phase product eduction tube (6) are penetrated out from the side wall of the pressure-bearing shell (23).

6. The ebullated bed hydrogenation reactor according to claim 5, wherein: the height difference between the liquid-solid mixed phase product eduction tube (5) and the liquid phase product eduction tube (6) is h1, and h1 is 40-90% of the inner diameter Dn of the pressure-bearing shell (23);

The inner diameter of the liquid-solid mixed phase product eduction tube (5) is equal to the inner diameter of the liquid phase product eduction tube (6).

7. The ebullated bed hydrogenation reactor according to claim 5 or 6, wherein: the inner diameter D of the straight cylinder section (1) is 50-90% of the inner diameter Dn of the pressure-bearing shell (23), and the height of the straight cylinder section (1) is 3-10% of the tangential height of the pressure-bearing shell (23);

the height difference between the upper end of the straight cylinder section (1) and the upper end of the light liquid guide pipe (4) is h2, and h2 is 60-100% of the inner diameter Dn of the pressure-bearing shell (23);

the height difference between the upper end of the light liquid guide pipe (4) and the upper end of the annular gap overflow pipe (2) is h3, and h3 is 10-60% of the inner diameter Dn of the pressure-bearing shell (23);

the height difference between the upper end of the light liquid guide pipe (4) and the axis of the liquid product eduction pipe (6) is h4, and h4 is 5-20% of the inner diameter Dn of the pressure-bearing shell (23).

8. Ebullated bed hydrogenation process employing the ebullated bed hydrogenation reactor according to any one of claims 5 to 7, characterized in that the process comprises the steps of:

step one, cyclone degassing: loading the gas-liquid-solid three-phase mixture into a fluidized bed hydrogenation reactor for reaction, and under the fluidization effect of the fluidized bed hydrogenation reactor, breaking the large bubbles under the inertia effect and continuing to move upwards to be discharged from a gas phase outlet (21); the rest gas phase, liquid phase and catalyst particles enter a gas-liquid-solid three-phase separator (22) from the upper end of an annular gap channel between a straight cylinder section (1) and an annular gap overflow pipe (2), a centrifugal force field is formed by the drainage effect of a rotational flow guide blade (3), small bubbles move towards the center of a light liquid guide pipe (4) under the effect of the centrifugal force field and continue to upwards along the light liquid guide pipe (4), enter the inner cavity top space of a pressure-bearing shell (23) from the upper end of the light liquid guide pipe (4), and are discharged from a gas phase outlet (21); part of liquid phase close to the center of the light liquid guide pipe (4) moves upwards along the light liquid guide pipe (4) under the action of internal rotational flow, and is finally discharged from the liquid phase product eduction pipe (6) as liquid phase product;

Step two, primary rotational flow solid removal: the catalyst particles with large particle size in the first step are thrown to the side wall of a gas-liquid-solid three-phase separator (22) under the action of a centrifugal force field, move downwards along a cone section (7) and an underflow pipe (8), and finally return to the inner cavity of a pressure-bearing shell (23) from a underflow port at the lower end of the underflow pipe (8) to continue to react; catalyst particles or powder with smaller particle size and partial liquid phase substances move upwards through an annular space between the annular space overflow pipe (2) and the light liquid flow guide pipe (4) under the action of the swirling flow field, and are finally discharged from the liquid-solid mixed phase product eduction pipe (5) as liquid-solid mixed phase products.

9. The ebullated bed hydrogenation reaction process according to claim 8, wherein: the method further comprises a step three;

step three, secondary rotational flow solid removal: after the liquid-solid mixed phase product in the second step is discharged out of the fluidized bed hydrogenation reactor, the liquid-solid mixed phase product continuously moves along a liquid-solid mixed phase product eduction tube (5) and a liquid-solid mixed phase product circulating tube (27) connected to a liquid-solid outlet of the liquid-solid mixed phase product eduction tube (5), the liquid-solid mixed phase product enters a secondary cyclone (26) connected to the lower end of the liquid-solid mixed phase product circulating tube (27) for further removing solids, and the clean liquid phase product obtained after the further solid removal enters the bottom of an inner cavity of a pressure-bearing shell (23) along a cyclone guide tube (28) connected to the secondary cyclone (26) and enters the upper part of the inner cavity of the pressure-bearing shell (23) under the action of a gas-liquid distributor (24) to continuously participate in the reaction.

10. The ebullated bed hydrogenation reaction process according to claim 8 or 9, characterized in that: the particle size range of the catalyst particles is 0.04-0.1 mm;

the particle size range of the large-particle-size catalyst particles is 0.07-0.1 mm;

the smaller particle size catalyst particles or powders have a particle size of less than 0.07mm;

at least two ebullated bed hydrogenation reactors are connected in series in a grading way;

the liquid phase outlet of the liquid phase product eduction tube (6) of the ebullated bed hydrogenation reactor is connected with the gas-liquid mixed phase inlet (25) of the ebullated bed hydrogenation reactor of the next stage through a pipeline;

the liquid level difference h5 between any two adjacent two-stage ebullated-bed hydrogenation reactors is greater than the on-way drag loss +0.5m.