CN113083169B - Fluidized bed hydrogenation reactor and using method thereof - Google Patents
Fluidized bed hydrogenation reactor and using method thereof Download PDFInfo
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Abstract
The present disclosure relates to a fluidized bed hydrogenation reactor and a method of using the same, providing a fluidized bed hydrogenation reactor comprising: the device comprises a pressure-bearing shell (3), a gas-liquid-solid three-phase cyclone separator arranged in the upper space of the pressure-bearing shell, a liquid-descending liquid-phase product eduction tube (14) arranged in the middle of the pressure-bearing shell, and a gas-liquid mixed phase inlet (1) and a gas-liquid outlet (7) and a liquid-phase outlet (15) which are arranged on the pressure-bearing shell. Also provides a using method of the fluidized bed hydrogenation reactor.
Description
Technical Field
The disclosure belongs to a revolutionary clean energy key equipment technology, and particularly relates to a fluidized bed hydrogenation reactor and a use method thereof.
Background
The fluidized bed reactor is a gas-liquid-solid three-phase fluidized bed reactor, and is widely applied to a hydrogenation process because of reduced pressure, difficulty in blockage and long-term operation. Ebullated-bed reactors have the following advantages due to their unique structure and mode of operation: the operation is flexible, and the operation can be carried out under high or low conversion rate; the catalyst can be periodically recovered or added from the reactor, and the reaction activity of the catalyst can be maintained under the condition of no work; expanding the catalyst bed layer by 30-50% through a circulating pump, and ensuring that enough free space exists among solid particles of the catalyst; the problems of accumulation, bed layer blockage or bed layer pressure drop increase in the process of passing through a catalyst bed layer by solid particles generated in the process of raw material entrainment or reaction can be avoided; fourthly, the use of the catalyst with small particle size can obviously reduce the limit of diffusion, improve the reaction rate and avoid the situation that metal deposition blocks catalyst pore channels; good heat transfer to minimize overheating of the catalyst bed and to reduce coke formation; the boiling bed reactor is operated approximately isothermally, and in an industrial boiling bed device, the temperature difference between any two points in the reactor is lower than 5 ℃, so that local overheating can be avoided.
The concept of ebullated bed reactors has been proposed for over 50 years as far as the equipment development of ebullated bed technology has been concerned, for over 40 years, but it is the primary reason for the high construction and operating costs of existing ebullated bed units, whether the H-Oil technology trades off for normal reactor operation at the expense of reaction space utilization and catalyst mass transfer efficiency, or, like the STRONG technology, trades off for normal reactor operation at the expense of more equipment manufacturing. In the existing technical level of reactor equipment, it is difficult to achieve the cross-over improvement of the whole technical level of the reactor only by gradual replacement of the catalyst. In order to break through the development bottleneck, it is foreseeable that the development of the ebullated-bed reactor in the future, besides relying on the former "three passes and one reverse" law to recognize the deepening and upgrading and updating of the catalyst, or the realization of the "possible development requirement" of the ebullated-bed reactor with the innovation of the reactor equipment, particularly the innovation of the outlet separator, can be considered: (1) the service life of the catalyst is prolonged, and coking is not easy to occur; (2) the catalyst is circularly operated in a fully mixed flow mode; (3) the space of the reactor is fully utilized; (4) the separation precision and efficiency are high; (5) the heat loss is small.
Chinese utility model patent CN 207828192U discloses a fluidized bed hydrogenation reaction system, and spindle-shaped baffle is equipped with to three-phase separator lower part, has reduced the catalyst volume of bringing, but its three-phase separation effect is not showing, only provides the rotatory separation between urceolus and inner tube and takes place coking phenomenon easily, and the catalyst life-span is short.
Chinese patent publication CN 102463077a discloses a three-phase ebullated-bed reactor, the upper part of which also comprises a three-phase separator device, which comprises an inner cylinder and an outer cylinder, and the upper and lower ends are all opened. The three-phase mixture upwards enters the inner cylinder, and solid particles enter an annular gap between the inner cylinder and the outer cylinder at the outlet of the inner cylinder due to transverse turbulence, and finally return to the reactor from the diffusion section. The device simple structure, but same gas-liquid-solid three-phase mixture receives the cross vortex effect to be limited, and solid particle can not high-efficiently separate with the liquid phase, and the microbubble also can remain in the liquid phase equally. Chinese patent publication CN 101721960a discloses a fluidized bed separator, which has a three-phase separator at its upper part, and its structure and principle are similar to CN 102463077 a. The three-phase separator comprises a sleeve structure of an inner cylinder and an outer cylinder, the upper section and the lower section of the inner cylinder and the outer cylinder are both of an opening structure, the upper sections of the inner cylinder and the outer cylinder are of inverted frustum-shaped structures, and the lower sections of the inner cylinder and the outer cylinder are both of upright frustum-shaped structures.
Chinese patent publication CN 108114510a discloses a gas-liquid-solid three-phase separator and a fluidized bed reactor containing the same, the three-phase separator includes three concentric straight cylinders with different inner diameters, the gas-liquid-solid three-phase mixture enters from the innermost draft tube, and is provided with a Z-shaped baffle plate to prevent bubbles from entering the liquid-solid separation zone, and the liquid-solid two-phase is separated between the outer cylinder and the wall of the reactor, which can reduce the entrainment of the catalyst by 80% -95%, and similarly, it cannot realize the fully mixed flow operation condition, and cannot fully utilize the inner space of the reactor.
Chinese utility model patent CN 210974072U discloses an anaerobic reactor three-phase separator device, through setting up the guide plate in the bottom both sides of separator, the minor part sewage can continue the upward movement along the inner wall about the reactor shell, and the floater wherein can flow the top of diffuser plate along the bottom of baffle to flow and separate on the guide plate, do not influence each other with the sewage that rises. However, for the fluidized bed reactor, the solid particles of the catalyst are small, the solid is difficult to be intercepted and separated under the action of a baffle, the separation precision is difficult to be ensured, and the fully mixed flow operation condition cannot be achieved.
Chinese patent publication CN 108148621a discloses a fluidized bed hydrogenation reactor and a fluidized bed hydrogenation method, wherein a three-phase separator is arranged in the upper part of the reactor to realize the separation of gas, liquid and solid phases. The three-phase separator is simple in structure, only provided with the inner cylinder and the outer cylinder, can meet the requirement of gas-liquid-solid three-phase separation in a small-scale and small-flow state, has a certain effect, is difficult to meet large-scale and high-efficiency separation, and cannot strengthen cyclone separation. The utility model CN 207929188U is the supplement and extension of CN 108148621A, and similarly, the problem that the enhanced driving force of the cyclone separation is not enough, and the separation precision and efficiency are not high.
Chinese utility model patent CN 201744345U discloses a fluidized bed reactor, including awl end, reaction cylinder, one-level cyclone and second grade cyclone, the reaction cylinder is arranged in to the separator is external, though separation efficiency is high, but need draw the reactant, and this process can lose the heat, and is more power consumptive.
The invention discloses a three-phase separator of a biomass pyrolysis liquid fluidized bed reactor and application thereof, wherein a cyclone structure is used for separating gas, liquid and solid phases, a liquid phase outlet pipe is arranged at the upper part, a non-return cone is arranged at the bottom part, the three-phase separator is reasonable and compact in structure, good in separation effect and large in operation elasticity, a three-phase mixture consisting of gas phase, liquid phase and catalyst particles directly enters the three-phase separator for separation, the three-phase separator is a complex flowing process, the separation precision is low, the separation efficiency is influenced, meanwhile, a bottom flow pipe has high solid concentration and is blocked by the non-return cone to dissipate heat, and the bottom of the bottom flow pipe is easy to coke under the conditions of high temperature and high pressure. Chinese patent publication CN 109967002A discloses a three-phase separator of a biomass pyrolysis liquid fluidized bed reactor and application thereof, the main structure of the three-phase separator is similar to that of CN 109967001A, and a liquid phase eduction tube is changed into a gas-liquid mixed outlet tube. In a traditional three-phase reactor, the size of bubbles is 2.5-15 mm, and the classical gas-liquid mixing theory is generally based on millimeter-centimeter-level gas-liquid particle characteristics; however, the volume mass transfer coefficient of the gas-liquid reaction is mainly influenced by the mass transfer coefficient and the area of the gas-liquid phase interface, and the efficiency is higher as the bubbles are smaller and the gas-liquid interface is more; however, when the bubbles are reduced to 0.1-2 mm, gas-liquid emulsified state is formed, and micro bubbles between 1 μm-1 mm are similar to rigid small balls, and are not easy to coalesce in the main body of the micro interface enhanced reaction device (see chinese patent ZL 201920155671.3), and thus are not easy to separate, and if such bubbles enter the liquid-solid cyclone in CN 109967001a and CN 109967002A, the separation of solid particles is disturbed, and the separation accuracy is not high.
Regarding the requirements of catalyst particle size, the above two patentsIn the publication, the particle diameter of the catalyst particles is defined to be at least 0.2 mm. According to the catalyst particle true density of 1500kg/m3The specific surface area of the catalyst with the particle diameter of 0.2mm is calculated to be 0.02m2About/g, the use requirement of small-particle-size catalyst particles cannot be met.
Therefore, in order to enable the ebullated-bed hydrogenation reactor to realize a fully mixed flow operation, to be suitable for a bubble-catalyst system with a high specific surface area to ensure separation accuracy, to realize in-situ on-line activation of catalyst particles, to have small heat loss and to be difficult to coke, the development of a hydrogenation reactor and a use method thereof, which can overcome the defects of the prior art, is urgently needed in the field.
Disclosure of Invention
The present disclosure provides a novel ebullated bed hydrogenation reactor and method of using the same, thereby solving the problems of the prior art.
In one aspect, the present disclosure provides an ebullated bed hydrogenation reactor comprising:
a pressure-bearing outer shell,
a gas-liquid-solid three-phase cyclone separator arranged in the upper space of the pressure-bearing shell,
a liquid-descending liquid-phase product lead-out pipe arranged in the middle of the pressure-bearing shell, and
and the gas-phase outlet, the liquid-phase outlet and the gas-liquid mixed-phase inlet are arranged on the pressure-bearing shell.
In a preferred embodiment, the gas-liquid-solid three-phase cyclone separator is formed by sequentially arranging a sieve mesh sleeve, a primary cyclone guide vane, a column section, a gas non-return conical plate, an overflow pipe, a secondary cyclone guide vane, a conical section, a cold hydrogen guide pipe and an underflow pipe from top to bottom,
the cold hydrogen leading pipe is coaxially arranged in the underflow pipe and is annular, and a cold hydrogen jet orifice is formed along the lower surface of the annular pipe; the sieve mesh sleeve is sleeved on the periphery of the overflow pipe, and the column section is sleeved on the periphery of the sieve mesh sleeve; the gas non-return conical plate is arranged on the sieve pore sleeve; the column section, the conical section and the liquid-descending liquid-phase product eduction tube are communicated from top to bottom; the first-stage rotational flow guide vane and the second-stage rotational flow guide vane are respectively arranged on the inner wall of the column section and the inner wall of the conical section.
In another preferred embodiment, the diameter of the liquid-phase product outlet pipe is 5-10% of the diameter of the pressure-bearing shell, the liquid-phase product outlet pipe and the pressure-bearing shell are arranged coaxially, the liquid-phase product outlet pipe penetrates through the whole reactor, and an outlet is formed in the lower end enclosure.
In another preferred embodiment, the gas non-return conical plate is fixed on the overflow pipe, and the included angle between the oblique side of the triangular section of the gas non-return conical plate and the horizontal line is 20-70 degrees; the first-stage rotational flow guide blade and the second-stage rotational flow guide blade consist of a plurality of rotational flow blades arranged on the inner wall of the column section and the inner wall of the cone section or consist of one spiral channel, two spiral channels or more spiral channels which are processed on the inner walls and are in an internal thread shape; the diameter of the column section is 10-90% of that of the pressure-bearing shell, the height of the column section is 2.5-10% of that of a tangent line of the pressure-bearing shell, and an included angle between a generatrix of the conical section and the horizontal plane is 20-80 degrees; the diameter of the sieve mesh sleeve is 20-80% of that of the pressure-bearing shell, small holes are formed in the sieve mesh sleeve, and the diameter of each small hole is 3-10 times of that of the catalyst particle; the height difference h between the column section and the sieve mesh sleeve1100-500 mm; height difference h between overflow pipe and liquid-phase product outlet pipe2Between 50 and 200 mm; height difference h between cold hydrogen lead pipe and liquid-phase product lead-out pipe3Is between 50 and 100 mm.
In another aspect, the present disclosure provides a method for using the above ebullated-bed hydrogenation reactor, which includes the following steps:
(i) cyclone degassing: at the material level position in the fluidized bed hydrogenation reactor, the three-phase mixture enters the fluidized bed hydrogenation reactor, and large bubbles break and escape into the upper space of the fluidized bed hydrogenation reactor; the mixture composed of the rest liquid phase, catalyst particles and small bubbles enters the column section of the gas-liquid-solid three-phase cyclone separator and the annular gap between the sieve mesh sleeves, a centrifugal force field is formed by the drainage of a primary cyclone guide vane, the small bubbles are driven to move towards the center of the centrifugal force field and enter the annular gaps of the overflow pipe and the sieve mesh sleeves through the small holes on the sieve mesh sleeves, and then are converged and enter the upper space of the reactor upwards; catalyst particles migrate to the periphery of a centrifugal force field under the action of centrifugal force to form a liquid-solid two-phase mixture, and the liquid-solid two-phase mixture enters a secondary cyclone guide vane from an annular gap between a gas non-return conical plate and a column section; and
(ii) and (3) cyclone de-solidification: the liquid-solid two-phase mixture in the step (i) passes through the secondary cyclone guide vane under the pushing of pressure difference, solid particles are thrown to the outer wall under the action of centrifugal force, and the liquid phase forms an upward inner cyclone at the position close to the center, enters an overflow pipe, rises and is finally discharged by a liquid-descending liquid-phase product outlet pipe; solid particles slide down along the wall surface, pass through the bottom of the gas-liquid-solid three-phase cyclone separator and return to the separator for reaction; the gas-liquid-solid three-phase cyclone is coaxially provided with a cold hydrogen guide pipe close to the bottom end, and cold hydrogen is continuously introduced in the three-phase reaction process so as to increase the cyclone separation driving force and prevent liquid phase countercurrent and coking phenomena.
In a preferred embodiment, the ebullated-bed hydrogenation reactor is used in two or more stages in series, wherein a two-phase mixture of air and water enters the inside of the first-stage reactor, so that the raw materials react inside the reactor, the three-phase mixture is separated by a gas-liquid-solid three-phase separator, and a clean liquid-phase product enters the next-stage hydrogenation reactor through a pipeline to continue reacting, so as to obtain a cleaner liquid-phase product; the reactor level difference h4 between each stage is greater than the on-way drag loss +1 m.
In another preferred embodiment, the reaction raw material is a liquid obtained by subjecting various biomasses to rapid thermal cracking, slow thermal cracking, hydro-liquefaction, gasification or carbonization thermal cracking processes.
In another preferred embodiment, the reaction feedstock is atmospheric residue, vacuum residue or distillate oil from petroleum.
In another preferred embodiment, the reaction feedstock is low temperature coal tar, medium temperature coal tar or high temperature coal tar from coal pyrolysis.
In another preferred embodiment, the catalyst particles have a particle size of between 0.05mm and 0.1 mm.
Has the advantages that:
the invention has the advantages that:
1. the full-mixed flow operation of the catalyst can be adopted, the catalyst inventory in the reactor reaches 80 percent, and the utilization rate of the reaction space is high.
2. A bubble-catalyst system with high specific surface area can be adopted, the sizes of bubbles and catalyst particles can be as small as 0.05mm, and the separation precision is ensured.
3. The catalyst can be activated in situ on line, the vibration in the pores of the particles is enhanced by using a rotational flow field, and pollutants in the pores of the catalyst particles are removed by the periodic resultant force of revolution, so that the in-situ activation effect is realized.
4. The heat loss of the liquid phase product outlet is small, and the liquid-descending liquid phase product eduction tube is arranged, so that the liquid phase product can continuously move to the outlet in the reactor after being separated by the three-phase cyclone separator, the heat preservation effect is good, and the heat loss is small.
Drawings
The accompanying drawings are included to provide a further understanding of the disclosure, and are incorporated in and constitute a part of this specification to further illustrate the disclosure and not limit the disclosure.
Fig. 1 is a schematic diagram of the structure of an ebullated bed hydrogenation reactor in a preferred embodiment of the present invention.
Fig. 2 is a schematic structural view of a three-phase separator in a preferred embodiment of the present invention.
FIG. 3 is a schematic representation of the use of ebullated-bed hydrogenation reactor cold die experiments in series in one embodiment of the present invention.
FIG. 4 is a schematic process flow diagram of an ebullated-bed hydrogenation reactor used in a 20000L/h straw pyrolysis liquor hydrodeoxygenation apparatus in an embodiment of the present invention.
Detailed Description
The inventor of the application finds out after extensive and intensive research that cyclone separation, sieve mesh separation and guide vane separation can be mainly adopted to separate gas, liquid and solid phases aiming at the problems of the fluidized bed hydrogenation reactor in the prior art. Based on the above findings, the present invention has been completed.
The gas-liquid-solid three-phase cyclone separator and the down-flow liquid-phase product eduction tube driven by cold hydrogen are arranged in the fluidized bed hydrogenation reactor, so that the three-phase separation of gas phase, liquid phase and catalyst solid particles in the fluidized bed hydrogenation reactor can be realized. The boiling bed hydrogenation reactor is suitable for a multi-section high-pressure hydrogenation process of an easily coking system such as biomass pyrolysis liquid, high carbon residue heavy oil and the like in series.
The ebullated bed hydrogenation reactor of the present invention may use catalyst particles as small as 0.1mm in diameter, with a surface area of about 0.04m2The specific surface area of the catalyst particles is doubled compared with that of the catalyst particles of 0.2 mm. The reason for realizing the function and ensuring the separation precision is that the gas-liquid-solid three-phase cyclone separator arranged in the fluidized bed hydrogenation reactor firstly performs a cyclone degassing process, and the influence of bubbles on the separation is reduced to a great extent, so that smaller bubbles can be used, the specific surface area of gas and liquid is improved, the gas-liquid mass transfer capacity is improved, and the reaction efficiency is finally improved. The invention is suitable for the complete mixed flow circulation operation of the catalyst, the space of the reactor can be fully utilized, the particle size of the catalyst is small, the specific surface area is increased, the mass transfer efficiency is improved, and the reaction is favorably carried out.
The material in the fluidized bed hydrogenation reactor is easy to coke due to a plurality of oxygen-containing species, and multi-stage hydrogenation is usually adopted, wherein hydrogenation is firstly carried out at a lower temperature, then hydrogenation is carried out at a higher temperature (see Chinese patent publication CN 104845668A), and a heating furnace is adopted for heating in an interstage mode. The structure of the invention reduces the temperature loss of the liquid phase outlet, and the liquid phase outlet enters the two-stage boiling bed hydrogenation reactor after being heated by combining with a small-load electric heater. The electricity consumption of the electric heater considers novel green energy sources such as water, electricity and the like, and the carbon emission reduction characteristic of biomass pyrolysis liquid hydrogenation upgrading can be further improved.
In the cyclone separation process, the centrifugal force applied by the centrifugal force field to the dispersed phase in the continuous fluid is far greater than the gravity to which the dispersed phase is subjected; meanwhile, the dispersed phase only needs to migrate to the side wall of the cyclone separator along the radial direction in the cyclone separator, so that the separation speed, the separation precision and the separation efficiency of the cyclone separator are far higher than those of a gravity settling means, and the volume of the equipment is far smaller than that of gravity settling equipment. Based on long-term research on the fully-mixed flow circulating fluidized bed and the cyclone separator, the applicant combines the characteristics of the fully-mixed flow circulating fluidized bed and the cyclone separator, couples the cyclone separator with the fully-mixed flow circulating fluidized bed, can quickly remove the gas phase, the liquid phase and the solid phase at the top of the fully-mixed flow circulating fluidized bed by utilizing the large density difference of the gas phase, the liquid phase and the solid phase to form a liquid-solid two-phase mixture, and then implements liquid-solid separation by combining the liquid-solid cyclone separator, so that a clean liquid-phase product can be quickly obtained and a catalyst is retained in a reactor. A macroscopic circulating flow exists between a liquid phase and a solid phase in the boiling bed hydrogenation reactor, namely the liquid phase and the solid phase are at the ascending speed from the center of the boiling bed hydrogenation reactor and at the descending speed from the side wall of the reactor. The cyclone separator is arranged on the central axis of the reactor, and the catalyst intercepted from the cyclone separator is mixed with the ascending material flow in the reactor when returning to the reaction area of the reactor, so that the concentration of the catalyst in the reactor is more uniform.
Because concentric overflow pipe and sieve mesh sleeve are installed at the top of reactor shell, the moving space of catalyst in the reactor is increased, so that the reactor has the advantages of high catalyst reserve and high reactor utilization rate.
The liquid phase outlet of the downcomer is combined with the structure of the three-phase cyclone, so that liquid phase products can be continuously and quickly led out. The boiling bed hydrogenation reactor is used in a series connection method, and the height difference of the liquid level of the reactor between every two stages needs to be controlled, so that the liquid phase outlet cutoff caused by fluctuation of gas phase flow is prevented. In the biomass hydrogenation process, the reactors in all sections need to be heated, and if the flow is cut off, the heating furnace can be burnt through due to overheating.
Adopt gas-liquid solid three-phase cyclone, cyclone degassing back cyclone is taken off admittedly earlier, adopt this structure after, separation accuracy improves by a wide margin, mainly because it carries out cyclone degassing process at first, has avoided the influence of bubble to follow-up cyclone and has taken off solid process, and second is external cold hydrogen drive, and it has mainly to prevent that gas-liquid solid three-phase cyclone bottom outlet department high concentration catalyst thick liquids coking, formation negative pressure are with the effect of reinforcing whirl thrust.
In a first aspect of the present disclosure, there is provided an ebullated-bed hydrogenation reactor comprising: the device comprises a pressure-bearing shell, a gas-liquid-solid three-phase cyclone separator arranged in the upper space of the pressure-bearing shell, a liquid-descending liquid-phase product eduction tube arranged in the middle of the pressure-bearing shell, and a gas-phase outlet, a liquid-phase outlet and a gas-liquid mixed-phase inlet which are arranged on the pressure-bearing shell.
In the disclosure, the gas-liquid-solid three-phase cyclone separator is formed by sequentially arranging a sieve mesh sleeve, a primary cyclone guide vane, a column section, a gas non-return conical plate, an overflow pipe, a secondary cyclone guide vane, a conical section, a cold hydrogen leading pipe and an underflow pipe from top to bottom, wherein the cold hydrogen leading pipe is coaxially arranged in the underflow pipe and is annular, and a cold hydrogen jet orifice is formed along the lower surface of the annular pipe; the sieve mesh sleeve is sleeved on the periphery of the overflow pipe, and the column section is sleeved on the periphery of the sieve mesh sleeve; the gas non-return conical plate is arranged on the sieve pore sleeve; the column section, the conical section and the liquid-descending liquid-phase product eduction tube are communicated from top to bottom; the first-stage and second-stage rotational flow guide vanes are respectively arranged on the inner wall of the column section and the inner wall of the cone section.
In the disclosure, the diameter of the liquid-descending liquid-phase product eduction tube is 5% -10% of the diameter of the pressure-bearing shell, the liquid-descending liquid-phase product eduction tube and the pressure-bearing shell are coaxially arranged, the liquid-descending liquid-phase product eduction tube penetrates through the inside of the whole reactor vessel, and an outlet is arranged at the lower end socket.
In the disclosure, the gas non-return conical plate is fixed on the overflow pipe, and the included angle between the oblique side of the triangular section and the horizontal line is 20-70 degrees.
In the disclosure, the first-stage and second-stage swirl guide vanes are composed of a plurality of swirl vanes arranged on the inner wall of the column section and the inner wall of the cone section or are composed of one helical channel, two helical channels or more helical channels which are processed on the inner wall and are in an internal thread shape.
In the disclosure, the diameter of the column section is 10-90% of the diameter of the pressure-bearing shell, the height of the column section is 2.5-10% of the tangential height of the pressure-bearing shell, and the included angle between the generatrix of the conical section and the horizontal plane is 20-80%.
In the disclosure, the diameter of the sieve pore sleeve is 20-80% of the diameter of the pressure-bearing shell; the sieve mesh sleeve is provided with small holes, and the diameter of each small hole is 3-10 times of the particle size of the catalyst particles.
In the disclosure, the height difference h1 between the column section and the sieve mesh sleeve is 100-500 mm; the height difference h2 between the overflow pipe and the liquid-phase product outlet pipe is 50-200 mm; the height difference h3 between the cold hydrogen guiding pipe and the liquid-descending liquid-phase product leading-out pipe is 50-100 mm.
In a second aspect of the present disclosure, there is provided a method for using the above ebullated-bed hydrogenation reactor, the method comprising the steps of:
(i) cyclone degassing: at the material level position in the fluidized bed hydrogenation reactor, the three-phase mixture enters the fluidized bed hydrogenation reactor, and large bubbles break and escape into the upper space of the fluidized bed hydrogenation reactor; the mixture composed of the rest liquid phase, catalyst particles and small bubbles enters the column section of the gas-liquid-solid three-phase cyclone separator and the annular gap between the sieve mesh sleeves, a centrifugal force field is formed by the drainage of a primary cyclone guide vane, the small bubbles are driven to move towards the center of the centrifugal force field and enter the annular gaps of the overflow pipe and the sieve mesh sleeves through the small holes on the sieve mesh sleeves, and then are converged and enter the upper space of the reactor upwards; catalyst particles migrate to the periphery of a centrifugal force field under the action of centrifugal force to form a liquid-solid two-phase mixture, and the liquid-solid two-phase mixture enters a secondary cyclone guide vane from an annular gap between a gas non-return conical plate and a column section; and
(ii) and (3) cyclone de-solidification: the liquid-solid two-phase mixture in the step (i) passes through the secondary cyclone guide vane under the pushing of pressure difference, solid particles are thrown to the outer wall under the action of centrifugal force, and the liquid phase forms an upward inner cyclone at the position close to the center, enters an overflow pipe, rises and is finally discharged by a liquid-descending liquid-phase product outlet pipe; solid particles slide down along the wall surface, pass through the bottom of the gas-liquid-solid three-phase cyclone separator and return to the separator for reaction; the gas-liquid-solid three-phase cyclone is coaxially provided with a cold hydrogen guide pipe close to the bottom end, and cold hydrogen is continuously introduced in the three-phase reaction process so as to increase the cyclone separation driving force and prevent liquid phase countercurrent and coking phenomena.
In the present disclosure, two or more ebullated bed hydrogenation reactors may be used in series for optimal effect; the method comprises the following steps that a two-phase mixture of air and water enters a reactor, so that raw materials react in the reactor, the three-phase mixture is separated through a three-phase separator, and a clean liquid-phase product enters a next-stage hydrogenation reactor through a pipeline to continue reacting, so that a cleaner liquid-phase product is obtained; the reactor level difference h4 between each stage needs to be greater than the on-way drag loss +1 m.
In the present disclosure, the reaction raw material is a liquid obtained by subjecting various biomasses to rapid thermal cracking, slow thermal cracking, hydrogenation liquefaction, gasification or carbonization thermal cracking processes.
In the present disclosure, the reaction raw material is atmospheric residue, vacuum residue or distillate oil derived from petroleum.
In the present disclosure, the reaction raw material is low-temperature coal tar, medium-temperature coal tar or high-temperature coal tar from coal pyrolysis.
In the present disclosure, the catalyst particles have a particle size between 0.05mm and 0.1 mm.
Reference is made to the accompanying drawings.
Fig. 1 is a schematic diagram of the structure of an ebullated bed hydrogenation reactor in a preferred embodiment of the present invention. As shown in fig. 1, the ebullated-bed hydrogenation reactor comprises: the device comprises a pressure-bearing shell 3, a gas-liquid-solid three-phase cyclone separator arranged in the upper space of the pressure-bearing shell, a liquid-descending liquid-phase product eduction tube 14 arranged in the middle of the pressure-bearing shell, a gas-phase outlet 7, a liquid-phase outlet 15 and a gas-liquid mixed-phase inlet 1 which are arranged on the pressure-bearing shell, and a distributor 2 arranged at the lower part of the pressure-bearing shell; the gas-liquid-solid three-phase cyclone separator is formed by sequentially arranging a sieve mesh sleeve 8, a primary cyclone guide vane 9, a column section 6, a gas non-return conical plate 10, an overflow pipe 11, a secondary cyclone guide vane 12, a conical section 5, a cold hydrogen guide pipe 13 and an underflow pipe 4 from top to bottom; the cold hydrogen leading pipe 13 is coaxially arranged in the underflow pipe and is annular, and a cold hydrogen jet orifice is formed along the lower surface of the annular pipe; the sieve mesh sleeve 8 is sleeved on the periphery of the overflow pipe 11, and the column section 6 is sleeved on the periphery of the sieve mesh sleeve 8; the gas non-return conical plate 10 is arranged on the sieve pore sleeve 8; the column section 6, the conical section 5 and the liquid-descending liquid-phase product eduction tube 14 are communicated from top to bottom; the first-stage cyclone guide vane 9 and the second-stage cyclone guide vane 12 are respectively arranged on the inner wall of the column section and the inner wall of the cone section;
the gas-liquid-solid three-phase cyclone separator provides space for separating a gas-liquid-solid three-phase mixture, and the diameter of a column section 6 of the gas-liquid-solid three-phase cyclone separator is 10-90% of that of a pressure-bearing shell 3; the three-phase mixture enters an annular gap between a sieve mesh sleeve 8 and a column section 6 of the gas-liquid-solid three-phase cyclone, and the gas phase enters the upper space of the reactor after large bubbles are broken; the rest three-phase mixture rotates through a first-stage rotational flow guide vane 9, solid particles are thrown to the outer wall by using density difference and centrifugal force and are settled under the action of gravity, and liquid moves upwards under the action of internal rotational flow when reaching the lower end of the sieve mesh sleeve 8 and finally enters a liquid-descending liquid-phase product eduction tube to be discharged;
the small holes on the sieve mesh sleeve 8 which is coaxially arranged with the three-phase cyclone have a crushing effect on micro bubbles in a liquid phase, solid particles carried by a bubble interface settle after passing through the small holes and being crushed, and gas phase is converged and then moves upwards to an upper space; the solid particles are settled under the action of gravity, move to a gas non-return conical plate and then are led to the conical section space of the three-phase cyclone to be mixed with the liquid phase, and only liquid and solid phases exist in the space, so that the gas phase in the three phases is removed;
the cone section of the three-phase cyclone provides a space for secondary cyclone separation for liquid-solid two-phase flow, the centrifugal force effect is more obvious, and solid particles can effectively migrate to the inner wall of the cyclone and slide down along the wall surface for sedimentation;
the second-stage rotational flow guide vane 12 is composed of a plurality of rotational flow vanes arranged on the inner wall of the conical section or is composed of a spiral channel which is processed on the inner wall of the column section and is in an internal thread shape; when the liquid-solid two-phase flow passes through the structure, liquid-solid separation is completed for the third time; the purified liquid phase rises along the overflow pipe 11 under the action of internal rotational flow and is discharged to the outside of the reactor from the liquid-phase product outlet pipe 14;
the lower part of the gas-liquid-solid three-phase cyclone is provided with a cold hydrogen lead pipe 13, and cold hydrogen is continuously introduced inwards, so that liquid phase is not easy to coke, a negative pressure enhanced cyclone driving force is formed, separated solid particles flow out from the bottom of the gas-liquid-solid three-phase cyclone, liquid phase countercurrent and coking phenomena are prevented, and the separation effect and precision are ensured.
Fig. 2 is a schematic structural view of a three-phase separator in a preferred embodiment of the present invention. As shown in figure 2, the gas-liquid-solid three-phase cyclone separator sequentially comprises a sieve mesh sleeve 8, a primary cyclone guide vane 9, a column section 6, a gas non-return conical plate 10, an overflow pipe 11, a secondary cyclone guide vane 12, a conical section 5 and a cold air pipe from top to bottomThe hydrogen leading pipe 13 and the underflow pipe 4 are arranged; the cold hydrogen leading pipe 13 is coaxially arranged in the underflow pipe and is annular, and a cold hydrogen jet orifice is formed along the lower surface of the annular pipe; the sieve mesh sleeve 8 is sleeved on the periphery of the overflow pipe 11, and the column section 6 is sleeved on the periphery of the sieve mesh sleeve 8; the gas non-return conical plate 10 is arranged on the sieve pore sleeve 8; the column section 6, the conical section 5 and the liquid-descending liquid-phase product eduction tube are communicated from top to bottom; the first-stage cyclone guide vane 9 and the second-stage cyclone guide vane 12 are respectively arranged on the inner wall of the column section and the inner wall of the cone section; wherein, D is the diameter of the pressure-bearing shell of the reactor, DsDenotes the diameter of the three-phase separator mesh sleeve, dyDenotes the diameter of the overflow pipe of the three-phase separator, dzDenotes the diameter of the column section of the three-phase separator, djThe diameter h of the liquid-phase product outlet pipe1Indicates the height difference between the column section and the sieve mesh sleeve, h2Indicates the height difference between the overflow pipe and the liquid-phase product outlet pipe3The height difference between the cold hydrogen lead pipe and the liquid-phase product lead-out pipe is shown, dkThe diameter of the small hole on the screen hole sleeve is shown, alpha is the angle of the conical section of the three-phase separator, beta1Indicating the angle of inclination, beta, of the first-stage swirl guide vane2Indicating the secondary swirl guide vane angle.
FIG. 3 is a schematic representation of the use of ebullated-bed hydrogenation reactor cold die experiments in series in one embodiment of the present invention. As shown in fig. 3, water is pumped into the reactor through a pump 36 from a gas-liquid mixed phase inlet 31 at the bottom of the ebullated bed hydrogenation reactor 33-1; air is pressurized by an air compressor 32 and then enters the reactor from a gas-liquid mixed phase inlet at the bottom of the fluidized bed hydrogenation reactor; under the action of momentum transfer with air, catalyst particles in a fluidized bed hydrogenation reactor reach a fluidized state; separating a gas-liquid-solid three-phase mixture in a fluidized bed hydrogenation reactor through a three-phase separator at the top of the reactor, discharging the obtained gas phase (and air) from a gas phase outlet of the fluidized bed hydrogenation reactor, discharging the obtained liquid phase from a liquid-descending liquid phase product eduction tube 34 of the fluidized bed hydrogenation reactor, continuing to react through a fluidized bed hydrogenation reactor 33-2 in series with two stages to realize deep purification and high-efficiency reaction of a liquid phase product, discharging the obtained gas phase (and air), and feeding the obtained liquid phase into a circulating tank 35 for recycling, wherein h is4To representThe difference in liquid level between the two reactors.
FIG. 4 is a schematic process flow diagram of an ebullated-bed hydrogenation reactor used in a 20000L/h straw pyrolysis liquor hydrodeoxygenation apparatus in an embodiment of the present invention. As shown in fig. 4, firstly, introducing a mixture of straw pyrolysis liquid and hydrogen (new hydrogen) into a heating furnace 41, introducing the heated two-phase mixture into a fluidized bed hydrogenation reactor 43-1 from the bottom, after the mixture is subjected to full reaction with a catalyst inside the reactor and a separation process of a three-phase separator, discharging the mixture through a down-flow liquid-phase product eduction tube 42-1 inside the reactor, returning the reacted oil back to the heating furnace again for heating, then introducing the oil into a fluidized bed hydrogenation reactor 43-2 through a gas-liquid mixed phase inlet 44, after the re-reaction and separation, discharging a crude product and a part of gas mixture through a down-flow liquid-phase product eduction tube 42-2 inside the reactor, introducing the crude product and the part of gas mixture into a medium-pressure separator 48 for separation, and lifting the product oil (liquid-phase product) to a fractionating tower 40 at the bottom of the medium-pressure separator under the action of a pump 49 for the next process; the hydrogen and part of the liquid phase mixture at the upper gas phase outlet of the two-stage reactor are cooled by an air cooler 45 and then enter a high-pressure separator 46, the liquid phase enters a medium-pressure separator from the bottom of the high-pressure separator, and the circulating hydrogen is returned to the inlet through an air compressor 47 at the upper part of the high-pressure separator to be mixed and reacted with the straw pyrolysis liquid again; returning a part of liquid-phase products in the medium-pressure separator to the inlet to continuously participate in the reaction; the final product is 2% naphtha, 20% gasoline, 50% diesel, 28% heavy diesel, etc.
Examples
The invention is further illustrated below with reference to specific examples. It is to be understood, however, that these examples are illustrative only and are not to be construed as limiting the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the manufacturer. All percentages and parts are by weight unless otherwise indicated.
Example 1:
the ebullated-bed hydrogenation reactor was used for a 3000L/h ebullated-bed hydrogenation reactor cold die experiment.
1. Process flow
As shown in fig. 3.
2. Major structure size of boiling bed hydrogenation separator
The main structure size of the boiling bed hydrogenation reactor is shown in the following table 1, and the size structure of the two-stage boiling bed hydrogenation separator is completely consistent.
Table 1: 3000L/h boiling bed hydrogenation reactor cold mould device structure size
3. Effects of the implementation
The test process of the 3000L/h boiling bed hydrogenation cold die device adopts water and air for test, and the test results are shown in the following table 2. From the test results, the catalyst reaches uniform fluidization, the catalyst does not have faults after continuously running for 30 hours, and the 0.1mm catalyst carrying-out amount is controlled to be less than 2 mu g/g.
Table 2: test result of 3000L/h boiling bed hydrogenation cold mould device
Example 2:
the fluidized bed hydrogenation reactor is used for a 20000L/h straw pyrolysis liquid hydrodeoxygenation device.
1. Process flow
As shown in fig. 4.
2. Main structure size of fluidized bed hydrogenation reactor
The main structure dimensions of the ebullated-bed hydrogenation reactor are shown in table 3 below, and the size structures of the two-stage ebullated-bed hydrogenation separators are completely consistent.
Table 3: boiling bed reactor structure size of 20000L/h sewage straw hydrolysate hydrodeoxygenation device
3. Effects of the implementation
The test process of the 20000L/h polluted straw hydrolysate hydrodeoxygenation device adopts the straw pyrolysis solution for testing, and the test results are shown in the following table 4. From the test results, the catalyst reaches uniform fluidization, no reactor coking occurs after the catalyst is continuously operated for 2000 hours, and the carrying-out quantity of the catalyst with the thickness of 0.1mm is controlled to be less than 2.5 mu g/g.
Table 4: 20000L/h straw pyrolysis liquid hydrodeoxygenation device test result
The above-listed embodiments are merely preferred embodiments of the present disclosure, and are not intended to limit the scope of the present disclosure. That is, all equivalent changes and modifications made according to the contents of the claims of the present application should be considered to be within the technical scope of the present disclosure.
All documents referred to in this disclosure are incorporated by reference into this application as if each were individually incorporated by reference. Furthermore, it should be understood that various changes or modifications to the disclosure may be made by those skilled in the art after reading the above teachings of the disclosure, and such equivalents may fall within the scope of the disclosure as defined by the appended claims.
Claims (9)
1. An ebullated bed hydrogenation reactor comprising:
a pressure-bearing outer shell (3),
a gas-liquid-solid three-phase cyclone separator arranged in the upper space of the pressure-bearing shell,
a liquid-descending liquid-phase product outlet pipe (14) arranged in the middle of the pressure-bearing shell, and
a gas phase outlet (7), a liquid phase outlet (15) and a gas-liquid mixed phase inlet (1) which are arranged on the pressure-bearing shell,
wherein, the gas-liquid-solid three-phase cyclone separator is sequentially formed by arranging a sieve mesh sleeve (8), a primary cyclone guide vane (9), a column section (6), a gas non-return conical plate (10), an overflow pipe (11), a secondary cyclone guide vane (12), a conical section (5), a cold hydrogen guide pipe (13) and an underflow pipe (4) from top to bottom,
the cold hydrogen leading pipe is coaxially arranged in the underflow pipe and is annular, and a cold hydrogen jet orifice is formed along the lower surface of the annular pipe; the sieve mesh sleeve is sleeved on the periphery of the overflow pipe, and the column section is sleeved on the periphery of the sieve mesh sleeve; the gas non-return conical plate is arranged on the sieve pore sleeve; the column section, the conical section and the liquid-descending liquid-phase product eduction tube are communicated from top to bottom; the first-stage rotational flow guide vane and the second-stage rotational flow guide vane are respectively arranged on the inner wall of the column section and the inner wall of the conical section.
2. The ebullated bed hydrogenation reactor of claim 1, wherein the diameter of the liquid-reducing liquid-phase product outlet pipe is 5-10% of the diameter of the pressure-bearing shell, the liquid-reducing liquid-phase product outlet pipe and the pressure-bearing shell are arranged coaxially, the liquid-reducing liquid-phase product outlet pipe penetrates through the whole reactor, and an outlet is formed in the lower end socket.
3. The ebullated bed hydrogenation reactor of claim 1 wherein the gas check cone plate is fixed to the overflow tube with the angled side of the triangular cross section forming an angle of 20 ° to 70 ° with the horizontal; the first-stage rotational flow guide blade and the second-stage rotational flow guide blade consist of a plurality of rotational flow blades arranged on the inner wall of the column section and the inner wall of the cone section or consist of one spiral channel, two spiral channels or more spiral channels which are processed on the inner walls and are in an internal thread shape; the diameter of the column section is 10-90% of that of the pressure-bearing shell, the height of the column section is 2.5-10% of that of a tangent line of the pressure-bearing shell, and an included angle between a generatrix of the conical section and the horizontal plane is 20-80 degrees; the diameter of the sieve mesh sleeve is 20-80% of that of the pressure-bearing shell, small holes are formed in the sieve mesh sleeve, and the diameter of each small hole is 3-10 times of that of the catalyst particle; the height difference h between the column section and the sieve mesh sleeve1100-500 mm; height difference h between overflow pipe and liquid-phase product outlet pipe2Between 50 and 200 mm; height difference h between cold hydrogen lead pipe and liquid-phase product lead-out pipe3Is between 50 and 100 mm.
4. A method of using the ebullated bed hydrogenation reactor of any one of claims 1-3, the method comprising the steps of:
(i) cyclone degassing: at the material level position in the fluidized bed hydrogenation reactor, the three-phase mixture enters the fluidized bed hydrogenation reactor, and large bubbles break and escape into the upper space of the fluidized bed hydrogenation reactor; the mixture composed of the rest liquid phase, catalyst particles and small bubbles enters the column section of the gas-liquid-solid three-phase cyclone separator and the annular gap between the sieve mesh sleeves, a centrifugal force field is formed by the drainage of a primary cyclone guide vane, the small bubbles are driven to move towards the center of the centrifugal force field and enter the annular gaps of the overflow pipe and the sieve mesh sleeves through the small holes on the sieve mesh sleeves, and then are converged and enter the upper space of the reactor upwards; catalyst particles migrate to the periphery of a centrifugal force field under the action of centrifugal force to form a liquid-solid two-phase mixture, and the liquid-solid two-phase mixture enters a secondary cyclone guide vane from an annular gap between a gas non-return conical plate and a column section; and
(ii) and (3) cyclone de-solidification: the liquid-solid two-phase mixture in the step (i) passes through the secondary cyclone guide vane under the pushing of pressure difference, solid particles are thrown to the outer wall under the action of centrifugal force, and the liquid phase forms an upward inner cyclone at the position close to the center, enters an overflow pipe, rises and is finally discharged by a liquid-descending liquid-phase product outlet pipe; solid particles slide down along the wall surface, pass through the bottom of the gas-liquid-solid three-phase cyclone separator and return to the fluidized bed hydrogenation reactor for reaction; the gas-liquid-solid three-phase cyclone is coaxially provided with a cold hydrogen guide pipe close to the bottom end, and cold hydrogen is continuously introduced in the three-phase reaction process so as to increase the cyclone separation driving force and prevent liquid phase countercurrent and coking phenomena.
5. The method of claim 4, wherein the ebullated-bed hydrogenation reactor is used in two or more stages in series, wherein a two-phase mixture of air and water is introduced into the reactor of the first stage, so that the raw material is reacted in the reactor, the three-phase mixture is separated by a gas-liquid-solid three-phase separator, and a clean liquid-phase product is introduced into the hydrogenation reactor of the next stage through a pipeline to be reacted continuously, so as to obtain a cleaner liquid-phase product; the reactor level difference h4 between each stage is greater than the on-way drag loss +1 m.
6. The method of claim 4 or 5, wherein the reaction raw material is a liquid obtained by subjecting various biomasses to a rapid thermal cracking process, a slow thermal cracking process, a hydrogenation liquefaction process, a gasification process or a carbonization thermal cracking process.
7. The process according to claim 4 or 5, wherein the reaction raw material is atmospheric residue, vacuum residue or distillate oil derived from petroleum.
8. The process according to claim 4 or 5, characterized in that the reaction raw material is low-temperature coal tar, medium-temperature coal tar or high-temperature coal tar from coal pyrolysis.
9. The method of claim 4 or 5, wherein the catalyst particles have a particle size of between 0.05mm and 0.1 mm.
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