CN110732297A - System and method for loading particles into a microchannel reactor - Google Patents
System and method for loading particles into a microchannel reactor Download PDFInfo
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- CN110732297A CN110732297A CN201810796769.7A CN201810796769A CN110732297A CN 110732297 A CN110732297 A CN 110732297A CN 201810796769 A CN201810796769 A CN 201810796769A CN 110732297 A CN110732297 A CN 110732297A
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- 238000011068 loading method Methods 0.000 title claims abstract description 41
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- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention relates to the technical field of microchannel reactors, and discloses systems and methods for loading particles into a microchannel reactor, wherein the systems comprise a conveying gas control unit, a particle storage tank, a dust removal device, a conveying pipeline, a distributor and the microchannel reactor, the conveying gas control unit is used for controlling the speed of gas entering the particle storage tank in stages, so that the gas flow in the initial stage is smaller than the initial fluidization speed of the particles, and the gas flow in other stages is not smaller than the initial fluidization speed, the distributor comprises a channel part connected with the conveying pipeline and a diameter expansion part, and the lower end surface of the diameter expansion part is matched with the upper end surface of the microchannel reactor, so that the distributed fluidization particles enter reaction microchannels of the microchannel reactor.
Description
Technical Field
The invention relates to the technical field of microchannel reaction, in particular to systems and methods for loading particles into a microchannel reactor.
Background
The microchannel reaction technology is which is a new technology of the chemical engineering subject of the twenty century, has incomparable advantages of a conventional reactor, and is particularly characterized in that a reaction channel is in a micron level, the surface area is large, the reactor has high mass transfer and heat transfer rates, the heat transfer coefficient is high, chemical reaction can occur under an isothermal condition, the phenomenon of temperature runaway is avoided, the application of high-activity and low-strength catalysts is realized, the engineering amplification is simple due to the modularized form, the reaction load per unit volume of the reactor is high, and the miniaturization of a large reactor is realized.
CN1607032A discloses methods for loading catalyst by dropping the catalyst into the reaction tube of a fixed-bed multitubular reactor, which is to insert chain-like substances into the reaction tube during the loading process so that the lower end of the chain-like substances is located higher than the upper end of the catalyst layer, which largely avoids the "bridging" of the catalyst during the loading process and the damage to the catalyst by the physical impact of the catalyst dropping.
CN1143537A discloses methods for uniformly loading solid particle catalysts into a tubular reactor, wherein the catalyst is divided into a plurality of thin flows with the same flow rate and loaded into the reactor at the same speed when the catalyst is loaded, the method is applied to the catalyst loading of the tubular reactor, the reactor consists of a plurality of tubes with the diameter of 15-50 mm, the size of the catalyst particles is 1-5 mm, the reactor has large volume and good operation space, and the device such as a diversion chain, a distributor and the like can be used for auxiliary loading, however, the reaction channel and the catalyst size of the microchannel reactor are both smaller than those of the conventional reaction by orders of magnitude, so that the diversion chain, the distributor and the like cannot be used.
CN101918128A discloses methods for loading and unloading particles into a microchannel reactor, which comprises placing ultrasonic generators on the upper end of the microchannel reactor, using ultrasonic waves to generate vibration during loading, so that catalyst particles are gradually added from the upper end of the reactor, and the catalyst particles can be densely filled into the microchannel, and providing reservoirs on the upper end of the microchannel reactor, wherein the reservoirs are filled with particles, the reservoirs comprise a slide and a slide , the slide can move to form an opening, gas can be introduced from the lower end of the microchannel reactor, the particles are blown out of the microchannel, then the flow rate of the gas is reduced, so that the particles can be refilled in the microchannel, and after several fluidization cycles, uniformly filled microchannels are obtained.
Disclosure of Invention
The present invention aims to overcome the above problems in the prior art and provide systems and methods for loading particles into a microchannel reactor, which not only can achieve uniform filling of particles, but also has the advantages of simple operation, etc.
According to th aspect of the invention, the invention provides systems for loading particles into a microchannel reactor, which comprise a conveying gas control unit, a particle storage tank, a dust removal device, a conveying pipeline, a distributor and the microchannel reactor, wherein the upper part of the particle storage tank is provided with a feeding port for adding particles, the lower part of the particle storage tank is provided with a gas inlet for introducing gas, and a gas distributor is arranged in the tank;
the conveying gas control unit can control the gas speed entering the particle storage tank in stages, so that the gas flow in the initial stage is smaller than the initial fluidization speed of the particles, and the gas flow in other stages is larger than the initial fluidization speed of the particles to realize the fluidization of the particles, thereby obtaining fluidized particles;
the dust removal device is used for removing the tank top gas obtained by contacting the gas of the initial stage with the particles so as to remove the lighter part in the particles;
the delivery conduit is for delivering the fluidized particulates to the distributor;
the distributor comprises a channel part connected with the conveying pipeline and a diameter expanding part, and the lower end face of the diameter expanding part is matched with the upper end of the microchannel reactor so that fluidized particles distributed by the distributor enter a reaction microchannel of the microchannel reactor;
the lower end of the microchannel reactor is provided with a lower porous support body, so that particles in fluidized particles entering the reaction microchannel are left in the microchannel and gas is discharged.
According to a second aspect of the present invention, there is provided a method of loading particles into a microchannel reactor, the method being performed in the system of aspect of the present invention, comprising:
1) introducing a gas into said fines storage tank at a flow rate less than the initial fluidization velocity of said fines to contact the fines, and venting the overhead gas from the contact through said dedusting apparatus to remove the lighter portion of the fines;
2) and increasing the gas flow velocity to be higher than the initial fluidization velocity, fluidizing the residual particles, introducing the obtained fluidized particles into the distributor for distribution, and uniformly entering reaction micro-channels of the micro-channel reactor.
The method of the invention can uniformly load the solid particles into each reaction channel in the microchannel reactor by combining with the system, the amount of the particles in different channels is basically the same, and the result that the reaction is deteriorated due to the bias current existing in the fluid distribution in the reaction process caused by uneven loading is avoided. For example, after loading the Fischer-Tropsch synthesis catalyst into the microchannel reactor, the reactor is introduced into the reaction system for Fischer-Tropsch synthesis reaction, the pressure drop of the reactor is small, the catalytic activity of the catalyst is high, and the selectivity of byproducts is low.
In addition, the system provided by the invention has the characteristics of simple structure, reusability and simple and convenient operation.
Drawings
FIG. 1 shows a schematic of the loading of catalyst into a microchannel reactor in embodiments of the invention.
Description of the reference numerals
1: a conveying gas control unit; 2: a catalyst tank; 3: a hose; 4: a dispenser; 5: a microchannel reactor; 6: a feed inlet.
Detailed Description
For numerical ranges, between the endpoints of each range and the individual points, and between the individual points may be combined with each other to yield new numerical ranges or ranges, which should be considered as specifically disclosed herein.
According to of the present invention, there is provided a system for loading particles into a microchannel reactor, the system comprising a transport gas control unit, a dust removal device, a particle reservoir, a transport conduit, a distributor, and a microchannel reactor;
the upper part (preferably the top) of the particle storage tank is provided with a feed inlet for adding particles, the lower part (preferably the bottom) of the particle storage tank is provided with a gas inlet for introducing gas, and a gas distributor is arranged in the tank;
the conveying gas control unit can control the gas velocity entering the particle storage tank in stages, so that the gas flow in the initial stage is smaller than the initial fluidization velocity of the particles, and the gas flow in other stages (hereinafter also referred to as "fluidization stage") is larger than the initial fluidization velocity to realize fluidization of the particles, thereby obtaining fluidized particles;
the dust removal device is used for removing the tank top gas obtained by contacting the gas of the initial stage with the particles so as to remove the lighter part in the particles;
the delivery conduit is for delivering the fluidized particulates to the distributor;
the distributor comprises a channel part connected with the conveying pipeline and a diameter expanding part, and the lower end face of the diameter expanding part is matched with the upper end of the microchannel reactor so that fluidized particles distributed by the distributor enter a reaction microchannel of the microchannel reactor;
the lower end of the microchannel reactor is provided with a lower porous support body, so that particles in fluidized particles entering the reaction microchannel are left in the microchannel and gas is discharged.
According to the system of the present invention, the particle storage tank may be a vertical cylindrical tank, and the upper and lower portions of the cylindrical shell are provided with arc-shaped end surfaces for increasing the effective height of the storage tank. Preferably, the height-to-diameter ratio (ratio of height to diameter) of the particulate reservoir is greater than 10. More preferably, the height-diameter ratio of the particle storage tank is 12 to 20, so that part of particles are prevented from remaining in the particle storage tank without being fluidized in the fluidization period.
The selection of the gas distributor is not particularly limited, as long as the gas can be uniformly dispersed and the material is not blocked.
According to the system of the present invention, the particulate loading system includes a dust removal device for removing smaller particulates from the top gas of the particulate tank after contact with the gas and particulates in the particulate tank and prior to non-fluidization during particulate loading, wherein the dust removal device may be connected above the particulate tank by a conduit having a valve .
According to the system of the invention, the transport gas control unit is used to control the gas velocity entering the particle storage tank in stages, including an initiation stage and a fluidization stage. Specifically, the gas flow is controlled to be smaller than the initial fluidization velocity of the fine particles in the initial stage, so that the lighter part of the fine particles can be sent to the tank top by the gas flow to be removed; and controlling the gas flow to be larger than the initial fluidization speed of the particles in the fluidization stage so as to realize fluidization of the whole particles and obtain fluidized particles. Typically, the transport gas control unit comprises a conduit connected to the gas inlet, and the control of the gas flow rate is achieved by providing a flow control valve on the conduit.
The system of the present invention utilizes a flowing gas phase (gas stream) as a carrier to carry the particles into the microchannel reactor, and thus, the particles can be any particles that can be fluidized by the gas stream. The particles may be spherical, cylindrical or of other shape, preferably spherical.
Generally, the particle size of the fine particles may be in the range of 15 to 500. mu.m, preferably 50 to 300. mu.m. Preferably, the particle size distribution in the fine particles is the median particle diameter (D)50) Particles of + -15 μm are larger than 70%, i.e. the particle size distribution is (D)50-15 μm) to (D)50+15 μm) range of greater than 70%. More preferably, the particles have a size distribution of more than 70% of the particles with a median particle size of. + -. 10 μm, i.e.a size distribution of (D)50-10 μm) to (D)50+10 μm) range of greater than 70%.
In addition, the compression strength of the particles is preferably greater than 5N/mm2More preferably greater than 10N/mm2。
According to the present invention, the particles may be a catalyst, and the catalyst may be any catalyst that can be reacted by using a microchannel reactor, such as a fischer-tropsch synthesis catalyst, a methanol synthesis catalyst, and the like. The fischer-tropsch synthesis catalyst is for example a cobalt based fischer-tropsch synthesis catalyst.
It will be understood by those skilled in the art that the term "lighter fraction" herein refers to particulates having relatively small particle size and lighter impurity components. For reactions where the particles are catalysts, the lighter fraction of the particles is detrimental to the reaction.
According to the system of the invention, the enlarged diameter portion of the distributor may be in the shape of a cone. Preferably, the expanded diameter portion of the distributor is in the shape of a regular pyramid or a regular cone, and the apex angle of the cone may be 30 ° to 120 °, more preferably 60 ° to 90 °.
According to the system of the present invention, the transport conduit is used to transport the fluidized particulates to the distributor, which may be selected from a hose or a rigid pipe, preferably a hose, which further reduces particle settling and attrition.
In the system according to the present invention, the microchannel reactor may be selected with reference to the prior art, and the present invention is not particularly limited thereto, and may be any microchannel reactor suitable for loading with particles. Typically, the microchannel reactor comprises at least 1 reaction microchannel, preferably more than 50 (e.g. 50 to 1000) of the reaction microchannels. The upper end face of the microchannel reactor is preferably rectangular. The microchannel reactor may be a layered structure reactor (e.g., formed by stacking a plurality of castellated metal sheets), and may include a plurality of the reaction microchannels between each layer of the layered structure. When the upper end face of the microchannel reactor is rectangular, in order to better realize the sealing with the reactor, the lower end face of the diameter expanding part of the distributor can also have a thickness which does not influence the loading effect, generally, the ratio of the thickness to the height of the whole diameter expanding part can be 1: 4-10, and the thickness is small, so that the shape of the whole diameter expanding part can not be influenced by the part.
Optionally, the microchannel reactor can also comprise a heat taking (heating) channel for introducing a heat-conducting medium, and the reaction microchannel and the heat taking (heating) channel can be alternately arranged and formed with for leading the particles and the heat-conducting medium to flow in a cocurrent mode, a crosscurrent mode and the like.
According to preferred embodiments, the reaction microchannels have a rectangular cross-section, each channel has a length of 1-1000 cm and a width and/or height of no greater than 1000 μm.
According to the system of the present invention, the bottom of the microchannel reactor is provided with a lower porous support for fixing the particles in the reaction microchannel, and for discharging the gas out of the reaction microchannel.
In addition, besides the lower porous support body, a lower end socket can be arranged on the microchannel reactor, a material flow channel is arranged in the lower end socket, the material flow channel can lead the gas exhausted by the lower porous support body to be exhausted through the lower end socket, and the material flow channel can lead the microchannel reactor to introduce or exhaust reactant flow when the microchannel reactor is used for reaction (such as Fischer-Tropsch synthesis reaction).
In order to allow the microchannel reactor loaded with the microparticles to be directly applied to a reaction system according to the system of the present invention, it is preferable that the system further comprises an upper end porous support for fixing the upper end of the microchannel reactor after the loading is completed.
The upper porous support may be selected from porous materials such as woven metal mesh, sintered metal plate, etc. The material of the porous material is preferably stainless steel. In addition, the pore size of the upper porous support is generally larger than the pore size of the lower porous support.
The upper end porous support body can also be fixed on the upper part (micro-channel inlet) of the micro-channel reactor through a spring, in addition, an upper end enclosure can be arranged on the micro-channel reactor besides the upper end porous support body, and a channel is arranged in the upper end enclosure, so that reactant flow can be introduced or discharged when the micro-channel reactor is used for reaction (such as Fischer-Tropsch synthesis reaction).
The various parts of the system of the present invention (i.e., the particle reservoirs, distributors, microchannel reactors, etc.) may not need to be connected before or after the loading of the particles is performed, which facilitates cleaning, maintenance, etc.
According to a second aspect of the present invention, there is provided a method of loading particles into a microchannel reactor, the method performed on the system of aspect of the present invention, comprising:
1) introducing a gas into said fines storage tank at a flow rate less than the initial fluidization velocity of said fines to contact the fines, and venting the overhead gas from the contact through said dedusting apparatus to remove the lighter portion of the fines;
2) and increasing the gas flow velocity to be higher than the initial fluidization velocity, fluidizing the rest particles, introducing the obtained fluidized particles into the distributor for distribution, and uniformly entering reaction micro-channels of the micro-channel reactor.
According to the method of the invention, the microchannel reactor is preferably cleaned and dried (for example, purged with air) in sequence before use, so as to ensure that impurities are not contained in the reaction channel and the inner wall is kept smooth and clean.
According to the process of the present invention, the gas may be any inert gas, preferably an inert gas which is environmentally friendly, such as air, nitrogen, argon, etc.
According to the method of the present invention, the initial fluidization velocity may be obtained from a fluidized bed cold die test or by theoretical calculation based on the catalyst pot size, catalyst particle size, catalyst void fraction, catalyst particle density, and gas density and viscosity. Specific calculation methods are well known in the art and will not be described herein.
In step 1), the gas flow rate is controlled to be less than the initial fluidization velocity in order to remove undesired smaller particles that are not advantageous for the reaction while avoiding excessive attrition of the particles during fluidization.
Preferably, the gas flow rate is more than 110% (e.g., 110 to 300%) of the initial fluidization velocity, and further is preferably 110 to 245% of the initial fluidization velocity.
According to specific preferred embodiments, step 2) comprises:
2-1: firstly, increasing the flow speed of the gas to be 110-130% of the initial fluidization speed until the particles coming out of the storage tank are obviously reduced;
2-2: and increasing the flow rate of the gas to be 180-245% of the initial fluidization speed until all the particles in the storage tank enter the microchannel reactor.
According to concrete embodiments, the catalyst is loaded into the microchannel reactor by the method of the invention as shown in figure 1. the microchannel reactor 5 is rectangular and is vertically placed, stainless steel metal sintered plates are arranged at the bottom of the reactor, a reactor lower head can be arranged and the bottom of the reactor (not shown) can be closed after springs are arranged, the top of the microchannel reactor 5 is connected with a distributor 4, the diameter-expanding part of the distributor 4 is a quadrangular pyramid, and the catalyst loading is carried out after all the equipment is connected.
Adding a certain amount of catalyst from a feeding port 6 at the top of the catalyst tank 2, opening a valve of a conveying gas control unit 1, introducing a conveying gas flow, firstly leading the gas to enter the tank at a speed lower than the initial fluidization speed to be contacted with particles, emptying the obtained tank top gas through a dust removal device, then increasing the conveying gas flow to enable catalyst particles to enter a fluidization state and begin to be carried out from the catalyst tank 2, leading the gas flow (i.e. fluidized particles) carrying the particles into a distributor 4 through a hose 3, uniformly entering each reaction microchannel of a microchannel reactor 5 after distribution, intercepting the catalyst particles by a stainless steel metal sintering plate, leading the gas out from the bottom through the stainless steel metal sintering plate, and slightly vibrating the microchannel reactor through a rubber hammer in the whole filling process.
After loading was complete, distributor 4 was removed and another stainless steel metal sintered plate was installed on top of the microchannel reactor to achieve immobilization of the particles.
According to the present invention, when the loaded catalyst is a fischer-tropsch synthesis catalyst, the microchannel reactor can be applied to a fischer-tropsch synthesis reaction system as a fischer-tropsch reaction site, wherein a mixture gas (mainly composed of hydrogen and carbon oxide) for fischer-tropsch synthesis can enter the reactor through a channel of a lower head installed at the bottom of the microchannel reactor to contact with the catalyst, and a reaction product can be discharged through a channel of the upper head.
When the micro-channel reactor loaded with the Fischer-Tropsch synthesis catalyst obtained by the method is used for carrying out Fischer-Tropsch reaction, the pressure drop of the reactor is small, and the catalyst can ensure higher activity and lower selectivity of byproduct methane.
The present invention will be described in detail below by way of examples.
The following examples 1-5 are used in conjunction with the system shown in fig. 1 for the present invention.
In the following examples and comparative examples,
the adopted microchannel reactor is a cuboid, the length of the end surface is 800mm, the width of the end surface is 800mm, 200 rectangular reaction microchannels are included, and the reactor is formed by laminating SS304 tooth-shaped metal sheets; each channel was 200mm in length, 5mm in width and 1mm in height, and the reactor was required to be filled with 160mL of catalyst.
The catalyst is a cobalt-based Fischer-Tropsch synthesis catalyst, and the specific preparation method comprises the following steps: dissolving cobalt nitrate in deionized water to obtain cobalt nitrate impregnation liquid; impregnating alumina powder with the impregnating solution, standing for 8h, drying at 120 deg.C for 4 hr, and calcining at 450 deg.C for 4 hr to obtain cobalt-based catalystWherein the content of cobalt is 25 wt% calculated by oxide, the particle size range of the catalyst is 50-200 μm, the median particle size is 150 μm, the particles between 140-160 μm account for 80% of the total amount, and the compressive strength of the catalyst is 15N/mm2。
The porous support body at the lower end is an SS304 metal sintered plate, and the aperture is 15 mu m;
the porous support body at the upper end is an SS304 metal sintered plate, and the aperture is 25 mu m;
the conveying pipeline is a hose with the inner diameter of 20 mm;
the expanded diameter portion of the distributor was a regular quadrangular pyramid with a circular mouth at the upper end face and an inner diameter of 20mm, the lower end face was a rectangle congruent with the upper end of the microchannel reactor, and the thickness of the lower end face (i.e., the height of the rectangular parallelepiped portion of the distributor 4 shown in the drawing) was 20% of the height of the entire expanded diameter portion.
Example 1
Before filling the catalyst, adopting absolute ethyl alcohol to clean each channel of the microchannel reactor, and purging with purified air to ensure that no impurities exist in the reaction channel. And arranging the lower porous support body at the bottom of the reactor, and arranging the lower end enclosure of the reactor after installing the spring.
The volume of the catalyst tank is 400mL, and the height-diameter ratio is 18; the cone apex angle of the enlarged diameter portion of the distributor was 60. The nitrogen gas is used as the conveying gas, and the nitrogen gas quantity required by the initial fluidization speed of the particles is 2500 mL/min.
The specific loading method is as follows:
1) adding 160mL of catalyst from a feed inlet on a catalyst tank, introducing nitrogen at the bottom, introducing the gas flow of 1500mL/min, introducing the gas at the top of the tank into a dust removal device for emptying, removing particles smaller than 80 mu m existing in the catalyst, introducing the gas at the top of the tank into a hose after 10 minutes, and starting filling the catalyst;
2) increasing the nitrogen amount to 3000mL/min, beating the four walls of the reactor by using a rubber hammer until the particles coming out of the catalyst tank are obviously reduced, and further increasing the nitrogen amount to 5000mL/min in the step to completely transfer the materials in the catalyst tank;
3) and after filling, removing a distributor on the upper part of the reactor, cleaning redundant powder, then placing the porous support material at the upper end on the upper part of the reactor, installing a spring, and then sealing the upper end socket of the reactor to prepare for accessing a reaction system.
Example 2
Before filling the catalyst, adopting absolute ethyl alcohol to clean each channel of the microchannel reactor, and purging with purified air to ensure that no impurities exist in the reaction channel. And arranging the lower porous support body at the bottom of the reactor, and arranging the lower end enclosure of the reactor after installing the spring.
The volume of the catalyst tank is 400mL, and the height-diameter ratio is 12; the cone apex angle of the enlarged diameter portion of the distributor is 90 deg.. The nitrogen gas is used as the conveying gas, and the nitrogen gas amount required by the initial fluidization speed of the particles is 3300 mL/min.
The specific loading method is as follows:
1) adding 160mL of catalyst from a feed inlet on a catalyst tank, introducing nitrogen at the bottom, introducing the gas flow of 2000mL/min, introducing the gas at the top of the tank into a dust removal device for emptying, removing particles smaller than 80 mu m existing in the catalyst, introducing the gas at the top of the tank into a hose after 10 minutes, and starting filling the catalyst;
2) increasing the nitrogen amount to 4000mL/min, knocking four walls of the reactor by a rubber hammer until particles coming out of the catalyst tank are obviously reduced, and further increasing the nitrogen amount to 8000mL/min in steps to completely transfer materials in the catalyst tank;
3) and after filling, removing a distributor on the upper part of the reactor, cleaning redundant powder, then placing the porous support material at the upper end on the upper part of the reactor, installing a spring, and then sealing the upper end socket of the reactor to prepare for accessing a reaction system.
Example 3
The catalyst was loaded using the loading system and method of example 1 except that the distributor enlarged diameter section was used with a cone apex angle of 120 °.
Example 4
The catalyst was loaded using the loading system and method of example 1 except that the distributor used had a cone apex angle of 30 °.
Example 5
Before filling the catalyst, adopting absolute ethyl alcohol to clean each channel of the microchannel reactor, and purging with purified air to ensure that no impurities exist in the reaction channel. And arranging the lower porous support body at the bottom of the reactor, and arranging the lower end enclosure of the reactor after installing the spring.
The volume of the catalyst tank is 400mL, and the height-diameter ratio is 10; the cone apex angle of the enlarged diameter portion of the distributor was 80. The nitrogen gas is used as the conveying gas, and the nitrogen gas amount required for reaching the initial fluidization speed is 4000mL/min through calculation.
The specific loading method is as follows:
1) adding 160mL of catalyst from a feed inlet on a catalyst tank, introducing nitrogen at the bottom, introducing gas flow of 3000mL/min, introducing tank top gas into a dust removal device for emptying, removing particles smaller than 80 mu m generated in the presence of the catalyst, introducing the tank top gas into a hose after 10 minutes, and starting filling of the catalyst;
2) increasing the nitrogen amount to 5000mL/min, knocking four walls of the reactor by using rubber hammers until particles coming out of the catalyst tank are obviously reduced, and further increasing the nitrogen amount to 11000mL/min in the step to completely transfer materials in the catalyst tank;
3) and after filling, removing a distributor at the upper part of the reactor, cleaning redundant powder, then placing a porous supporting material at the upper end at the upper part of the reactor, installing a spring, and then sealing the upper end socket of the reactor to prepare for accessing a reaction system.
Comparative example 1
The microchannel reactor was charged with the catalyst according to the method of example 1, except that the charging system was directly charged using a corridor without using a catalyst tank, a hose and a distributor, and the lower part of the funnel was a small slit-shaped hole to facilitate charging by the catalyst into the reaction microchannel, the charging process was maintained as uniform as possible in speed to equalize the charging height, and the four walls of the reactor were simultaneously tapped with rubber hammers to clean the excess powder after the charging was completed, and then the upper end porous support material was placed on the upper part of the reactor, and the upper end of the reactor was closed after mounting a spring to prepare for the introduction into the reaction system.
Comparative example 2
The catalyst was loaded with reference to the system of example 1, except that the system of the comparative example did not employ a dust removal device. Before filling the catalyst, adopting absolute ethyl alcohol to clean each channel of the microchannel reactor, and purging with purified air to ensure that no impurities exist in the reaction channel. And arranging the lower porous support body at the bottom of the reactor, and arranging the lower end enclosure of the reactor after installing the spring.
The volume of the catalyst tank is 600mL, and the height-diameter ratio is 15; the cone apex angle of the enlarged diameter portion of the distributor was 60. The nitrogen gas is used as the conveying gas, and the nitrogen gas amount required for reaching the initial fluidization speed is 4000mL/min through calculation.
The specific loading method is as follows:
1) 160mL of catalyst is added from a feed inlet on a catalyst tank, nitrogen at the bottom is introduced, the gas flow is 5000mL/min, the top gas of the tank is introduced into a hose, and the filling of the catalyst is started;
2) increasing the nitrogen amount to 12000mL/min, and knocking the four walls of the reactor by using rubber hammers until the particles coming out of the catalyst tank are obviously reduced;
3) and after filling, removing a distributor on the upper part of the reactor, cleaning redundant powder, then placing a porous supporting material at the upper end on the upper part of the reactor, installing a spring, and then sealing the upper end socket of the reactor to prepare for accessing a reaction system.
In comparison with examples 1-5, there is a problem that the catalyst is not completely transferred during the packing process.
Test example
The microchannel reactors loaded with the catalysts in the examples 1 to 5 and the comparative examples 1 to 2 are respectively connected to a Fischer-Tropsch synthesis reaction system.
(1) Reduction of the catalyst
Under normal pressure, the catalyst is put in nitrogen atmosphere, and the gas space velocity is 1000mL/mLCatalyst and process for preparing sameHeating to 120 ℃ at a specified speed of 30 ℃/h under the condition of/h, controlling the maximum temperature difference of each point of the reactor to be not more than 1 ℃ in the heating process, and keeping the temperature for 8 h;
after the constant temperature is finished, the catalyst is put in a hydrogen-nitrogen mixed gas (the volume fraction of hydrogen is 5 percent) and the gas space velocity is 3000mL/mLCatalyst and process for preparing sameHeating to 28 deg.C/h at a specified rate of 10 deg.C/h under the condition of/hControlling the maximum temperature difference of each point of the reactor to be not more than 2 ℃ in the temperature rising process at 0 ℃, and keeping the temperature for 12 hours after the temperature rises;
after the constant temperature is finished, the catalyst is put in a hydrogen-nitrogen mixed gas (the volume fraction of hydrogen is 5 percent) and the gas space velocity is 2000mL/mLCatalyst and process for preparing sameHeating to 400 ℃ at a specified speed of 20 ℃/h under the condition of/h, controlling the maximum temperature difference of each point of the reactor to be not more than 3 ℃ in the heating process, detecting that the water content in the exhaust gas is 2mg/L after the temperature is heated to a constant temperature for 6h, increasing the volume fraction of hydrogen in the mixed gas of hydrogen and nitrogen to be 40%, detecting that the water content in the exhaust gas is 2mg/L after 6h, changing the exhaust gas into pure hydrogen, finishing reduction after the constant temperature is 6h, and starting to cool at 30 ℃/h.
(2) Carrying out the Fischer-Tropsch reaction
The reduced catalyst is prepared under the following reaction conditions: the pressure is 2.5MPa, the temperature is 220 ℃, and the composition of the synthesis gas (raw material gas) is H2Volume fraction 60%, volume fraction 30% CO, N2Volume fraction of 10 percent and space velocity of 10000mL/mLCatalyst and process for preparing sameAnd/h, carrying out Fischer-Tropsch synthesis reaction, and analyzing products by gas chromatography.
The catalyst activity and product selectivity after 100h of reaction were monitored. Wherein,
percent CO conversion ═ mole of CO in feed-mole of CO in discharge/mole of CO in feed ] × 100%;
CH4selectivity%4Mole number/(moles of CO in feed-moles of CO in discharge)]×100％；
C5 +Selectivity of hydrocarbons%5 +Moles of hydrocarbons/(moles of CO in feed-moles of CO in discharge)]×100％。
The results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the catalyst loading by the method of the present invention not only resulted in a small pressure drop in the reactor, but also resulted in uniform loading and no hot spots, and by-product CH was generated4The selectivity is lower than that of the comparative example, and the target product C5 +The selectivity to hydrocarbons is also significantly better than the comparative example.
In addition, when the vertex angle of the cone of the diameter expanding part of the distributor is controlled within the range of , the better loading effect is realized by comparing the embodiment 1-2 with the embodiment 3-4;
comparing examples 1-2 with example 5, it can be seen that by controlling the nitrogen flow in the fluidization phase, excessive catalyst attrition can be avoided, and thus the loading effect is improved;
comparing examples 1-5 with comparative example 2, it can be seen that, by using a small gas flow in combination with a dust removal device to remove the lighter part of the particles before fluidizing the catalyst, the total pressure drop of the catalyst during the reaction can be reduced and a better reaction effect can be obtained.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (11)
- A system for loading particles into a microchannel reactor, which comprises a conveying gas control unit, a particle storage tank, a dust removal device, a conveying pipeline, a distributor and the microchannel reactor, wherein the upper part of the particle storage tank is provided with a feed inlet for adding particles, the lower part of the particle storage tank is provided with a gas inlet for introducing gas, and a gas distributor is arranged in the tank;the conveying gas control unit can control the gas speed entering the particle storage tank in stages, so that the gas flow in the initial stage is smaller than the initial fluidization speed of the particles, and the gas flow in other stages is larger than the initial fluidization speed to realize fluidization of the particles, and obtain fluidized particles;the dust removal device is used for removing the tank top gas obtained by contacting the gas of the initial stage with the particles so as to remove the lighter part in the particles;the delivery conduit is for delivering the fluidized particulates to the distributor;the distributor comprises a channel part connected with the conveying pipeline and a diameter expanding part, and the lower end face of the diameter expanding part is matched with the upper end of the microchannel reactor so that fluidized particles distributed by the distributor enter a reaction microchannel of the microchannel reactor;the lower end of the microchannel reactor is provided with a lower porous support body, so that particles in fluidized particles entering the reaction microchannel are left in the microchannel and gas is discharged.
- 2. The system of claim 1, wherein the particulate reservoir has an aspect ratio of greater than 10, preferably 12 to 20; and/orThe volume of the particle storage tank is 2-5 times, preferably 2-3 times of the volume of the particles needing to be loaded in the microchannel reactor.
- 3. The system according to claim 1 or 2, wherein the particles have a size in the range of 15 to 500 μm, preferably 50 to 300 μm;preferably, the particle size distribution of the particles is more than 70% in the median particle size of +/-15 μm, and more preferably, the particle size distribution of the particles is more than 70% in the median particle size of +/-10 μm;preferably, the compression strength of the particles is greater than 5N/mm2。
- 4. The system of claim 1, wherein the microchannel reactor comprises more than 50 of the reaction microchannels, preferably the upper end of the microchannel reactor is rectangular.
- 5. The system of claim 1 or 4, wherein the reaction microchannel has a rectangular cross section, each channel has a length of 1 to 1000cm and a width and/or height of not more than 1000 μm.
- 6. The system according to claim 1, wherein the shape of the diverging section of the distributor is a cone, preferably the shape of the diverging section of the distributor is a regular pyramid or a regular cone, the apex angle of the cone is 30 ° to 120 °, and the further steps are preferably 60 ° to 90 °.
- 7. The system of claim 1, further comprising an upper porous support for holding the upper end of the microchannel reactor after particulate loading is complete.
- A method of loading particles into a microchannel reactor of , the method performed on the system of any of of claims 1-7, comprising:1) introducing a gas into said fines storage tank at a flow rate less than the initial fluidization velocity of said fines to contact the fines, and venting the overhead gas from the contact through said dedusting apparatus to remove the lighter portion of the fines;2) and increasing the gas flow velocity to be higher than the initial fluidization velocity, fluidizing the rest particles, introducing the obtained fluidized particles into the distributor for distribution, and uniformly entering reaction micro-channels of the micro-channel reactor.
- 9. The process according to claim 8, wherein the particulate is a catalyst, preferably a fischer-tropsch synthesis catalyst or a methanol synthesis catalyst.
- 10. The process according to claim 8 or 9, wherein in step 1), the flow rate of the gas is 40-80% of the initial fluidization velocity.
- 11. A process according to claim 8 or 9, wherein in step 2) the gas flow rate is more than 110%, preferably 110-245% of the initial fluidization velocity.
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