CN113019467A - Porous carrier catalyst loading device and process based on impregnation centrifugation - Google Patents
Porous carrier catalyst loading device and process based on impregnation centrifugation Download PDFInfo
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- CN113019467A CN113019467A CN202110240196.1A CN202110240196A CN113019467A CN 113019467 A CN113019467 A CN 113019467A CN 202110240196 A CN202110240196 A CN 202110240196A CN 113019467 A CN113019467 A CN 113019467A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
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Abstract
The invention discloses a porous carrier catalyst loading device and a process based on impregnation centrifugation. The vacuum pressure gauge is fixed on the sealing cover, and a sealing ring is arranged between the sealing cover and the tank body; the peripheral surface of the top of the tank body is provided with a metal hasp; the bottom of the tank body is provided with a shockproof foot pad; the bottom of the tank body is provided with a circular truncated cone protruding structure, the upper bottom surface of the circular truncated cone protruding structure is provided with a through hole, the motor is fixed below the upper top surface, and the method comprises the following steps: pretreating a porous carrier; preparing a precursor solution; the precursor solution is supported on a porous support. The invention can realize the catalyst loading of porous carriers with different materials, porosities and shapes; the uniform loading of the catalyst on the porous structure is realized, and the pore blocking after drying is avoided; catalyst loading can be carried out on a plurality of carriers simultaneously, so that the impregnation time of the carriers is reduced; meanwhile, the method has good effects of realizing the homogenization and the rapid loading of the catalyst and increasing the loading capacity of the catalyst.
Description
Technical Field
The invention relates to a porous carrier catalyst loading technology, in particular to a porous carrier catalyst loading device and a porous carrier catalyst loading process based on impregnation centrifugation, which are used for loading a porous foam carrier in a catalyst precursor solution, so that the catalyst precursor solution can be quickly and uniformly loaded in the porous carrier, and the loading capacity of a catalyst and the catalytic reaction performance of the carrier can be improved.
Technical Field
The metal and ceramic foam material with the porous structure has the advantages of light weight, small reaction pressure drop, strong heat and mass transfer performance, large specific surface area and the like, can improve the loading capacity and the loading strength of the catalyst, and can be widely used as a carrier of the catalyst in the microreactor. Common materials are nickel foam, copper foam, alumina foam, FeCrAl foam and porous silicon carbide foam. The carrier with the porous structure provides a channel or a cavity with a micron size, so that the catalyst is fully contacted with reactants, and the performance of catalytic reaction is improved.
The catalyst carrier is usually carried out by adopting an impregnation method, and the process mainly comprises the following steps: and (3) putting the carrier into the catalyst precursor solution for soaking, taking out and drying, and then repeating the operation until the required catalyst quality is obtained by loading. On one hand, because the viscosity of a precursor solution is higher, the impregnation process is difficult to enter the internal structure of the porous foam material, and the working hour of the impregnation process is longer; on the other hand, after excessive impregnation, excessive precursor solution is dried to easily cause pore blockage, so that the porous structure in the catalyst is unevenly loaded, reactants cannot be fully contacted with the catalyst, and the pressure drop of the reaction device is increased while the catalytic performance of the porous carrier is influenced.
In order to solve the problems, a catalyst rapid loading process and a catalyst rapid loading device are required to be designed according to the structural characteristics of the porous carrier, so that the dynamic uniform loading of the catalyst is realized, the excessively impregnated precursor solution is removed, and the catalytic performance of the porous carrier is improved.
Disclosure of Invention
In order to solve the technical problems of the existing porous foam material surface supported catalyst, the technical scheme of the invention is as follows:
porous carrier catalyst loading device based on impregnation centrifugation
The porous carrier catalyst loading device comprises a vacuum pressure gauge, a metal hasp, a sealing cover, a sealing ring, a vacuum joint, an air compressor joint, a cylindrical tank body, a drainage joint, a shockproof foot pad, a rotating circular plate, a connecting flange, a porous carrier, a carrying supporting plate and a motor;
the vacuum pressure gauge is fixedly arranged in the center of the top surface of the sealing cover, the sealing cover and the cylindrical tank body are sequentially arranged from top to bottom, a sealing ring is arranged between the sealing cover and the cylindrical tank body, and the sealing cover, the sealing ring and the cylindrical tank body are tightly pressed through metal hasps;
two metal hasps are symmetrically arranged on the peripheral surface of the top of the cylindrical tank body, the fixed end of each metal hasp is arranged on the peripheral surface of the top of the cylindrical tank body, and the movable end of each metal hasp is buckled and pressed on the raised edge of the sealing cover;
the outer circumferential surface of the cylindrical tank body is fixedly provided with a vacuum joint, an air compressor joint and a drainage joint from top to bottom in sequence, and the bottom of the cylindrical tank body is fixedly provided with shockproof foot pads at intervals along the circumference; a circular truncated cone protruding structure is arranged in the middle of the bottom of the cylindrical tank body, a through hole is formed in the center of the upper bottom surface of the circular truncated cone protruding structure, and the motor is fixed below the upper top surface of the circular truncated cone protruding structure;
an output shaft of the motor penetrates through the through hole and then is connected with the bottom end of the connecting flange, and the top end of the connecting flange is connected with the bottom surface of the rotating circular plate; the carrying supporting plate is fixed on the rotary circular plate through a connecting rod, and the porous carrier is placed at the bottom of the carrying supporting plate and is fixed through a clamping mechanism.
Rotatory plectane edge open along the circumference symmetrically and have N to mounting structure, N is more than or equal to 1's natural number, every is all including installation hole site and arch installation screens to mounting structure, arch installation screens is opened at rotatory plectane edge, it has the installation hole site to open on the rotatory plectane that is close to arch installation screens, the center of arch installation screens and the center of installation hole site are on same water flat line, every is to installing structure on N to carrying the thing layer board, every is to carrying the thing layer board and comprises two year thing layer boards, realize both ends mass balance, reduce the motor moment of torsion.
The top end of the carrying supporting plate is fixed on a mounting hole position of the rotating circular plate after being bent, an included angle between the top end of the carrying supporting plate and the middle end of the carrying supporting plate is equal to an included angle between a bus of the circular truncated cone protruding structure and the horizontal plane, the bent angle of the top end of the carrying supporting plate is equal to an included angle between the bus of the circular truncated cone protruding structure and the horizontal plane, and the included angle is 45-90 degrees.
The middle of the bottom end of the carrying supporting plate is provided with a convex block vertical to the bottom end by adopting a plate bending process, and the bottom of the porous carrier is placed on the convex block and used for realizing bottom support of the porous carrier. The middle of the bottom end of the carrying supporting plate is provided with a right-angle bend with the length of 15-30mm, so that the bottom support of the porous carrier is realized.
The clamping mechanism comprises a pressing bolt, a pressing plate and a compression spring, the pressing plate is sleeved on the pressing bolt, the pressing plate is pressed on the porous carrier after the two pressing bolts penetrate through respective mounting holes, two ends of the compression spring are sleeved on the pressing bolt between the pressing plate and the bottom of the carrying supporting plate to be connected with the pressing plate and the carrying supporting plate, two sides of the bottom of the carrying supporting plate are respectively provided with a round through hole as the mounting holes, and then the porous carrier is pressed on the carrying supporting plate.
The porous carrier is foam copper, foam nickel, foam aluminum, silicon carbide foam or FeCrAl foam with a porous structure.
The motor adopts a direct-current brushless speed reduction motor, and realizes stable rotation under the condition of set rotating speed.
The vacuum pressure gauge adopts a radial oil-filled shock-proof vacuum pressure gauge, and the internal pressure is accurately controlled.
Second, porous carrier catalyst loading process based on impregnation centrifugation
Step 1: putting the porous carrier into an ultrasonic cleaning machine for pretreatment, and drying the porous carrier for later use after the pretreatment is finished;
step 2: dissolving metal nitrate into deionized water, and adding gamma-Al containing additive2O3Fully stirring the slurry to obtain a catalyst precursor solution;
and step 3: opening a sealing cover, placing the porous carrier pretreated in the step 1) on a carrying supporting plate, adjusting a compression bolt, compressing a pressing plate on the surface of the porous carrier, and further compressing the porous carrier on the carrying supporting plate;
then pouring the precursor solution into a cavity between the cylindrical tank body and the circular truncated cone protruding structure until the precursor solution is completely immersed into the porous carrier, then covering the sealing cover, and then pressing the movable end of the metal hasp on the sealing cover to seal the interior of the cylindrical tank body;
then, the vacuum joint is connected with an external vacuum pump to work, the external vacuum pump is closed when the vacuum pressure gauge shows that the vacuum degree reaches-95 kPa to-80 kPa, a motor is started, and the motor drives the porous carrier to rotate at the speed of 0-100rpm, so that the porous carrier is fully impregnated;
and 4, step 4: connecting an air compressor joint with an external air compressor to work, simultaneously opening a water drainage joint, discharging the precursor solution in the cylindrical tank body to an external water drainage pipe connected with the water drainage joint, then adjusting a motor to drive the porous carrier to rotate at a rotating speed of 100-2500 rpm, and adjusting the operation time of the motor to be 0-60min according to the viscosity of the precursor solution and the porosity of the porous carrier;
and 5: and (3) unbuckling the movable end of the metal hasp from the sealing cover, then opening the sealing cover, taking out the porous carrier, putting the porous carrier into a drying furnace, drying at the temperature of 70-90 ℃, weighing after drying, completing catalyst loading if the designed catalyst loading mass is reached, and otherwise, repeating the steps 1) to 4) until the loading is completed.
In the step 2, the metal nitrate is one or more of copper nitrate, zinc nitrate, cerium nitrate, zirconium nitrate and palladium nitrate.
In the step 2, gamma-Al2O3Gamma-Al in the slurry2O3Has a particle size of 1-10 μm, gamma-Al2O3The mass fraction of the additive is 5-30%, wherein the additive is one or more of aluminum sol (CA), polyvinyl alcohol (PVA), polyethylene glycol (PEG), hydroxyethyl methyl cellulose (HEMC) and nano-silica sol.
The invention provides a porous carrier catalyst loading process and a device based on impregnation centrifugation, which can realize accurate control of internal pressure by using a radial oil-filled shock-resistant vacuum pressure gauge; the position of the compression bolt is adjusted, and the pressing force is transmitted through the pressing plate, so that the porous carrier can be well fixed on the carrying supporting plate, and the catalyst loading of the porous carrier with different materials, porosities and shapes can be realized; an external vacuum pump is connected with a vacuum joint, so that the vacuum condition in the container can be achieved, and then a motor is started to drive the porous carrier to rotate at a low speed, so that the air soaked in the porous carrier of the catalyst precursor solution can be quickly discharged, and the carrier can be fully soaked; the air compressor joint is connected with the air compressor, and the drainage joint is opened, so that redundant precursor solution in the device can be quickly discharged; the motor is used for driving the porous carrier on the carrying supporting plate to rotate at a high speed, and the centrifugal action of the high-speed rotation of the carrier is used for throwing out redundant catalyst precursor solution in the pores of the carrier, so that the uniform loading of the catalyst on the porous structure is realized, and the phenomenon of hole blockage after drying is avoided. The device and the process can realize the homogenization and the rapid loading of the catalyst of the porous carrier.
The invention has the beneficial effects that:
the invention can realize the catalyst loading of porous carriers with different materials, porosities and shapes; discharging redundant catalyst precursor solution in pores of the carrier by utilizing the centrifugal action of high-speed rotation of the carrier, realizing uniform loading of the catalyst on a porous structure, and avoiding pore blockage after drying; catalyst loading can be carried out on a plurality of carriers simultaneously, so that the impregnation time of the carriers is reduced; meanwhile, the method has good effects of realizing the homogenization and the rapid loading of the catalyst and increasing the loading capacity of the catalyst.
Drawings
FIG. 1 is a flow diagram of a catalyst loading process of the present invention;
FIG. 2 is a schematic structural diagram of a main body of an embodiment of the present invention;
FIG. 3 is a top view of the internal structure of an embodiment of the present invention;
FIG. 4 is a perspective view of an embodiment of the present invention;
FIG. 5 is a schematic illustration of the placement of a porous support according to an embodiment of the present invention;
FIG. 6 is a schematic view of the structure of a rotating circular plate;
FIG. 7 is a schematic structural view of a connecting flange;
FIG. 8 is a schematic structural view of a porous carrier;
figure 9 is a schematic view of a carrier plate;
fig. 10(a) is a laser confocal micrograph of a porous metal support obtained by a direct immersion method, and fig. 10(b) is a laser confocal micrograph of a surface of a porous metal support treated by the process of the present invention.
In the figure, 1 vacuum pressure gauge, 2 metal hasp, 3 sealing cover, 4 sealing ring, 5 vacuum joint, 6 air compressor joint, 7 cylindrical tank, 8 drainage joint, 9 shockproof foot pad, 10 rotary circular plate, 11 connecting flange, 12 porous carrier, 13 carrying supporting plate, 14 pressing bolt, 15 pressing plate, 16 motor and 17 compression spring.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and the embodiments are given in conjunction with the present technology, but the scope of the present invention is not limited thereto.
As shown in fig. 2 and 4, the device of the present invention comprises a vacuum pressure gauge 1, a metal hasp 2, a sealing cover 3, a sealing ring 4, a vacuum joint 5, an air compressor joint 6, a cylindrical tank 7, a water discharge joint 8, a shockproof foot pad 9, a rotary circular plate 10, a connecting flange 11, a porous carrier 12, a carrying pallet 13 and a motor 16;
the vacuum pressure gauge 1 is fixedly arranged at the center of the top surface of the sealing cover 3 through threads, the sealing cover 3 and the cylindrical tank body 7 are sequentially arranged from top to bottom, a sealing ring 4 is arranged between the sealing cover 3 and the cylindrical tank body 7, and the sealing cover 3, the sealing ring 4 and the cylindrical tank body 7 are tightly pressed through a metal hasp 2 to form internal sealing;
the outer peripheral surface of the top of the cylindrical tank body 7 is symmetrically provided with two metal hasps 2, the fixed end of each metal hasp 2 is arranged on the outer peripheral surface of the top of the cylindrical tank body 7, and the movable end of each metal hasp 2 is buckled on the protruding edge of the sealing cover 3;
as shown in fig. 4, a vacuum joint 5, an air compressor joint 6 and a drain joint 8 are fixedly installed on the outer circumferential surface of the cylindrical tank 7 from top to bottom in sequence, the vacuum joint 5, the air compressor joint 6 and the drain joint 8 are implemented on the same vertical line, the vacuum joint 5 is connected with an external vacuum pump, the air compressor joint 6 is connected with an air compressor, and the drain joint 8 is connected with a drain pipe with a switch outside; the bottom of the cylindrical tank body 7 is uniformly fixed with shockproof foot pads 9 at intervals along the circumference through bolts; a circular truncated cone protruding structure is arranged in the middle of the bottom of the cylindrical tank body 7, a through hole is formed in the center of the upper bottom surface of the circular truncated cone protruding structure, and the motor 16 is fixed below the upper top surface of the circular truncated cone protruding structure;
as shown in fig. 5 and 7, the output shaft of the motor 16 penetrates through the through hole and is connected with the bottom end of the connecting flange 11, and the top end of the connecting flange 11 is connected with the bottom surface of the rotating circular plate 10; the motor 16 is a brushless dc speed-reducing motor, and can rotate stably at a predetermined speed. The rotary circular plate 10, the connecting flange 11 and the motor 16 are sequentially and coaxially connected from top to bottom, the motor 16 is placed in the circular truncated cone protruding structure, and a cavity is formed between the cylindrical tank 7 and the circular truncated cone protruding structure and used for storing a catalyst precursor solution; the carrier plate 13 is fixed to the rotating circular plate 10 by a connecting rod, and the porous carrier 12 is placed on the bottom of the carrier plate 13 and fixed by a clamping mechanism.
As shown in fig. 5 and 6, the edge of the rotating circular plate 10 is symmetrically provided with N pairs of mounting structures along the circumference, N is a natural number greater than or equal to 1, each pair of mounting structures includes a mounting hole position and an arched mounting position, the arched mounting position is arranged at the edge of the rotating circular plate 10, the rotating circular plate 10 close to the arched mounting position is provided with a mounting hole position, the center of the arched mounting position and the center of the mounting hole position are on the same horizontal line, each pair of mounting structures is provided with N pairs of carrying supporting plates 13, each pair of carrying supporting plates 13 is composed of two carrying supporting plates 13, mass balance at two ends is realized, and the torque of the motor is reduced.
As shown in fig. 5 and 9, the top end of the carrying supporting plate 13 is bent and then fixed on the mounting hole position of the rotating circular plate 10, the included angle between the top end of the carrying supporting plate 13 and the middle end of the carrying supporting plate 13 is equal to the included angle between the generatrix of the circular truncated cone protruding structure and the horizontal plane, the bent angle of the top end of the carrying supporting plate 13 is equal to the included angle between the generatrix of the circular truncated cone protruding structure and the horizontal plane, and the included angle is 45-90.
A lug perpendicular to the bottom end is arranged in the middle of the bottom end of the carrying supporting plate 13 by adopting a plate bending process, and the bottom of the porous carrier 12 is placed on the lug and used for realizing bottom support of the porous carrier 12. The middle of the bottom end of the carrying supporting plate 13 is provided with a right-angle bend with the length of 15-30mm, so that the bottom support of the porous carrier 12 is realized.
As shown in fig. 3 and 5, the clamping mechanism includes a pressing bolt 14, a pressing plate 15 and a compression spring 17, the pressing plate 15 is sleeved on the pressing bolt 14, two pressing bolts 14 pass through respective mounting holes to press the pressing plate 15 on the porous carrier 12, the compression spring 17 is sleeved on the pressing bolt 14 between the pressing plate 15 and the bottom of the carrying supporting plate 13, two ends of the compression spring 17 are connected with the pressing plate 15 and the carrying supporting plate 13, two sides of the bottom of the carrying supporting plate 13 are respectively provided with a round through hole as a mounting hole, so that the porous carrier 12 is pressed on the carrying supporting plate 13.
As shown in fig. 8, the porous support 12 is a copper foam, a nickel foam, an aluminum foam, a silicon carbide foam or a FeCrAl foam having a porous structure.
As shown in fig. 1, the impregnation and centrifugation catalyst loading process of the porous carrier is realized based on the impregnation and centrifugation porous carrier catalyst loading device, and comprises the following specific steps:
step 1: putting the porous carrier 12 into an ultrasonic cleaning machine for pretreatment, removing dust, oil stain and rust on the surface of the porous carrier 12, and drying for later use after the pretreatment is finished;
step 2: dissolving one or more metal nitrates prepared according to the proportion of the catalyst into deionized water, and then adding gamma-Al containing additive2O3Fully stirring the slurry to obtain a catalyst precursor solution; wherein, gamma-Al2O3Gamma-Al in the slurry2O3Has a particle size of 1-10 μm, gamma-Al2O3The mass fraction of the additive is 5-30%, wherein the additive is one or more of aluminum sol (CA), polyvinyl alcohol (PVA), polyethylene glycol (PEG), hydroxyethyl methyl cellulose (HEMC) and nano-silica sol;
and step 3: opening the sealing cover 3, placing the porous carrier 12 pretreated in the step 1 on the bottom of the carrying supporting plate 13, adjusting the compression bolt 14, compressing the pressure plate 15 on the surface of the porous carrier 12, and further compressing the porous carrier 12 on the carrying supporting plate 13;
then pouring the precursor solution into a cavity between the cylindrical tank body 7 and the circular truncated cone protruding structure until the precursor solution is completely immersed into the porous carrier 12, then covering the sealing cover 3, and then pressing the movable end of the metal hasp 2 on the sealing cover 3 to seal the interior of the cylindrical tank body 7;
then, the vacuum joint 5 is connected with an external vacuum pump to work, the external vacuum pump is closed when the vacuum pressure gauge 1 shows that the vacuum degree reaches-95 kPa to-80 kPa, the motor 16 is started, and the motor 16 drives the porous carrier 12 to rotate at the speed of 0-100rpm, so that the porous carrier 12 is fully impregnated;
and 4, step 4: connecting an air compressor connector 6 with an external air compressor to work, simultaneously opening a water drainage connector 8, discharging a precursor solution in a cylindrical tank 7 to an external water drainage pipe connected with the water drainage connector 8, then adjusting a motor 16 to drive a porous carrier 12 to rotate at a rotating speed of 100rpm-2500rpm, adjusting the running time of the motor 16 to be 0-60min according to the viscosity of the precursor solution and the porosity of the porous carrier, throwing out the redundant catalyst precursor solution in the pores of the porous carrier 12 by using the centrifugal action of the rotation of the porous carrier 12, and preventing the pores of the porous carrier 12 from being blocked after subsequent drying;
and 5: and (3) unbuckling the movable end of the metal hasp 2 from the sealing cover 3, then opening the sealing cover 3, taking out the porous carrier 12, putting the porous carrier into a drying furnace for drying at the temperature of 70-90 ℃, weighing after drying, completing catalyst loading if the designed catalyst loading mass is reached, and otherwise, repeating the steps 1 to 4 until the loading is completed.
In specific implementation, the metal nitrate is one or more of copper nitrate, zinc nitrate, cerium nitrate, zirconium nitrate and palladium nitrate. The vacuum pressure gauge 1 adopts a radial oil-filled shock-proof vacuum pressure gauge to realize accurate control of internal pressure.
The examples are as follows:
the typical embodiment of the device is used for the catalyst loading of a porous carrier in a microreactor for hydrogen production by methanol reforming, and the porous copper foam is used for loadingCu/ZnO/CeO carrier2For example, the loading process was as follows:
foam copper pretreatment: a2 mm thick 110ppi copper foam plate was cut into a size of 65mm x 65mm, put into a 180W ultrasonic cleaner and pretreated with absolute ethanol for 5min to remove surface stains, and then dried.
The preparation process of the catalyst precursor solution comprises the following steps: adding Cu (NO)3)2、Zn(NO3)2、Ce(NO3)4Dissolving in a small amount of deionized water at a molar ratio of 5:2:1, adding gamma-Al with particle size of about four microns and solid content of less than 30 wt%2O30.5 wt% of HEMC was added to the slurry to increase the adhesive strength and viscosity, and the mixture was sufficiently stirred to obtain a catalyst precursor solution. Wherein, gamma-Al2O3The slurry is prepared by mixing gamma-Al2O3Wet milling the balls in a ball mill at 250r/min for 24 h.
And (3) a loading process: firstly, a catalyst precursor solution is poured into the cylindrical tank body 7, the pretreated foam copper is placed on the carrying supporting plate 13 and fixed by the pressing plate 15, and the sealing cover 3 is sealed by the metal hasp 2 after the installation is finished. The vacuum pump connected to the vacuum connection 5 was started, the vacuum pressure gauge 1 was observed to bring the interior of the apparatus to about-88 kPa, and the vacuum pump was turned off, which was favorable for exhausting the air of the porous carrier. Starting a motor to drive the foamy copper to be soaked for 10min at the rotating speed of 0-100rpm, and realizing full soaking.
After excessive impregnation, the air compressor connected to the air compressor connection 6 is started, the water drain connection 8 is opened, and the excess precursor solution is quickly drained by means of pressure difference. And starting the motor again to drive the foamy copper carrier to rotate at the rotating speed of 1250rpm, discharging the precursor solution of the redundant catalyst in the pores by using the centrifugal action, and taking out the foamy copper carrier with the uniformly loaded catalyst after about 2min of treatment. The above-described loading process can be repeated after drying until the catalyst coating layer reaches a desired quality or thickness, as required by the process. The average thickness t of the catalyst precursor solution can be calculated using the following formula:
wherein t represents an average thickness, m1Denotes the mass after load, m0Denotes the initial mass of the support, s0Denotes the surface area of the support, p0The catalyst precursor solution density is shown.
Fig. 10(a) is a laser confocal micrograph of a porous metal carrier obtained after being immersed for 10 hours by a direct immersion method, and due to a complex pore structure inside the porous metal fiber, a precursor solution is not easy to discharge, a phenomenon of pore blocking is formed, and the porous metal carrier is not favorable for use after loading; fig. 10(b) is a laser confocal micrograph of the surface of a porous metal carrier treated once by loading according to the present invention, wherein the excess precursor solution in the pores is drained, and the uniform alumina coating is loaded on the fiber, which is repeated several times, so that the desired quality or thickness can be obtained without causing pore blocking.
Claims (10)
1. A porous carrier catalyst loading device based on impregnation centrifugation is characterized in that: the device comprises a vacuum pressure gauge (1), a metal hasp (2), a sealing cover (3), a sealing ring (4), a vacuum joint (5), an air compressor joint (6), a cylindrical tank body (7), a drainage joint (8), a shockproof foot pad (9), a rotating circular plate (10), a connecting flange (11), a porous carrier (12), a carrying supporting plate (13) and a motor (16);
the vacuum pressure gauge (1) is fixedly arranged at the center of the top surface of the sealing cover (3), the sealing cover (3) and the cylindrical tank body (7) are sequentially arranged from top to bottom, a sealing ring (4) is arranged between the sealing cover (3) and the cylindrical tank body (7), and the sealing cover (3), the sealing ring (4) and the cylindrical tank body (7) are pressed tightly through a metal hasp (2);
two metal hasps (2) are symmetrically arranged on the peripheral surface of the top of the cylindrical tank body (7), the fixed end of each metal hasp (2) is arranged on the peripheral surface of the top of the cylindrical tank body (7), and the movable end of each metal hasp (2) is buckled on the protruding edge of the sealing cover (3);
a vacuum joint (5), an air compressor joint (6) and a drainage joint (8) are fixedly installed on the outer circumferential surface of the cylindrical tank body (7) from top to bottom in sequence, and shockproof foot pads (9) are fixedly installed at the bottom of the cylindrical tank body (7) at intervals along the circumference; a circular truncated cone protruding structure is arranged in the middle of the bottom of the cylindrical tank body (7), a through hole is formed in the center of the upper bottom surface of the circular truncated cone protruding structure, and the motor (16) is fixed below the upper top surface of the circular truncated cone protruding structure;
an output shaft of the motor (16) penetrates through the through hole and then is connected with the bottom end of the connecting flange (11), and the top end of the connecting flange (11) is connected with the bottom surface of the rotating circular plate (10); the carrying supporting plate (13) is fixed on the rotary circular plate (10) through a connecting rod, and the porous carrier (12) is placed at the bottom of the carrying supporting plate (13) and is fixed through a clamping mechanism.
2. The impregnation centrifugation-based porous carrier catalyst support device according to claim 1, wherein: the edge of the rotating circular plate (10) is symmetrically provided with N pairs of mounting structures along the circumference, N is a natural number greater than or equal to 1, each pair of mounting structures comprises a mounting hole position and an arched mounting clamping position, each pair of mounting structures is provided with N pairs of carrying supporting plates (13), and each pair of carrying supporting plates (13) consists of two carrying supporting plates (13).
3. The impregnation centrifugation-based porous carrier catalyst support device according to claim 1, wherein: the top end of the carrying supporting plate (13) is bent and then fixed on a mounting hole position of the rotating circular plate (10), the bending angle of the top end of the carrying supporting plate (13) is equal to the included angle between a bus of the circular truncated cone protruding structure and the horizontal plane, and the included angle is 45-90 degrees.
4. The impregnation centrifugation-based porous carrier catalyst support device according to claim 1, wherein: the middle of the bottom end of the carrying supporting plate (13) is provided with a convex block vertical to the bottom end by adopting a plate bending process, and the bottom of the porous carrier (12) is placed on the convex block.
5. The impregnation centrifugation-based porous carrier catalyst support device according to claim 1, characterized in that: clamping mechanism include clamp bolt (14), clamp plate (15) and compression spring (17), clamp plate (15) suit is on clamp bolt (14), clamp bolt (14) pass behind the mounting hole with clamp plate (15) compress tightly on porous carrier (12), the cover is equipped with compression spring (17) on clamp bolt (14) between clamp plate (15) and year thing layer board (13) bottom, it has a round through-hole as the mounting hole respectively to open the both sides of year thing layer board (13) bottom, and then makes porous carrier (12) compress tightly on carrying layer board (13).
6. The impregnation centrifugation-based porous carrier catalyst support device according to claim 1, characterized in that: the porous carrier (12) is foamed copper, foamed nickel, foamed aluminum, silicon carbide foam or FeCrAl foam with a porous structure.
7. The impregnation centrifugation-based porous carrier catalyst support device according to claim 1, wherein: the motor (16) adopts a direct current brushless speed reducing motor.
8. A process for carrying out porous carrier catalyst loading based on impregnation centrifugation of a porous carrier catalyst loading device according to any one of claims 1 to 7, characterized in that: comprises the following steps:
step 1: putting the porous carrier (12) into an ultrasonic cleaning machine for pretreatment, and drying for later use after the pretreatment is finished;
step 2: dissolving metal nitrate into deionized water, and adding gamma-Al containing additive2O3Fully stirring the slurry to obtain a catalyst precursor solution;
and step 3: opening a sealing cover (3), placing the porous carrier (12) pretreated in the step 1) on a carrying supporting plate (13), adjusting a compression bolt (14), compressing a pressure plate (15) on the surface of the porous carrier (12), and further compressing the porous carrier (12) on the carrying supporting plate (13);
then pouring the precursor solution into a cavity between the cylindrical tank body (7) and the circular truncated cone protruding structure until the precursor solution is completely immersed into the porous carrier (12), then covering the sealing cover (3), and pressing the movable end of the metal hasp (2) on the sealing cover (3) to seal the interior of the cylindrical tank body (7);
then, the vacuum joint (5) is connected with an external vacuum pump to work, the external vacuum pump is closed when the vacuum pressure gauge (1) displays that the vacuum degree reaches-95 kPa to-80 kPa, a motor (16) is started, and the motor (16) drives the porous carrier (12) to rotate at the speed of 0-100rpm, so that the porous carrier (12) is fully impregnated;
and 4, step 4: connecting an air compressor connector (6) with an external air compressor to work, simultaneously opening a water drainage connector (8), discharging a precursor solution in a cylindrical tank body (7) to an external water drainage pipe connected with the water drainage connector (8), then adjusting a motor (16) to drive a porous carrier (12) to rotate at a rotating speed of 100rpm-2500rpm, and adjusting the running time of the motor (16) to be 0-60min according to the viscosity of the precursor solution and the porosity of the porous carrier;
and 5: and (3) releasing the movable end of the metal hasp (2) from the sealing cover (3), then opening the sealing cover (3), taking out the porous carrier (12), drying the porous carrier in a drying furnace at the temperature of 70-90 ℃, weighing the porous carrier after drying, completing catalyst loading if the porous carrier reaches the designed catalyst loading mass, and otherwise, repeating the steps 1) to 4) until the loading is completed.
9. The process of impregnation centrifugal catalyst loading of a porous support achieved according to claim 8, characterized in that: in the step 2, the metal nitrate is one or more of copper nitrate, zinc nitrate, cerium nitrate, zirconium nitrate and palladium nitrate.
10. The process of impregnation centrifugal catalyst loading of a porous support achieved according to claim 8, characterized in that: in the step 2, gamma-Al2O3Gamma-Al in the slurry2O3Has a particle size of 1-10 μm, gamma-Al2O3The mass fraction of the additive is 5-30%, and the additive is one or more of aluminum sol, polyvinyl alcohol, polyethylene glycol, hydroxyethyl methyl cellulose and nano silicon dioxide sol.
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