CN117816083B - A catalyst in-situ preparation device and application method thereof - Google Patents
A catalyst in-situ preparation device and application method thereof Download PDFInfo
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- CN117816083B CN117816083B CN202410247894.8A CN202410247894A CN117816083B CN 117816083 B CN117816083 B CN 117816083B CN 202410247894 A CN202410247894 A CN 202410247894A CN 117816083 B CN117816083 B CN 117816083B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/22—Evaporating by bringing a thin layer of the liquid into contact with a heated surface
- B01D1/222—In rotating vessels; vessels with movable parts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/001—Drying-air generating units, e.g. movable, independent of drying enclosure
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- F26B21/50—
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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Abstract
The invention discloses a catalyst in-situ preparation device and an application method thereof, which relate to the technical field of catalyst preparation, wherein a tank body is used for loading materials, and a rotating mechanism is used for controlling the tank body to rotate in a vertical plane; the liquid circulation system is used for circularly cleaning the materials; the air inlet system is used for pressurizing, drying or reducing the materials; the pipeline type air heater is used for heating the gas; the tank body heater is used for heating the tank body and heating the materials; the blind flange is used for sealing the upper end of the tank body; the flange with the filter membrane is used for communicating the upper end of the tank body and intercepting and filtering materials; the flat bottom valve is used for controlling the opening and closing of the lower end of the tank body; the quick connector is used for quickly connecting a liquid circulation system or an air inlet system; the vacuum system is used for connecting the flange with the filter membrane to vacuumize the tank body. The invention can prepare the catalyst in situ in one tank body, and can effectively improve the preparation efficiency and the preparation quality of the catalyst.
Description
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a catalyst in-situ preparation device and an application method thereof.
Background
At present, when a hydrothermal-reduction method is used for preparing a fuel cell catalyst, a plurality of working procedures are involved before and after, and materials are required to be transferred for a plurality of times in different devices so as to carry out operations of cleaning, filtering, drying, dipping, reduction and the like; the whole preparation process has a plurality of problems, for example, a large amount of waste water is generated in the cleaning process, the product pollution and loss are easily caused in the process of multiple transfer, the spontaneous combustion of the high-activity catalyst is easily caused in the drying process, and the like; these problems seriously affect the preparation efficiency and the preparation quality of the catalyst.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a catalyst in-situ preparation device and an application method thereof.
The invention provides a catalyst in-situ preparation device which comprises a fixed frame, a tank body, a liquid circulation system, an air inlet system and a vacuum system, wherein the tank body is arranged on the side surface of the fixed frame based on a rotating mechanism, the tank body is used for loading materials, and the rotating mechanism is used for controlling the tank body to rotate in a vertical plane; the liquid circulation system and the air inlet system are fixedly arranged in the fixing frame; the liquid circulation system is used for communicating the upper end and the lower end of the tank body to perform liquid circulation and circularly cleaning materials; the air inlet system is used for communicating the lower end of the tank body to supply air and pressurizing, drying or reducing materials; the air inlet system comprises a pipeline type air heater for heating the air;
the surface of the tank body is provided with a tank body heater, and the tank body heater is used for heating the tank body and heating materials; a blind flange or a flange with a filter membrane is arranged at the upper end of the tank body; the blind flange is used for sealing the upper end of the tank body; the flange with the filter membrane is used for communicating the upper end of the tank body and intercepting and filtering materials; the lower end of the tank body is provided with a flat bottom valve which is used for controlling the opening and closing of the lower end of the tank body; the flat bottom valve is connected with a quick connector which is used for quickly connecting the liquid circulation system or the air inlet system; the vacuum system is independently arranged at the side of the fixing frame and is used for connecting the flange with the filter membrane to vacuumize the tank body.
Specifically, the liquid circulation system comprises a liquid storage tank and a diaphragm pump, wherein the liquid storage tank is arranged at the upper end of the fixing frame and is used for storing liquid and serving as a transfer station for liquid circulation; the diaphragm pump is arranged at the lower end of the fixing frame and is used for driving liquid to move; the liquid storage tank is communicated with the diaphragm pump based on a pipeline;
When liquid circulation is carried out, the upper end of the tank body is provided with a filter membrane flange, the liquid storage tank is connected with the filter membrane flange on the basis of a pipeline, and the diaphragm pump is connected with the quick connector on the basis of the pipeline.
Specifically, rotary mechanism is the motor, the body of motor is fixed to be set up the side of mount, the output of motor with jar body fixed connection.
Specifically, the tank heater is a silica gel heating pad, and the silica gel heating pad wraps the outer peripheral surface of the tank.
Specifically, the upper part of the tank body is of a cylindrical structure, and the lower part of the tank body is of a conical structure.
The invention also provides an application method of the catalyst in-situ preparation device, which comprises the following steps:
s1, modifying a carrier raw material;
Putting a carrier raw material and a modifier into a tank body, mounting a blind flange at the upper end of the tank body, and obtaining a first modified carrier after soaking for a preset time;
S2, filtering for the first time;
Replacing the blind flange with a filter membrane, and starting a rotating mechanism to drive the tank body to rotate until the flange with the filter membrane faces downwards;
connecting an air inlet system with a quick connector, introducing clean compressed gas into the tank body, and pressurizing and filtering out redundant modifier, wherein the first modified carrier is reserved in the tank body; or (b)
Connecting a vacuum system with the flange with a filter membrane, vacuumizing the tank body, filtering out redundant modifier under negative pressure, and retaining the first modified carrier in the tank body;
s3, cleaning the first modified carrier;
Starting the rotating mechanism to drive the tank body to rotate until the flange with the filter membrane faces upwards, respectively connecting the flange with the filter membrane and the quick connector with a liquid circulating system, and circularly cleaning the first modified carrier by pure water to obtain a second modified carrier after cleaning for a preset time;
S4, filtering for the second time;
Starting the rotating mechanism to drive the tank body to rotate until the flange with the filter membrane faces downwards;
Connecting the air inlet system with the quick connector, introducing clean compressed gas into the tank body, pressurizing and filtering out redundant water, and retaining the second modified carrier in the tank body; or (b)
Connecting the vacuum system with the flange with a filter membrane, vacuumizing the tank body, filtering out redundant water under negative pressure, and retaining the second modified carrier in the tank body;
S5, drying the second modified carrier
Starting the rotating mechanism to drive the tank body to rotate until the flange with the filter membrane faces upwards;
The vacuum system is connected with the flange with the filter membrane in a first drying mode, and the tank body is vacuumized; starting a tank heater to heat the tank; starting the rotating mechanism to drive the tank body to swing and rotate, and turning over the second modified carrier; or (b)
Connecting the air inlet system with the quick connector in a second drying mode, and introducing clean compressed gas into the tank body to agitate the second modified carrier; and opening a pipeline type air heater to heat the compressed gas;
S6, loading a second modified carrier;
the dried second modified carrier is reserved in the tank body, a metal precursor solution is added into the tank body, the blind flange is arranged at the upper end of the tank body, and a catalyst precursor is obtained after impregnating for a preset time;
S7, drying the catalyst precursor;
Replacing the blind flange with the filter membrane flange, wherein the filter membrane flange faces upwards;
The vacuum system is connected with the flange with the filter membrane in a first drying mode, and the tank body is vacuumized; starting the tank heater to heat the tank; opening the rotating mechanism to drive the tank body to swing and rotate, and turning over the catalyst precursor; or (b)
Connecting the air inlet system with the quick connector in a second drying mode, and introducing clean compressed gas into the tank body to agitate the catalyst precursor; and turning on the pipeline type air heater to heat the compressed gas;
s8, reducing the catalyst precursor;
the dried catalyst precursor is reserved in the tank body, and the flange with the filter membrane faces upwards; connecting the air inlet system with the quick connector, starting the pipeline type air heater and/or the tank body heater, and introducing hydrogen into the tank body to perform reduction treatment on the catalyst precursor to obtain a catalyst finished product;
S9, pouring out a catalyst finished product;
And (3) removing the connection between the air inlet system and the quick connector, removing the flange with the filter membrane, installing a receiving barrel at the upper end of the tank body, starting the rotating mechanism to drive the tank body to rotate until the receiving barrel is positioned below, and pouring out the catalyst finished product.
Specifically, the modification of the carrier raw material further comprises: starting the rotating mechanism to drive the tank body to swing and rotate, and turning over the carrier raw material and the modifier;
The second modified support load further comprises: and opening the rotating mechanism to drive the tank body to swing and rotate, and turning over the second modified carrier and the metal precursor solution.
Specifically, based on the vertical direction, the swinging rotation angle of the tank body is-120 degrees and +120 degrees.
Specifically, the temperature range for drying the second modified carrier is 60-150 ℃;
the temperature range used for drying the catalyst precursor is 60-150 ℃.
Specifically, the second modified carrier load further comprises:
ball milling beads are put into the tank body, wherein the ball milling beads are zirconium beads or glass beads or PTFE beads.
Compared with the prior art, the invention has the beneficial effects that:
In the invention, the tank body is used for loading materials (including powder materials such as carriers, catalysts and the like), is a container for preparing the catalysts, and can be matched with other mechanisms to carry out the operations of cleaning, filtering, drying, dipping, reduction and the like of the materials; the rotating mechanism is used for controlling the tank body to rotate in a vertical plane, and can turn materials, so that the operations of filtering, drying, dipping, discharging and the like of the materials are facilitated; the liquid circulation system is used for communicating the upper end and the lower end of the tank body to perform liquid circulation, so that materials can be circularly cleaned, and the generation of waste water is reduced; the air inlet system is used for communicating the lower end of the tank body to supply air, so that air with different properties can be supplied as required to pressurize, dry or reduce the material, and the air can stir the material, so that the efficiency of drying or reduction is improved; the gases with different properties have different functions, and when the high-activity catalyst is dried, protective gas can be filled into the tank body to reduce the risk of spontaneous combustion; the pipeline type air heater is used for heating the gas, so that the material can be dried or reduced conveniently; the tank body heater is used for heating the tank body and heating the materials, so that the materials can be dried or reduced conveniently; the tank body can use a blind flange or a filter membrane flange as required, the blind flange is used for sealing the upper end of the tank body, and the filter membrane flange is used for communicating the upper end of the tank body to intercept and filter materials; the lower end of the tank body is provided with a flat bottom valve for controlling the opening and closing of the lower end of the tank body, and no dead zone exists; the flat bottom valve can be quickly connected with a liquid circulation system or an air inlet system through a quick connector; the vacuum system is used for connecting the flange with the filter membrane to vacuumize the tank body, so that negative pressure filtration and accelerated drying are facilitated.
The invention can clean, filter, dry, impregnate and reduce the material in the same tank, which is convenient for preparing the catalyst in situ, and can reduce the transfer times of the material, thereby reducing the pollution and loss of the product and the waste of time; the materials can be circularly cleaned, so that the generation of waste water is reduced; the protective gas can be filled to protect the dry materials, so that the risk of spontaneous combustion of the materials is reduced, and the quality is controllable and safe; therefore, the invention can effectively improve the preparation efficiency and the preparation quality of the catalyst.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings which are required in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural view of an in-situ catalyst preparation apparatus according to an embodiment of the present invention;
FIG. 2 is an enlarged schematic view of the area A in FIG. 1;
FIG. 3 is a flow chart of a method of application of a catalyst in situ preparation apparatus in an embodiment of the invention;
FIG. 4 is a schematic view of a blind flange for installing a can body according to an embodiment of the present invention;
Fig. 5 is a schematic structural view of a flange with a filter membrane mounted on a tank body in an embodiment of the invention.
In the drawing, 100, a fixing frame; 200. a tank body; 210. a tank heater; 221. a seal ring; 222. a flange through hole; 223. a filtering membrane; 230. a flat bottom valve; 240. a quick connector; 300. a liquid circulation system; 310. a liquid storage tank; 320. a diaphragm pump; 400. an air intake system; 410. a duct type air heater; 500. a vacuum system; 600. a rotating mechanism.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a catalyst in-situ preparation device, and fig. 1 shows a schematic structural diagram of the catalyst in-situ preparation device in the embodiment of the invention, which comprises a fixing frame 100, a tank body 200, a liquid circulation system 300, an air inlet system 400 and a vacuum system 500, wherein the tank body 200 is arranged on the side surface of the fixing frame 100 based on a rotating mechanism 600, the tank body 200 is used for loading materials, and the rotating mechanism 600 is used for controlling the tank body 200 to rotate in a vertical plane; the liquid circulation system 300 and the air intake system 400 are fixedly disposed in the fixing frame 100; the liquid circulation system 300 is used for communicating the upper end and the lower end of the tank 200 to perform liquid circulation and perform circulation cleaning on materials; the air inlet system 400 is used for communicating with the lower end of the tank 200 to supply air and pressurizing, drying or reducing materials; the air intake system 400 includes a duct type air heater 410 for heating the gas; a tank heater 210 is arranged on the surface of the tank 200, and the tank heater 210 is used for heating the tank 200 and heating materials; a blind flange or a flange with a filter membrane is arranged at the upper end of the tank body 200; the blind flange is used for sealing the upper end of the tank body 200; the flange with the filter membrane is used for communicating the upper end of the tank body 200 and intercepting and filtering materials; the lower end of the tank 200 is provided with a flat bottom valve 230, and the flat bottom valve 230 is used for controlling the opening and closing of the lower end of the tank 200; the flat bottom valve 230 is connected with a quick connector 240, and the quick connector 240 is used for quickly connecting the liquid circulation system 300 or the air intake system 400; the vacuum system 500 is independently arranged at the side of the fixing frame 100, and the vacuum system 500 is used for connecting the flange with the filter membrane to vacuumize the tank 200.
In the invention, the tank 200 is used for loading materials (including powder materials such as carriers, catalysts and the like), is a container for preparing the catalysts, and can be matched with other mechanisms to carry out the operations of cleaning, filtering, drying, dipping, reduction and the like of the materials; the rotating mechanism 600 is used for controlling the tank 200 to rotate in a vertical plane, and can turn materials, so that the operations of filtering, drying, dipping, discharging and the like can be conveniently performed on the materials; the liquid circulation system 300 is used for communicating the upper end and the lower end of the tank body 200 to perform liquid circulation, so that materials can be circularly cleaned, and the generation of waste water is reduced; the air inlet system 400 is used for communicating the lower end of the tank body 200 to supply air, so that air with different properties can be supplied as required to pressurize, dry or reduce materials, and the air can stir the materials, so that the drying or reduction efficiency is improved; gases with different properties have different roles, and when the high-activity catalyst is dried, protective gas can be filled into the tank 200 to reduce the risk of spontaneous combustion; the pipeline type air heater 410 is used for heating the gas, so that the drying or reduction of the materials is facilitated; the tank heater 210 is used for heating the tank 200 to heat the material, so as to facilitate drying or reduction of the material; the tank body 200 can use a blind flange or a filter membrane flange as required, wherein the blind flange is used for sealing the upper end of the tank body 200, and the filter membrane flange is used for communicating the upper end of the tank body 200 to intercept and filter materials; the lower end of the can 200 is provided with a flat bottom valve 230 for controlling the opening and closing of the lower end of the can 200 without dead zone; the flat bottom valve 230 may be quickly connected to the fluid circulation system 300 or the air intake system 400 via the quick connector 240; the vacuum system 500 is used for connecting the flange with the filter membrane to vacuumize the tank 200, so that negative pressure filtration and accelerated drying are facilitated.
The invention can clean, filter, dry, impregnate and reduce the material in the same pot 200, which is convenient for preparing the catalyst in situ, and can reduce the transfer times of the material, thereby reducing the pollution and loss of the product and the waste of time; the materials can be circularly cleaned, so that the generation of waste water is reduced; the protective gas can be filled to protect the dry materials, so that the risk of spontaneous combustion of the materials is reduced, and the quality is controllable and safe; therefore, the invention can effectively improve the preparation efficiency and the preparation quality of the catalyst.
Fig. 2 shows an enlarged schematic view of the area a in fig. 1, and a sealing ring 221 is disposed between the flange with a filter membrane (or the blind flange) and the can 200, which is beneficial to improving the tightness between the flange and the can 200.
Further, the blind flange is used for sealing the upper end of the can body 200, so that the leakage of materials in the can body 200 can be prevented; the flange with the filter membrane is provided with a flange through hole 222 and a filter membrane 223, and the filter membrane 223 covers the flange through hole 222 and can prevent material loss while communicating the internal space of the tank body 200; the flange with the filter membrane not only can be used for connecting the tank body 200 with other systems, but also can play a role of a filter when the tank body 200 is inverted, namely, the filter can intercept and filter materials.
Specifically, the flat bottom valve 230 is an electric valve or a manual valve, is resistant to flushing and corrosion, has no dead zone, and is favorable for fully cleaning, dipping, drying, reducing and the like materials in the tank 200.
In some embodiments, the conduit between the air intake system 400 and the quick connector 240 is provided with a flow control valve for regulating the flow and pressure of the gas.
In some embodiments, referring to fig. 1, the liquid circulation system 300 includes a liquid storage tank 310 and a diaphragm pump 320, wherein the liquid storage tank 310 is installed at an upper end of the fixing frame 100, and is used for storing liquid and serving as a transfer station for liquid circulation; the diaphragm pump 320 is installed at the lower end of the fixing frame 100, and is used for driving the liquid to move; the liquid storage tank 310 and the diaphragm pump 320 are communicated based on a pipeline; when liquid circulation is performed, a flange with a filter membrane is arranged at the upper end of the tank body 200, the liquid storage tank 310 is connected with the flange with the filter membrane based on a pipeline, and the diaphragm pump 320 is connected with the quick connector 240 based on the pipeline.
Specifically, the liquid storage tank 310 is a 316L stainless steel tank or a high polymer material tank, and is firm, durable and corrosion-resistant; a filter screen can be arranged at the water outlet of the liquid storage tank 310 to prevent impurities from entering the diaphragm pump 320; the tank 310 may store a sufficient amount of pure water to facilitate the circulation of the liquid, and the tank 310 may be changed in water if necessary.
The parts of the diaphragm pump 320, which are in contact with the materials, are made of corrosion-resistant materials, can be 316L stainless steel or high polymer materials, and are durable. The pipeline between the diaphragm pump 320 and the quick connector 240 is provided with a flow regulating valve for regulating the water flow, so that on one hand, the water flow is ensured to be large enough, and the materials in the tank body 200 are fully fluidized; on the other hand, the damage of the filter membrane with the filter membrane flange caused by the large water flow is avoided. The pipe between the diaphragm pump 320 and the tank 310 is provided with a shut-off valve, which can shut off the circulation of the liquid when an emergency is encountered.
After the liquid circulation system 300 is started, pure water in the liquid storage tank 310 enters from the flat bottom valve 230 at the lower end of the tank body 200 under the drive of the diaphragm pump 320, flows out from the flange with the filter membrane at the upper end of the tank body 200, and returns to the liquid storage tank 310; the material in the tank 200 is fluidized by the impact of the water flow so that the material is sufficiently washed.
In some embodiments, the rotating mechanism 600 is a motor, the body of the motor is fixedly disposed on the side surface of the fixing frame 100, and the output end of the motor is fixedly connected with the can 200, so that the rotating angle of the can 200 can be accurately controlled, and meanwhile, the response speed of the motor is relatively high, so that the rotating direction of the can 200 can be easily changed.
In some embodiments, referring to fig. 1, the upper portion of the tank 200 has a cylindrical structure, and the lower portion of the tank 200 has a conical structure, which can collect materials so that the materials can sufficiently receive the impact of water or gas. When water flow or gas enters from the lower end of the tank body 200, the materials are impacted, and as the upper part of the tank body 200 is of a cylindrical structure and the lower part is of a conical structure, the lower part is small and the upper part is large, so that the materials have sufficient diffusion space; then, the material is recollected to the bottom along the inner wall of the conical structural region of the can 200 under the action of gravity, and continues to receive the impact of water flow or gas. Thus, the material can be ensured to be fully contacted with water flow, gas and the like, and the material is favorable for being fully washed, fully dried or fully reduced.
Specifically, the structural size of the tank 200 is optimized through simulation, so that the materials can be fully fluidized.
Generally, many materials are dried by loading the materials into a tray and then sending the materials into drying equipment for drying; however, the conventional drying equipment cannot be filled with the protective gas, and even if the conventional drying equipment can be filled with the protective gas, the problem that oxygen is difficult to completely exhaust due to too large volume and large dead space is caused, so that the spontaneous combustion of the high-activity catalyst is easy to occur in the drying process. Compared with the conventional drying equipment, the size of the tank 200 is smaller, the air tightness is good, no dead zone exists, the tank 200 can be easily filled with protective gas through the air inlet system 400, oxygen is discharged, the atmosphere of the full protective gas is formed, and the condition that the high-activity catalyst is spontaneously combusted in the drying process can be effectively avoided.
In some embodiments, the tank heater 210 is a silica gel heating pad, the silica gel heating pad wraps the outer peripheral surface of the tank 200, and the silica gel heating pad has good adhesion with the tank 200, which is beneficial to improving the heating efficiency.
The invention can clean, filter, dry, impregnate and reduce the material in the same pot 200, which is convenient for preparing the catalyst in situ, and can reduce the transfer times of the material, thereby reducing the pollution and loss of the product and the waste of time; the materials can be circularly cleaned, so that the generation of waste water is reduced; the protective gas can be filled to protect the dry materials, so that the risk of spontaneous combustion of the materials is reduced, and the quality is controllable and safe; therefore, the invention can effectively improve the preparation efficiency and the preparation quality of the catalyst.
FIG. 3 shows a flow chart of a method of application of a catalyst in situ preparation apparatus in an embodiment of the invention, comprising the steps of:
s1, modifying a carrier raw material;
Putting a carrier raw material and a modifier into a tank 200, installing a blind flange at the upper end of the tank 200 (refer to fig. 4), and obtaining a first modified carrier after impregnating for a preset time;
Specifically, the carrier raw material is a porous carrier material, and the porous carrier material comprises one or more of carbon black, activated carbon, mesoporous carbon, carbon nanotubes, graphene, aluminum oxide and diatomite. The modifier is an acidic liquid or an alkaline liquid, and is used as required to enhance the hydrophilicity of the carrier raw material so as to facilitate the subsequent adsorption of the metal precursor solution. The soaking time is 60-180 min, which is favorable for ensuring that the carrier raw material is fully modified and enhancing the hydrophilicity of the carrier raw material; depending on the type of carrier material, the amount of the material to be fed, etc., the impregnation may be carried out for 60min, 90min, 120min, 150min or 180min.
Furthermore, the feeding volume of the carrier raw material cannot exceed one half of the volume of the tank body, so that the carrier raw material is ensured to have enough fluidization space during subsequent cleaning, and the difficult processing of procedures such as filtration, drying, reduction and the like caused by excessive carrier raw material is avoided.
In some embodiments, the carrier material modification further comprises: the rotating mechanism 600 is started to drive the tank 200 to swing, and the carrier raw material and the modifier are turned over, so that the carrier raw material and the modifier are fully mixed, and the carrier raw material is fully modified.
Specifically, based on the vertical direction, the swinging rotation angle of the tank 200 is-120 degrees and +120 degrees, that is, the tank 200 swings left and right, and based on the vertical direction, the swinging angles to the left and right are 120 degrees, so that the carrier raw material and the modifier are fully mixed.
S2, filtering for the first time;
The blind flange is replaced by a flange with a filter membrane (refer to fig. 5), and the rotating mechanism 600 is started to drive the tank 200 to rotate until the flange with the filter membrane faces downwards, so that the redundant modifier is filtered out;
In some embodiments, the air inlet system 400 is connected with the quick connector 240, clean compressed air is introduced into the tank 200, the excess modifier is filtered out under pressure, and the first modified carrier remains in the tank 200; the pressurization can effectively improve the filtering speed and shorten the filtering time; the compressed air is easy to obtain and convenient to use.
In some embodiments, a vacuum system 500 is connected with the flange with the filter membrane, the tank 200 is vacuumized, the excess modifier is filtered out under negative pressure, and the first modified carrier is remained in the tank 200; the negative pressure can also effectively improve the filtering speed and shorten the filtering time.
In some embodiments, the pore diameter of the filtering membrane 223 with the filtering membrane flange is 0.2-10 μm, so that water and gas can normally pass through the filtering membrane 223 and materials can be intercepted; the pore size of the filter membrane 223 may be 0.22 μm, 0.45 μm, 1 μm, or 5 μm, or 10 μm, as desired.
S3, cleaning the first modified carrier;
Starting the rotating mechanism 600 to drive the tank body 200 to rotate until the flange with the filter membrane faces upwards, respectively connecting the flange with the filter membrane and the quick connector 240 with the liquid circulating system 300, and circularly cleaning the first modified carrier by pure water for a preset time to obtain a second modified carrier; the residual modifier in the first modified carrier can be washed off by circulating washing, so that the obtained second modified carrier is neutral, and the influence of the modifier on the metal precursor solution loaded on the subsequent second modified carrier is avoided.
When the circulating cleaning is carried out, pure water enters the tank body 200 from the lower end of the tank body 200, and the first modified carrier is flushed until the water overflows from the flange with the filter membrane, so that the liquid circulation is established; after the liquid circulation is established, the first modified carrier can be fully fluidized in water, and the circulation cleaning lasts for 30-120 min, so that the first modified carrier can be fully cleaned; depending on the amount of first modified support, the liquid may be circulated for 30min, 60min or 120min.
After the circulation cleaning is finished, the connection between the liquid circulation system 300 and the flange with the filter membrane and the quick connector 240 are released, so that the liquid circulation system 300 is prevented from interfering with the next operation.
S4, filtering for the second time;
Opening the rotating mechanism 600 to drive the tank 200 to rotate until the flange with the filter membrane faces downwards, so as to facilitate filtering out excessive water;
in some embodiments, the air inlet system 400 is connected with the quick connector 240, clean compressed gas is introduced into the tank 200, excess water is filtered out under pressure, and the second modified carrier remains in the tank 200; the pressurization can effectively improve the filtering speed and shorten the filtering time; the compressed air is easy to obtain and convenient to use.
In some embodiments, the vacuum system 500 is connected with the flange with the filter membrane, the tank 200 is vacuumized, the redundant water is filtered out under the negative pressure, and the second modified carrier is remained in the tank 200; the negative pressure can also effectively improve the filtering speed and shorten the filtering time.
S5, drying the second modified carrier;
Opening the rotating mechanism 600 to drive the tank 200 to rotate until the flange with the filter membrane faces upwards;
In some embodiments, the vacuum system 500 is flange-connected with the filter membrane to vacuum the tank 200 by a first drying method; opening a tank heater 210 to heat the tank 200; the rotating mechanism 600 is started to drive the tank 200 to swing and rotate, and the second modified carrier is turned over.
In the drying process, the second modified carrier in the tank 200 is heated and turned over, and the moisture gradually vaporizes; the vacuum system 500 can rapidly extract vaporized moisture, and form a negative pressure state around the second modified carrier, and a large humidity gradient is formed between the inner layer and the outer layer of the second modified carrier and between the surface and surrounding medium, so that the vaporization speed of the moisture is accelerated, the drying speed of the second modified carrier is effectively improved, and finally the second modified carrier can be dried to be in a loose powder state.
Specifically, the temperature of the tank heater 210 is set to 60-150 ℃, that is, the temperature range for drying the second modified carrier is 60-150 ℃, so that the safety and the risk are low; specifically, a certain temperature may be selected for drying, such as 60 ℃, or 80 ℃, or 100 ℃, or 110 ℃, or 120 ℃, or 130 ℃, or 140 ℃, or 150 ℃; the step-type heating drying can also be selected, the first stage is performed at 60-80 ℃, the second stage is performed at 100-120 ℃, and the third stage is performed at 130-150 ℃, so that the drying efficiency is both considered, the energy consumption is reduced, and the microstructure of the carrier is protected.
Further, based on the vertical direction, the swinging rotation angle of the tank 200 is-120 ° and +120°, that is, the tank 200 swings left and right, and based on the vertical direction, the swinging angles of the tank 200 are 120 ° to the left and right, so that the second modified carrier in the tank 200 can be fully turned, which is beneficial to accelerating the drying efficiency of the second modified carrier.
In some embodiments, a second drying mode is adopted to connect the air inlet system 400 and the quick connector 240, and clean compressed gas is introduced into the tank 200 to agitate the second modified carrier; and turns on the duct type air heater 410 to heat the compressed gas; during the drying process, the can 200 remains stationary and cannot rotate.
In the drying process, the heated compressed gas enters the tank 200, can stir and heat the second modified carrier, so that the second modified carrier is sufficiently heated, the moisture in the second modified carrier can be rapidly vaporized, and the vaporized moisture is wrapped and clamped and discharged from the flange with the filter membrane, so that the drying efficiency is extremely high; the second modified carrier after complete drying is in a loose powder state. The flange with the filter membrane can be connected with an exhaust hose, so that hot and moisture-containing gas can be conveniently drained to a designated place.
Specifically, the temperature of the pipeline type air heater 410 is set to be 60-150 ℃, namely the temperature range for drying the second modified carrier is 60-150 ℃, so that the pipeline type air heater is safe and has low risk; specifically, a certain temperature may be selected for drying, such as 60 ℃, or 80 ℃, or 100 ℃, or 110 ℃, or 120 ℃, or 130 ℃, or 140 ℃, or 150 ℃; the step-type heating drying can also be selected, the first stage is performed at 60-80 ℃, the second stage is performed at 100-120 ℃, and the third stage is performed at 130-150 ℃, so that the drying efficiency is both considered, the energy consumption is reduced, and the microstructure of the carrier is protected.
Further, the compressed gas is compressed air or compressed nitrogen; compressed air is easy to obtain and convenient to use; the compressed nitrogen can provide inert atmosphere, isolate air and avoid spontaneous combustion of the combustible carrier in the drying process.
S6, loading a second modified carrier;
the dried second modified carrier is reserved in the tank 200, a metal precursor solution is added into the tank 200, the blind flange is arranged at the upper end of the tank 200 (refer to fig. 4), and a catalyst precursor is obtained after soaking for a preset time;
In some embodiments, the metal precursor solution includes chloroplatinic acid solution, cupric chloride solution, nickel chloride solution, ferric chloride solution, and the like, and platinum-based catalyst, copper-based catalyst, nickel-based catalyst, iron-based catalyst, and the like can be prepared.
Specifically, the dosage of the metal precursor solution is determined according to the self concentration, the dosage of the second modified carrier and the preset load; the feeding volume of the metal precursor solution is at least 2 times of the volume of the second modified carrier, so that the metal precursor solution can fully submerge the second modified carrier, and the metal precursor solution and the second modified carrier are easier to uniformly mix. Optionally, the volume of the metal precursor solution is 2 times, or 3 times, or 4 times that of the second modified support, which is favorable for fully mixing the metal precursor solution and the second modified support, is convenient for the second modified support to fully absorb the metal precursor solution, and does not cause too much water to be difficult to dry.
Further, the soaking time is 60-180 min, which is favorable for ensuring that the second modified carrier fully loads the metal precursor solution; the impregnation may be performed for 60min, 90min, 120min, 150min or 180min depending on the kind, the amount of the metal precursor solution, etc.
In some embodiments, the second modified-support loading further comprises: the rotating mechanism 600 is started to drive the tank 200 to swing and rotate, and the second modified carrier and the metal precursor solution are turned over, so that the second modified carrier and the metal precursor solution are fully mixed, and the metal precursor solution carries the metal precursor into micropores of the second modified carrier fully, so that the second modified carrier fully loads the metal precursor.
Specifically, based on the vertical direction, the swinging rotation angle of the tank 200 is-120 ° and +120°, that is, the tank 200 swings left and right, and based on the vertical direction, the swinging angles to the left and right are 120 °, so as to ensure that the second modified carrier and the metal precursor solution are fully mixed.
In some embodiments, the second modified-support loading further comprises: ball milling beads are put into the tank 200, and the ball milling beads can improve the mixing efficiency of the second modified carrier and the metal precursor solution and improve the mixing uniformity of the second modified carrier and the metal precursor solution.
Specifically, the particle size range of the ball-milling beads is 0.5-1 cm, so that the mixing efficiency and the mixing uniformity of the metal precursor solution and the second modified carrier can be effectively improved, and the subsequent screening is facilitated; the ball milling beads are zirconium beads, glass beads or PTFE beads, and are heat-resistant, corrosion-resistant and not dissolved out.
S7, drying the catalyst precursor;
replacing the blind flange with the filter membrane flange (see fig. 5), wherein the filter membrane flange faces upwards;
the second modified carrier is immersed in the metal precursor solution to obtain a catalyst precursor, and then is directly dried with liquid without filtering; during the drying process, the concentration of the solution gradually increases, and the loading amount of the second modified support can be increased.
In some embodiments, the vacuum system 500 is flange-connected with the filter membrane to vacuum the tank 200 by a first drying method; turning on the can heater 210 to heat the can 200; the rotation mechanism 600 is turned on to drive the can 200 to swing and turn the catalyst precursor.
During the drying process, the catalyst precursor with liquid in the tank 200 is heated and turned over, and the moisture gradually vaporizes; the vacuum system 500 can reduce the pressure in the tank 200, thereby reducing the boiling point of the solution, enabling evaporation and boiling to be performed simultaneously, and accelerating the evaporation speed of water. Meanwhile, vacuumizing is carried out, vaporized moisture is rapidly pumped out, a negative pressure state is formed around the catalyst precursor, a large humidity gradient is formed between the inner layer and the outer layer of the catalyst precursor and between the surface and surrounding media, the vaporization speed of the moisture is accelerated, the drying speed of the catalyst precursor is effectively improved, and finally the catalyst precursor in a loose powder state can be obtained; at this time, the metal precursor in the metal precursor solution is sufficiently loaded into the second modified support in preparation for subsequent reduction.
Specifically, the temperature of the tank heater 210 is set to 60-150 ℃, i.e., the temperature range for drying the catalyst precursor is 60-150 ℃, which is safe and has low risk; specifically, a certain temperature may be selected for drying, such as 60 ℃, or 80 ℃, or 100 ℃, or 110 ℃, or 120 ℃, or 130 ℃, or 140 ℃, or 150 ℃; or step heating to dry, treating the catalyst precursor with liquid at 60-80 deg.c to change the catalyst precursor into slurry state from suspension state, heating to 100-120 deg.c and further drying; when the catalyst precursor with liquid in the slurry state is changed into a micro-wet state, heating to 130-150 ℃ for thorough drying until the catalyst precursor is dried into a loose powder state; such stepped temperature-rising drying is advantageous in reducing energy consumption, and in protecting the microstructure of the second modified support, and in ensuring the bonding strength of the second modified support and the metal precursor.
Further, based on the vertical direction, the swinging rotation angle of the tank 200 is-120 ° and +120°, that is, the tank 200 swings left and right, and based on the vertical direction, the swinging angles to the left and right are 120 °, so that the catalyst precursor in the tank 200 can be fully turned, which is beneficial to accelerating the drying efficiency of the catalyst precursor.
In some embodiments, a second drying mode is used to connect the air inlet system 400 and the quick connector 240, and clean compressed gas is introduced into the tank 200 to agitate the catalyst precursor; and turns on the duct type air heater 410 to heat the compressed gas; during the drying process, the can 200 remains stationary and cannot rotate.
In the drying process, the heated compressed gas enters the tank 200, can stir and heat the catalyst precursor with liquid, fully heats the catalyst precursor with liquid, can quickly vaporize moisture, and can discharge the vaporized moisture from the flange with the filter membrane, so that the drying efficiency is extremely high; the completely dried catalyst precursor is in a loose powder state, and at the moment, the metal precursor of the metal precursor solution is fully loaded into the second modified carrier to prepare for subsequent reduction. The flange with the filter membrane can be connected with an exhaust hose, so that hot and moisture-containing gas can be conveniently drained to a designated place.
Specifically, the temperature of the pipe-type air heater 410 is set to 60-150 ℃, that is, the temperature range for drying the catalyst precursor is 60-150 ℃, so that the safety and the risk are low; specifically, a certain temperature may be selected for drying, such as 60 ℃, or 80 ℃, or 100 ℃, or 110 ℃, or 120 ℃, or 130 ℃, or 140 ℃, or 150 ℃; or step heating to dry, treating the catalyst precursor with liquid at 60-80 deg.c to change the catalyst precursor into slurry state from suspension state, heating to 100-120 deg.c and further drying; when the catalyst precursor with liquid in the slurry state is changed into a micro-wet state, heating to 130-150 ℃ for thorough drying until the catalyst precursor is dried into a loose powder state; such stepped temperature-rising drying is advantageous in reducing energy consumption, and in protecting the microstructure of the second modified support, and in ensuring the bonding strength of the second modified support and the metal precursor.
Further, the compressed gas is compressed air or compressed nitrogen; compressed air is easy to obtain and convenient to use; the compressed nitrogen can provide inert atmosphere, isolate air and avoid spontaneous combustion of combustible materials in the drying process.
S8, reducing the catalyst precursor;
Retaining the dried catalyst precursor in the tank 200 with the filter membrane flange facing upwards; connecting the air inlet system 400 with the quick connector 240, and starting the pipeline type air heater 410 and/or the tank heater 210, and introducing hydrogen into the tank 200 to perform reduction treatment on the catalyst precursor to obtain a catalyst finished product; during the reduction process, the canister 200 remains stationary and cannot rotate.
Hydrogen enters the tank 200 and the catalyst precursor is reduced under heating, namely, the metal precursor is reduced into a metal simple substance, and the metal simple substance is attached to the carrier to form the metal-based catalyst. Specifically, the reduction treatment includes two stages:
Firstly, evacuating air in the tank body 200 by using hydrogen so as to ensure the safety of the reduction process;
in the second stage, the temperature of the tank 200 reaches a preset condition, and the reduction reaction is started.
Wherein the heating conditions may be provided by the duct type air heater 410 and/or the tank heater 210; preferably, the duct type air heater 410 and the tank heater 210 are activated simultaneously, providing more stable temperature conditions for the reduction process. Specifically, the temperature of the reduction treatment is in the range of 150-240 ℃, the treatment temperature is selected according to the amount of the catalyst precursor in the range, and the more the amount of the catalyst precursor is, the higher the temperature of the reduction treatment is, so that the reduction efficiency is ensured; alternatively, the temperature of the reduction treatment may be 150 ℃, 170 ℃, 190 ℃, 210 ℃ or 240 ℃.
The waste gas generated by the reduction reaction is discharged from the flange with the filter membrane, and the flange with the filter membrane is connected with the corrosion-resistant pipeline, so that the waste gas is discharged to the absorption tower for treatment, and the waste gas is prevented from polluting the environment and endangering the health of human bodies. The completion of the reduction can be determined by detecting the acidity or basicity of the exhaust gas discharged from the flange with the filter membrane.
After the reduction is finished, the hydrogen in the tank body 200 is discharged through the nitrogen, so that the catalyst finished product is naturally cooled to the room temperature in the nitrogen atmosphere.
S9, pouring out a catalyst finished product;
the connection between the air inlet system 400 and the quick connector 240 is released, the flange with the filter membrane is detached, the material receiving barrel is installed at the upper end of the tank body 200, the rotating mechanism 600 is started to drive the tank body 200 to rotate until the material receiving barrel is positioned below, the catalyst finished product is poured out, the unloading is easy, and the operation is simple.
If ball-milling beads are put into the previous loading procedure, the ball-milling beads in the catalyst finished product are also required to be sieved out, and then the catalyst is weighed, packaged and put in storage for standby.
The invention can clean, filter, dry, impregnate and reduce the materials in the same tank 200, which is convenient for preparing the catalyst in situ; in addition, under the cooperation of the air inlet system 400, the rotating mechanism 600, the vacuum system 500 and the like, the operations of pressurizing or negative pressure filtering, turning or stirring materials, vacuumizing and drying, pneumatic drying and the like can be realized, and the efficiency of filtering, drying and the like is effectively improved; in addition, the invention can reduce the material transferring times, thereby reducing the product pollution and loss and reducing the time waste; the materials can be circularly cleaned, so that the generation of waste water is reduced; the material can be filtered under pressure or negative pressure, and the filtering efficiency is high; the protective gas can be filled to protect the dry materials, so that the risk of spontaneous combustion of the materials is reduced, and the quality is controllable and safe.
Therefore, the invention can effectively improve the preparation efficiency and the preparation quality of the catalyst.
The foregoing has described in detail the apparatus for in-situ preparation of a catalyst and the method for application thereof according to the embodiments of the present invention, and specific examples should be adopted to illustrate the principles and embodiments of the present invention, and the description of the foregoing examples is only for aiding in understanding the method and core idea of the present invention; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present invention, the present description should not be construed as limiting the present invention in view of the above.
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| CN111994918A (en) * | 2020-08-27 | 2020-11-27 | 宁夏美邦寰宇化学有限公司 | Preparation method and preparation system of titanium silicalite molecular sieve catalyst |
| CN112675610A (en) * | 2020-12-30 | 2021-04-20 | 无锡先导智能装备股份有限公司 | Catalyst filtering system, control method thereof and catalyst preparation system |
| CN112710128A (en) * | 2020-12-30 | 2021-04-27 | 无锡先导智能装备股份有限公司 | Catalyst drying system, control method thereof and catalyst preparation system |
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| CN111420585A (en) * | 2019-07-16 | 2020-07-17 | 镇江市思泰智能装备技术有限公司 | A kind of catalyst slurry automatic preparation system and preparation method |
| CN111994918A (en) * | 2020-08-27 | 2020-11-27 | 宁夏美邦寰宇化学有限公司 | Preparation method and preparation system of titanium silicalite molecular sieve catalyst |
| CN112675610A (en) * | 2020-12-30 | 2021-04-20 | 无锡先导智能装备股份有限公司 | Catalyst filtering system, control method thereof and catalyst preparation system |
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