Catalyst mass production molding device and molding method

Abstract

The present application relates to a catalyst mass production molding device and molding method, and belongs to the field of catalyst production molding technology. It includes a freeze-drying assembly, a post-processing assembly and a cooling system. The freeze-drying assembly includes a feed assembly, an insulation box, a freeze-drying chamber and a temperature regulating coil. The temperature regulating coil is in contact with the freeze-drying chamber. The freeze-drying chamber is arranged inside the insulation box. The feed assembly located outside the insulation box is connected to the feed port of the freeze-drying chamber. The freeze-drying chamber is connected to an external vacuum pumping device through an exhaust pipe, and a heating device is provided on the freeze-drying chamber. The post-processing assembly includes a crushing box and a discharge assembly, and the cooling system is connected to the inlet and outlet of the temperature regulating coil. The present application uses vacuum freeze-drying technology to shape the bio-enzyme catalyst so that it is transformed from a slurry into powder particles. The whole process is at low temperature, the enzyme activity yield is greater than 95%, and the residual moisture is less than 3%, which makes the catalyst more stable and is particularly suitable for catalysts made from heat-sensitive enzymes.

Description

Technical Field

[0001] The present application belongs to the technical field of catalyst preparation and molding, and specifically relates to a catalyst mass preparation and molding device and molding method. Background Art

[0002] Bio-enzyme catalysts are widely used in food, textiles, bioenergy, medicine and other fields. Their catalytic efficiency is much higher than that of inorganic catalysts and their added value is higher.

[0003] Existing bio-enzyme catalysts often concentrate the fermentation broth into a slurry, then spray-dry it into a powder for molding. Although this process has the advantage of continuous production, it has the problem of significant activity loss. High temperature can cause irreversible denaturation and inactivation of proteins. Under high temperature conditions, the enzyme activity loss rate is generally greater than 30%. High temperature can also destroy the hydrogen bonds and hydrophobic interactions of enzyme proteins, causing the tertiary structure to collapse and the active center conformation to change. For example, the enzyme activity yield of alkaline pectinase produced by Bacillus subtilis is less than 10% at an inlet air temperature of 160°C. Summary of the Invention

[0004] The technical problem to be solved by the present application is: to overcome the deficiencies of the prior art and provide a catalyst mass preparation molding device and molding method. The present application uses vacuum freeze-drying technology to mold the biological enzyme catalyst, so that it is transformed from a slurry into powder particles. The entire process is at low temperature, the enzyme activity yield is greater than 95%, and the residual moisture is less than 3%, making the catalyst more stable, and is particularly suitable for catalysts made from heat-sensitive enzymes.

[0005] The technical solution adopted by this application to solve the problems existing in the prior art is:

[0006] A catalyst mass production molding device comprises a freeze-drying assembly, a post-processing assembly and a cooling system.

[0007] The freeze-drying assembly includes a feeding assembly, an insulation box, a freeze-drying chamber and a temperature control coil. The temperature control coil is in contact with the freeze-drying chamber. The freeze-drying chamber is arranged inside the insulation box. The feeding assembly located outside the insulation box is connected to the feeding port of the freeze-drying chamber. The freeze-drying chamber is connected to the external vacuum equipment through an exhaust pipe. The freeze-drying chamber is provided with a heating device.

[0008] The post-processing assembly includes a crushing box, and a plurality of layers of vibrating screens arranged at intervals are arranged inside the crushing box. The crushing box is connected to the discharge assembly.

[0009] The freeze-drying bin, the heat preservation box and the crushing box are connected through a passage, and an electrically or pneumatically controlled door panel is provided on the passage.

[0010] The cooling system is connected to the inlet and outlet of the temperature regulating coil.

[0011] Preferably, the feed assembly and the discharge assembly have the same structure, and both include a first air-controlled valve, an intermediate tank, a second air-controlled valve, a terminal pipe and a sub-control device.

[0012] The inlets and outlets at the upper and lower ends of the intermediate tank are respectively connected to the first air-controlled valve and the second air-controlled valve. The second air-controlled valve is arranged between the intermediate tank and the terminal pipe. The sub-control device is connected to the first air-controlled valve and the second air-controlled valve through two valve-closing control air pipes and two valve-opening control air pipes. The sub-control device is externally connected to an external high-pressure air pipe.

[0013] Preferably, the sub-control device includes a valve body and a cover plate that are detachably connected.

[0014] The valve body is provided with an air intake cavity connected to an external high-pressure air pipe. The air intake cavity is connected to the extension control air cavity and the contraction control air cavity arranged at intervals. The extension control air cavity is connected to two first air cavities, the first cavity is connected to the valve opening control air pipe, the contraction control air cavity is connected to two second air cavities, and the second cavity is connected to the valve closing control air pipe.

[0015] The valve body is provided with four valve stem movable holes, and the planes where the axes of the valve stem movable holes are located are perpendicular to the planes where the axes of the first air cavity and the second air cavity are located.

[0016] Two valve stem movable holes are connected to the two first air cavities through-and-through, and the other two valve stem movable holes are connected to the two second air cavities through-and-through.

[0017] A valve opening control valve column is provided inside the valve stem movable hole connected to the first air cavity, and a first through hole matched with the first air cavity is provided on the first cylinder of the valve opening control valve column.

[0018] A valve control valve column is arranged inside the valve stem movable hole connected to the second air cavity, and a second through hole connected to the second air cavity is arranged on the second cylinder of the valve closing control valve column.

[0019] A control assembly for controlling the sliding of a valve opening control valve column and a valve closing control valve column is arranged outside the cover plate.

[0020] Preferably, a continuous vacuum air cavity is provided inside the valve body, and both ends of the vacuum air cavity are respectively connected to the vacuum tube and the connecting pipe, and the end of the connecting pipe is passed through to the interior of the intermediate tank.

[0021] The two valve stem movable holes which are in continuous connection with the second air cavity are in continuous connection with the vacuum air cavity.

[0022] The second cylindrical body of the valve closing control valve column is provided with a third through hole which is matched with the vacuum air cavity.

[0023] Preferably, the end surface where the heat preservation box is connected to the crushing box is provided with a discharge channel, and the corresponding position of the crushing box is provided with a feed channel, and the feed channel is connected with the discharge channel.

[0024] The discharge channel is provided with a second door panel, and the second telescopic device drives the second door panel to move, thereby achieving communication and isolation between the discharge channel and the feed channel.

[0025] The lower half of the end face of the freeze-drying bin facing the discharge channel is open, and a slot is provided in the inner wall of the upper half of the end face. A first door panel is slidably provided inside the slot. A first telescopic device fixedly connected to the freeze-drying bin controls the up and down movement of the first door panel. The first door panel moves down to the lowest point, covering the open area of ​​the lower half of the end face of the freeze-drying bin facing the discharge channel.

[0026] An open area at the lower half of the end surface of the freeze-drying bin facing the discharge channel is connected to the discharge channel through a connecting frame.

[0027] Preferably, the freeze-drying chamber is supported inside the thermal insulation box by an externally provided heat-insulating support frame.

[0028] Preferably, a push plate is provided inside the freeze-drying chamber, the bottom surface and left and right side surfaces of the push plate are in contact with the inner wall of the freeze-drying chamber, the top of the push plate is threadedly connected to a screw through a threaded hole, the end of the screw is connected to a first motor, and the first motor drives the push plate away from or close to the first door panel through the screw.

[0029] Preferably, the cooling system includes an internal circulation system and an external circulation system. The external circulation system exchanges heat with the internal circulation system through an exchanger. The external circulation system is connected to a temperature regulating coil to cool the freeze-drying chamber.

[0030] Preferably, the internal circulation system includes a liquid nitrogen storage tank, a first delivery pump and a first heat exchanger connected in series.

[0031] The external circulation system includes a nitrogen storage tank connected in series with the temperature regulating coil, a second delivery pump and a first heat exchanger.

[0032] The flowing medium in the inner circulation system is liquid nitrogen, and the flowing medium in the outer circulation system is nitrogen gas. The liquid nitrogen passes through the first heat exchanger to reduce the temperature of the nitrogen gas.

[0033] A catalyst mass production molding method, based on the above-mentioned catalyst mass production molding device, comprises the following steps:

[0034] S01, the vacuum equipment vacuums the freeze-drying chamber through the vacuum pipe, so that the air pressure inside the freeze-drying chamber is maintained between 1~30Pa, and the freeze-drying chamber is cooled by the cooling system to reduce the temperature inside the freeze-drying chamber to between -40℃ and -50℃;

[0035] S02. The slurry enters the freeze-drying chamber through the feeding assembly. During the feeding process, the first air control valve is opened first, and the second air control valve is closed, and the slurry is injected into the intermediate tank;

[0036] Then close the first air control valve, and the vacuum equipment evacuates the intermediate tank through the connecting pipe to maintain the internal pressure between 1 and 30 Pa. The internal pressure of the intermediate tank is lower than the internal pressure of the freeze-drying chamber. Then open the second air control valve and the slurry flows into the freeze-drying chamber.

[0037] S03. After the slurry is frozen in the freeze-drying chamber for 2 to 4 hours, the temperature inside the freeze-drying chamber is raised to between -25°C and -20°C, and the air pressure inside the freeze-drying chamber is reduced to 10Pa to 15Pa for primary drying;

[0038] The control method for the temperature rise of the thermostatic coil adopts any one of the following two schemes or a combination of the two:

[0039] 1. By increasing the power of the second delivery pump, the flow rate of nitrogen in the external circulation system is increased, thereby reducing the heat exchange efficiency between nitrogen and liquid nitrogen in the first heat exchanger, thereby increasing the temperature of the nitrogen and thus increasing the temperature of the thermostatic coil;

[0040] 2. Turn off the first delivery pump;

[0041] S04, after the primary drying is maintained for 4 to 6 hours, the secondary drying process is entered, and the temperature of the secondary drying is increased to 25°C to 55°C. When the temperature inside the freeze-drying chamber reaches 0°C, the first delivery pump and the second delivery pump (49) are turned off, and the heating device is turned on. The heating device adopts electric heating to heat the freeze-drying chamber;

[0042] During the secondary drying process, the air pressure inside the freeze-drying chamber is adjusted to less than 5 Pa, and the secondary drying time is maintained for 2 to 3 hours;

[0043] S05. After completing the secondary drying, the freeze-drying chamber pushes the bulk catalyst into the crushing box, and the bulk catalyst is broken into particles by the vibrating screen. The particles then enter the discharge assembly through the vibrating screen and are finally discharged through the discharge assembly.

[0044] Compared with the prior art, this application has the following beneficial effects:

[0045] (1) Vacuum freeze-drying technology is used to form the slurry of the bio-enzyme catalyst into powder particles. The low-temperature anoxic environment and the biochemical dehydration mechanism work together to increase the enzyme activity retention rate by 20-90% compared to the spray drying process, and the enzyme activity retention rate reaches more than 95%. At the same time, the residual water rate is ≤3%, and the room temperature stability is improved. It is particularly suitable for heat-sensitive enzyme catalysts and high-enzyme added catalysts.

[0046] (2) The temperature range below 0℃ in the freeze-drying chamber is adjusted by the cooling system, and the temperature range above 0℃ is adjusted by the electric heating device. This not only saves energy and reduces consumption, but also is more conducive to achieving step-by-step temperature increase during the secondary drying process, making temperature control more precise. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] The present application is further described below with reference to the accompanying drawings and examples.

[0048] Figure 1 This is a structural diagram of a catalyst mass production molding device for this application.

[0049] Figure 2 This is a freeze-drying assembly structure diagram for a catalyst mass production molding device in this application.

[0050] Figure 3 This is the first partial cross-sectional view of the insulation box in the freeze-drying assembly of this application.

[0051] Figure 4 This is the second partial cross-sectional view of the insulated box in the freeze-drying assembly of this application.

[0052] Figure 5 This is the structural diagram of the freeze-drying assembly after removing the insulation box.

[0053] Figure 6 This is the structural diagram of the feed assembly in the freeze-drying assembly of this application.

[0054] Figure 7 This is a cross-sectional view of the rubber connecting pipe in the freeze-drying assembly of this application.

[0055] Figure 8 This is the structural diagram of the sub-control device in the freeze-drying assembly of this application.

[0056] Figure 9 This is the exploded view of the sub-control device in the freeze-drying assembly for this application.

[0057] Figure 10 This is the first cross-sectional view of the sub-control device in the freeze-drying assembly of this application.

[0058] Figure 11 This is the second cross-sectional view of the sub-control device in the freeze-drying assembly of this application.

[0059] Figure 12 This is the third cross-sectional view of the sub-control device in the freeze-drying assembly of this application.

[0060] Figure 13 This is the structure diagram of the valve column in the sub-control device of this application.

[0061] Figure 14 for Figure 13 A cross-sectional view of

[0062] Figure 15 This is the structure diagram of the valve column of the closing valve control device in this application.

[0063] Figure 16 for Figure 15 A cross-sectional view of

[0064] Figure 17 This is the structural diagram of the freeze-drying assembly after removing the insulation box and the feeding assembly.

[0065] Figure 18 for Figure 17 Front view of

[0066] Figure 19 This is the freeze-drying chamber structure diagram of the freeze-drying assembly in this application.

[0067] Figure 20 for Figure 19 A cross-sectional view of

[0068] Figure 21 This is the structure diagram of the temperature regulating coil in the freeze drying assembly for this application.

[0069] Figure 22 This is the structural diagram of the heat insulation support frame in the freeze-drying assembly of this application.

[0070] Figure 23 This is the door panel structure diagram of the freeze-drying assembly for this application.

[0071] Figure 24 This is the first structural diagram of the post-processing assembly in a catalyst mass production molding device of this application.

[0072] Figure 25 This is the second structural diagram of the post-processing assembly of this application.

[0073] Figure 26 for Figure 25 Cross-sectional view after removing the discharge assembly,

[0074] Figure 27 for Figure 26 A partial enlarged view of point A in the middle.

[0075] Figure 28 for Figure 26 A partial enlarged view of point B in the middle.

[0076] Figure 29 This is a diagram of the cooling system in a large-scale catalyst preparation and molding device for this application.

[0077] In the figure: 1-feed pipe, 2-first air control valve, 3-intermediate tank, 4-second air control valve, 5-end pipe, 6-rubber connecting pipe, 601-clamping ring area, 7-fixing frame, 8-sub-control device, 801-valve body, 802-cover plate, 803-inlet cavity, 804-extension control cavity, 805-contraction control cavity, 806-first branch cavity, 807-first pressure relief cavity, 808-first pressure relief hole, 809-second branch cavity, 8010-second pressure relief cavity, 8011-second pressure relief hole, 8012-valve stem movable hole, 8013-vacuum cavity, 9-valve opening control valve column, 901-first cylinder, 902-first control rod, 903-first clamping ball head, 904-first through hole, 905-first L-shaped hole, 10-valve closing control valve column, 1001-second cylinder, 1002-second control rod, 1003-second clamping ball head, 1004-second through hole, 1005-second L-shaped hole, 1006-third through hole, 11-lever, 1101-waist-shaped hole, 12-servo motor, 13-external high-pressure air pipe, 14-valve closing control air pipe, 15-valve opening control air pipe, 16-vacuum tube, 17-connecting pipe, 18-insulation box, 1801-discharge channel, 1802-U-shaped groove, 1803-upper connecting plate, 19-freeze-drying chamber, 1901-feeding port, 1902-exhaust hole, 1903-rib, 1904-slot, 20-first door panel, 21-first telescopic device, 22-push plate, 2201-slanted area, 23-screw, 24-first motor, 25-temperature regulating coil, 26-exhaust hood, 2601-exhaust pipe, 27-connecting frame, 28-insulation support frame, 29-vibrator, 30-heating device, 31-second door panel , 33-second telescopic device, 33-crushing box, 3301-feeding channel, 3302-lower connecting plate, 3303-annular limit frame, 3304-spring top plate, 3305-discharge port, 34-filter plate, 35-spring, 36-camshaft, 37-second motor, 38-grating, 39-liquid nitrogen storage tank, 40-first delivery pump, 41-first heat exchanger, 42-temperature controller, 43-three-way valve, 44-reflux storage tank, 45-compressor, 46-second heat exchanger, 47-expander, 48-nitrogen storage tank, 49-second delivery pump. DETAILED DESCRIPTION

[0078] Combined with the attached drawings Figures 1 to 29 A catalyst mass production molding device and molding method of the present application are further described in detail, but this does not limit the present application.

[0079] A catalyst mass production molding device, comprising Figure 1 As shown, it includes a freeze-drying assembly, a post-processing assembly and a cooling system.

[0080] The freeze-drying assembly includes a feeding assembly, an insulation box 18, a freeze-drying chamber 19 and a temperature control coil 25. The temperature control coil 25 is in contact with the freeze-drying chamber 19. The temperature control coil 25 includes two groups of serpentine tubes connected in series. The two groups of serpentine tubes are respectively tightly attached to the outer walls on the left and right sides of the freeze-drying chamber 19.

[0081] The freeze drying chamber 19 is arranged inside the heat preservation box 18, and the freeze drying chamber 19 is supported inside the heat preservation box 18 by an externally arranged heat insulation support frame 28. Figure 22 As shown, the insulation support frame 28 includes a bottom plate, bottom support beams, side support beams, and a top support beam. Vertically arranged protrusions 1903 are provided on the left and right side walls of the freeze-drying chamber 19. The side support beams of the insulation support frame 28 have recessed slots, into which the protrusions 1903 are secured. Vertically arranged U-shaped grooves 1802 are provided on the inner wall of the insulated box 18, into which the side support beams of the insulation support frame 28 are secured.

[0082] The insulating support frame 28 is made of rubber, providing both thermal insulation and vibration within the freeze-drying chamber 19. To this end, several vibrators 29 are mounted on the bottom plate of the insulating support frame 28, with their oscillators abutting the bottom surface of the freeze-drying chamber 19. Once the slurry is injected into the freeze-drying chamber 19, the vibrators 29 can be activated to vibrate the slurry.

[0083] By combining high-speed vibration with a vacuum environment, the slurry rapidly boils near its freezing point, absorbing heat and instantly freezing into a micron-sized "smoothie" structure. During the freezing process, vibration inhibits ice crystal growth, preventing the particle agglomeration caused by ice crystal extrusion during traditional freezing. This results in a highly dispersed powder after drying, rather than the porous lumps of traditional freeze-dried materials. Vibration also increases heat exchange, boosting the sublimation rate by 3-5 times, thereby reducing energy consumption.

[0084] The feed assembly, located outside the insulated box 18, is connected to the feed port 1901 of the freeze-drying chamber 19. A row of exhaust holes 1902 are located on the top surface of the freeze-drying chamber 19. A vacuum hood 26, covering all of the exhaust holes 1902, is installed outside the freeze-drying chamber 19. The vacuum hood 26 is connected to an external vacuum pump via an exhaust pipe 2601. A heating device 30 is installed on the freeze-drying chamber 19. This device uses electrical heating to keep the interior of the freeze-drying chamber 19 heated to approximately 50°C.

[0085] During the vacuum freeze-drying process of the bio-enzyme catalyst, the internal temperature of the freeze-drying chamber 19 is adjusted within a range of -50°C to 50°C. The refrigerant of the cooling system uses liquid nitrogen, which is more suitable for temperatures below 0°C. Therefore, a heating device 30 is added to adjust the temperature of the freeze-drying chamber 19 to a range above 0°C.

[0086] The feed assembly includes a first air control valve 2 , an intermediate tank 3 , a second air control valve 4 , a terminal pipe 5 and a sub-control device 8 , and the sub-control device 8 is fixedly connected to the intermediate tank 3 via a fixing frame 7 .

[0087] The inlets and outlets at the upper and lower ends of the intermediate tank 3 are respectively connected to the first air-controlled valve 2 and the second air-controlled valve 4. The second air-controlled valve 4 is arranged between the intermediate tank 3 and the terminal pipe 5. The sub-control device 8 is connected to the first air-controlled valve 2 and the second air-controlled valve 4 through two valve-closing control air pipes 14 and two valve-opening control air pipes 15. The sub-control device 8 is externally connected to an external high-pressure air pipe 13.

[0088] Depend on Figure 8 As shown, the sub-control device 8 is connected to the outside of the external high-pressure gas pipe 13, the valve closing control gas pipe 14, the valve opening control gas pipe 15, the vacuum tube 16 and the connecting pipe 17, and the end of the connecting pipe 17 is passed through the interior of the intermediate tank 3.

[0089] The external high-pressure gas pipe 13 is connected to an external high-pressure gas supply device, and the vacuum pipe 16 is connected to an external vacuum pumping device.

[0090] The two valve closing control air pipes 14 and the two valve opening control air pipes 15 are connected to the control air interfaces of the first air-controlled valve 2 and the second air-controlled valve 4 respectively.

[0091] Depend on Figures 8 to 16 As shown, the sub-control device 8 includes a detachably connected valve body 801 and a cover plate 802, which are fixedly connected by bolts.

[0092] The valve body 801 is internally provided with an air intake chamber 803 connected to the external high-pressure air pipe 13. The air intake chamber 803 is interconnected with an extension control chamber 804 and a contraction control chamber 805, which are spaced apart. The extension control chamber 804 is interconnected with two first branch air chambers 806, which are interconnected with the valve opening control air pipe 15. The contraction control chamber 805 is interconnected with two second branch air chambers 809, which are interconnected with the valve closing control air pipe 14.

[0093] The axes of the air inlet cavity 803 , the extension control cavity 804 , the contraction control cavity 805 , the first branch cavity 806 and the second branch cavity 809 are all located in the same plane.

[0094] A continuous vacuum air cavity 8013 is provided inside the valve body 801 , and both ends of the vacuum air cavity 8013 are connected to the vacuum tube 16 and the connecting tube 17 respectively.

[0095] The valve body 801 is provided with four valve stem movable holes 8012. The axes of the valve stem movable holes 8012 lie perpendicular to the planes of the axes of the first air chamber 806, the second air chamber 809, and the vacuum air chamber 8013. Two valve stem movable holes 8012 are connected to the two first air chambers 806, while the other two valve stem movable holes 8012 are connected to the two second air chambers 809 and the vacuum air chamber 8013.

[0096] A valve opening control valve column 9 is provided inside the valve stem movable hole 8012 connected to the first air cavity 806 , and a first through hole 904 cooperating with the first air cavity 806 is provided on the first cylinder 901 of the valve opening control valve column 9 .

[0097] A valve control valve column 10 is arranged inside the valve stem movable hole 8012 which is connected to the second air cavity 809. The second cylinder 1001 of the valve closing control valve column 10 is provided with a second through hole 1004 which is connected to the second air cavity 809 and a third through hole 1006 which is connected to the vacuum air cavity 8013.

[0098] A control assembly for controlling the sliding of the valve opening control valve column 9 and the valve closing control valve column 10 is provided on the outside of the cover plate 802 .

[0099] In this embodiment, the control assembly includes a lever 11 and a servo motor 12. The output shaft of the servo motor 12 is fixedly connected to the center of the lever 11, and the servo motor 12 controls the swing of the lever 11. A waist-shaped hole 1101 is provided on both sides of the output shaft of the servo motor 12 on the lever 11.

[0100] The valve opening control valve column 9 includes a first cylinder 901 and a first control rod 902 that are coaxially fixedly connected. The end of the first control rod 902 is passed through the outside of the cover plate 802. The end of the first control rod 902 is provided with two first clamping ball heads 903 arranged at intervals. The end of the first control rod 902 is passed through the waist-shaped hole 1101, and the two first clamping ball heads 903 clamp the lever 11 in the middle.

[0101] The valve closing control valve column 10 includes a second cylinder 1001 and a second control rod 1002 that are coaxially fixedly connected. The end of the second control rod 1002 is passed through the outside of the cover plate 802. The end of the second control rod 1002 is provided with two second clamping ball heads 1003 arranged at intervals. The end of the second control rod 1002 is passed through the waist-shaped hole 1101, and the two second clamping ball heads 1003 clamp the lever 11 in the middle.

[0102] The ends of the first control rod 902 and the second control rod 1002 are respectively located in the waist-shaped holes 1101 on both sides of the lever 11. In this way, when the servo motor 12 drives the lever 11 to swing, it drives the first cylinder 901 and the second cylinder 1001 to move in opposite directions, thereby ensuring that the valve closing control air pipe 14 and the valve opening control air pipe 15 are in two different states of intake and exhaust.

[0103] To achieve pressure relief during the operation of the first and second air-controlled valves 2 and 4, a first pressure relief chamber 807 and a second pressure relief chamber 8010 are provided within the valve body 801. The first pressure relief chamber 807 is connected to the two first branch air chambers 806 at both ends, while the second pressure relief chamber 8010 is connected to the two second branch air chambers 809 at both ends. The first pressure relief chamber 807 is connected to the exterior of the valve body 801 via a first pressure relief hole 808, while the second pressure relief chamber 8010 is connected to the exterior of the valve body 801 via a second pressure relief hole 8011.

[0104] Correspondingly, a first L-shaped hole 905 is provided on the first cylindrical body 901 , and a second L-shaped hole 1005 is provided on the second cylindrical body 1001 .

[0105] When the first air-controlled valve 2 or the second air-controlled valve 4 is in the open state, the first cylinder 901 is pressed down by the lever 11, and the second cylinder 1001 is lifted by the lever 11. At this time, the first through hole 904 is connected to the first branch air cavity 806, and the extended control air cavity 804 is connected to the valve opening control air pipe 15 through the first branch air cavity 806. The high-pressure air in the valve opening control air pipe 15 controls the opening of the first air-controlled valve 2 or the second air-controlled valve 4.

[0106] At this time, the two ends of the second L-shaped hole 1005 on the second cylinder 1001 are respectively connected to the valve closing control air pipe 14 and the second pressure relief chamber 8010, and the exhaust generated by the first air-controlled valve 2 or the second air-controlled valve 4 is discharged through the valve closing control air pipe 14, the second L-shaped hole 1005, the second pressure relief chamber 8010 and the second pressure relief hole 8011.

[0107] When the first or second air-controlled valve 2 or 4 is closed, the second cylindrical body 1001 is pressed downward by the lever 11, while the first cylindrical body 901 is lifted by the lever 11. At this point, the second through-hole 1004 is connected to the second branch air cavity 809, and the third through-hole 1006 is connected to the vacuum air cavity 8013. High-pressure air enters the first or second air-controlled valve 2 or 4 through the valve-closing control air pipe 14, controlling its closure.

[0108] At this time, the two ends of the first L-shaped hole 905 on the first cylinder 901 are respectively connected to the valve opening control air pipe 15 and the first pressure relief chamber 807, and the exhaust gas generated by the first air-controlled valve 2 or the second air-controlled valve 4 is discharged through the valve opening control air pipe 15, the first L-shaped hole 905, the first pressure relief chamber 807 and the first pressure relief hole 808.

[0109] The two valve closing control valve rods 10 respectively control the closing of the first air control valve 2 and the second air control valve 4. If only one is closed, then only one third through hole 1006 on the second cylinder 1001 is connected to the vacuum air cavity 8013, and the other second cylinder 1001 also blocks the vacuum air cavity 8013, making it impossible to evacuate the intermediate tank 3.

[0110] Only when the first and second air-controlled valves 2 and 4 are simultaneously closed, and the third through-holes 1006 on the two second cylindrical bodies 1001 are both connected to the vacuum chamber 8013, will the entire vacuum chamber 8013 be unobstructed, allowing the intermediate tank 3 to be evacuated. Therefore, the configuration of the sub-control device 8 enables coordinated control of the vacuuming of the first and second air-controlled valves 2 and 4, and the intermediate tank 3.

[0111] A feed pipe 1 is connected to the end of the first air-controlled valve 2 that is away from the intermediate tank 3 , and the feed pipe 1 is connected to the slurry supply system pipeline.

[0112] To achieve thermal insulation and allow for free space during freeze-drying chamber 19 vibration, terminal tube 5 is connected to freeze-drying chamber 19's feed port 1901 via rubber connecting tube 6. A through-hole is provided in insulated chamber 18, through which rubber connecting tube 6 passes. A snap ring area 601 is provided where the rubber connecting tube 6 contacts the through-hole. The upper and lower snap rings of snap ring area 601 are respectively secured to the top surface of insulated chamber 18, optimizing the sealing effect.

[0113] The post-processing assembly includes a crushing box 33, which houses several layers of spaced-apart vibrating screens. The crushing box 33 is connected to the discharge assembly, which has the same structure as the feed assembly, including a first air-controlled valve 2, an intermediate tank 3, a second air-controlled valve 4, a terminal pipe 5, and a sub-control device 8. The discharge port 3305 at the bottom of the crushing box 33 is connected to the first air-controlled valve 2.

[0114] The setting of the sub-control device 8 and the intermediate tank 3 in the feeding assembly and the discharging assembly can serve the purpose of pre-vacuuming, thereby avoiding excessive pressure rise in the freeze-drying chamber 19 when the feeding assembly and the discharging assembly are connected to the freeze-drying assembly, requiring the vacuuming equipment to be started again, thereby achieving the purpose of reducing energy consumption.

[0115] The freeze-drying chamber 19, the insulated container 18, and the crushing container 33 are connected by a passageway equipped with an electrically or pneumatically controlled door panel. Specifically, a discharge passage 1801 is provided at the end where the insulated container 18 connects to the crushing container 33. A corresponding feed passage 3301 is provided at the corresponding position of the crushing container 33, and the feed passage 3301 is connected to the discharge passage 1801.

[0116] An upper connecting plate 1803 is fixed to the outside of the heat preservation box 18, and a lower connecting plate 3302 is fixed to the outside of the crushing box 33. The upper connecting plate 1803 and the lower connecting plate 3302 are overlapped and fixedly connected by bolts.

[0117] The discharge channel 1801 is provided with a second door panel 31 , and the second telescopic device 32 drives the second door panel 31 to move, thereby achieving communication and isolation between the discharge channel 1801 and the feed channel 3301 .

[0118] The freeze-drying bin 19 is open in the lower half of the end face facing the discharge channel 1801, and a slot 1904 is provided in the inner wall of the upper half of the end face. A first door panel 20 is slidingly provided inside the slot 1904. A first telescopic device 21 fixedly connected to the freeze-drying bin 19 controls the up and down movement of the first door panel 20. The first door panel 20 moves down to the lowest point, covering the open area of ​​the lower half of the end face of the freeze-drying bin 19 facing the discharge channel 1801.

[0119] The open area of ​​the lower half of the end surface of the freeze-drying bin 19 facing the discharge channel 1801 is connected to the discharge channel 1801 through the connecting frame 27. The bottom surface of the connecting frame 27 is an inclined surface, which is convenient for discharging.

[0120] The freeze-drying chamber 19 is equipped with a push plate 22. The bottom and left and right sides of the push plate 22 abut against the inner wall of the freeze-drying chamber 19. The top of the push plate 22 is threadedly connected to a screw 23 through a threaded hole. The end of the screw 23 is connected to a first motor 24. The first motor 24 drives the push plate 22 away from or toward the first door panel 20 via the screw 23. After vacuum freeze-drying is completed, the first and second door panels 20 and 31 are opened. The screw 23 is driven by the first motor 24 to rotate, driving the push plate 22 toward the crushing box 33, pushing the catalyst powder inside the freeze-drying chamber 19. To optimize the ejection effect, the bottom of the push plate 22 is formed into a beveled area 2201.

[0121] Depend on Figures 24 to 28 As shown, the crushing box 33 is equipped with two layers of vibrating screens, with the upper layer of the vibrating screen being lower than the height of the feed channel 3301. The vibrating screens include a filter plate 34, a cam 36, and a second motor 37, which is fixedly connected to the crushing box 33. One end of the filter plate 34 is hinged to the crushing box 33, and a cam 36 is located below the other end. The cam 36 is connected to the output shaft of the second motor 37.

[0122] A spring 35 is provided above the filter plate 34, located on the side of the cam 36. A spring top plate 3304 is provided above the spring 35, and the spring top plate 3304 is fixedly connected to the inner wall of the crushing box 33. An annular limiting frame 3303 is fixed to the inner wall of the crushing box 33, and the filter plate 34 rests on the annular limiting frame 3303.

[0123] Since the catalyst powder after vacuum freeze drying tends to aggregate and form lumps, the bonding force between the individual particles is weak and can be broken up by a vibrating screen. In this embodiment, the aperture of the upper filter plate 34 is larger than that of the lower filter plate 34 to avoid clogging.

[0124] Three groups of gratings are provided inside the crushing box 33 , and the three groups of gratings are respectively arranged above the upper filter plate 34 , between the two filter plates 34 , and below the lower filter plate 34 .

[0125] The three sets of gratings are used to obtain the amount of catalyst powder squeezed above each filter plate 34, and then the speed of the two second motors 37 is adjusted to increase or decrease the vibration frequency of the filter plate 34. The specific adjustment method is as follows:

[0126] The height of the catalyst powder above the upper filter plate 34 is set to a, the height of the catalyst powder above the lower filter plate 34 is set to b, and the height of the catalyst powder at the bottom of the crushing box 33 is set to c.

[0127] When c reaches the threshold, the two second motors 37 are turned off, and the discharge assembly is turned on to perform discharge.

[0128] When c is less than the threshold:

[0129] If a>b, the speed of the second motor 37 of the upper vibrating screen is increased so that the speed of the second motor 37 of the upper vibrating screen is greater than the speed of the second motor 37 of the lower vibrating screen;

[0130] If a<b, then reduce the speed of the second motor 37 of the upper vibrating screen so that the speed of the second motor 37 of the upper vibrating screen is less than the speed of the second motor 37 of the lower vibrating screen;

[0131] If a=b, the second motors 37 of the upper and lower vibrating screens have the same rotational speed.

[0132] Depend on Figure 29 As shown, the cooling system includes an internal circulation system and an external circulation system. The external circulation system exchanges heat with the internal circulation system through an exchanger. The external circulation system is connected to the temperature regulating coil 25 to cool the freeze-drying chamber 19.

[0133] The internal circulation system includes a liquid nitrogen storage tank 39, a first delivery pump 40 and a first heat exchanger 41 connected in series; the external circulation system includes a nitrogen storage tank 48, a second delivery pump 49 and a first heat exchanger 41 connected in series with the temperature control coil 25.

[0134] The flowing medium in the inner circulation system is liquid nitrogen, and the flowing medium in the outer circulation system is nitrogen gas. The liquid nitrogen passes through the first heat exchanger 41 to reduce the temperature of the nitrogen gas.

[0135] After the liquid nitrogen and nitrogen gas undergo heat exchange, the nitrogen gas temperature decreases and the liquid nitrogen temperature increases. Once the liquid nitrogen temperature reaches a threshold, it vaporizes and forms nitrogen gas. Therefore, in the internal circulation system, the liquid nitrogen outlet pipeline of the first heat exchanger 41—that is, the pipeline between the first heat exchanger 41 and the liquid nitrogen storage tank 39—is equipped with an electrically connected thermostat 42 and a three-way valve 43. One outlet of the three-way valve 43 is connected to the liquid nitrogen storage tank 39, and the other outlet is connected to the reflux storage tank 44.

[0136] When the temperature controller 42 with temperature detection function detects that the medium temperature is higher than the threshold value, it determines that the medium contains nitrogen, controls the three-way valve 43 to change the through-path, and the medium flows into the reflux storage tank 44 for storage.

[0137] A compressor 45 , a second heat exchanger 46 , and an expander 47 are sequentially connected between the reflux storage tank 44 and the liquid nitrogen storage tank 39 . Through these devices, the nitrogen inside the reflux storage tank 44 is liquefied again to form liquid nitrogen.

[0138] The medium is compressed by the compressor 45 and its temperature rises to above 50°C. At this time, the temperature of the nitrogen inside the external circulation system is below 0°C. Therefore, the external circulation system is connected to the second heat exchanger 46. After the nitrogen inside the external circulation system passes through the temperature control coil 25, it flows into the second heat exchanger 46, cooling the medium in the internal circulation system after being compressed by the compressor 45.

[0139] A catalyst mass production molding method, based on the above-mentioned catalyst mass production molding device, comprises the following steps:

[0140] S01, the vacuuming equipment vacuums the freeze-drying chamber 19 through the vacuum pipe 2601, so that the air pressure inside the freeze-drying chamber 19 is maintained between 1 and 30 Pa, and the freeze-drying chamber 19 is cooled by the cooling system to reduce the internal temperature of the freeze-drying chamber 19 to between -40°C and -50°C;

[0141] S02, the slurry enters the freeze-drying chamber 19 through the feeding assembly. During the feeding process, the first air control valve 2 is opened, the second air control valve 4 is closed, and the slurry is injected into the intermediate tank 3;

[0142] Then close the first air control valve 2, and the vacuum equipment evacuates the intermediate tank 3 through the connecting pipe 17 to maintain the internal pressure between 1 and 30 Pa. The internal pressure of the intermediate tank 3 is lower than the internal pressure of the freeze-drying chamber 19. Then open the second air control valve 4, and the slurry flows into the freeze-drying chamber 19.

[0143] S03, after the slurry is frozen in the freeze-drying chamber 19 for 2 to 4 hours, the temperature inside the freeze-drying chamber 19 is raised to between -25°C and -20°C, and the air pressure inside the freeze-drying chamber 19 is reduced to 10Pa to 15Pa for primary drying;

[0144] The temperature control method of the temperature regulating coil 25 adopts any one of the following two schemes or a combination of the two schemes:

[0145] 1. By increasing the power of the second delivery pump 49 and increasing the flow rate of nitrogen in the external circulation system, the heat exchange efficiency between the nitrogen and the liquid nitrogen in the first heat exchanger 41 is reduced, thereby increasing the temperature of the nitrogen and thereby increasing the temperature of the thermostatic coil 25;

[0146] 2. Turn off the first delivery pump 40;

[0147] S04. After the primary drying is maintained for 4 to 6 hours, the secondary drying process is entered. The temperature of the secondary drying is increased to 25°C to 55°C. When the temperature inside the freeze-drying chamber 19 reaches 0°C, the first delivery pump 40 and the second delivery pump 49 are turned off, and the heating device 30 is turned on. The heating device 30 uses electric heating to heat the freeze-drying chamber 19.

[0148] During the secondary drying process, the air pressure inside the freeze-drying chamber is adjusted to less than 5Pa, and the secondary drying time is maintained for 2 to 3 hours;

[0149] S05. After completing the secondary drying, the freeze-drying chamber 19 pushes the bulk catalyst into the crushing box 33, and the bulk catalyst is broken into particles by the vibrating screen. The particles enter the discharge assembly through the vibrating screen and are finally discharged through the discharge assembly.

[0150] The above describes the implementation methods of the present application in detail in conjunction with the accompanying drawings, but the present application is not limited to the above implementation methods. Various changes can be made within the scope of knowledge possessed by ordinary technicians in the relevant technical field without departing from the purpose of the present application.

Claims

1. A catalyst mass production molding device, characterized by: Including freeze drying assembly, post-processing assembly and cooling system; The freeze-drying assembly includes a feed assembly, an insulation box (18), a freeze-drying chamber (19), and a temperature regulating coil (25). The temperature regulating coil (25) is in contact with the freeze-drying chamber (19). The freeze-drying chamber (19) is arranged inside the insulation box (18). The feed assembly located outside the insulation box (18) is connected to the feed port (1901) of the freeze-drying chamber (19). The freeze-drying chamber (19) is connected to an external vacuum pumping device via an exhaust pipe (2601). A heating device (30) is provided on the freeze-drying chamber (19). The post-processing assembly includes a crushing box (33), wherein a plurality of layers of vibrating screens are arranged at intervals inside the crushing box (33), and the crushing box (33) is connected to the discharge assembly; The freeze-drying chamber (19), the heat preservation box (18) and the crushing box (33) are connected by a passage, and the passage is provided with an electrically or pneumatically controlled door panel; The cooling system is connected to the inlet and outlet of the temperature regulating coil (25).

2. A catalyst mass production molding device according to claim 1, characterized in that: The feed assembly and the discharge assembly have the same structure, both comprising a first air control valve (2), an intermediate tank (3), a second air control valve (4), a terminal pipe (5) and a sub-control device (8); The inlet and outlet ports at the upper and lower ends of the intermediate tank (3) are respectively connected to the first air control valve (2) and the second air control valve (4). The second air control valve (4) is arranged between the intermediate tank (3) and the terminal pipe (5). The sub-control device (8) is connected to the first air control valve (2) and the second air control valve (4) through two valve closing control air pipes (14) and two valve opening control air pipes (15). The sub-control device (8) is externally connected to an external high-pressure air pipe (13).

3. A catalyst mass production molding device according to claim 2, characterized in that: The sub-control device (8) comprises a detachably connected valve body (801) and a cover plate (802); The valve body (801) is provided with an air inlet cavity (803) connected to an external high-pressure air pipe (13). The air inlet cavity (803) is connected to the extended control air cavity (804) and the contraction control air cavity (805) arranged at intervals. The extended control air cavity (804) is connected to two first branch air cavities (806). The first branch air cavity (806) is connected to the valve opening control air pipe (15). The contraction control air cavity (805) is connected to two second branch air cavities (809). The second branch air cavity (809) is connected to the valve closing control air pipe (14). The valve body (801) is provided with four valve stem movable holes (8012), and the planes where the axes of the valve stem movable holes (8012) lie are perpendicular to the planes where the axes of the first air cavity (806) and the second air cavity (809) lie. Two valve stem movable holes (8012) are connected to the two first air cavities (806), and the other two valve stem movable holes (8012) are connected to the two second air cavities (809); A valve opening control valve column (9) is provided inside the valve stem movable hole (8012) connected to the first air cavity (806), and a first through hole (904) is provided on the first cylindrical body (901) of the valve opening control valve column (9) for connecting with the first air cavity (806); A valve control valve column (10) is provided inside the valve stem movable hole (8012) connected to the second air cavity (809), and a second through hole (1004) is provided on the second cylindrical body (1001) of the valve closing control valve column (10) for connecting with the second air cavity (809); A control assembly for controlling the sliding of a valve opening control valve column (9) and a valve closing control valve column (10) is provided on the outside of the cover plate (802).

4. A catalyst mass production molding device according to claim 3, characterized in that: The valve body (801) is provided with a continuous vacuum air cavity (8013) inside, and the two ends of the vacuum air cavity (8013) are respectively connected to the vacuum tube (16) and the connecting tube (17), and the end of the connecting tube (17) is passed through to the inside of the intermediate tank (3); The two valve stem movable holes (8012) that are in continuous communication with the second air cavity (809) are in continuous communication with the vacuum air cavity (8013); A third through hole (1006) is provided on the second cylindrical body (1001) of the valve closing control valve column (10) and is connected to the vacuum air cavity (8013).

5. A catalyst mass production molding device according to any one of claims 1 to 4, characterized in that: The end surface of the heat preservation box (18) connected to the crushing box (33) is provided with a discharge channel (1801), and the corresponding position of the crushing box (33) is provided with a feed channel (3301), and the feed channel (3301) is connected to the discharge channel (1801); The discharge channel (1801) is provided with a second door panel (31), and the second telescopic device (32) drives the second door panel (31) to move, thereby achieving communication and isolation between the discharge channel (1801) and the feed channel (3301); The freeze-drying bin (19) is arranged with an open lower half of the end surface facing the discharge channel (1801), a slot (1904) is provided in the inner wall of the upper half of the end surface, a first door panel (20) is slidably provided inside the slot (1904), a first telescopic device (21) fixedly connected to the freeze-drying bin (19) controls the first door panel (20) to move up and down, and the first door panel (20) moves down to the lowest point, covering the open area of ​​the lower half of the end surface of the freeze-drying bin (19) facing the discharge channel (1801); The open area of ​​the lower half of the end surface of the freeze-drying chamber (19) facing the discharge channel (1801) is connected to the discharge channel (1801) through the connecting frame (27).

6. A catalyst mass production molding device according to claim 5, characterized in that: The freeze-drying chamber (19) is supported inside the heat preservation box (18) by an externally provided heat-insulating support frame (28).

7. A catalyst mass production molding device according to claim 5, characterized in that: A push plate (22) is provided inside the freeze-drying bin (19), and the bottom surface and left and right side surfaces of the push plate (22) are in contact with the inner wall of the freeze-drying bin (19). The top of the push plate (22) is threadedly connected to a screw rod (23) through a threaded hole, and the end of the screw rod (23) is connected to a first motor (24). The first motor (24) drives the push plate (22) away from or close to the first door panel (20) through the screw rod (23).

8. A catalyst mass production molding device according to claim 1 or 2 or 3 or 4 or 6 or 7, characterized in that: The cooling system includes an internal circulation system and an external circulation system. The external circulation system exchanges heat with the internal circulation system through an exchanger. The external circulation system is connected to the temperature regulating coil (25) to cool the freeze-drying chamber (19).

9. A catalyst mass production molding device according to claim 8, characterized in that: The internal circulation system includes a liquid nitrogen storage tank (39), a first delivery pump (40), and a first heat exchanger (41) connected in series; The external circulation system includes a nitrogen storage tank (48) connected in series with the temperature regulating coil (25), a second delivery pump (49) and a first heat exchanger (41); The flow medium in the inner circulation system is liquid nitrogen, and the flow medium in the outer circulation system is nitrogen gas. The liquid nitrogen passes through the first heat exchanger (41) to reduce the temperature of the nitrogen gas.

10. A method for preparing and molding a catalyst in large quantities, based on the device for preparing and molding a catalyst in large quantities according to claim 9, characterized in that: The following steps are involved: S01, the vacuuming device vacuums the freeze-drying chamber (19) through the vacuum pipe (2601), so that the air pressure inside the freeze-drying chamber (19) is maintained between 1 and 30 Pa, and the freeze-drying chamber (19) is cooled by the cooling system, so that the internal temperature of the freeze-drying chamber (19) is reduced to between -40°C and -50°C; S02, the slurry enters the freeze-drying chamber (19) through the feeding assembly. During the feeding process, the first air control valve (2) is opened, the second air control valve (4) is closed, and the slurry is injected into the intermediate tank (3); Then, the first air control valve (2) is closed, and the vacuum device is used to vacuum the intermediate tank (3) through the connecting pipe (17), so that the internal air pressure of the intermediate tank (3) is maintained between 1 and 30 Pa, and the internal air pressure of the intermediate tank (3) is lower than the internal air pressure of the freeze-drying chamber (19). Then, the second air control valve (4) is opened, and the slurry flows into the freeze-drying chamber (19); S03, after the slurry is frozen in the freeze-drying chamber (19) for 2 to 4 hours, the temperature inside the freeze-drying chamber (19) is raised to between -25°C and -20°C, and the air pressure inside the freeze-drying chamber (19) is reduced to 10Pa to 15Pa for primary drying; The temperature control method of the temperature regulating coil (25) adopts any one of the following two schemes or a combination of the two schemes:

1. By increasing the power of the second delivery pump (49), the flow rate of nitrogen in the external circulation system is increased, thereby reducing the heat exchange efficiency between the nitrogen and the liquid nitrogen in the first heat exchanger (41), thereby increasing the temperature of the nitrogen and thereby increasing the temperature of the temperature regulating coil (25); 2. Turn off the first delivery pump (40); S04, after the primary drying is maintained for 4 to 6 hours, the secondary drying process is entered, and the temperature of the secondary drying is increased to 25°C to 55°C. When the internal temperature of the freeze-drying chamber (19) reaches 0°C, the first delivery pump (40) and the second delivery pump (49) are turned off, and the heating device (30) is turned on. The heating device (30) uses electric heating to heat the freeze-drying chamber (19); During the secondary drying process, the air pressure inside the freeze-drying chamber is adjusted to less than 5 Pa, and the secondary drying time is maintained for 2 to 3 hours; S05. After the secondary drying is completed, the freeze-drying chamber (19) pushes the bulk catalyst into the crushing box (33), and the bulk catalyst is broken into particles by the vibrating screen. The particles enter the discharge assembly through the vibrating screen and are finally discharged through the discharge assembly.

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