Molding device and molding method for macroscopic preparation of catalyst

Abstract

The invention relates to a catalyst macroscopic preparation forming device and method, and belongs to the technical field of catalyst preparation forming. Comprising a freeze-drying assembly, a post-processing assembly and a cold supply system. The freeze-drying assembly comprises a feeding assembly, a heat preservation box, a freeze-drying bin and a temperature adjusting coil pipe, the temperature adjusting coil pipe abuts against the freeze-drying bin, the freeze-drying bin is arranged in the heat preservation box, the feeding assembly located outside the heat preservation box is connected with a feeding port of the freeze-drying bin, the freeze-drying bin is connected with external vacuumizing equipment through an exhaust pipe, and a heating device is arranged on the freeze-drying bin. The post-processing assembly comprises a smashing box and a discharging assembly, and the cold supply system is connected with an inlet and an outlet of the temperature adjusting coil pipe. The bio-enzyme catalyst is subjected to forming treatment through a vacuum freeze drying technology, the slurry is changed into powder particles, the whole process is low in temperature, the enzyme activity yield is larger than 95%, the water residue is smaller than 3%, the stability of the catalyst is higher, and the method is particularly suitable for the catalyst prepared from a heat-sensitive enzyme.

Description

Technical Field

[0001] This application belongs to the technical field of catalyst preparation and forming, and specifically relates to a device and method for macro-preparing and forming a catalyst. Background Art

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

[0003] Existing bio-enzyme catalysts often concentrate the fermentation broth into a slurry and then make it into powder through spray hot air drying for forming. Although this process has the advantage of continuous production, there are significant problems of 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, leading to the collapse of the tertiary structure and the change of the active center conformation. For example, the yield of alkaline pectinase produced by Bacillus subtilis is <10% at an inlet air temperature of 160°C. Summary of the Invention

[0004] The technical problem to be solved by this application is: to overcome the deficiencies of the prior art and provide a device and method for macro-preparing and forming a catalyst. This application uses vacuum freeze-drying technology to form a bio-enzyme catalyst, turning it from a slurry into powder particles. The whole process is at low temperature, with an enzyme activity recovery rate greater than 95% and a moisture residue less than 3%, making the catalyst more stable, especially 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: A device for macro-preparing and forming a catalyst includes a freeze-drying assembly, a post-treatment assembly, and a cooling system.

[0006] The freeze-drying assembly includes a feeding assembly, a heat preservation box, a freeze-drying chamber, and a temperature control coil. The temperature control coil abuts against the freeze-drying chamber. The freeze-drying chamber is arranged inside the heat preservation box. The feeding assembly located outside the heat preservation box is connected to the feeding port of the freeze-drying chamber. The freeze-drying chamber is connected to an external vacuum pumping device through an air extraction pipe. A heating device is provided on the freeze-drying chamber.

[0007] The post-treatment assembly includes a crushing box. Inside the crushing box, there are several layers of vibrating screens arranged at intervals. The crushing box is connected in a through manner with a discharging assembly.

[0008] The freeze-drying chamber, the heat preservation box, and the crushing box are connected through a channel, and a door panel controlled electrically or pneumatically is provided on the channel.

[0009] The cooling system is connected to the inlet and outlet of the temperature control coil.

[0010] Preferably, the feeding assembly and the discharging assembly have the same structure, and both include a first pneumatic control valve, an intermediate tank, a second pneumatic control valve, an end pipe, and a sub-control device.

[0011] The inlets and outlets at the upper and lower ends of the intermediate tank are respectively connected to the first pneumatic control valve and the second pneumatic control valve. The second pneumatic control valve is arranged between the intermediate tank and the end pipe. The sub-control device is connected to the first pneumatic control valve and the second pneumatic control valve through two valve closing control air pipes and two valve opening control air pipes, and an external high-pressure air pipe is connected to the outside of the sub-control device.

[0012] Preferably, the sub-control device includes a valve body and a cover plate that are detachably connected.

[0013] An air inlet cavity connected to the external high-pressure air pipe is provided inside the valve body. The air inlet cavity is connected in a through manner to an extended control air cavity and a contraction control air cavity that are arranged at intervals. The extended control air cavity is connected in a through manner to two first branch air cavities, and the first branch air cavities are connected in a through manner to the valve opening control air pipes. The contraction control air cavity is connected in a through manner to two second branch air cavities, and the second branch air cavities are connected in a through manner to the valve closing control air pipes.

[0014] Four valve rod moving holes are provided on the valve body. The plane where the axes of the valve rod moving holes are located is perpendicular to the plane where the axes of the first branch air cavities and the second branch air cavities are located.

[0015] Two valve rod moving holes are connected in a through manner to the two first branch air cavities, and the other two valve rod moving holes are connected in a through manner to the two second branch air cavities.

[0016] A valve opening control valve column is provided inside the valve rod moving hole connected in a through manner to the first branch air cavity. A first through hole that is cooperatively connected to the first branch air cavity is provided on the first cylinder of the valve opening control valve column.

[0017] A valve closing control valve column is provided inside the valve rod moving hole connected in a through manner to the second branch air cavity. A second through hole that is cooperatively connected to the second branch air cavity is provided on the second cylinder of the valve closing control valve column.

[0018] A control assembly for controlling the sliding of the valve opening control valve column and the valve closing control valve column is provided outside the cover plate.

[0019] Preferably, a through vacuum air cavity is provided inside the valve body. The two ends of the vacuum air cavity are respectively connected in a through manner to a vacuum pipe and a connecting pipe, and the end of the connecting pipe penetrates into the intermediate tank.

[0020] The two valve rod moving holes connected in a through manner to the second branch air cavities are connected in a through manner to the vacuum air cavity.

[0021] A third through hole that is cooperatively connected to the vacuum air cavity is provided on the second cylinder of the valve closing control valve column.

[0022] Preferably, an outlet channel is provided on the end face where the heat preservation box is connected to the crushing box, and a feed channel is provided at the corresponding position of the crushing box. The feed channel is connected to the outlet channel in a through manner.

[0023] A second door panel is provided on the outlet channel, and the second telescopic device drives the second door panel to move, so as to realize the connection and isolation between the outlet channel and the feed channel.

[0024] The lower half of the end face of the freeze-drying chamber facing the outlet channel is arranged in an open manner, and a slot is provided in the inner wall of the upper half of the end face. A first door panel is slidably arranged inside the slot, and a first telescopic device fixedly connected to the freeze-drying chamber controls the up and down movement of the first door panel. When the first door panel moves down to the lowest point, the open area in the lower half of the end face of the freeze-drying chamber facing the outlet channel is covered.

[0025] The open area in the lower half of the end face of the freeze-drying chamber facing the outlet channel is connected to the outlet channel in a through manner through a connecting frame.

[0026] Preferably, the freeze-drying chamber is supported inside the heat preservation box by an externally provided heat insulation support frame.

[0027] Preferably, a push plate is provided inside the freeze-drying chamber. The bottom surface and the 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 with a screw rod through a threaded hole. The end of the screw rod is connected with a first motor, and the first motor drives the push plate to move away from or close to the first door panel through the screw rod.

[0028] 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 control coil to cool the freeze-drying chamber.

[0029] Preferably, the internal circulation system includes a liquid nitrogen storage tank, a first delivery pump, and a first heat exchanger connected in series.

[0030] The external circulation system includes a nitrogen storage tank, a second delivery pump, and a first heat exchanger connected in series with the temperature control coil.

[0031] The flowing medium in the internal circulation system is liquid nitrogen, and the flowing medium in the external circulation system is nitrogen. The liquid nitrogen reduces the temperature of the nitrogen through the first heat exchanger.

[0032] A method for macroscopically preparing and forming a catalyst, based on the above-mentioned device for macroscopically preparing and forming a catalyst, includes the following steps: S01. The vacuum pumping device pumps the freeze-drying chamber through a suction pipe to keep the air pressure inside the freeze-drying chamber between 1 and 30 Pa, and cools the freeze-drying chamber through the cooling system to reduce the internal temperature of the freeze-drying chamber to between -40°C and -50°C; 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; Then close the first gas 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 gas control valve, and the slurry flows into the freeze-drying chamber. 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; The control method for the temperature rise of the thermostatic coil adopts any one of the following two solutions or a combination of the two: 1. By increasing the power of the second delivery pump and increasing the flow rate of nitrogen in the external circulation system, the heat exchange efficiency between nitrogen and liquid nitrogen in the first heat exchanger is reduced, thereby increasing the temperature of nitrogen and thus raising the temperature of the thermostatic coil; 2. Turn off the first delivery pump; 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; 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; S05. After completing the secondary drying, the freeze-drying chamber pushes the block catalyst into the crushing box, and the block 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.

[0033] Compared with the prior art, the present invention has the following beneficial effects: (1) The vacuum freeze-drying technology is used to form the slurry of the biological enzyme catalyst into powder particles. The low-temperature anoxic environment and the biochemical dehydration mechanism cooperate with each other, so that the enzyme activity retention rate is increased by 20~90% compared with 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 especially suitable for heat-sensitive enzyme catalysts and high-added enzyme catalysts.

[0034] (2) The temperature range below 0°C in the freeze-drying chamber is adjusted by a cooling system, and the temperature range above 0°C is adjusted by an electric heating device. This not only saves energy and reduces consumption, but also facilitates the realization of step-by-step temperature increase during the secondary drying process, making temperature control more precise. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] The present application will be further described below in conjunction with the accompanying drawings and embodiments.

[0036] Figure 1 It is a structural diagram of a device for macro-preparing and forming a catalyst of the present application. Figure 2 It is a structural diagram of the freeze-drying assembly in the device for macro-preparing and forming a catalyst of the present application. Figure 3 It is a first partial cross-sectional view of the insulation box in the freeze-drying assembly of the present application. Figure 4 It is a second partial cross-sectional view of the insulation box in the freeze-drying assembly of the present application. Figure 5 It is a structural diagram of the freeze-drying assembly after removing the insulation box of the present application. Figure 6 It is a structural diagram of the feeding assembly in the freeze-drying assembly of the present application. Figure 7 It is a cross-sectional view of the rubber connecting pipe in the freeze-drying assembly of the present application. Figure 8 It is a structural diagram of the sub-control device in the freeze-drying assembly of the present application. Figure 9 It is an exploded view of the sub-control device in the freeze-drying assembly of the present application. Figure 10 It is a first cross-sectional view of the sub-control device in the freeze-drying assembly of the present application. Figure 11 It is a second cross-sectional view of the sub-control device in the freeze-drying assembly of the present application. Figure 12 It is a third cross-sectional view of the sub-control device in the freeze-drying assembly of the present application. Figure 13 It is a structural diagram of the valve-opening control valve column in the sub-control device of the present application. Figure 14 It is Figure 13 a cross-sectional view of Figure 15 It is a structural diagram of the valve-closing control valve column in the sub-control device of the present application. Figure 16 It is Figure 15 a cross-sectional view of Figure 17 It is a structural diagram of the freeze-drying assembly after removing the insulation box and the feeding assembly of the present application. Figure 18 It is Figure 17 a front view of Figure 19 It is a structural diagram of the freeze-drying chamber in the freeze-drying assembly of the present application. Figure 20 It is Figure 19 a cross-sectional view of Figure 21 It is a structural diagram of the temperature-regulating coiled pipe in the freeze-drying assembly of the present application. Figure 22 This is the structural diagram of the heat insulation support frame in the freeze-drying assembly of this application. Figure 23 This is the structural diagram of the door panel in the freeze-drying assembly of this application. Figure 24 This is the first structural diagram of the post-treatment assembly in a catalyst macroscale preparation and forming device of this application. Figure 25 This is the second structural diagram of the post-treatment assembly of this application. Figure 26 It is Figure 25 The cross-sectional view after removing the discharge assembly. Figure 27 It is Figure 26 The partial enlarged view at position A in Figure 28 It is Figure 26 The partial enlarged view at position B in Figure 29 This is the cooling system diagram in a catalyst macroscale preparation and forming device of this application.

[0037] In the figure: 1 - Feed pipe, 2 - First pneumatic control valve, 3 - Intermediate tank, 4 - Second pneumatic control valve, 5 - End pipe, 6 - Rubber connecting pipe, 601 - Snap ring area, 7 - Fixed bracket, 8 - Sub-control device, 801 - Valve body, 802 - Cover plate, 803 - Intake cavity, 804 - Extended control air cavity, 805 - Shrinkage control air cavity, 806 - First branch air cavity, 807 - First pressure relief cavity, 808 - First pressure relief hole, 809 - Second branch air cavity, 8010 - Second pressure relief cavity, 8011 - Second pressure relief hole, 8012 - Valve stem moving hole, 8013 - Vacuum air cavity, 9 - Valve opening control valve column, 901 - First cylinder, 902 - First control rod, 903 - First snap 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 snap 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 pipe, 17 - Connecting pipe, 18 - Insulation box, 1801 - Discharge channel, 1802 - U-shaped groove, 1803 - Upper connecting plate, 19 - Freeze-drying chamber, 1901 - Feed inlet, 1902 - Air extraction hole, 1903 - Rib, 1904 - Slot, 20 - First door panel, 21 - First telescopic device, 22 - Pusher plate, 2201 - Inclined plane area, 23 - Screw, 24 - First motor, 25 - Temperature control coil, 26 - Air extraction hood, 2601 - Air extraction pipe, 27 - Connecting frame, 28 - Heat insulation support frame, 29 - Vibrator, 30 - Heating device, 31 - Second door panel, 33 - Second telescopic device, 33 - Crushing box, 3301 - Feed channel, 3302 - Lower connecting plate, 3303 - Annular limiting 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 transfer pump, 41 - First heat exchanger, 42 - Temperature controller, 43 - Three-way valve, 44 - Return storage tank, 45 - Compressor, 46 - Second heat exchanger, 47 - Expander, 48 - Nitrogen storage tank, 49 - Second transfer pump. Detailed implementation manners

[0038] With reference to the attached drawings Figures 1 to 29 A further detailed description is given to a catalyst macro-preparation forming device and a forming method of the present application, but it is not a limitation to the present application.

[0039] A catalyst macro-preparation forming device comprises Figure 1 as shown, and includes a freeze-drying assembly, a post-treatment assembly and a cooling system.

[0040] The freeze-drying assembly described above includes a feeding assembly, a heat preservation box 18, a freeze-drying chamber 19, and a temperature-regulating coil 25. The temperature-regulating coil 25 abuts against the freeze-drying chamber 19. The temperature-regulating coil 25 includes two sets of serpentine tubes connected in series, and the two sets of serpentine tubes are respectively closely attached to the outer walls on the left and right sides of the freeze-drying chamber 19.

[0041] 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 external heat insulation support frame 28. As Figure 22 shown, the heat insulation support frame 28 includes a bottom plate, a bottom support beam, a side support beam, and a top support beam. Convex strips 1903 arranged vertically are protruded on the left and right side walls of the freeze-drying chamber 19, and a clamping groove is recessed on the side support beam of the heat insulation support frame 28, and the convex strips 1903 are clamped inside the clamping strip. A U-shaped groove 1802 arranged vertically is provided on the inner wall of the heat preservation box 18, and the side support beam of the heat insulation support frame 28 is clamped inside the U-shaped groove 1802.

[0042] The heat insulation support frame 28 is made of rubber material, which can not only play a heat insulation role, but also ensure that the freeze-drying chamber 19 can vibrate. For this reason, a plurality of vibrators 29 are provided on the bottom plate of the heat insulation support frame 28, and the vibrators of the vibrators 29 abut against the bottom surface of the freeze-drying chamber 19. After the slurry is injected into the freeze-drying chamber 19, the vibrators 29 can be turned on to vibrate the slurry.

[0043] By combining high-speed vibration with a vacuum environment, the slurry rapidly boils and absorbs heat near the freezing point, and is instantly frozen into a micron-level "ice sand" structure. During the freezing process, vibration inhibits the growth of ice crystals, avoiding particle agglomeration caused by ice crystal extrusion in traditional freezing, so that the dried material is a highly dispersed powder, rather than the porous block of traditional freeze-drying. At the same time, vibration can also increase heat exchange, increasing the sublimation rate by 3 to 5 times, thereby reducing energy consumption.

[0044] The feeding assembly located outside the heat preservation box 18 is connected to the feeding port 1901 of the freeze-drying chamber 19. A row of air extraction holes 1902 is provided on the top surface of the freeze-drying chamber 19. An air extraction hood 26 that completely covers the air extraction holes 1902 is provided outside the freeze-drying chamber 19. The air extraction hood 26 is connected to an external vacuum pumping device through an air extraction pipe 2601. A heating device 30 is provided on the freeze-drying chamber 19. The heating device 30 uses electric heating, and the temperature inside the freeze-drying chamber 19 needs to be heated to about 50°C.

[0045] In the entire vacuum freeze-drying process of the biocatalyst, the temperature inside the freeze-drying chamber 19 is adjusted in the range of -50°C to 50°C. The refrigerant of the cooling system uses liquid nitrogen, which is more suitable for below 0°C. Therefore, a heating device 30 is added to adjust the temperature range of the freeze-drying chamber 19 above 0°C.

[0046] The described feeding assembly includes a first pneumatic control valve 2, an intermediate tank 3, a second pneumatic control valve 4, an end pipe 5, and a sub-control device 8. The sub-control device 8 is fixedly connected to the intermediate tank 3 through a fixing bracket 7.

[0047] The inlets and outlets at the upper and lower ends of the intermediate tank 3 are respectively connected to the first pneumatic control valve 2 and the second pneumatic control valve 4. The second pneumatic control valve 4 is arranged between the intermediate tank 3 and the end pipe 5. The sub-control device 8 is connected to the first pneumatic control valve 2 and the second pneumatic control valve 4 through two valve-closing control air pipes 14 and two valve-opening control air pipes 15. An external high-pressure air pipe 13 is connected to the outside of the sub-control device 8.

[0048] As shown by Figure 8 the external high-pressure air pipe 13, valve-closing control air pipe 14, valve-opening control air pipe 15, vacuum pipe 16, and connecting pipe 17 that are connected through the outside of the sub-control device 8. The end of the connecting pipe 17 penetrates into the interior of the intermediate tank 3.

[0049] The external high-pressure air pipe 13 is connected to an external high-pressure air supply device, and the vacuum pipe 16 is connected to an external vacuum pumping device.

[0050] The two valve-closing control air pipes 14 and the two valve-opening control air pipes 15 are respectively connected to the control air interfaces of the first pneumatic control valve 2 and the second pneumatic control valve 4.

[0051] As shown by Figures 8 to 16 the described sub-control device 8 includes a valve body 801 and a cover plate 802 that are detachably connected, and the two are fixedly connected by bolts.

[0052] An air inlet chamber 803 connected to the external high-pressure air pipe 13 is provided inside the valve body 801. The air inlet chamber 803 is connected in communication with an extended control air chamber 804 and a contracted control air chamber 805 that are arranged at intervals. Two first branch air chambers 806 are connected in communication with the extended control air chamber 804, and the first branch air chambers 806 are connected in communication with the valve-opening control air pipes 15. Two second branch air chambers 809 are connected in communication with the contracted control air chamber 805, and the second branch air chambers 809 are connected in communication with the valve-closing control air pipes 14.

[0053] The axes of the air inlet chamber 803, extended control air chamber 804, contracted control air chamber 805, first branch air chamber 806, and second branch air chamber 809 are all in the same plane.

[0054] A through vacuum air chamber 8013 is provided inside the valve body 801. The two ends of the vacuum air chamber 8013 are respectively connected in communication with the vacuum pipe 16 and the connecting pipe 17.

[0055] Four valve stem moving holes 8012 are provided on the valve body 801, and the plane where the axes of the valve stem moving holes 8012 are located is perpendicular to the plane where the axes of the first branch air cavity 806, the second branch air cavity 809, and the vacuum air cavity 8013 are located. Two valve stem moving holes 8012 are connected to the two first branch air cavities 806 in a penetrating manner, and the other two valve stem moving holes 8012 are connected to the two second branch air cavities 809 and the vacuum air cavity 8013 in a penetrating manner.

[0056] A valve opening control valve column 9 is arranged inside the valve stem moving hole 8012 that is connected to the first branch air cavity 806 in a penetrating manner. A first through hole 904 that is cooperatively connected to the first branch air cavity 806 is provided on the first cylinder 901 of the valve opening control valve column 9.

[0057] A valve closing control valve column 10 is arranged inside the valve stem moving hole 8012 that is connected to the second branch air cavity 809 in a penetrating manner. A second through hole 1004 that is cooperatively connected to the second branch air cavity 809 and a third through hole 1006 that is cooperatively connected to the vacuum air cavity 8013 are provided on the second cylinder 1001 of the valve closing control valve column 10.

[0058] A control assembly for controlling the sliding of the valve opening control valve column 9 and the valve closing control valve column 10 is arranged outside the cover plate 802.

[0059] 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 central position of the lever 11, and the servo motor 12 controls the swinging of the lever 11. A waist-shaped hole 1101 is provided on each side of the output shaft of the servo motor 12 on the lever 11.

[0060] The valve opening control valve column 9 includes a first cylinder 901 and a first control rod 902 that are coaxially and fixedly connected. The end of the first control rod 902 penetrates to the outside of the cover plate 802. Two first clamping ball heads 903 arranged at intervals are provided at the end of the first control rod 902. The end of the first control rod 902 penetrates into the waist-shaped hole 1101, and the two first clamping ball heads 903 clamp the lever 11 in the middle.

[0061] The valve closing control valve column 10 includes a second cylinder 1001 and a second control rod 1002 that are coaxially and fixedly connected. The end of the second control rod 1002 penetrates to the outside of the cover plate 802. Two second clamping ball heads 1003 arranged at intervals are provided at the end of the second control rod 1002. The end of the second control rod 1002 penetrates into the waist-shaped hole 1101, and the two second clamping ball heads 1003 clamp the lever 11 in the middle.

[0062] The ends of the first control lever 902 and the second control lever 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 air control pipe 14 for closing the valve and the air control pipe 15 for opening the valve are in two different states of air intake and exhaust.

[0063] In order to achieve pressure relief during the movement of the first pneumatic control valve 2 and the second pneumatic control valve 4, a first pressure relief chamber 807 and a second pressure relief chamber 8010 are provided inside the valve body 801. Both ends of the first pressure relief chamber 807 are connected to two first branch air chambers 806 in a through manner, and both ends of the second pressure relief chamber 8010 are connected to two second branch air chambers 809 in a through manner. The first pressure relief chamber 807 is connected to the outside of the valve body 801 through a first pressure relief hole 808, and the second pressure relief chamber 8010 is connected to the outside of the valve body 801 through a second pressure relief hole 8011.

[0064] Correspondingly, a first L-shaped hole 905 is provided on the first cylinder 901, and a second L-shaped hole 1005 is provided on the second cylinder 1001.

[0065] When the first pneumatic control valve 2 or the second pneumatic control 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 chamber 806 in a through manner, so that the extended control air chamber 804 is connected to the air control pipe 15 for opening the valve through the first branch air chamber 806, and the high-pressure air in the air control pipe 15 for opening the valve controls the opening of the first pneumatic control valve 2 or the second pneumatic control valve 4.

[0066] At this time, both ends of the second L-shaped hole 1005 on the second cylinder 1001 are respectively connected to the air control pipe 14 for closing the valve and the second pressure relief chamber 8010, and the exhaust gas generated by the first pneumatic control valve 2 or the second pneumatic control valve 4 is discharged through the air control pipe 14 for closing the valve, the second L-shaped hole 1005, the second pressure relief chamber 8010, and the second pressure relief hole 8011.

[0067] When the first pneumatic control valve 2 or the second pneumatic control valve 4 is in the closed state, the second cylinder 1001 is pressed down by the lever 11, and the first cylinder 901 is lifted by the lever 11. At this time, the second through hole 1004 is connected to the second branch air chamber 809 in a through manner, and the third through hole 1006 is connected to the vacuum air chamber 8013 in a through manner. The high-pressure air enters the first pneumatic control valve 2 or the second pneumatic control valve 4 through the air control pipe 14 for closing the valve to control its closing.

[0068] At this time, both ends of the first L-shaped hole 905 on the first cylinder 901 are respectively connected to the air control pipe 15 for opening the valve and the first pressure relief chamber 807, and the exhaust gas generated by the first pneumatic control valve 2 or the second pneumatic control valve 4 is discharged through the air control pipe 15 for opening the valve, the first L-shaped hole 905, the first pressure relief chamber 807, and the first pressure relief hole 808.

[0069] The two valve closing control valve columns 10 respectively control the closing of the first air-controlled valve 2 and the second air-controlled 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.

[0070] Only when the first air-controlled valve 2 and the second air-controlled valve 4 are closed at the same time, and the third through holes 1006 on the two second cylinders 1001 are connected to the vacuum air cavity 8013, the entire vacuum air cavity 8013 is in a smooth state, and the intermediate tank 3 can be evacuated. Therefore, through the setting of the sub-control device 8, the linkage control of the first air-controlled valve 2, the second air-controlled valve 4 and the intermediate tank 3 can be achieved.

[0071] A feed pipe 1 is connected to one end of the first gas-controlled valve 2 that is away from the intermediate tank 3 , and the feed pipe 1 is connected to a slurry supply system pipeline.

[0072] In order to achieve heat insulation and leave free space during the vibration of the freeze-drying chamber 19, the terminal tube 5 is connected to the feed port 1901 of the freeze-drying chamber 19 through the rubber connecting tube 6. A through hole is provided on the insulated box 18, and the rubber connecting tube 6 passes through the through hole. A clamping ring area 601 is provided in the area where the rubber connecting tube 6 contacts the through hole. The upper and lower clamping rings of the clamping ring area 601 are respectively clamped on both sides of the top surface of the insulated box 18 to optimize the sealing effect.

[0073] The post-processing assembly includes a crushing box 33, and a plurality of layers of vibrating screens are arranged at intervals inside the crushing box 33. The crushing box 33 is connected to the discharge assembly, and the structure of the discharge assembly is the same as that of the feeding assembly, and also includes the first air control valve 2, the intermediate tank 3, the second air control valve 4, the terminal pipe 5 and the sub-control device 8. The discharge port 3305 at the bottom of the crushing box 33 is connected to the first air control valve 2.

[0074] The provision of the sub-control device 8 and the intermediate tank 3 in the feed assembly and the discharge assembly can serve the purpose of pre-vacuuming, thereby preventing the pressure in the freeze-drying chamber 19 from rising too much when the feed assembly and the discharge assembly are connected to the freeze-drying assembly, necessitating the restart of the vacuuming equipment, thereby achieving the purpose of reducing energy consumption.

[0075] The freeze-drying bin 19, the heat preservation box 18 and the crushing box 33 are connected by a passage, and an electrically or pneumatically controlled door panel is provided on the passage. Specifically, the end surface where the heat preservation box 18 and the crushing box 33 are connected is provided with a discharge passage 1801, and the corresponding position of the crushing box 33 is provided with a feed passage 3301, and the feed passage 3301 is connected with the discharge passage 1801.

[0076] An upper connecting plate 1803 is fixedly mounted outside the incubator 18, and a lower connecting plate 3302 is fixedly mounted outside the crushing box 33. The upper connecting plate 1803 and the lower connecting plate 3302 are placed on each other and fixedly connected by bolts.

[0077] A second door panel 31 is provided on the discharge channel 1801. The second telescopic device 32 drives the second door panel 31 to move, so as to realize the connection and isolation between the discharge channel 1801 and the feed channel 3301.

[0078] The lower half of the end face of the freeze-drying chamber 19 facing the discharge channel 1801 is arranged in an open manner. A slot 1904 is provided in the inner wall of the upper half of the end face. A first door panel 20 is slidably arranged inside the slot 1904. The first telescopic device 21 fixedly connected to the freeze-drying chamber 19 controls the up and down movement of the first door panel 20. When the first door panel 20 moves down to the lowest point, the open area of the lower half of the end face of the freeze-drying chamber 19 facing the discharge channel 1801 is covered.

[0079] The open area of the lower half of the end face of the freeze-drying chamber 19 facing the discharge channel 1801 is connected to the discharge channel 1801 through a connecting frame 27. The bottom surface of the connecting frame 27 is inclined to facilitate discharging.

[0080] A push plate 22 is arranged inside the freeze-drying chamber 19. The bottom surface and the left and right side surfaces of the push plate 22 are in contact with the inner wall of the freeze-drying chamber 19. A screw rod 23 is threadedly connected to the top of the push plate 22 through a threaded hole. The end of the screw rod 23 is connected to a first motor 24. The first motor 24 drives the push plate 22 to move away from or close to the first door panel 20 through the screw rod 23. After the vacuum freeze-drying is completed, the first door panel 20 and the second door panel 31 are opened. The first motor 24 drives the screw rod 23 to rotate, driving the push plate 22 to move towards the crushing box 33, so as to push out the catalyst powder inside the freeze-drying chamber 19. In order to optimize the pushing effect, the bottom of the push plate 22 is an inclined surface area 2201.

[0081] As Figures 24 to 28 shown, two layers of vibrating sieves are arranged inside the crushing box 33. The height of the upper vibrating sieve is lower than the height of the feed channel 3301. The vibrating sieve includes a filter plate 34, a cam 36 and a second motor 37. The second motor 37 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 arranged below the other end. The cam 36 is connected to the output shaft of the second motor 37.

[0082] A spring 35 is arranged above the filter plate 34. The spring 35 is located on the side of the cam 36. Above the spring 35, there is a spring top plate 3304, and the spring top plate 3304 is fixedly connected to the inner wall of the crushing box 33. An annular limiting frame 3303 is fixedly mounted on the inner wall of the crushing box 33, and the filter plate 34 is placed on the annular limiting frame 3303.

[0083] Since the catalyst powder after vacuum freeze-drying will aggregate together to form lumps, but the bonding force between individual particles is not high, it can be broken up by a vibrating screen. In this embodiment, the pore size of the upper filter plate 34 is larger than that of the lower filter plate 34 to avoid material blockage.

[0084] Inside the crushing box 33, three sets of gratings are provided, and the three sets of gratings are respectively arranged above the upper filter plate 34, between the two filter plates 34, and below the lower filter plate 34.

[0085] By the three sets of gratings to obtain the quantity of the catalyst powder extruded above each filter plate 34, and then adjust the rotational speeds of the two second motors 37 to increase or decrease the vibration frequency of the filter plate 34. The specific adjustment method is as follows: The height value of the catalyst powder above the upper filter plate 34 is set as a, the height value of the catalyst powder above the lower filter plate 34 is set as b, and the height value of the catalyst powder at the bottom of the crushing box 33 is set as c.

[0086] When c reaches the threshold value, turn off the two second motors 37 and turn on the discharging assembly to discharge the material.

[0087] When c is less than the threshold value: If a > b, then increase the rotational speed of the second motor 37 of the upper vibrating screen to make the rotational speed of the second motor 37 of the upper vibrating screen greater than that of the second motor 37 of the lower vibrating screen; If a < b, then decrease the rotational speed of the second motor 37 of the upper vibrating screen to make the rotational speed of the second motor 37 of the upper vibrating screen less than that of the second motor 37 of the lower vibrating screen; If a = b, then the rotational speeds of the second motors 37 of the upper and lower vibrating screens are the same.

[0088] As Figure 29 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 control coil 25 to refrigerate the freeze-drying chamber 19.

[0089] 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.

[0090] The flowing medium in the internal circulation system is liquid nitrogen, and the flowing medium in the external circulation system is nitrogen. The liquid nitrogen reduces the temperature of the nitrogen through the first heat exchanger 41.

[0091] After the liquid nitrogen exchanges heat with nitrogen, the temperature of the nitrogen decreases and the temperature of the liquid nitrogen increases. After the temperature of the liquid nitrogen rises to the threshold value, it will vaporize to form nitrogen. Therefore, in the internal circulation system, on the liquid nitrogen outlet pipeline of the first heat exchanger 41, that is, on the pipeline between the first heat exchanger 41 and the liquid nitrogen storage tank 39, a thermostat 42 and a three-way valve 43 are electrically connected to each other. One outlet of the three-way valve 43 is connected to the liquid nitrogen storage tank 39, and the other outlet is connected to a reflux storage tank 44.

[0092] When the thermostat 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 internal storage.

[0093] 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.

[0094] After being compressed by the compressor 45, the temperature of the medium rises above 50°C. At this time, the temperature of the nitrogen inside the external circulation system is lower than 0°C. Therefore, the external circulation system is connected to the second heat exchanger 46. When the nitrogen inside the external circulation system passes through the temperature control coil 25 and then flows into the second heat exchanger 46, it cools down the medium compressed by the compressor 45 in the internal circulation system.

[0095] A method for macro-preparing and forming a catalyst, based on the above-mentioned device for macro-preparing and forming a catalyst, includes the following steps: S01. The vacuum pumping device evacuates the freeze-drying chamber 19 through the air extraction pipe 2601 so that the air pressure inside the freeze-drying chamber 19 is maintained between 1 and 30 Pa. 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, first open the first pneumatic control valve 2 and close the second pneumatic control valve 4, and the slurry is injected into the intermediate tank 3. Then close the first pneumatic control valve 2, and the vacuum pumping device evacuates the intermediate tank 3 through the connecting pipe 17 so that the internal air pressure is maintained between 1 and 30 Pa. The internal air pressure of the intermediate tank 3 is less than the internal air pressure of the freeze-drying chamber 19. Then open the second pneumatic control valve 4, 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 internal temperature of the freeze-drying chamber 19 is raised to between -25°C and -20°C, and the internal air pressure of the freeze-drying chamber 19 is reduced to 10 Pa to 15 Pa for primary drying. The control method for the temperature rise of the temperature control coil 25 adopts any one or a combination of the following two schemes: 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 thus 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 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; During the secondary drying process, the air pressure inside the freeze-drying chamber is adjusted to less than 5Pa, and the secondary drying is maintained for 2 to 3 hours; S05. After completing the secondary drying, the freeze-drying chamber 19 pushes the block catalyst into the crushing box 33, breaks the block catalyst into particles through the vibrating screen, and enters the discharge assembly through the vibrating screen, and is finally discharged through the discharge assembly.

[0096] The implementation methods of the present application are described in detail above in conjunction with the accompanying drawings, but the present application is not limited to the above implementation methods, and various changes can be made within the knowledge scope of ordinary technicians in the relevant technical field without departing from the purpose of the present application.

Claims

1. A device for macro-preparing and forming a catalyst, characterized in that: It includes a freeze-drying assembly, a post-treatment assembly and a cooling system; The freeze-drying assembly includes a feeding assembly, a heat preservation box (18), a freeze-drying chamber (19) and a temperature control coil (25). The temperature control coil (25) abuts against the freeze-drying chamber (19). The freeze-drying chamber (19) is arranged inside the heat preservation box (18). The feeding assembly located outside the heat preservation box (18) is connected to the feeding port (1901) of the freeze-drying chamber (19). The freeze-drying chamber (19) is connected to an external vacuum pumping device through an exhaust pipe (2601). A heating device (30) is provided on the freeze-drying chamber (19); The post-treatment assembly includes a crushing box (33). Inside the crushing box (33), there are several layers of vibrating screens arranged at intervals. The crushing box (33) is connected in through connection with a discharging assembly; The freeze-drying chamber (19), the heat preservation box (18) and the crushing box (33) are connected through a channel, and a door panel controlled by electricity or pneumatic is provided on the channel; The cooling system is connected to the inlet and outlet of the temperature control coil (25).

2. The device for macro-preparing and forming a catalyst according to claim 1, characterized in that: The feeding assembly and the discharging assembly have the same structure, and both include a first pneumatic control valve (2), an intermediate tank (3), a second pneumatic control valve (4), a terminal pipe (5) and a sub-control device (8); The inlets and outlets at the upper and lower ends of the intermediate tank (3) are respectively connected to the first pneumatic control valve (2) and the second pneumatic control valve (4). The second pneumatic 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 pneumatic control valve (2) and the second pneumatic control valve (4) through two valve closing control air pipes (14) and two valve opening control air pipes (15). An external high-pressure air pipe (13) is connected to the outside of the sub-control device (8).

3. The device for macro-preparing and forming a catalyst according to claim 2, characterized in that: The sub-control device (8) includes a valve body (801) and a cover plate (802) which are detachably connected; An air inlet cavity (803) connected to the external high-pressure air pipe (13) is provided inside the valve body (801). The air inlet cavity (803) is connected in through connection with an extended control air cavity (804) and a contraction control air cavity (805) arranged at intervals. The extended control air cavity (804) is connected in through connection with two first branch air cavities (806). The first branch air cavity (806) is connected in through connection with the valve opening control air pipe (15). The contraction control air cavity (805) is connected in through connection with two second branch air cavities (809). The second branch air cavity (809) is connected in through connection with the valve closing control air pipe (14); Four valve rod moving holes (8012) are provided on the valve body (801). The plane where the axes of the valve rod moving holes (8012) are located is perpendicular to the plane where the axes of the first branch air cavity (806) and the second branch air cavity (809) are located; Two valve rod moving holes (8012) are connected in through connection with two first branch air cavities (806), and the other two valve rod moving holes (8012) are connected in through connection with two second branch air cavities (809); Inside the valve stem moving hole (8012) that is connected in communication with the first air cavity (806), there is a valve opening control valve column (9). On the first cylinder body (901) of the valve opening control valve column (9), there is a first through hole (904) that is connected in cooperation with the first air cavity (806); Inside the valve stem moving hole (8012) that is connected in communication with the second air cavity (809), there is a valve closing control valve column (10). On the second cylinder body (1001) of the valve closing control valve column (10), there is a second through hole (1004) that is connected in cooperation with the second air cavity (809); Outside the cover plate (802), there is a control assembly that controls the sliding of the valve opening control valve column (9) and the valve closing control valve column (10).

4. The macroscale preparation and forming device for a catalyst according to claim 3, wherein: Inside the valve body (801), there is a through vacuum air cavity (8013). The two ends of the vacuum air cavity (8013) are respectively connected in communication with a vacuum tube (16) and a connecting tube (17). The end of the connecting tube (17) penetrates into the intermediate tank (3); The two valve stem moving holes (8012) that are connected in communication with the second air cavity (809) are connected in communication with the vacuum air cavity (8013); On the second cylinder body (1001) of the valve closing control valve column (10), there is a third through hole (1006) that is connected in cooperation with the vacuum air cavity (8013).

5. The macroscale preparation and forming device for a catalyst according to any one of claims 1 to 4, wherein: On the end face where the heat preservation box (18) is connected to the pulverizing box (33), there is a discharge channel (1801). At the corresponding position of the pulverizing box (33), there is a feed channel (3301). The feed channel (3301) is connected in communication with the discharge channel (1801); On the discharge channel (1801), there is a second door panel (31). The second telescopic device (32) drives the second door panel (31) to move, realizing the connection and isolation between the discharge channel (1801) and the feed channel (3301); The lower half of the end face of the freeze-drying chamber (19) facing the discharge channel (1801) is arranged in an open manner. Inside the inner wall of the upper half of the end face, there is a slot (1904). Inside the slot (1904), a first door panel (20) slides. The first telescopic device (21) fixedly connected to the freeze-drying chamber (19) controls the up and down movement of the first door panel (20). When the first door panel (20) moves down to the lowest point, it covers the open area of the lower half of the end face of the freeze-drying chamber (19) facing the discharge channel (1801); The open area of the lower half of the end face of the freeze-drying chamber (19) facing the discharge channel (1801) is connected in communication with the discharge channel (1801) through a connecting frame (27).

6. The macroscale preparation and forming device for a catalyst according to claim 5, wherein: The freeze-drying chamber (19) is supported inside the heat preservation box (18) by an externally arranged heat insulation support frame (28).

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

8. A catalyst macro-preparation and forming 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 a temperature control coil (25) to refrigerate the freeze-drying chamber (19).

9. A catalyst macro-preparation and forming 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 with each other; 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); The flowing medium in the internal circulation system is liquid nitrogen, and the flowing medium in the external circulation system is nitrogen. The liquid nitrogen reduces the temperature of the nitrogen through the first heat exchanger (41).

10. A method for macroscale preparation and shaping of a catalyst, based on the apparatus for macroscale preparation and shaping of a catalyst described in claim 9 above, characterized in that, It includes the following steps: S01. A vacuum pumping device pumps the freeze-drying chamber (19) through a suction pipe (2601) to maintain the air pressure inside the freeze-drying chamber (19) between 1 and 30 Pa. The freeze-drying chamber (19) is cooled through the cooling system to reduce the internal temperature of the freeze-drying chamber (19) to between -40°C and -50°C; S02. The slurry enters the interior of the freeze-drying chamber (19) through the feeding assembly. During the feeding process, first, the first pneumatic control valve (2) is opened, and the second pneumatic control valve (4) is closed. The slurry is injected into the intermediate tank (3); Then, the first pneumatic control valve (2) is closed. The vacuum pumping device pumps the intermediate tank (3) through a connecting pipe (17) to maintain the air pressure inside it between 1 and 30 Pa. The air pressure inside the intermediate tank (3) is less than the air pressure inside the freeze-drying chamber (19). Then, the second pneumatic 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 internal temperature of the freeze-drying chamber (19) is raised to between -25°C and -20°C, and the internal air pressure of the freeze-drying chamber (19) is reduced to 10 Pa to 15 Pa for primary drying; The control method for the temperature rise of the temperature control coil (25) adopts any one or a combination of the following two schemes: One. By increasing the power of the second delivery pump (49), increasing the flow rate of nitrogen in the external circulation system, reducing its heat exchange efficiency with liquid nitrogen in the first heat exchanger (41), increasing the temperature of the nitrogen, and thus raising the temperature of the temperature control coil (25); Two. Close 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 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); 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; S05. After the secondary drying is completed, the freeze-drying chamber (19) pushes the bulk catalyst into the crushing box (33), where the bulk catalyst is crushed into particles by a vibrating screen, and enters the discharge assembly through the vibrating screen, and is finally discharged through the discharge assembly.

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