A sample pulverizing device

Abstract

The utility model provides a kind of sample pulverizing device, solve the raw material medicine pulverizing device of the principle of mechanical grinding to be easy to introduce metal or other impurities in raw material medicine powder, and it is difficult to obtain the problem of good ultrafine powder of monodispersity.The top of the utility model box is fixed with the top opening of the discharge port, the lower end of the discharge port is inserted into the box and is connected with the upper end of the storage cylinder;Liquid nitrogen tank is equipped in the box, the outlet of liquid nitrogen tank is connected with the inlet of cooling coil through liquid nitrogen delivery pipe, first solenoid valve is equipped on liquid nitrogen delivery pipe, cooling coil is spirally coiled on storage cylinder, the outlet of cooling coil is connected with the gas inlet of gas storage tank through nitrogen recovery pipe, first telescopic device can be equipped in the box, the movable end of first telescopic device is fixedly connected with gate, gate is slidably abutted at the lower end of storage cylinder;High-frequency micro-amplitude vibration pulverizing device is equipped in the box, the top of high-frequency micro-amplitude vibration pulverizing device is equipped with sample vessel that can be taken and placed.

Description

Technical Field

[0001] This utility model relates to the field of pharmaceutical equipment technology, and in particular to a sample crushing device. Background Technology

[0002] Active pharmaceutical ingredients (APIs), also known as active drug components, are prepared by chemical synthesis, plant extraction, or biotechnology. They are generally processed by adding excipients to produce drugs that can be used directly. In order to increase the contact area between the API and other excipients during processing and other processing factors, the API is often subjected to ultra-fine pulverization.

[0003] In existing technologies, the pulverization of active pharmaceutical ingredients (APIs) mostly employs mechanical grinding principles. For example, the ultra-micro pulverization mechanism for biochemical APIs disclosed in patent application number 202323077699.5 includes a base plate and a grinding chamber fixedly connected to the upper surface of the base plate. The back of the grinding chamber is provided with a grinding structure for grinding the API. The grinding structure includes a motor fixedly connected to the back of the grinding chamber. The output shaft of the motor is fixedly connected to a rotating rod. A drive gear is fixedly connected to the outer side of the rotating rod. A driven gear meshes with the right side of the drive gear. A driven rod is fixedly connected to the inner side of the center of the driven gear. Grinding cylinders are fixedly connected to the outer sides of both the rotating rod and the driven rod. Several ceramic balls are fixedly connected to the outer surface of the grinding cylinder. A cooling component for cooling the API is provided on the left side of the grinding chamber. The following disadvantages exist when using this type of raw material pulverizing device that uses mechanical grinding principle: (1) The grinding media (such as the balls in the ball mill jar) are in contact with the material for a long time, which may introduce metal or other impurities; (2) The heat generated by mechanical friction may cause the raw material to decompose or denature; (3) The particle size distribution of the pulverized raw material powder is uneven, making it difficult to obtain ultrafine powder with good monodispersity. Utility Model Content

[0004] In order to solve the problem that the raw material pulverizing device using the mechanical grinding principle in the background art is prone to introducing metal or other impurities into the raw material powder and is difficult to obtain ultrafine powder with good monodispersity, this utility model proposes a sample pulverizing device.

[0005] The technical solution of this utility model is: a sample crushing device, including a box body, a top opening of a feeding port fixedly provided on the top of the box body, a detachable cover provided on the upper opening of the feeding port, the lower end of the feeding port passing through the box body and connected to the upper end of a flexible hose, the lower end of the flexible hose being connected to the upper end of a storage cylinder, the storage cylinder being a tubular structure with open top and bottom, and the storage cylinder being fixedly installed in the box body. The box contains a liquid nitrogen tank. The outlet of the liquid nitrogen tank is connected to the inlet of the cooling coil through a liquid nitrogen delivery pipe. A first solenoid valve is installed on the liquid nitrogen delivery pipe. The cooling coil is spirally wound on the storage cylinder. The outlet of the cooling coil is connected to the air inlet of the storage tank through a nitrogen recovery pipe. A safety valve and a second solenoid valve are installed on the nitrogen recovery pipe. A mounting frame is fixedly installed inside the box. The mounting frame is equipped with a first telescopic device that can extend and retract left and right. A gate is fixedly connected to the movable end of the first telescopic device. The gate slides against the lower end of the storage cylinder and can be moved away from the lower end of the storage cylinder. The chamber is equipped with a high-frequency micro-vibration pulverizer. The top of the high-frequency micro-vibration pulverizer is equipped with a sample container that can be placed and removed. The sample container is located below the gate and directly below the lower port of the storage cylinder. The storage cylinder is equipped with a temperature sensor for monitoring its internal temperature; The front panel of the box has a transparent access opening, and a door is hinged to the access opening. The movable end of the door is detachably connected to the front panel of the box via a second latch. The door is equipped with a controller, and the temperature sensor is connected to the controller. The temperature sensor is also connected to the first solenoid valve, the second solenoid valve, the first telescopic device, and the high-frequency micro-vibration crushing device.

[0006] Preferably, the high-frequency micro-amplitude vibration crushing device includes a base, with a number of piezoelectric ceramic sheets embedded in the bottom of the base. All the piezoelectric ceramic sheets are connected in series and connected to the controller. The bottom of the base is provided with a removable sealing plate for sealing the piezoelectric ceramic sheets.

[0007] Preferably, the base has a holder at the top, and the bottom of the sample container is inserted into the holder.

[0008] Preferably, the top of the sample vessel slides against the bottom of the gate, and the gate can simultaneously close the upper port of the sample vessel and the lower port of the storage cylinder.

[0009] Preferably, the sample container has a hollow structure that is narrow at the top and wide at the bottom. From the inside to the outside, the sample container includes a working cavity surface and an elastic conductive layer. The elastic conductive layer is in contact with the high-frequency micro-amplitude vibration crushing device. The working cavity surface is made of silicon nitride ceramic, zirconium oxide ceramic or high-purity sapphire, and the elastic conductive layer is made of titanium alloy or beryllium copper alloy.

[0010] Preferably, the high-frequency micro-vibration crushing device is slidably disposed at the bottom of the box, and a second telescopic device capable of extending and retracting back and forth is provided inside the box. The movable end of the second telescopic device is fixedly connected to the high-frequency micro-vibration crushing device. The second telescopic device can push the high-frequency micro-vibration crushing device out of the pick-and-place port on the front panel of the box. The second telescopic device is connected to the controller.

[0011] Preferably, the storage cylinder is equipped with a low-frequency vibration device, which is connected to the controller. A first vacuum-insulated flexible metal hose connects the liquid nitrogen delivery pipe to the cooling coil, and a second vacuum-insulated flexible metal hose connects the cooling coil to the nitrogen recovery pipe.

[0012] Preferably, the outlet of the gas storage tank is connected to the upper part of the storage cylinder through a nitrogen delivery pipe, and the nitrogen delivery pipe is equipped with a third vacuum-insulated flexible metal hose and a third solenoid valve. The bottom of the storage cylinder is connected to one end of the nitrogen emission pipe. The nitrogen emission pipe is equipped with a powder filter and a fourth solenoid valve. The powder filter is located between the fourth solenoid valve and the storage cylinder. The other end of the nitrogen emission pipe passes through the housing and is connected to the exhaust port. The exhaust port is equipped with a filter screen. The fourth solenoid valve is connected to the controller.

[0013] Preferably, the storage cylinder is equipped with a pressure sensor for monitoring its internal pressure, and the pressure sensor is communicatively connected to the controller.

[0014] Preferably, a backflush pipe is connected to the outlet of the cooling coil, and a fifth solenoid valve is provided on the backflush pipe. The fifth solenoid valve is connected to the controller. The end of the backflush pipe away from the cooling coil is connected to the nitrogen discharge pipe. The connection point between the backflush pipe and the nitrogen discharge pipe is located between the powder filter and the fourth solenoid valve.

[0015] Advantages of this utility model: (1) Deep low temperature pulverization: By using liquid nitrogen circulation cooling, the heat-sensitive and high-value-added raw material samples are pulverized in a brittle state, which fundamentally solves the problems of decomposition and denaturation caused by mechanical friction heat.

[0016] (2) High efficiency utilization of cooling capacity: The innovative liquid nitrogen vaporization and recovery design recovers the nitrogen used for refrigeration to the storage tank, which not only recovers the cooling capacity, but also provides a free source of inert gas for the system, saving energy and protecting the environment.

[0017] (3) Fully inert and oxygen-free: Through nitrogen replacement and a closed circulation system, the risk of oxidation and moisture absorption of the sample during the crushing process is completely eliminated.

[0018] (4) Ultra-high purity guarantee: The working cavity surface of the sample vessel in contact with the raw drug is made of inert material, which ensures that the sample is not contaminated by impurities such as metal ions.

[0019] (5) Precise energy transfer: The composite vibration structure of "piezoelectric ceramic-elastic conductive layer-working cavity surface" is adopted to realize low loss and high efficiency transmission of high frequency micro-amplitude vibration. The crushing force is precisely controllable and can obtain fine powder with uniform particle size distribution.

[0020] (6) The liquid nitrogen pipeline adopts a vacuum-insulated flexible metal hose, which can effectively insulate heat and absorb and offset vibration stress, prevent the pipeline from fatigue breaking due to vibration, and eliminate the risk of leakage.

[0021] (7) A safety valve is installed on the nitrogen recovery pipe to ensure that the pressure is within a safe range.

[0022] (8) Through the linkage of temperature and pressure sensors and multiple solenoid valves, the automatic control of the entire process of inerting, cooling, crushing and collection is realized. The operation is simple and the repeatability is good.

[0023] (9) The integrated online pulse backflushing cleaning system can automatically clean the powder filter, solving the key technical problem of easy clogging by fine powder. It does not require opening the cover to interrupt the process, greatly improving the continuous working ability and reliability of the equipment. Attached Figure Description

[0024] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0025] Figure 1 This is a schematic diagram of the internal main structure of Example 1; Figure 2 This is a schematic diagram of the external main structure of Example 1; Figure 3 for Figure 1 A schematic diagram of the internal structure of the sample vessel and the high-frequency micro-vibration pulverizer in the image. Figure 4 for Figure 1 Enlarged view of the structure at point A in the image; In the diagram, 1. Box body, 2. Feed port, 3. Cover, 4. First lock, 5. Hose, 6. Storage cylinder, 7. Gate, 8. First telescopic device, 9. Pressure sensor, 10. Temperature sensor, 11. Low-frequency vibration device, 12. Track, 13. Slider, 14. High-frequency micro-vibration crushing device, 1401. Base, 1402. Piezoelectric ceramic sheet, 1403. Sealing plate, 1404. Card holder, 1405. Connecting plate, 15. Sample container, 1501. Working chamber surface, 1502. Elasticity 16. Conductive layer; 17. Second telescopic device; 18. Liquid nitrogen tank; 19. First vacuum-insulated flexible metal hose; 20. First solenoid valve; 21. Cooling coil; 22. Second vacuum-insulated flexible metal hose; 23. Safety valve; 24. Second solenoid valve; 25. Gas storage tank; 26. Third vacuum-insulated flexible metal hose; 27. Third solenoid valve; 28. Powder filter; 29. ​​Fourth solenoid valve; 30. Exhaust port; 31. Fifth solenoid valve; 32. Box door; 33. Second latch; 34. Controller. Detailed Implementation

[0026] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0027] Example 1: A sample pulverizing device, such as Figure 1 As shown, the device includes a box body 1. The top of the box body 1 is fixedly provided with a top opening for a discharge port 2. The upper opening of the discharge port 2 is provided with a detachable cover 3. The discharge port 2 and the cover 3 are detachably connected by a first latch 4.

[0028] The lower end of the discharge port 2 is inserted into the box 1 and connected to the upper end of the hose 5. The lower end of the hose 5 is connected to the upper end of the storage cylinder 6. The storage cylinder 6 is a tubular structure that is open at both ends and is fixedly installed inside the box 1.

[0029] The housing 1 contains a liquid nitrogen tank 17. The outlet of the liquid nitrogen tank 17 is connected to the inlet of the cooling coil 20 through a liquid nitrogen delivery pipe. A first vacuum-insulated flexible metal hose 18 is connected between the liquid nitrogen delivery pipe and the cooling coil 20. A first solenoid valve 19 is installed on the liquid nitrogen delivery pipe. The cooling coil 20 is spirally wound on the storage cylinder 6. The outlet of the cooling coil 20 is connected to the air inlet of the gas storage tank 24 through a nitrogen recovery pipe. A second vacuum-insulated flexible metal hose 21 is connected between the cooling coil 20 and the nitrogen recovery pipe. A safety valve 22 and a second solenoid valve 23 are installed on the nitrogen recovery pipe.

[0030] The outlet of the gas storage tank 24 is connected to the upper part of the storage cylinder 6 through a nitrogen delivery pipe. The nitrogen delivery pipe is equipped with a third vacuum insulated flexible metal hose 25 and a third solenoid valve 26. The bottom of the storage cylinder 6 is connected to one end of the nitrogen discharge pipe. The nitrogen discharge pipe is equipped with a powder filter 27 and a fourth solenoid valve 28. The powder filter 27 is located between the fourth solenoid valve 28 and the storage cylinder 6. The other end of the nitrogen discharge pipe passes through the box 1 and is connected to the exhaust port 29. The exhaust port 29 is equipped with a filter screen. The fourth solenoid valve 28 is connected to the controller 33 for control.

[0031] A backflush pipe is connected to the outlet of the cooling coil 20. A fifth solenoid valve 30 is installed on the backflush pipe. The fifth solenoid valve 30 is connected to the controller 33. The end of the backflush pipe away from the cooling coil 20 is connected to the nitrogen discharge pipe. The connection point between the backflush pipe and the nitrogen discharge pipe is located between the powder filter 27 and the fourth solenoid valve 28.

[0032] The storage cylinder 6 is equipped with a pressure sensor 9 for monitoring its internal pressure and a temperature sensor 10 for monitoring its internal temperature.

[0033] A low-frequency vibration device 11 is provided on the storage cylinder 6. In this embodiment, the low-frequency vibration device 11 is a vibration motor with a vibration frequency in the range of 10~50 Hz. The low-frequency vibration device 11 is connected to the controller 33. The design purpose of the low-frequency vibration device 11 is: (1) to break the "arch bridge" effect formed by the powder in the storage cylinder and sample container, and ensure that the material can flow smoothly downward; (2) to make the material generate micro-movement in the sample container, to ensure that the material is cooled evenly and efficiently, and to avoid local overheating or cooling dead corners; (3) to create a uniform, stable and loose material environment for high-frequency pulverization, and to ensure the uniformity of pulverization; (4) to help the pulverized powder fall more completely into the collection container when the gate is opened.

[0034] An installation frame is fixedly installed inside the housing 1. The installation frame is equipped with a first telescopic device 8 that can extend and retract left and right. A gate 7 is fixedly connected to the movable end of the first telescopic device 8. The gate 7 slides against the lower port of the storage cylinder 6 and can be moved away from the lower port of the storage cylinder 6.

[0035] The housing 1 has a track 12 extending in the front-to-back direction. A slider 13 slides on the track 12. A high-frequency micro-vibration crushing device 14 is installed on the top of the slider 13. Under the favorable conditions created by low frequency, the high-frequency micro-vibration crushing device 14 performs precise and efficient "surgical" disintegration on brittle materials. Figure 3As shown, the high-frequency micro-amplitude vibration pulverizing device 14 includes a metal base 1401, which serves as both a support and a heat dissipation channel. Several piezoelectric ceramic plates 1402 with a vibration frequency of 18-25 kHz are embedded in the bottom of the base 1401. All the piezoelectric ceramic plates 1402 are connected in series and then connected to the controller 33. A removable sealing plate 1403 is provided at the bottom of the base 1401 to seal the piezoelectric ceramic plates 1402. A retaining seat 1404 is provided at the top of the base 1401.

[0036] The base 1401 has connecting plates 1405 fixed on both the left and right sides. The housing 1 has a second telescopic device 16 that can extend and retract back and forth. The movable end of the second telescopic device 16 is fixedly connected to the connecting plate 1405 of the high-frequency micro-vibration crushing device 14. The second telescopic device 16 can push the high-frequency micro-vibration crushing device 14 out of the pick-up and put-out port on the front panel of the housing 1. The second telescopic device 16 is connected to the controller 33 for control.

[0037] The high-frequency micro-vibration pulverizer 14 has a sample container 15 that can be picked up and put in at the top, and the bottom of the sample container 15 is inserted into the card holder 1404.

[0038] The sample container 15 is located below the gate 7 and directly below the lower port of the storage cylinder 6. The top of the sample container 15 slides against the bottom of the gate 7, and the gate 7 can simultaneously close the upper port of the sample container 15 and the lower port of the storage cylinder 6.

[0039] The sample container 15 has a hollow structure that is narrower at the top and wider at the bottom. From the inside out, the sample container 15 includes a working chamber surface 1501 and an elastic conductive layer 1502. The elastic conductive layer 1502 is in contact with the high-frequency micro-vibration pulverizing device 14. The working chamber surface 1501 is made of a high-purity, high-hardness, and high-wear-resistant inert material, such as silicon nitride ceramic, zirconium oxide ceramic, or high-purity sapphire. The working chamber surface 1501 is the surface that directly contacts the raw material powder. Its high hardness ensures wear resistance, its chemical inertness ensures the purity of the sample, and its smooth surface reduces powder adhesion. The elastic conductive layer 1502 is made of a high-strength, high-fatigue-life, and low-energy-loss metal alloy, such as titanium alloy or beryllium copper alloy. The elastic conductive layer 1502 can efficiently transmit the high-frequency micro-vibration of the bottom piezoelectric ceramic sheet 1402 to the top working chamber surface 1501, buffering and distributing the internal stress caused by the difference in thermal expansion coefficients and vibration, preventing the brittle working chamber surface 1501 from cracking.

[0040] The front panel of the box 1 has a transparent opening for taking out and putting in, and a door 31 is hinged to the opening. The movable end of the door 31 is detachably connected to the front panel of the box 1 through a second latch 32.

[0041] The door 31 is equipped with a controller 33. The temperature sensor 10 is connected to the controller 33. The temperature sensor 10 is connected to the first solenoid valve 19, the second solenoid valve 23, the pressure sensor 9, the first telescopic device 8, and the high-frequency micro-amplitude vibration crushing device 14.

[0042] In this embodiment, the telescopic device uses an electric push rod. In other embodiments, a hydraulic cylinder or a pneumatic cylinder can be used instead.

[0043] The sample pulverizing device described in this application operates as an intelligent, closed-loop process integrating cryogenic treatment, inert environment protection, and high-frequency micro-vibration pulverization. Its working principle can be divided into the following core steps: (1) Preparation and loading stage: Open the cover 3, put the heat-sensitive raw material sample to be crushed into the storage cylinder 6 through the feed port 2, put the cover 3 back on the top of the feed port 2, and use the first lock 4 to lock the cover 3 on the top of the feed port 2.

[0044] (2) Inert environment creation and pre-cooling stage: Air purging: Controller 33 opens the third solenoid valve 26 and the fourth solenoid valve 25, allowing nitrogen in the gas storage tank 24 to enter the upper part of the storage cylinder 6 through the nitrogen delivery pipe. The nitrogen flows downwards, purging the air in the storage cylinder 6 and its connecting pipes from the nitrogen discharge pipe at the bottom. This process is monitored by pressure sensor 9 to ensure that the air is fully replaced.

[0045] Deep cooling: Controller 33 opens the first solenoid valve 19 and the second solenoid valve 23, allowing liquid nitrogen to flow from the liquid nitrogen tank 17. This liquid nitrogen then passes through the first vacuum-insulated flexible metal hose 18 and the liquid nitrogen delivery pipe into the cooling coil 20 spirally wound around the storage cylinder 6. The liquid nitrogen absorbs heat and vaporizes within the cooling coil 20, providing powerful cooling to the storage cylinder 6 and its entire interior space.

[0046] Cold energy recovery: The vaporized low-temperature nitrogen gas is recovered to the gas storage tank 24 through the second vacuum insulated flexible metal hose 21, realizing the recycling of cold energy and inert gas.

[0047] (3) Deep cryogenic embrittlement and initial crushing stage: When the temperature sensor 10 detects that the temperature inside the storage cylinder 6 reaches the preset deep cryogenic target (such as -50℃), the controller 33 starts the low frequency vibration device 11 to make the storage cylinder and the internal airflow vibrate, which helps the material to be initially dispersed and heat exchanged.

[0048] (4) "Dissociative" pulverization stage: The controller 33 controls the first telescopic device 8 to move the gate 7 away from the lower port of the storage cylinder 6 and the upper port of the sample vessel 15. The raw material that has undergone cryogenic embrittlement and initial pulverization falls into the sample vessel 15. The gate 7 is then moved back to the position between the lower port of the storage cylinder 6 and the upper port of the sample vessel 15, closing the upper port of the sample vessel 15. The high-frequency micro-amplitude vibration pulverization device 14 is started. The high-frequency vibration generated by the piezoelectric ceramic sheet 1402 is efficiently transmitted to the working cavity surface 1501 of the sample vessel 15 through the base 1401 and the elastic conductive layer 1501, performing precise and efficient "dissociative" pulverization on the raw material sample in a cryogenic embrittlement state, avoiding thermal damage and over-pulverization.

[0049] (5) Removal of raw material powder: Open the box door 31, and use the controller 33 to control the second telescopic device 16 to push the high-frequency micro-vibration pulverizer 14 and sample container 15 out of the box 1. Take out the raw material in the sample container 15, clean the sample container 15, and put the sample container 15 back on the high-frequency micro-vibration pulverizer 14. Use the controller 33 to pull the high-frequency micro-vibration pulverizer 14 and sample container 15 back into the box 1 for reset.

[0050] (6) Filter self-cleaning: If the powder filter 27 becomes clogged during or after the crushing process, the controller 33 controls the fifth solenoid valve 30 to open briefly. The high-pressure nitrogen gas at the outlet of the cooling coil 20 impacts the powder filter 33 in the reverse direction through the backflush pipe, shaking off the powder adhering to its surface and recycling it into the storage cylinder 6. This achieves online, non-destructive automatic cleaning and ensures the reliability of the system's long-term operation.

[0051] It will be apparent to those skilled in the art that this invention is not limited to the details of the exemplary embodiments described above, and that it can be implemented in other specific forms without departing from the spirit or essential characteristics of this invention. Therefore, the embodiments should be considered illustrative and non-limiting in all respects, and the scope of this invention is defined by the appended claims and not by the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within this invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

Claims

1. A sample pulverizing device, characterized in that: Includes a box body (1), the top of the box body (1) is fixedly provided with a top opening for a discharge port (2), the upper opening of the discharge port (2) is provided with a detachable cover (3), the lower end of the discharge port (2) is inserted into the box body (1) and connected to the upper end of a hose (5), the lower end of the hose (5) is connected to the upper end of a storage cylinder (6), the storage cylinder (6) is a tubular structure that is open from top to bottom, and the storage cylinder (6) is fixedly installed inside the box body (1); The housing (1) is equipped with a liquid nitrogen tank (17). The outlet of the liquid nitrogen tank (17) is connected to the inlet of the cooling coil (20) through a liquid nitrogen delivery pipe. A first solenoid valve (19) is provided on the liquid nitrogen delivery pipe. The cooling coil (20) is spirally wound on the storage cylinder (6). The outlet of the cooling coil (20) is connected to the air inlet of the gas storage tank (24) through a nitrogen recovery pipe. A safety valve (22) and a second solenoid valve (23) are provided on the nitrogen recovery pipe. An installation frame is fixedly provided inside the box (1). The installation frame is provided with a first telescopic device (8) that can extend and retract left and right. A gate (7) is fixedly connected to the movable end of the first telescopic device (8). The gate (7) slides against the lower port of the storage cylinder (6), and the gate (7) can be moved away from the lower port of the storage cylinder (6). The box (1) is equipped with a high-frequency micro-amplitude vibration crushing device (14). The top of the high-frequency micro-amplitude vibration crushing device (14) is equipped with a sample container (15) that can be picked up and placed. The sample container (15) is located below the gate (7) and directly below the lower port of the storage cylinder (6). The storage cylinder (6) is equipped with a temperature sensor (10) for monitoring its internal temperature; The front panel of the box (1) has a transparent opening for taking out and putting in, and a door (31) is hinged to the opening. The movable end of the door (31) is detachably connected to the front panel of the box (1) through a second latch (32). The door (31) is equipped with a controller (33), the temperature sensor (10) is connected to the controller (33) for communication, and the temperature sensor (10) is connected to the first solenoid valve (19), the second solenoid valve (23), the first telescopic device (8), and the high-frequency micro-amplitude vibration crushing device (14) for control.

2. The sample pulverizing device as described in claim 1, characterized in that: The high-frequency micro-amplitude vibration crushing device (14) includes a base (1401), and a number of piezoelectric ceramic sheets (1402) are embedded in the bottom of the base (1401). All the piezoelectric ceramic sheets (1402) are connected in series and connected to the controller (33). The bottom of the base (1401) is provided with a detachable sealing plate (1403) for sealing the piezoelectric ceramic sheets (1402).

3. The sample pulverizing device as described in claim 2, characterized in that: The base (1401) has a card holder (1404) on top, and the bottom of the sample container (15) is inserted into the card holder (1404).

4. The sample pulverizing device as described in claim 3, characterized in that: The top of the sample vessel (15) slides against the bottom of the gate (7), and the gate (7) can simultaneously close the upper port of the sample vessel (15) and the lower port of the storage cylinder (6).

5. A sample pulverizing device as described in claim 1 or 3, characterized in that: The sample vessel (15) is a hollow structure that is narrow at the top and wide at the bottom. The sample vessel (15) includes a working cavity surface (1501) and an elastic conductive layer (1502) from the inside to the outside. The elastic conductive layer (1502) is in contact with the high-frequency micro-amplitude vibration crushing device (14). The working cavity surface (1501) is made of wear-resistant inert material, and the elastic conductive layer (1502) is made of alloy.

6. A sample pulverizing apparatus as described in any one of claims 1-3, characterized in that: The high-frequency micro-vibration crushing device (14) is slidably disposed at the bottom of the box (1). The box (1) is provided with a second telescopic device (16) that can extend and retract in the front and back. The movable end of the second telescopic device (16) is fixedly connected to the high-frequency micro-vibration crushing device (14). The second telescopic device (16) can push the high-frequency micro-vibration crushing device (14) out of the pick-and-place port on the front panel of the box (1). The second telescopic device (16) is connected to the controller (33).

7. The sample pulverizing device as described in claim 1, characterized in that: The storage cylinder (6) is equipped with a low-frequency vibration device (11), which is connected to the controller (33). A first vacuum-insulated flexible metal hose (18) is connected between the liquid nitrogen delivery pipe and the cooling coil (20), and a second vacuum-insulated flexible metal hose (21) is connected between the cooling coil (20) and the nitrogen recovery pipe.

8. A sample pulverizing device as described in claim 1 or 7, characterized in that: The outlet of the gas storage tank (24) is connected to the upper part of the storage cylinder (6) through a nitrogen delivery pipe. The nitrogen delivery pipe is equipped with a third vacuum insulated flexible metal hose (25) and a third solenoid valve (26). The bottom of the storage cylinder (6) is connected to one end of the nitrogen discharge pipe. The nitrogen discharge pipe is equipped with a powder filter (27) and a fourth solenoid valve (28). The powder filter (27) is located between the fourth solenoid valve (28) and the storage cylinder (6). The other end of the nitrogen discharge pipe passes through the box (1) and is connected to the exhaust port (29). The exhaust port (29) is equipped with a filter screen. The fourth solenoid valve (28) is connected to the controller (33).

9. The sample pulverizing device as described in claim 8, characterized in that: The storage cylinder (6) is equipped with a pressure sensor (9) for monitoring its internal pressure, and the pressure sensor (9) is connected to the controller (33) in communication.

10. The sample pulverizing device as described in claim 9, characterized in that: A backflush pipe is connected to the outlet of the cooling coil (20). A fifth solenoid valve (30) is provided on the backflush pipe. The fifth solenoid valve (30) is connected to the controller (33). The end of the backflush pipe away from the cooling coil (20) is connected to the nitrogen discharge pipe. The connection node between the backflush pipe and the nitrogen discharge pipe is located between the powder filter (27) and the fourth solenoid valve (28).

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