Apparatus and method for freeze-drying process

Abstract

The invention relates to the technical field of freeze-drying equipment, in particular to equipment and a method for a freeze-drying process. Comprising a cabinet body which is detachably provided with a sealing cover; the fixing ring is detachably installed on the cabinet body, the fixing ring is rotationally connected with at least two first rotating rods, all the first rotating rods are jointly rotationally connected with a bottom plate and a top plate, and the top plate is located above the bottom plate and fixedly connected with a sealing ring matched with the sealing cover in a sealing mode; the first rotating rod is slidably connected with fixing cylinders in a linear array, the fixing cylinders with the same height are jointly and fixedly connected with a sliding plate, and the top plate is rotatably connected with a second rotating rod. A synchronous extrusion mode is adopted, so that multiple layers of cover plates can move synchronously in the cover pressing process, the distance between every two adjacent cover plates is shortened synchronously, samples on each layer are extruded at the same time, and the effect of uniformly extruding the samples on each layer with the same extrusion force is achieved.

Description

Technical Field

[0001] The present invention relates to the technical field of freeze-drying equipment, and in particular to equipment and methods used in freeze-drying technology. Background Art

[0002] A freeze dryer is a device that freezes samples and then sublimates the water in the samples under a vacuum environment to achieve the purpose of drying. In the pharmaceutical industry, freeze drying is a very important formulation technology, mainly used in the production of injections, vaccines, protein drugs or easily hydrolyzed drugs. It removes water from the product by freeze drying, greatly improving the stability of the product and extending the shelf life.

[0003] The freeze dryers commonly used in the pharmaceutical industry are divided into: multi-manifold freeze dryers, capping freeze dryers, etc. When drying injections, capping freeze dryers are generally used. Its working process is: pre-freezing (shaping the vials containing injections, during this process the vials and the stoppers are only in contact), freeze drying again under a vacuum environment (continue to lower the temperature of the injection in the vial and make the injection in the vial in the form of ice crystals), capping (pressing the stopper on the vial into it), sublimation drying (sublimating the ice crystal-like drugs in the vial directly into water vapor without passing through the liquid state), backfilling with gas and unloading.

[0004] The existing capping type freeze dryer adopts a layer-by-layer pressing method during the capping process, but the disadvantage of this method is that the capping of the lower sample will be triggered only after the sample on the upper side completes the capping step, which will increase the time required for the capping step. Moreover, since the stopper is squeezed into the vial, the space occupied by the stopper in the freeze dryer will be reduced, which will also increase the vacuum around the sample, causing the vacuum level around the lower sample to deviate from the originally designed freeze-drying conditions, affecting the efficiency and uniformity of ice crystal sublimation. Summary of the invention

[0005] The present invention adopts the following technical scheme to solve the above-mentioned technical problems, and is an apparatus and method for freeze-drying process, comprising: a cabinet body, on which a sealing cover is detachably installed; a fixing ring, which is detachably installed on the cabinet body, the fixing ring is rotatably connected with at least two first rotating rods, and all the first rotating rods are rotatably connected with a bottom plate and a top plate, the top plate is located above the bottom plate and is fixedly connected with a sealing ring that is sealed with the sealing cover, a linear array of fixed cylinders are slidably connected to the first rotating rod, and the fixed cylinders of the same height are commonly fixed with a sliding plate, the top plate is rotatably connected with a second rotating rod, and the first rotating rod and the second rotating rod are connected by a sprocket chain transmission; fixing pins, the number of which is the same as that of the fixing cylinders, are fixedly connected in adjacent fixing cylinders, the first rotating rod is provided with a linear array of spiral grooves, and the fixing pins are squeezed and matched with adjacent spiral grooves.

[0006] Preferably, the initial position of the fixing pin is located at the middle and lower part of the adjacent spiral groove, and a gap is left between the top plate and the adjacent fixing cylinder.

[0007] Preferably, a plurality of guide frames are fixedly connected to the upper side of the cabinet body, and a plurality of balls are spherically connected to the opposite sides of the plurality of guide frames, and the plurality of balls on the guide frames are in contact with and cooperate with the sealing cover.

[0008] Preferably, the pitches of the spiral grooves in the linear array on the same first rotating rod increase in a step-by-step manner from bottom to top, and the pitches of the spiral grooves on the same first rotating rod are arithmetically distributed.

[0009] Preferably, the fixed cylinders of equal height are slidably connected with a pressure plate for squeezing the sample, a spring is fixed between the pressure plate and the adjacent sliding plate, a linear array of limiting components is arranged in the sealing cover, and the limiting components are used to limit the adjacent pressure plates.

[0010] Preferably, the limiting assembly includes: a fixed column, fixedly connected to the adjacent pressure plate and slidably matched with the adjacent sliding plate, the fixed column is provided with a limiting groove; a fixed plate, fixedly connected to the adjacent sliding plate, the fixed plate is slidably connected with a sliding pin, the sliding pin is limitedly matched with the limiting groove on the adjacent fixed column, a tension spring is fixedly connected between the sliding pin and the adjacent fixed plate, and a driving assembly is provided on the top plate, and the driving assembly is used to drive the second rotating rod to rotate.

[0011] Preferably, the driving assembly includes: a connecting frame fixedly connected to the top plate, a first fixed shell fixedly connected to a side of the connecting frame away from the top plate, the first fixed shell rotatably connected to a rotating shell, the rotating shell fixedly connected to a connecting shell, the rotating shell is located between the first fixed shell and the connecting shell, and the connecting shell is fixedly connected to a handle that rotatably cooperates with the second rotating rod; a plurality of second fixed shells, all fixedly connected to the connecting shell, the second fixed shell is slidably connected to a sliding member that slidably cooperates with the connecting shell, a tension spring is fixedly connected between the sliding member and the adjacent second fixed shell, the second rotating rod is provided with a plurality of blind holes, the sliding member is limitedly cooperated with adjacent blind holes on the second rotating rod, the sliding member is fixedly connected to balls in a symmetrical and linear array, and the balls on the sliding member are in contact and cooperate with adjacent blind holes on the second rotating rod.

[0012] Preferably, the sliding plate close to the top plate is fixedly connected with an elastic bag, the elastic bag is squeezed and matched with the adjacent pressure plate, the elastic bag is fixedly connected to the first fixed shell and is connected with a connecting pipe, the connecting pipe passes through the adjacent sliding plate and the top plate, the first fixed shell is connected with the rotating shell, the rotating shell is connected with several second fixed shells, and hydraulic oil is stored in the elastic bag, the adjacent connecting pipe, the first fixed shell, the rotating shell and several second fixed shells; a sliding ring is slidably connected in the rotating shell.

[0013] Preferably, the second rotating rod is fixedly connected with a ratchet, and the ratchet is located between the handle and the connecting shell. The handle is rotatably connected to a side close to the connecting shell with a plurality of limiting members, and a torsion spring is arranged between the limiting member and the handle, and the plurality of limiting members are all in limited cooperation with the ratchet.

[0014] Preferably, the method for using the freeze-drying process equipment comprises the following steps: The first step is to pre-freeze the sample before freeze-drying, remove the sealing cover, and then place the sample on the tray, and then put multiple trays into the required position for work; In the second step, after the tray is placed, the sealing cover is placed back on the cabinet, and the cabinet performs freeze-drying on the samples; The third step is to rotate the handle after the freeze-drying is completed. The handle drives the second rotating rod to rotate through the connecting shell and a plurality of sliding parts. The second rotating rod transmits the power to the first rotating rod through the sprocket chain. Step 4: During the rotation of the first rotating rod, the adjacent fixing pins are squeezed through the spiral groove, so that the pressing plate performs a capping process on the sample; Step 5, during the process of pressing the sample, the pressing plate is made to fit with the sample, and the sliding plate continues to move to squeeze the elastic bag and reduce the distance between it and the adjacent pressing plate; Step 6: After the elastic bag is squeezed, the hydraulic oil is delivered to all the second fixed shells, disconnecting all the sliding parts from the second rotating rod. After all the sliding parts are no longer in contact with the adjacent blind holes in the second rotating rod, the handle will rotate idly and will not drive the second rotating rod to rotate synchronously, thereby completing the sample capping, and then the cabinet will perform sublimation drying on the sample; Step 7: After the sublimation drying process of the sample is completed, the handle is rotated in the reverse direction to make the first rotating rod rotate in the reverse direction, and the adjacent fixing pins are squeezed through the spiral groove, so that the fixing cylinder drives the adjacent sliding plate to reset and move, and the pressing plate is separated from the contact with the sample; Step 8: After the pressing plate is no longer in contact with the sample, the sealing cover is removed and the trays are taken out in sequence, thereby completing the sublimation drying process of the sample; In the ninth step, after taking out the sample, the limit of the adjacent fixed column is released by the sliding pin, so that the pressure plate no longer squeezes the elastic bag, and all the sliding parts are moved to be inserted into the adjacent blind holes on the second rotating rod to complete the reset of the sliding parts.

[0015] The beneficial effects of the present invention are as follows: the present invention adopts a synchronous extrusion method, so that during the capping process, the multi-layer cover plates can move synchronously, and the distance between two adjacent cover plates can be shortened synchronously, and each layer of the sample is extruded simultaneously, so as to achieve the effect of uniformly extruding each layer of the sample with the same extrusion force; When the sealing cover is removed, the sealing cover is vertically guided by the contact between the ball in the guide frame and the sealing cover, so as to prevent the sealing cover from hitting adjacent parts during placement, thereby affecting the placement of the sample; During the process of capping the sample, the distance between the pressing plate and the adjacent sliding plate is used to control the timing of the handle's idling, so as to avoid excessive movement of the pressing plate caused by excessive rotation of the second rotating rod, resulting in excessive squeezing of the sample, thereby affecting the quality of the sample itself. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention; Figure 2 It is a sectional view of the three-dimensional structure of the present invention; Figure 3 It is a three-dimensional structural cross-sectional view of the sealing cover of the present invention; Figure 4 It is a three-dimensional structural cross-sectional view of the top plate of the present invention; Figure 5 is a three-dimensional structural cross-sectional view of the sliding plate of the present invention; Figure 6 It is a three-dimensional structural cross-sectional view of the handle of the present invention; Figure 7 It is a three-dimensional structural cross-sectional view of the rotating shell of the present invention; Figure 8 It is a three-dimensional structural cross-sectional view of the sliding ring of the present invention.

[0017] In the figure: 10-cabinet, 11-sealing cover, 12-fixing ring, 13-first rotating rod, 14-bottom plate, 15-top plate, 16-fixing cylinder, 17-sliding plate, 18-second rotating rod, 19-guide frame, 20-fixing pin, 21-spiral groove, 30-pressing plate, 31-fixing column, 32-fixing plate, 33-sliding pin, 40-connecting frame, 41-first fixed shell, 42-rotating shell, 43-connecting shell, 44-handle, 45-second fixed shell, 46-sliding member, 50-elastic capsule, 51-sliding ring, 52-ratchet, 53-limiting member. DETAILED DESCRIPTION

[0018] The present invention will be further described below in conjunction with specific embodiments. The illustrative embodiments and descriptions of the present invention are used to explain the present invention but are not intended to limit the present invention.

[0019] The capping process of a capping type freeze dryer usually occurs before the freeze drying step. Specifically, it is carried out after the medicine is pre-frozen and before the sublimation drying stage begins. At this time, the medicine has been frozen, but the sublimation step of removing moisture has not yet begun. At this time, the samples (vials and stoppers) in the freeze dryer need to be capped. During the capping process, since the existing method of pressing down layer by layer is adopted, the time required for the capping step will be increased, and the vacuum degree around the samples that have not been capped will be increased, thereby affecting the efficiency and uniformity of ice crystal sublimation. The present invention adopts a synchronous extrusion method, so that during the capping process, the multiple layers of cover plates can move synchronously and the distance between two adjacent cover plates can be shortened synchronously, so as to achieve the effect of uniformly extruding each layer of samples.

[0020] See also Figure 1-Figure 5 , equipment for freeze-drying process, including: a cabinet 10, the cabinet 10 is detachably mounted with a sealing cover 11; a fixing ring 12, which is detachably mounted on the cabinet 10, the fixing ring 12 is rotatably connected with at least two first rotating rods 13, all the first rotating rods 13 are rotatably connected with a bottom plate 14 and a top plate 15, the top plate 15 is located above the bottom plate 14 and is fixed with a sealing ring that is sealed with the sealing cover 11, a linear array of fixed cylinders 16 are slidably connected to the first rotating rods 13, the fixed cylinders 16 of the same height are fixed with a sliding plate 17, the top plate 15 is rotatably connected with a second rotating rod 18, the first rotating rod 13 and the second rotating rod 18 are connected through a sprocket chain transmission; fixing pins 20, the number of which is the same as the fixing cylinder 16, fixedly connected to the adjacent fixing cylinder 1 6, a linear array of spiral grooves 21 is provided on the first rotating rod 13, and the fixing pin 20 is pressed and matched with the adjacent spiral grooves 21; the initial position of the fixing pin 20 is located in the middle and lower part of the adjacent spiral grooves 21, and a gap is left between the top plate 15 and the adjacent fixed cylinder 16; the pitch of the linear array of spiral grooves 21 on the same first rotating rod 13 increases in a step-like manner from bottom to top, and the pitch of the spiral grooves 21 on the same first rotating rod 13 is equidistantly distributed; the fixed cylinders 16 of the same height are slidably connected with a pressing plate 30, which is used to squeeze the sample, and a spring is fixed between the pressing plate 30 and the adjacent sliding plate 17, and a linear array of limiting components is provided in the sealing cover 11, and the limiting components are used to limit the adjacent pressing plates 30.

[0021] In the above scheme, it is intended to solve the problem that the existing layer-by-layer pressing method will prolong the time required for the capping step and increase the vacuum degree around the samples that have not been capped. The samples mentioned in the present invention are existing syringe bottles and stoppers. A vacuum pump is arranged on the left side of the cabinet 10 to form a vacuum environment in the sealing cover 11. The sealing cover 11 is made of a transparent hard material. The sealing strip can be installed at the position where the lower side of the sealing cover 11 and the upper side of the cabinet 10 fit according to actual conditions to ensure the sealing between the cabinet 10 and the sealing cover 11. There are two first rotating rods 13 in the present invention. The two first rotating rods 13 are located on the left and right sides of the middle of the fixing ring 12, the bottom plate 14 and the top plate 15 and are symmetrically distributed. The central axis of the first rotating rod 13 is parallel to the central axis of the fixing ring 12, the bottom plate 14, the top plate 15 and the sealing cover 11. The central axis of the fixing ring 12, the central axis of the bottom plate 14, the central axis of the top plate 15 and the central axis of the sealing cover 11 all coincide.

[0022] like Figure 3 As shown, the rear sides of the fixing ring 12, the top plate 15 and the bottom plate 14 are fixedly connected with a limiting rod which passes through the rear sides of all the sliding plates 17 and all the pressure plates 30. The limiting rod located at the rear side of the fixing ring 12 and the two first rotating rods 13 located in the middle of the fixing ring 12 form an isosceles triangle, which is used to prevent the sliding plate 17 and the three first rotating rods 13 from eccentric wear. The use of two first rotating rods 13 and the limiting rod can also facilitate the placement and removal of the tray. In the present invention, there are two sealing rings on the outside of the top plate 15 to ensure the sealing inside the sealing cover 11. The fixed cylinders 16 in the linear array are three vertically distributed, and the lengths of the three fixed cylinders 16 are different. From bottom to top, the lengths of the three fixed cylinders 16 gradually increase to adapt to the lengths of adjacent spiral grooves 21. The tray will be placed on the two sliding plates 17 on the lower side. The gap between the top plate 15 and the adjacent fixed cylinders 16 is used to reserve space for all the sliding plates 17 to move upward. The space is cleared and all the pressing plates 30 can move upward, so that the device can be applied to larger cillin bottles, increasing the application range of the device. The number of fixing pins 20 in the adjacent fixing cylinders 16 is two in a circular array in the present invention. The number of spiral grooves 21 in a linear array on the two first rotating rods 13 on the front side is three groups in the present invention, and the number of spiral grooves 21 in each group is two, and the two spiral grooves 21 are distributed in a circular array. There are two fixing pins 20 and two adjacent spiral grooves 21, which are used to ensure the stability of the adjacent fixed cylinders 16 during movement. Under the action of the equidistant distribution of the pitch of the linear array spiral grooves 21 on the first rotating rod 13, the three sliding plates 17 drive the adjacent pressing plates 30 to move downward in a manner of proportionally reducing the distance, so as to achieve the effect of uniformly squeezing each layer of samples with the same squeezing force. The position of the adjacent pressing plates 30 is limited by the limit assembly to avoid excessive squeezing of the samples, resulting in a reduction in the structural strength of the samples.

[0023] See also Figure 2A plurality of guide frames 19 are fixedly connected to the upper side of the cabinet 10 , and a plurality of balls are spherically connected to the opposite sides of the plurality of guide frames 19 , and the plurality of balls on the guide frames 19 are in contact with and cooperate with the sealing cover 11 .

[0024] In the above scheme, the number of guide frames 19 in the present invention is at least two symmetrical ones, which are used to ensure the stability of the sealing cover 11 during movement. The facing sides of the guide frames 19 are arc-shaped, which are used to fit the curvature of the outer side of the sealing cover 11. The distance between the facing sides of the guide frames 19 is greater than the diameter of the sealing cover 11, which is used to provide space for adjacent balls to rotate. The balls on the guide frames 19 are located on the front and rear sides thereof, which are used to provide vertical guidance for the sealing cover 11. The center of the balls on the guide frames 19 is located inside the guide frames 19, which is used to prevent the balls from moving out of the adjacent guide frames 19 during rotation.

[0025] See also Figure 4 and Figure 5 The limiting assembly includes: a fixed column 31, which is fixedly connected to the adjacent pressure plate 30 and slidably cooperates with the adjacent sliding plate 17, and a limiting groove is arranged on the fixed column 31; a fixed plate 32, which is fixedly connected to the adjacent sliding plate 17, and the fixed plate 32 is slidably connected with a sliding pin 33, and the sliding pin 33 is limitedly cooperated with the limiting groove on the adjacent fixed column 31, and a tension spring is fixedly connected between the sliding pin 33 and the adjacent fixed plate 32, and a driving assembly is arranged on the top plate 15, and the driving assembly is used to drive the second rotating rod 18 to rotate.

[0026] In the above scheme, the limiting groove on the fixed column 31 is directed away from the central axis of the sealing cover 11 to facilitate the subsequent unlocking of the fixed column 31. The distance between the fixed column 31 and the central axis of the sealing cover 11 is smaller than the distance between the adjacent fixed plate 32 and the central axis of the sealing cover 11. When the sliding pin 33 is not inserted into the limiting groove on the adjacent fixed column 31, the tension spring adjacent to the sliding pin 33 is in a stretched state.

[0027] See also Figure 3 and Figure 6-Figure 8The driving assembly includes: a connecting frame 40, which is fixed to the top plate 15, and a first fixed shell 41 is fixed to the side of the connecting frame 40 away from the top plate 15. The first fixed shell 41 is rotatably connected to a rotating shell 42, and the rotating shell 42 is fixed to a connecting shell 43. The rotating shell 42 is located between the first fixed shell 41 and the connecting shell 43, and the connecting shell 43 is fixed to a handle 44 that rotatably cooperates with the second rotating rod 18; a plurality of second fixed shells 45 are all fixed to the connecting shell 43, and the second fixed shell 45 is slidably connected to a sliding member 46 that slidably cooperates with the connecting shell 43, and a tension spring is fixed between the sliding member 46 and the adjacent second fixed shell 45, and the second rotating rod 18 is provided with a plurality of blind holes, and the sliding member 46 is limitedly cooperated with the adjacent blind holes on the second rotating rod 18, and the sliding member 46 is fixed with a symmetrical and linear array of balls, and the balls on the sliding member 46 are in contact with and cooperate with the adjacent blind holes on the second rotating rod 18.

[0028] In the above scheme, there are two connecting frames 40 in the present invention, which are used to ensure the stability of the first fixed shell 41. The first fixed shell 41 is connected to the rotating shell 42 in a limited rotational connection, so that the rotating shell 42 can rotate along the central axis of the first fixed shell 41 during the rotation process, so as to avoid eccentric rotation of the rotating shell 42, which leads to eccentric wear between the rotating shell 42 and the first fixed shell 41. There is no friction between the handle 44 and the second rotating rod 18. There are four second fixed shells 45 in the present invention (the second fixed shells 45 are at least two, which are used to ensure the stability of the second rotating rod 18 after the adjacent sliding members 46 are inserted into the adjacent blind holes on the second rotating rod 18). After the sliding member 46 is inserted into the adjacent blind hole on the second rotating rod 18, the handle 44 can drive the second rotating rod 18 to rotate clockwise (viewed from top to bottom) through all the sliding members 46. At this time, the tension spring adjacent to the sliding member 46 is in an unstretched state. After the sliding member 46 is no longer inserted into the adjacent blind hole on the second rotating rod 18, the handle 44 rotates idly along the second rotating rod 18. At this time, the tension spring adjacent to the sliding member 46 is in a stretched state. Taking the sliding member 46 on the left as an example, the symmetrical and linear array of balls are respectively located on the front and rear sides of the adjacent sliding members 46, so that the sliding member 46 can slide in or out of the blind hole on the second rotating rod 18 smoothly.

[0029] See also Figure 3 and Figure 4 and Figure 6-Figure 8 The sliding plate 17 close to the top plate 15 is fixedly connected with an elastic bag 50, and the elastic bag 50 is squeezed and matched with the adjacent pressure plate 30. The elastic bag 50 is fixedly connected to the first fixed shell 41 and is connected with a connecting pipe. The connecting pipe runs through the adjacent sliding plate 17 and the top plate 15. The first fixed shell 41 is connected with the rotating shell 42, and the rotating shell 42 is connected with several second fixed shells 45. Hydraulic oil is stored in the elastic bag 50, the adjacent connecting pipe, the first fixed shell 41, the rotating shell 42 and the several second fixed shells 45; the sliding ring 51 is slidably connected in the rotating shell 42.

[0030] In the above scheme, the elastic bag 50 is located at the bottom of the upper sliding plate 17. When the elastic bag 50 is squeezed by the adjacent pressing plate 30 (this situation will occur when the sample is pressed), the connecting tube adjacent to the elastic bag 50 is a hose, and the length of the hose is greater than the length shown in the figure (the connecting tube has residues during use), which is used to enable the sliding plate 17 located on the upper side to drive the elastic bag 50 and the connecting tube to move downward, so that the remaining part of the connecting tube can be pulled.

[0031] See also Figure 6 and Figure 7 The second rotating rod 18 is fixedly connected with a ratchet 52, and the ratchet 52 is located between the handle 44 and the connecting shell 43. The handle 44 is rotatably connected to one side close to the connecting shell 43 with a plurality of limit members 53. A torsion spring is arranged between the limit member 53 and the handle 44, and the plurality of limit members 53 are limitedly matched with the ratchet 52.

[0032] In the above scheme, there are two limit members 53 in the present invention, which are used to enable any one of the two limit members 53 to contact the ratchet 52 when the handle 44 rotates counterclockwise, thereby driving the ratchet 52 to rotate counterclockwise. The limit member 53 is arc-shaped. After all the sliding members 46 no longer contact the adjacent blind holes on the second rotating rod 18, the handle 44 will not drive the ratchet 52 to rotate through the two limit members 53 when it rotates clockwise.

[0033] Before using the device to freeze-dry samples, the staff will first pre-freeze the samples, and then place the pre-frozen samples on the trays in sequence. The staff will then move the sealing cover 11 upwards, and the sealing cover 11 will move upwards along the balls in the two guide frames 19 during the upward movement. After the sealing cover 11 is removed, the staff will place multiple trays on the bottom plate 14 and the upper side of the two sliding plates 17 at the lower side, that is, Figure 3 Status in.

[0034] After placing multiple trays, the staff will replace the sealing cover 11 on the upper side of the cabinet 10. During the process of replacing the sealing cover 11, the outer side of the sealing cover 11 moves downward along the ball bearings on the two guide frames 19, and the inner side of the sealing cover 11 moves downward along the sealing ring on the top plate 15, thereby realizing vertical guiding of the sealing cover 11 to prevent the sealing cover 11 from colliding with adjacent parts during the placement process, thereby affecting the placement of the sample.

[0035] When the lower side of the sealing cover 11 is attached to the upper side of the cabinet 10 , the cabinet 10 performs freeze-drying on the sample, and the environment in the sealing cover 11 is controlled by a vacuum pump during the freeze-drying process.

[0036] After the freeze-drying of the sample is completed, the vacuum pump is no longer in effect, and then the staff injects gas into the sealing cover 11 to make the sealing cover 11 at atmospheric pressure. Then the staff rotates the handle 44 clockwise, and the handle 44 drives the second rotating rod 18 to rotate through the connecting shell 43 and all the sliding parts 46. The second rotating rod 18 transmits power to the two first rotating rods 13 through two sets of sprocket chains, so that the two first rotating rods 13 rotate along the top plate 15 and the fixed ring 12. Now take the rotation process of one of the spiral grooves 21 on one of the first rotating rods 13 as an example. During the rotation of the first rotating rod 13, the spiral groove 21 squeezes the adjacent fixing pin 20, so that the adjacent fixing pin 20 drives the adjacent sliding plate 17 and the adjacent pressing plate 30 to move downward through the adjacent fixing cylinder 16.

[0037] In the process of capping the samples, the three sliding plates 17 drive the adjacent pressing plates 30 to move downward. Under the effect of the equidistant pitch distribution of the linear array spiral grooves 21 on the first rotating rod 13, the three sliding plates 17 drive the adjacent pressing plates 30 to move downward in an equidistant manner, so that each layer of samples can be squeezed by the adjacent pressing plates 30. Taking the movement process of the upper pressing plate 30 as an example, when the pressing plate 30 moves downward until its lower side contacts the plug of the sample, the lower sides of the two lower pressing plates 30 also contact the plug of the sample. When the pressing plate 30 continues to move downward, the effect of evenly squeezing each layer of samples with the same squeezing force is achieved.

[0038] When the stopper in the sample is squeezed into the vial by the adjacent pressing plate 30, the pressing plate 30 adheres to the sample and stops moving downward. The sliding plate 17 continues to move downward, which will reduce the distance between it and the adjacent pressing plate 30 (the spring adjacent to the pressing plate 30 is squeezed in this process). Taking the movement process of the upper pressing plate 30 as an example, during the process of shortening the distance between the pressing plate 30 and the adjacent sliding plate 17, the pressing plate 30 adheres to the sample and thus remains stationary. During the movement of the sliding plate 17, the elastic bag 50 is squeezed and the adjacent fixed column 31 is moved relative to the adjacent sliding plate 17.

[0039] During the squeezing of the elastic bag 50, the hydraulic oil therein is transported to the first fixed shell 41 through the adjacent connecting pipe, thereby increasing the pressure in the first fixed shell 41 and the rotating shell 42, thereby causing the sliding ring 51 to move upward and squeeze the hydraulic oil in the rotating shell 42 into all the second fixed shells 45, increasing the pressure in all the second fixed shells 45, and causing the adjacent sliding member 46 in the second fixed shell 45 to move to the side away from the second rotating rod 18 (the adjacent tension spring is stretched during the movement of the sliding member 46), thereby causing the sliding member 46 to gradually break away from the contact with the adjacent blind hole in the second rotating rod 18.

[0040] When the fixed column 31 slides until the central axis of the adjacent sliding pin 33 coincides with the central axis of the limiting groove in the adjacent fixed column 31, the sliding pin 33 is inserted into the limiting groove on the adjacent fixed column 31, thereby limiting the distance between the pressure plate 30 and the adjacent sliding plate 17 and protecting the spring between the pressure plate 30 and the adjacent sliding plate 17. During this process, the hydraulic oil in the elastic bag 50 enters all the second fixed shells 45, and all the sliding members 46 have moved to break away from the contact with the blind hole on the second rotating rod 18. At this time, the staff continues to clockwise When the needle rotates the handle 44, the handle 44, the connecting shell 43 and their attached parts all rotate idly around the second rotating rod 18 (the two limit members 53 will not drive the ratchet 52 to rotate when rotating clockwise around the ratchet 52). At this time, the staff will no longer rotate the handle 44, and the distance between the pressing plate 30 and the adjacent sliding plate 17 will no longer be shortened, so as to avoid excessive movement of the pressing plate 30 due to excessive rotation of the second rotating rod 18, resulting in excessive squeezing of the sample, thereby affecting the quality of the sample itself (excessive squeezing may cause the vial to rupture or the sealing failure of the stopper).

[0041] After completing the step of capping the sample, the cabinet 10 performs sublimation drying treatment on the sample, and the specific steps are consistent with the prior art.

[0042] After completing the sublimation drying process of the sample, the staff rotates the handle 44 counterclockwise, and the handle 44 drives the ratchet 52 and the second rotating rod 18 to rotate counterclockwise through the two limit members 53. The second rotating rod 18 transmits the power to the two first rotating rods 13 through the two sets of sprocket chains, so that the two first rotating rods 13 rotate in the opposite direction. Under the action of the spiral groove 21 and the adjacent fixing pin 20, the fixing pin 20 drives the adjacent sliding plate 17 and its accessory parts to move upward synchronously through the adjacent fixing cylinder 16, and the pressing plate 30 is separated from the contact with the sample.

[0043] When the distance between the sample and the adjacent pressing plate 30 is sufficient to allow the sample to be removed, the staff will stop turning the handle 44, and all the fixed cylinders 16 will stop moving. The staff will then remove the sealing cover 11 and take out the trays one by one, thereby completing the freeze-drying process of the sample.

[0044] After the staff takes out the sample, they pull the sliding pin 33 to the right (stretching the adjacent tension spring during the movement of the sliding pin 33) so that the sliding pin 33 releases the limit on the adjacent fixed column 31. Under the action of the adjacent spring, the pressure plate 30 drives the adjacent fixed column 31 to move downward along the adjacent sliding plate 17, thereby realizing the reset movement of the pressure plate 30.

[0045] During the resetting movement of the pressure plate 30 on the upper side, the elastic bag 50 is no longer squeezed. The elastic bag 50 is reset under the action of its own elastic force and extracts the hydraulic oil in the first fixed shell 41 through the adjacent connecting pipe, reducing the pressure in the first fixed shell 41 and the rotating shell 42, so that the sliding ring 51 moves downward and reduces the pressure in the rotating shell 42 and the second fixed shell 45. Under the action of the adjacent tension springs of all the sliding members 46, all the sliding members 46 move toward each other and are gradually inserted into the adjacent blind holes on the second rotating rod 18. The subsequent processing process of the sample can be repeated as described above.

[0046] In addition, the present invention also provides a method for using the freeze-drying process equipment, comprising the following steps: The first step is to pre-freeze the sample before freeze-drying, remove the sealing cover 11, and then place the sample on the tray, and then put multiple trays into the required positions for work; In the second step, after the tray is placed, the sealing cover 11 is placed back on the cabinet 10, and the cabinet 10 performs freeze-drying on the sample; Step 3: After the freeze-drying is completed, the handle 44 is rotated, and the handle 44 drives the second rotating rod 18 to rotate through the connecting shell 43 and a plurality of sliding members 46, and the second rotating rod 18 transmits the power to the first rotating rod 13 through the sprocket chain; Step 4: During the rotation of the first rotating rod 13, the spiral groove 21 squeezes the adjacent fixing pins 20, so that the pressing plate 30 performs a capping process on the sample; Step 5: During the process of capping the sample, the pressing plate 30 is made to fit with the sample, and the sliding plate 17 continues to move to squeeze the elastic capsule 50 and reduce the distance between it and the adjacent pressing plate 30; Step 6: After the elastic bag 50 is squeezed, the hydraulic oil is delivered to all the second fixed shells 45, and the connection between all the sliding members 46 and the second rotating rod 18 is disconnected. After all the sliding members 46 are no longer in contact with the adjacent blind holes in the second rotating rod 18, the handle 44 rotates idle and does not drive the second rotating rod 18 to rotate synchronously, thereby completing the pressing of the sample, and then the cabinet 10 performs sublimation drying treatment on the sample; Step 7: After the sublimation drying process of the sample is completed, the handle 44 is rotated in the reverse direction, so that the first rotating rod 13 rotates in the reverse direction, and the adjacent fixing pin 20 is squeezed through the spiral groove 21, so that the fixing cylinder 16 drives the adjacent sliding plate 17 to reset and move, and the pressing plate 30 is separated from the contact with the sample; Step 8: After the pressing plate 30 is no longer in contact with the sample, the sealing cover 11 is removed, and the trays are taken out in sequence, thereby completing the sublimation drying process of the sample; In the ninth step, after the sample is taken out, the limit of the adjacent fixed column 31 is released by the sliding pin 33, so that the pressure plate 30 no longer squeezes the elastic bag 50, and all the sliding members 46 are moved to be inserted into the adjacent blind holes on the second rotating rod 18 to complete the reset of the sliding members 46.

[0047] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. Equipment used for freeze-drying process, including: A cabinet (10), wherein the cabinet (10) is detachably mounted with a sealing cover (11); It is characterized by further comprising: A fixing ring (12) is detachably mounted on the cabinet (10), the fixing ring (12) is rotatably connected to at least two first rotating rods (13), all of the first rotating rods (13) are rotatably connected to a bottom plate (14) and a top plate (15), the top plate (15) is located above the bottom plate (14) and is fixedly connected to a sealing ring that seals with the sealing cover (11), a linear array of fixing cylinders (16) are slidably connected to the first rotating rods (13), the fixing cylinders (16) of the same height are fixedly connected to a sliding plate (17), the top plate (15) is rotatably connected to a second rotating rod (18), and the first rotating rod (13) and the second rotating rod (18) are connected via a sprocket chain transmission; The fixing pins (20) are the same in number as the fixing tubes (16) and are fixedly connected to adjacent fixing tubes (16). The first rotating rod (13) is provided with a linear array of spiral grooves (21), and the fixing pins (20) are pressed and matched with adjacent spiral grooves (21).

2. The freeze-drying process according to claim 1, characterized in that The initial position of the fixing pin (20) is located at the middle and lower part of the adjacent spiral groove (21), and a gap is left between the top plate (15) and the adjacent fixing cylinder (16).

3. The freeze-drying process according to claim 2, characterized in that: A plurality of guide frames (19) are fixedly connected to the upper side of the cabinet (10), and a plurality of balls are spherically connected to the opposite sides of the plurality of guide frames (19), and the plurality of balls on the guide frames (19) are in contact with and cooperate with the sealing cover (11).

4. The freeze-drying process according to claim 3, characterized in that: The pitches of the spiral grooves (21) in the linear array on the same first rotating rod (13) increase in a step-like manner from bottom to top, and the pitches of the spiral grooves (21) on the same first rotating rod (13) are equidistantly distributed.

5. The freeze-drying process according to claim 4, characterized in that: The fixed cylinders (16) of equal height are slidably connected to a pressing plate (30), the pressing plate (30) being used to press the sample, a spring being fixedly connected between the pressing plate (30) and the adjacent sliding plate (17), and a linear array of limiting components being arranged in the sealing cover (11), the limiting components being used to limit the adjacent pressing plates (30).

6. The freeze-drying process according to claim 5, characterized in that The limiting component comprises: A fixed column (31) is fixedly connected to the adjacent pressing plate (30) and slidably cooperates with the adjacent sliding plate (17), and a limiting groove is provided on the fixed column (31); The fixed plate (32) is fixedly connected to the adjacent sliding plate (17); the fixed plate (32) is slidably connected with a sliding pin (33); the sliding pin (33) is limitedly matched with a limiting groove on the adjacent fixed column (31); a tension spring is fixedly connected between the sliding pin (33) and the adjacent fixed plate (32); a driving assembly is arranged on the top plate (15); the driving assembly is used to drive the second rotating rod (18) to rotate.

7. The freeze-drying process according to claim 6, characterized in that The drive assembly comprises: a connecting frame (40) fixedly connected to the top plate (15); a first fixed shell (41) fixedly connected to a side of the connecting frame (40) away from the top plate (15); the first fixed shell (41) being rotatably connected to a rotating shell (42); the rotating shell (42) being fixedly connected to a connecting shell (43); the rotating shell (42) being located between the first fixed shell (41) and the connecting shell (43); and the connecting shell (43) being fixedly connected to a handle (44) rotatably matched with the second rotating rod (18); A plurality of second fixed shells (45) are fixedly connected to the connecting shell (43); the second fixed shell (45) is slidably connected to a sliding member (46) that slidably cooperates with the connecting shell (43); a tension spring is fixedly connected between the sliding member (46) and an adjacent second fixed shell (45); the second rotating rod (18) is provided with a plurality of blind holes; the sliding member (46) is limitedly cooperated with adjacent blind holes on the second rotating rod (18); the sliding member (46) is fixedly connected to symmetrical and linearly arrayed balls; the balls on the sliding member (46) are in contact and cooperate with adjacent blind holes on the second rotating rod (18).

8. The freeze-drying process according to claim 7, characterized in that: The sliding plate (17) close to the top plate (15) is fixedly connected with an elastic bag (50), the elastic bag (50) is pressed and matched with the adjacent pressing plate (30), the elastic bag (50) is fixedly connected and connected with the first fixed shell (41) by a connecting pipe, the connecting pipe passes through the adjacent sliding plate (17) and the top plate (15), the first fixed shell (41) is connected with the rotating shell (42), the rotating shell (42) is connected with a plurality of the second fixed shells (45), and hydraulic oil is stored in the elastic bag (50), the adjacent connecting pipe, the first fixed shell (41), the rotating shell (42) and the plurality of the second fixed shells (45); A sliding ring (51) is slidably connected inside the rotating shell (42).

9. The freeze-drying process according to claim 8, characterized in that: The second rotating rod (18) is fixedly connected with a ratchet (52), and the ratchet (52) is located between the handle (44) and the connecting shell (43). A side of the handle (44) close to the connecting shell (43) is rotatably connected with a plurality of limiting members (53), a torsion spring is provided between the limiting member (53) and the handle (44), and the plurality of limiting members (53) are all in limiting cooperation with the ratchet (52).

10. A method for using a freeze-drying process device, which is completed by using the freeze-drying process device according to claim 9, characterized in that: The method for freeze-drying a sample comprises the following steps: In the first step, the sample is pre-frozen before freeze-drying, the sealing cover (11) is removed, and the sample is then placed on a tray, and then multiple trays are placed in the required positions for the work; In the second step, after the tray is placed, the sealing cover (11) is placed back on the cabinet (10), and the cabinet (10) performs freeze-drying on the sample; The third step is to rotate the handle (44) after the freeze-drying is completed. The handle (44) drives the second rotating rod (18) to rotate through the connecting shell (43) and a plurality of sliding members (46). The second rotating rod (18) transmits power to the first rotating rod (13) via the sprocket chain. Step 4: During the rotation of the first rotating rod (13), the adjacent fixing pins (20) are squeezed through the spiral groove (21), so that the pressing plate (30) performs a pressing process on the sample; Step 5: During the process of pressing the sample, the pressing plate (30) is made to fit the sample, and the sliding plate (17) continues to move to squeeze the elastic bag (50) and reduce the distance between the elastic bag (50) and the adjacent pressing plate (30); In the sixth step, after the elastic bag (50) is squeezed, the hydraulic oil is delivered to all the second fixed shells (45), and the connection between all the sliding parts (46) and the second rotating rod (18) is disconnected. After all the sliding parts (46) are no longer in contact with the adjacent blind holes in the second rotating rod (18), the handle (44) rotates idle and does not drive the second rotating rod (18) to rotate synchronously, thereby completing the pressing of the sample, and then the cabinet (10) performs sublimation drying treatment on the sample; Step 7: After the sublimation drying process of the sample is completed, the handle (44) is rotated in the reverse direction, so that the first rotating rod (13) rotates in the reverse direction, and the adjacent fixing pin (20) is squeezed through the spiral groove (21), so that the fixing cylinder (16) drives the adjacent sliding plate (17) to reset and move, and the pressing plate (30) is separated from the contact with the sample; Step 8: After the pressing plate (30) is no longer in contact with the sample, the sealing cover (11) is removed and the trays are taken out in sequence, thereby completing the sublimation drying process of the sample; In the ninth step, after the sample is taken out, the limiting position of the adjacent fixed column (31) is released by the sliding pin (33), so that the pressure plate (30) no longer squeezes the elastic bag (50), and all the sliding members (46) are moved to be inserted into the adjacent blind holes on the second rotating rod (18), so as to complete the reset of the sliding members (46).

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