Apparatus and method for determining silicone oil leakage and residue in a lyophilizer pre-chamber

Abstract

The application provides a device and method for judging silicone oil leakage and residue of a pre-chamber of a freeze dryer, which comprises the following steps: after a batch of freeze drying tasks is completed by the freeze dryer, a device for judging silicone oil leakage and residue of the pre-chamber of the freeze dryer is used to perform silicone oil background detection; when silicone oil is detected in the silicone oil background detection, the pre-chamber of the freeze dryer is cleaned according to a production procedure, and after the cleaning, second silicone oil detection is performed in a pressure maintaining stage; and artificial intelligence algorithm is used to perform deep analysis on the detection data, and silicone oil leakage and residue are automatically identified, so that the accuracy and reliability of the judgment are improved. According to the application, silicone oil existing in the pre-chamber of the freeze dryer can be quickly and accurately detected without affecting production, meanwhile, the sterile environment of the pre-chamber of the freeze dryer is ensured, product quality problems and equipment failures are avoided, and the operation stability and reliability of the freeze dryer are improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of freeze dryer detection, in particular to a device and method for judging the leakage and residue of silicone oil in the pre-chamber of a freeze dryer. BACKGROUND

[0002] Freeze dryers are widely used in the pharmaceutical, food and other industries. However, the leakage and residue of silicone oil in the pre-chamber of a freeze dryer cannot be ignored. This not only leads to product contamination and quality degradation, but also causes a series of serious consequences, even causing equipment failure, increasing maintenance costs, and affecting production progress.

[0003] Currently, some existing methods for detecting the leakage and residue of silicone oil in the pre-chamber of a freeze dryer have many significant shortcomings. First, many detection methods perform poorly in terms of detection speed. Spectroscopy and sensors can only detect specific substances, with slow reaction speed and insufficient detection limit. Chromatography can be used for quantitative analysis, but the detection period is long. In today's fast-paced production environment, time is efficiency, and some detection methods require a long time to complete sample collection, analysis and result derivation, making it difficult to meet the urgent need for rapid detection on the production line. This leads to stagnation of the production process, reducing overall production efficiency.

[0004] Furthermore, the operation process of some detection methods is extremely complex. This not only requires a high level of professional technical expertise from the detection personnel, but also requires them to undergo long-term training and practice to master it. This undoubtedly increases labor costs, and in actual operation, complex steps are prone to human error, further affecting the accuracy and reliability of the detection results.

[0005] In addition, the detection equipment relied upon by some detection methods is expensive and has high maintenance costs. This is a heavy economic burden for enterprises, especially for small and medium-sized enterprises, which may not be able to adopt these detection methods due to cost issues, thereby facing greater risks in production.

[0006] In view of this, it is particularly critical to timely and accurately judge the leakage and residue of silicone oil in the pre-chamber of a freeze dryer. This not only ensures high-quality production of products, but also effectively prevents equipment failure and ensures the stability and efficiency of the production process. SUMMARY

[0007] In view of the defects in the prior art, the purpose of the present application is to provide a device and method for judging the leakage and residue of silicone oil in the pre-chamber of a freeze dryer.

[0008] The device for judging the leakage and residue of silicone oil in the pre-chamber of a freeze dryer comprises a silicone oil detection device, an air pipe, a stainless steel hose, a pneumatic diaphragm valve, a pre-chamber of a freeze dryer, a first vacuum gauge, a high-pressure air source of a freeze dryer, a host computer, a second electromagnetic valve, a first electromagnetic valve, a silicone oil detection cavity, a second vacuum gauge, an alarm device, a molecular pump, a diaphragm pump, and a verification hole.

[0009] The silicone oil detection cavity is connected to the molecular pump, the molecular pump is connected to the diaphragm pump, and the diaphragm pump and the molecular pump enable the silicone oil detection cavity to have a negative pressure environment.

[0010] The second vacuum gauge is installed on the silicone oil detection cavity and displays the vacuum degree of the silicone oil detection cavity.

[0011] One end of the first electromagnetic valve is connected to the silicone oil detection cavity through a stainless steel straight pipe, and the other end of the first electromagnetic valve is connected to the pneumatic diaphragm valve through a stainless steel hose.

[0012] The pneumatic diaphragm valve is fixed to the verification hole of the pre-chamber of the freeze dryer.

[0013] The host computer in the silicone oil detection device is installed with silicone oil detection control software and is responsible for silicone oil detection data processing; the host computer controls the opening and closing of the first electromagnetic valve and the second electromagnetic valve.

[0014] One end of the second electromagnetic valve is connected to the high-pressure air source of the freeze dryer through an air pipe, and the other end of the second electromagnetic valve is connected to the pneumatic diaphragm valve air path control interface through an air pipe; the second electromagnetic valve controls the opening and closing of the pneumatic diaphragm valve.

[0015] The first vacuum gauge is connected to the pre-chamber of the freeze dryer and displays the vacuum degree in the pre-chamber of the freeze dryer.

[0016] The alarm device is connected to the host computer, and when the silicone oil detection value exceeds the set warning value, the alarm device issues an alarm.

[0017] Preferably, the second electromagnetic valve and the first electromagnetic valve have an interlocking function; when the vacuum degree of the pre-chamber of the freeze dryer is higher than 50 pa during the silicone oil detection process, the host computer issues an instruction to close the second electromagnetic valve to protect the silicone oil detection device; when the vacuum degree of the silicone oil detection cavity is higher than 0.1 pa during the silicone oil detection process, the host computer issues an instruction to close the second electromagnetic valve and the first electromagnetic valve to prevent external gas from polluting the pre-chamber of the freeze dryer.

[0018] Preferably, the molecular pump is installed on the silicone oil detection cavity through a fastener, the diaphragm pump is connected to the molecular pump through an air pipe, the diaphragm pump extracts a first-stage vacuum for the silicone oil detection cavity, and the molecular pump extracts a second-stage vacuum for the silicone oil detection cavity.

[0019] Preferably, the second vacuum gauge is connected to the silicone oil detection cavity through a KF16 clamp and measures the vacuum degree value of the silicone oil detection cavity.

[0020] Preferably, the first electromagnetic valve is connected to the silicone oil detection cavity through a stainless steel straight pipe, the opening and closing of the first electromagnetic valve is controlled by the host, and the first electromagnetic valve is opened during the detection process to allow silicone molecules to enter the silicone oil detection cavity for detection.

[0021] Preferably, one end of the pneumatic diaphragm valve is fixed to the verification hole of the front box of the freeze dryer through an ISO38 clamp, and the other end of the pneumatic diaphragm valve is connected to the first electromagnetic valve through a KF16 stainless steel corrugated pipe to form a sample injection channel.

[0022] Preferably, one end of the second electromagnetic valve is connected to the high-pressure gas source of the freeze dryer through a 6mm air pipe, and the other end of the second electromagnetic valve is connected to the pneumatic diaphragm valve through a 6mm air pipe, and the second electromagnetic valve and the pneumatic diaphragm valve are synchronously opened and closed, and when the vacuum degree of the silicone oil detection cavity is lower than 0.09Pa, the host sends an instruction to open the second electromagnetic valve, and the pneumatic diaphragm valve is opened to perform silicone oil detection.

[0023] Preferably, the first vacuum gauge is installed on the front box of the freeze dryer through a clamp to detect the vacuum degree of the front box of the freeze dryer; and when the vacuum degree of the first vacuum gauge is greater than 50Pa during the silicone oil detection process, the host sends an instruction to close the second electromagnetic valve and the first electromagnetic valve, so that the detection device in the silicone oil detection cavity is closed.

[0024] Preferably, the alarm device sends an alarm when the vacuum degree of the silicone oil detection cavity is greater than 0.1Pa during the silicone oil detection process, and sends an alarm when the vacuum degree of the first vacuum gauge is greater than 50Pa.

[0025] The method for judging silicone oil leakage and residue of the front box of the freeze dryer provided by the application comprises the following steps:

[0026] The device for judging silicone oil leakage and residue of the front box of the freeze dryer is connected, the silicone oil detection control software is opened, the host controls the opening of the first electromagnetic valve, and the vacuumizing program of the freeze dryer is started;

[0027] When the vacuum degree of the silicone oil detection cavity is less than 0.05Pa and the vacuum degree of the front box of the freeze dryer is less than 50Pa, the host controls the opening of the second electromagnetic valve to perform silicone oil detection;

[0028] The freeze drying area of the freeze dryer is 10 square meters or less, and the heating program of the freeze dryer is not started; and the freeze drying area of the freeze dryer is more than 10 square meters, and the freeze dryer is heated and pressure maintained.

[0029] After completing a batch of freeze drying tasks, the device for judging silicone oil leakage and residue of the front box of the freeze dryer is used for background silicone oil detection, silicone oil composition is detected in the background silicone oil detection, the front box of the freeze dryer is cleaned according to the production program, and the second silicone oil composition detection is performed in the pressure maintaining stage after the cleaning; and the two silicone oil detection data are introduced into a preset machine learning algorithm training model, and the control software judges the silicone oil leakage and residue according to different freeze dryer models, working conditions and historical data.

[0030] Compared with the prior art, the present application has the following beneficial effects:

[0031] The present application provides a device for judging the leakage and residue of silicone oil in the pre-chamber of a freeze dryer, which can quickly and accurately detect the leakage and residue of silicone oil in the pre-chamber of a freeze dryer without affecting production, find problems in time and take corresponding measures, avoid product quality problems and equipment failures caused by silicone oil leakage and residue, and improve the operation stability and reliability of the freeze dryer. BRIEF DESCRIPTION OF DRAWINGS

[0032] Other features, objects and advantages of the present application will become more apparent from the following detailed description of non-limiting embodiments with reference to the attached drawings:

[0033] Figure 1 is a schematic diagram of the connection mode of the device for judging the leakage and residue of silicone oil in the pre-chamber of a freeze dryer of the present application;

[0034] Figure 2 is a 5m 2 background trend graph of silicone oil detection of a freeze dryer;

[0035] Figure 3 is a 5m 2 trend graph of silicone oil detection of a freeze dryer;

[0036] Figure 4 is a 35m 2 background trend graph of silicone oil detection of a freeze dryer;

[0037] Figure 5 is a 35m 2 trend graph of silicone oil detection of a freeze dryer.

[0038] In the figure, the silicone oil detection device 1, the air pipe 2, the stainless steel hose 3, the pneumatic diaphragm valve 4, the pre-chamber 5 of the freeze dryer, the first vacuum gauge 6, the high-pressure gas source 7 of the freeze dryer; the main machine 11, the second electromagnetic valve 12, the first electromagnetic valve 13, the silicone oil detection cavity 14, the second vacuum gauge 15, the alarm device 16, the molecular pump 17, the diaphragm pump 18; the verification hole 51. DETAILED DESCRIPTION

[0039] The present application will be described in detail below in conjunction with specific embodiments. The following embodiments will help those skilled in the art to further understand the present application, but do not limit the present application in any form. It should be noted that those skilled in the art can make several changes and improvements without departing from the concept of the present application. These all belong to the protection scope of the present application.

[0040] Example 1

[0041] As Figure 1As shown, the application provides a device for judging the leakage and residue of silicone oil in the front box of a freeze dryer. The silicone oil detection cavity 14 is connected with a molecular pump 17, and the molecular pump 17 is connected with a diaphragm pump 18. The diaphragm pump 18 and the molecular pump 17 provide a negative pressure environment for the silicone oil detection cavity 14.

[0042] The second vacuum gauge 15 is installed on the silicone oil detection cavity 14 to display the vacuum degree of the silicone oil detection cavity 14.

[0043] One end of the first electromagnetic valve 13 is connected with the silicone oil detection cavity 14 through a stainless steel straight pipe, and the other end of the first electromagnetic valve 13 is connected with the pneumatic diaphragm valve 4 through a stainless steel hose 3.

[0044] The pneumatic diaphragm valve 4 is fixed on the verification hole 51 of the front box 5 of the freeze dryer.

[0045] The host 11 in the silicone oil detection device 1 is installed with silicone oil detection control software and is responsible for silicone oil detection data processing. The host 11 controls the opening and closing of the first electromagnetic valve 13 and the second electromagnetic valve 12.

[0046] One end of the second electromagnetic valve 12 is connected with the high-pressure gas source 7 of the freeze dryer through a 6mm diameter air pipe 2, and the other end of the second electromagnetic valve 12 is connected with the pneumatic diaphragm valve 4 gas path control interface through a 6mm diameter air pipe 2. The second electromagnetic valve 12 controls the opening and closing of the pneumatic diaphragm valve 4.

[0047] The first vacuum gauge 6 is connected with the front box 5 of the freeze dryer to display the vacuum degree in the front box 5 of the freeze dryer.

[0048] The second electromagnetic valve 12 and the first electromagnetic valve 13 have interlocking functions. When the vacuum degree of the front box 5 of the freeze dryer is higher than 50pa during the silicone oil detection process, the host 11 sends a command to close the second electromagnetic valve 12 to protect the silicone oil detection device 1. When the vacuum degree of the silicone oil detection cavity 14 is higher than 0.1pa during the silicone oil detection process, the host sends a command to close the second electromagnetic valve 12 and the first electromagnetic valve 13 to prevent external gas from polluting the front box of the freeze dryer and to ensure a sterile environment.

[0049] The vacuum degree of the silicone oil detection cavity 14 is not higher than 0.1pa because the working condition vacuum degree of the detector in the silicone oil detection cavity 14 cannot be higher than 0.1pa. The vacuum degree of the front box 5 of the freeze dryer is not higher than 50pa because when the vacuum degree of the front box 5 of the freeze dryer is higher than 50pa, the silicone oil detection cavity 14 does not satisfy the condition that the vacuum degree is lower than 0.1pa.

[0050] When the silicone oil detection value exceeds the set warning value, the alarm device 16 sends an alarm.

[0051] The codes 7, 5 and 51 in the schematic diagram of the connection mode of the freeze-dryer front box silicone oil leakage and residual device are not components of the freeze-dryer front box silicone oil leakage and residual device, and 7, 5 and 51 are components of the freeze-dryer to be detected.

[0052] Figure 1 The silicone oil detection device 1 comprises a host 11, a second electromagnetic valve 12, a first electromagnetic valve 13, a silicone oil detection cavity 14, a second vacuum gauge 15, an alarm device 16, a molecular pump 17 and a diaphragm pump 18. The shell of the silicone oil detection device 1 is made of ABS flame-retardant material. The molecular pump 17 is installed on the silicone oil detection cavity 14 by fasteners. The diaphragm pump 18 is connected to the molecular pump 17 through an air pipe. The diaphragm pump 18 extracts a primary vacuum for the silicone oil detection cavity 14. The molecular pump 17 extracts a secondary vacuum for the silicone oil detection cavity 14. The second vacuum gauge 15 is connected to the silicone oil detection cavity 14 through a KF16 clamp to measure the vacuum value of the silicone oil detection cavity 14. The first electromagnetic valve 13 is connected to the silicone oil detection cavity 14 through a stainless steel straight pipe. The opening and closing of the first electromagnetic valve 13 is controlled by the host 11. The first electromagnetic valve 13 is opened during the detection process, and silicone molecules enter the silicone oil detection cavity 14 for detection. At the same time, when the vacuum degree of the silicone oil detection cavity 14 is greater than 0.1 Pa, the host closes the first electromagnetic valve 13 to protect the detection device in the silicone oil detection cavity 14. One end of the pneumatic diaphragm valve 4 is fixed to the freeze-dryer front box verification hole through an ISO38 clamp. The other end of the pneumatic diaphragm valve 4 is connected to the first electromagnetic valve 13 through a KF16 stainless steel corrugated pipe to form a sample inlet channel. The pneumatic diaphragm valve 4 can avoid the influence of the external environment on the freeze-dryer front box and ensure the original sterile environment of the freeze-dryer front box. One end of the second electromagnetic valve 12 is connected to the freeze-dryer compressed air source through a 6mm air pipe. The other end of the second electromagnetic valve 12 is connected to the pneumatic diaphragm valve 4 through a 6mm air pipe. The second electromagnetic valve 12 and the pneumatic diaphragm valve 4 are synchronously opened and closed. When the vacuum degree of the silicone oil detection cavity 14 is less than 0.09 Pa, the host 11 sends a command to open the second electromagnetic valve 12, and the pneumatic diaphragm valve 4 is opened for silicone oil detection. When the vacuum degree of the silicone oil detection cavity 14 is greater than 0.1 Pa during the detection process, the host sends a command to close the second electromagnetic valve 12 and the first electromagnetic valve 13. The second electromagnetic valve 12 is closed, and the pneumatic diaphragm valve 4 is closed. The first electromagnetic valve 13 is closed to protect the detection device in the silicone oil detection cavity 14 and avoid external gas from entering the freeze-dryer front box. The first vacuum gauge 6 is installed on the freeze-dryer front box through a clamp to detect the vacuum degree of the freeze-dryer front box. When the vacuum degree of the first vacuum gauge 6 is greater than 50 Pa during the silicone oil detection process, the host sends a command to close the second electromagnetic valve 12 and the first electromagnetic valve 13 to protect the detection device in the silicone oil detection cavity 14.

[0053] The alarm device 16 issues an alarm when the vacuum value of the silicone oil detection chamber 14 is greater than 0.1 Pa during the silicone oil detection process, and the alarm device 16 issues an alarm when the vacuum value of the first vacuum gauge 6 is greater than 50 Pa during the silicone oil detection process.

[0054] This invention provides a method for determining silicone oil leakage and residue in the front chamber of a freeze dryer, comprising the following steps:

[0055] After a batch of products is freeze-dried, a device for detecting silicone oil leakage and residue in the freeze dryer's front chamber is connected. The freeze dryer starts its vacuuming program, setting the vacuum level to 20 Pa. The device for detecting silicone oil leakage and residue in the freeze dryer's front chamber is activated with a single button. Once the vacuum level in the freeze dryer's front chamber reaches 20 Pa and the silicone oil detection trend chart stabilizes, the pneumatic diaphragm valve 4 is opened for silicone oil detection. If silicone oil is detected, the freeze dryer is cleaned, and a second silicone oil detection is performed under the same conditions. At 20 Pa, there are relatively more silicone oil molecules volatilized in the freeze dryer's front chamber, while simultaneously meeting the requirement that the pressure in the silicone oil detection chamber 14 be below 0.1 Pa, resulting in a high silicone oil detection response. The freeze dryer consumes little energy to achieve a vacuum level of 20 Pa.

[0056] 10m 2 The following tests were performed directly using a freeze dryer, 10m 2 The above freeze dryers require heating and pressure maintenance to accelerate the evaporation of silicone oil molecules. At 10m... 2 As a boundary, based on the volume of the freeze dryer's front chamber and the test results of adding 1ml of silicone oil, 10m 2 For freeze dryers below the specified size, silicone oil molecules can be directly detected by adding 1 ml of silicone oil; 10 ml... 2 Freeze dryers of higher specifications cannot detect this directly; they require heating and pressure holding to detect it because of the 10m... 2 The freeze dryer described above has a large front chamber volume, and the mass-to-nucleus ratio of silicone oil molecules is much larger than that of air. Heating and pressurizing accelerate the volatilization of silicone oil, allowing silicone oil molecules to fill the entire front chamber space in a short time, which is beneficial for detection.

[0057] Given the lack of expertise among personnel using a device to determine silicone oil leakage and residue in the front chamber of a freeze dryer, the control software utilizes machine learning algorithms to train a model for in-depth analysis of the two detection data. This enables it to more accurately determine silicone oil leakage and residue based on different freeze dryer models, operating conditions, and historical data.

[0058] The deep analysis of the two detection data by training the model by using the machine learning algorithm comprises: first, establishing a detection formula, the formula including a freeze dryer model, freeze dryer working conditions including a vacuum degree value, a temperature, a silicon oil leakage detection warning value, a silicon oil residue detection warning value and a threshold value, performing background detection data without silicon oil residue and leakage under the formula as comparison data, and subsequently, when performing silicon oil detection, the software intelligently compares according to the historical data and the detection data to determine the silicon oil residue and the silicon oil leakage.

[0059] Example 2

[0060] A domestic large-scale freeze dryer manufacturer provides a freeze dryer (5m 2 ) which is used in combination with the device for judging the silicon oil leakage and residue of the front box of the freeze dryer in the present application to perform the simulation detection of the silicon oil of the front box of the freeze dryer.

[0061] First, the background detection of the front box of the freeze dryer is performed, and the background detection graph of the silicon oil of the front box of the freeze dryer is as shown in Figure 2 , and no silicon oil component is detected.

[0062] The silicon oil is taken out from the silicon oil pipe loaded on the freeze dryer, 0.5ml of the silicon oil sample is loaded into a standard vial, the vial loaded with 0.5ml of the silicon oil is placed on the plate layer of the front box of the freeze dryer, the vacuum program of the freeze dryer is started, 20Pa is set, the silicon oil detection device in the present application is started, and the silicon oil detection is performed, and the silicon oil detection trend graph is as shown in Figure 3 , the silicon oil content is detected to suddenly rise after the pneumatic diaphragm valve is opened, the silicon oil detection intensity is in an upward state with time, and the silicon oil component is detected.

[0063] Example 3

[0064] A domestic large-scale freeze dryer manufacturer provides a freeze dryer (35m 2 ) which is used in combination with the device for judging the silicon oil leakage and residue of the front box of the freeze dryer in the present application to perform the simulation detection of the silicon oil of the front box of the freeze dryer.

[0065] First, the background detection of the front box of the freeze dryer is performed, and the background detection graph of the silicon oil of the front box of the freeze dryer is as shown in Figure 4 , and no silicon oil component is detected.

[0066] The silicon oil is taken out from the silicon oil pipe loaded on the freeze dryer, 1ml of the silicon oil sample is loaded into a standard vial, the vial loaded with 1ml of the silicon oil is placed on the plate layer of the front box of the freeze dryer, the vacuum program of the freeze dryer is started, 20Pa is set, the heating program of the freeze dryer is started, the vacuum degree and the plate layer temperature of the front box of the freeze dryer reach the set value and then pressure is maintained, the silicon oil detection device in the present application is started, and the silicon oil detection is performed, and the detection trend graph is as shown in Figure 5 , the silicon oil detection content is detected to suddenly rise, the silicon oil detection intensity trend graph is in an upward trend with time, and the silicon oil component is detected.

[0067] In the description of the present application, it needs to be understood that the terms "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the present application.

[0068] Those skilled in the art know that, in addition to implementing the system, device and each module thereof provided by the present application in the form of pure computer readable program code, the same program can also be implemented in the form of logic gates, switches, application specific integrated circuits, programmable logic controllers and embedded microcontrollers by logically programming the method steps. Therefore, the system, device and each module thereof provided by the present application can be considered as a hardware component, and the modules included therein for implementing various programs can also be considered as structures within the hardware component; the modules for implementing various functions can also be considered as both software programs for implementing methods and structures within hardware components.

[0069] The specific embodiments of the present application are described above. It needs to be understood that the present application is not limited to the specific embodiments described above, and those skilled in the art can make various changes or modifications within the scope of the claims, which does not affect the essential content of the present application. The embodiments of the present application and the features in the embodiments can be arbitrarily combined with each other without conflict.

Claims

1. A device for determining silicone oil leakage and residue in a pre-vacuum chamber of a freeze dryer, characterized by, The application relates to a silicone oil detection device. The silicone oil detection device comprises a silicone oil detection device (1), an air pipe (2), a stainless steel hose (3), a pneumatic diaphragm valve (4), a freeze dryer front box (5), a first vacuum gauge (6), a freeze dryer high-pressure gas source (7), a host computer (11), a second electromagnetic valve (12), a first electromagnetic valve (13), a silicone oil detection cavity (14), a second vacuum gauge (15), an alarm device (16), a molecular pump (17), a diaphragm pump (18) and a verification hole (51). The silicone oil detection cavity (14) is connected with the molecular pump (17), the molecular pump (17) is connected with the diaphragm pump (18), and the diaphragm pump (18) and the molecular pump (17) enable the silicone oil detection cavity (14) to have a negative pressure environment. The second vacuum gauge (15) is installed on the silicone oil detection cavity (14) and displays the vacuum degree of the silicone oil detection cavity (14). One end of the first electromagnetic valve (13) is connected with the silicone oil detection cavity (14) through a stainless steel straight pipe, and the other end of the first electromagnetic valve (13) is connected with the pneumatic diaphragm valve (4) through the stainless steel hose (3). The pneumatic diaphragm valve (4) is fixed on the verification hole (51) of the freeze dryer front box (5). The host computer (11) in the silicone oil detection device is installed with silicone oil detection control software and is responsible for silicone oil detection data processing; the host computer (11) controls the first electromagnetic valve (13) and the second electromagnetic valve (12) to be opened and closed. One end of the second electromagnetic valve (12) is connected with the freeze dryer high-pressure gas source (7) through the air pipe (2), and the other end of the second electromagnetic valve (12) is connected with the pneumatic diaphragm valve (4) gas path control interface through the air pipe (2), and the second electromagnetic valve (12) controls the opening and closing of the pneumatic diaphragm valve (4). The first vacuum gauge (6) is connected to the freeze dryer front box (5) and displays the vacuum degree in the freeze dryer front box (5). The alarm device (16) is connected with the host computer (11), and when the silicone oil detection value exceeds the set warning value, the alarm device (16) issues an alarm.

2. The apparatus for determining silicone oil leakage and residue of a pre-vacuum chamber of a freeze dryer according to claim 1, wherein The second electromagnetic valve (12) and the first electromagnetic valve (13) have an interlocking function, when the vacuum degree of the freeze dryer front box (5) is higher than 50pa during the silicone oil detection process, the host computer (11) issues an instruction to close the second electromagnetic valve (12) to protect the silicone oil detection device (1); when the vacuum degree of the silicone oil detection cavity (14) is higher than 0.1pa during the silicone oil detection process, the host computer (11) issues an instruction to close the second electromagnetic valve (12) and the first electromagnetic valve (13) to prevent external gas from polluting the freeze dryer front box.

3. The apparatus for determining silicone oil leakage and residue of a pre-vacuum chamber of a freeze dryer according to claim 1, wherein The molecular pump (17) is installed on the silicone oil detection cavity (14) through a fastener, the diaphragm pump (18) is connected with the molecular pump (17) through an air pipe, the diaphragm pump (18) extracts primary vacuum for the silicone oil detection cavity (14), and the molecular pump (17) extracts secondary vacuum for the silicone oil detection cavity (14).

4. The apparatus for determining silicone oil leakage and residue of a pre-vacuum chamber of a freeze dryer according to claim 1, wherein The second vacuum gauge (15) is connected to the silicone oil detection cavity (14) through a KF16 clamp and measures the vacuum degree value of the silicone oil detection cavity (14).

5. The apparatus for determining silicone oil leakage and residue in a pre-vacuum chamber of a freeze dryer according to claim 1, wherein The first electromagnetic valve (13) is connected to the silicone oil detection cavity (14) through a stainless steel straight pipe, the opening and closing of the first electromagnetic valve (13) is controlled by the host computer (11), the first electromagnetic valve (13) is opened during the detection process, and silicone molecules enter the silicone oil detection cavity (14) to be detected.

6. The apparatus for determining silicone oil leakage and residue of a pre-vacuum chamber of a freeze dryer according to claim 1, wherein The pneumatic diaphragm valve (4) is fixed to the verification hole (51) of the freeze dryer front box (5) through an ISO38 clamp at one end, and is connected to the first electromagnetic valve (13) through a KF16 stainless steel bellows at the other end, forming a sample injection channel.

7. The apparatus for determining silicone oil leakage and residue of a pre-vacuum chamber of a freeze dryer according to claim 1, wherein The second electromagnetic valve (12) is connected to the freeze dryer high-pressure gas source (7) through a 6mm air pipe at one end, and is connected to the pneumatic diaphragm valve (4) through a 6mm air pipe at the other end. The second electromagnetic valve (12) and the pneumatic diaphragm valve (4) are opened and closed synchronously. When the vacuum degree of the silicone oil detection cavity (14) is lower than 0.09Pa, the host computer (11) sends a command to open the second electromagnetic valve (12), and the pneumatic diaphragm valve (4) is opened to detect the silicone oil.

8. The apparatus for determining silicone oil leakage and residue of a pre-vacuum chamber of a freeze dryer according to claim 1, wherein The first vacuum gauge (6) is installed on the freeze dryer front box (5) through a clamp to detect the vacuum degree of the freeze dryer front box (5). During the silicone oil detection process, when the vacuum degree of the first vacuum gauge (6) is greater than 50Pa, the host computer (11) sends a command to close the second electromagnetic valve (12) and the first electromagnetic valve (13) to detect the detector in the silicone oil detection cavity (14).

9. The apparatus for determining silicone oil leakage and residue in a pre-vacuum chamber of a lyophilizer according to claim 1, wherein The alarm device (16) sends an alarm when the vacuum degree of the silicone oil detection cavity (14) is greater than 0.1Pa during the silicone oil detection process, and sends an alarm when the vacuum degree of the first vacuum gauge (6) is greater than 50Pa.

10. A method of determining silicone oil leakage and residue in a pre-vacuum chamber of a freeze dryer, comprising: The device for judging the silicone oil leakage and residue of the freeze dryer front box according to any one of claims 1 to 9 comprises the following steps: Connect the device for judging the silicone oil leakage and residue of the freeze dryer front box, open the silicone oil detection control software, and the host computer controls the opening of the first electromagnetic valve to start the freeze dryer vacuum pumping program. When the vacuum degree of the silicone oil detection cavity is less than 0.05Pa and the vacuum degree of the freeze dryer front box is less than 50Pa, the host computer controls the opening of the second electromagnetic valve to perform silicone oil detection. The freeze dryer with a freeze-drying area of 10 square meters or less does not start the heating program, and the freeze dryer with a freeze-drying area of more than 10 square meters heats and pressurizes. After completing a batch of freeze-drying tasks, the device for judging the silicone oil leakage and residue of the freeze dryer front box is used for silicone background detection. When the silicone background detection detects silicone components, the freeze dryer front box is cleaned according to the production program, and the second silicone component detection is performed during the pressurization stage after cleaning. The silicone detection data of the two times are imported into the preset machine learning algorithm training model, and the control software judges the silicone leakage and residue according to different freeze dryer models, working conditions and historical data.

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