Device and method for judging leakage and residue of silicone oil in front box of freeze dryer

By providing a system including silicone oil detection device and related equipment, the problem of slow detection of silicone oil leakage and residue in front of the freeze-dryer is solved, and the operational stability of the freeze-dryer is achieved is achieved. Effect.

CN119469617AActive Publication Date: 2025-02-18SHANGHAI YUDA INDUSTRIAL CO LTD
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Patent Information

Application Number
CN202411567875.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-05
Publication Date
2025-02-18
Estimated Expiration
2044-11-05

AI Technical Summary

Technical Problem

The prior art has problems such as slow detection speed, insufficient detection limit, complex operation process and high equipment maintenance costs in detecting silicone oil leakage and residue in front of the freeze-dryer, which is difficult to meet the needs of rapid testing on the production line.

Method used

Provided is a silicone oil detection device, a gas pipe, a stainless steel hose, a pneumatic diaphragm valve, a lyophilized front box, a vacuum gauge, a high-pressure air source, a main unit, a solenoid valve, a silicone oil detection chamber, a molecular pump, a diaphragm pump and an alarm device. The system uses the host to control the solenoid valve and vacuum pump to achieve fast and accurate silicone oil detection, and uses machine learning algorithms to perform data analysis to judge the leakage and residue of silicone oil.

Benefits of technology

It realizes rapid and accurate detection of the leakage and residue of silicone oil in the front box of the lyophilized machine without affecting production, improves the operating stability and reliability of the lyophilized machine, and avoids product quality caused by leakage and residue of silicone oil. Problems and equipment failures.

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Patent Text Reader

Abstract

The invention provides a device and method for judging leakage and residue of silicone oil in a front box of a freeze dryer, and the method comprises the steps: carrying out silicone oil background detection by adopting the device for judging the leakage and residue of the silicone oil in the front box of the freeze dryer after the freeze dryer completes a batch of freeze-drying tasks; the silicone oil background detects the silicone oil, the front box of the freeze dryer is cleaned according to a production procedure, the secondary silicone oil detection is performed in a pressure maintaining stage after cleaning, the detection data is deeply analyzed by adopting an artificial intelligence algorithm, the leakage and residue of the silicone oil are automatically identified, and the judgment accuracy and reliability are improved. The silicone oil in the freeze dryer front box can be rapidly and accurately detected under the condition that production is not affected, meanwhile, the sterile environment of the freeze dryer front box is guaranteed, the product quality problem and the equipment fault are avoided, and the operation stability and reliability of the freeze dryer are improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of freeze dryer detection, and in particular to a device and method for judging the leakage and residue of silicone oil in a front box of a freeze dryer. Background Art

[0002] Freeze dryers are widely used in many industries such as pharmaceuticals and food. However, the leakage and residue of silicone oil in the front box of the freeze dryer cannot be underestimated. This not only causes product contamination and quality degradation, but also leads to a series of serious consequences, even causing equipment failure, increasing maintenance costs, and affecting production progress.

[0003] Some existing methods for detecting silicone oil leakage and residue in the front box of freeze dryers have many significant shortcomings. First of all, 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. Although chromatography can be used for quantitative analysis, the detection cycle 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 results, which makes it difficult to meet the urgent need for rapid detection on the production line. This leads to stagnation of the production process and reduces overall production efficiency.

[0004] Furthermore, the operation procedures of some testing methods are extremely complicated. This not only places high demands on the professional and technical level of the testers, but also requires them to undergo long-term training and practice to master them. This undoubtedly increases labor costs, and in actual operations, complex steps are prone to human errors, further affecting the accuracy and reliability of the test results.

[0005] In addition, some detection methods rely on expensive detection equipment and 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, thus facing greater risks in production.

[0006] In view of this, it is particularly important to timely and accurately determine the leakage and residual status of silicone oil in the front box of the freeze dryer. This can not only ensure the high-quality production of products, but also effectively prevent equipment failures and ensure the stability and efficiency of the production process. Summary of the invention

[0007] In view of the defects in the prior art, the object of the present invention is to provide a device and method for judging the leakage and residue of silicone oil in the front box of a freeze dryer.

[0008] The device for judging the leakage and residue of silicone oil in the front box of the freeze dryer provided by the present invention comprises: a silicone oil detection device, an air pipe, a stainless steel hose, a pneumatic diaphragm valve, a front box of the freeze dryer, a first vacuum gauge, a high-pressure gas source of the freeze dryer, a host, a second solenoid valve, a first solenoid 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 a molecular pump, and the molecular pump is connected to a diaphragm pump. The diaphragm pump and the molecular pump provide the silicone oil detection cavity with a negative pressure environment;

[0010] The second vacuum gauge is installed on the silicone oil detection cavity to display the vacuum degree of the silicone oil detection cavity;

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

[0012] The pneumatic diaphragm valve is fixed on the verification hole of the front box of the freeze dryer;

[0013] The host 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 controls the opening and closing of the first solenoid valve and the second solenoid valve;

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

[0015] The first vacuum gauge is connected to the front box of the freeze dryer to display the vacuum degree in the front box 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 sounds an alarm.

[0017] Preferably, the second solenoid valve and the first solenoid valve have an interlocking function. When the vacuum degree of the front box of the freeze dryer is higher than 50 Pa during the silicone oil detection process, the host issues a command to close the second solenoid valve to protect the silicone oil detection device; when the vacuum degree of the silicone oil detection chamber is higher than 0.1 Pa during the silicone oil detection process, the host issues a command to close the second solenoid valve and the first solenoid valve to prevent external gas from contaminating the front box of the freeze dryer.

[0018] Preferably, the molecular pump is mounted on the silicone oil detection cavity through fasteners, the diaphragm pump is connected to the molecular pump through an air pipe, the diaphragm pump extracts a primary vacuum for the silicone oil detection cavity, and the molecular pump extracts a secondary 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 to measure the vacuum value of the silicone oil detection cavity.

[0020] Preferably, the first solenoid valve is connected to the silicone oil detection cavity through a stainless steel straight pipe. The opening and closing of the first solenoid valve is controlled by the host. During the detection process, the first solenoid valve is opened, and the silicone oil molecules 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 freeze dryer front box through an ISO38 clamp, and the other end of the pneumatic diaphragm valve is connected to the first solenoid valve through a KF16 stainless steel bellows to form a test sample injection channel.

[0022] Preferably, one end of the second solenoid valve is connected to the high-pressure air source of the freeze dryer through a 6mm air pipe, and the other end of the second solenoid valve is connected to the pneumatic diaphragm valve through a 6mm air pipe. The second solenoid valve and the pneumatic diaphragm valve are opened and closed synchronously. When the vacuum degree of the silicone oil detection chamber is lower than 0.09Pa, the host sends a command to open the second solenoid 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; during the silicone oil detection process, when the vacuum value of the first vacuum gauge is greater than 50Pa, the host sends an instruction to close the second solenoid valve and the first solenoid valve, thereby detecting the detection device in the silicone oil detection cavity.

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

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

[0026] Connect the device for detecting silicone oil leakage and residue in the front box of the freeze dryer, open the silicone oil detection control software, and control the host to open the first solenoid valve and start the vacuum pumping program of the freeze dryer;

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

[0028] The freeze dryer with a freeze drying area of ​​10 square meters or less will not start the heating program, and the freeze dryer with a freeze drying area of ​​more than 10 square meters will heat and maintain pressure;

[0029] After the freeze dryer completes a batch of freeze-drying tasks, a device for judging the leakage and residue of silicone oil in the front box of the freeze dryer is used to perform a silicone oil background test. The silicone oil background detects the silicone oil component, and the front box of the freeze dryer is cleaned according to the production procedure. After cleaning, a second silicone oil component test is performed during the pressure holding stage. The two silicone oil test data are imported into the preset machine learning algorithm training model. 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 invention has the following beneficial effects:

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

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

[0033] Figure 1 It is a schematic diagram of a connection method of a device for judging silicone oil leakage and residue in a front box of a freeze dryer according to the present invention;

[0034] Figure 2 5m 2 Freeze dryer silicone oil detection background trend chart;

[0035] Figure 3 5m 2 Freeze dryer silicone oil detection trend chart;

[0036] Figure 4 35m 2 Freeze dryer silicone oil detection background trend chart;

[0037] Figure 5 35m 2 Freeze dryer silicone oil detection trend chart.

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

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

[0040] Example 1

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

[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 solenoid valve 13 is connected to the silicone oil detection chamber 14 through a stainless steel straight pipe, and the other end of the first solenoid valve 13 is connected to 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 freeze dryer front box 5;

[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 solenoid valve 13 and the second solenoid valve 12;

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

[0047] The first vacuum gauge 6 is connected to 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 solenoid valve 12 and the first solenoid valve 13 have an interlocking function. When the vacuum degree of the freeze dryer front box 5 is higher than 50 Pa during the silicone oil detection process, the host 11 issues a command to close the second solenoid valve 12 to protect the silicone oil detection device 1; when the vacuum degree of the silicone oil detection chamber 14 is higher than 0.1 Pa during the silicone oil detection process, the host issues a command to close the second solenoid valve 12 and the first solenoid valve 13 to prevent external gas from contaminating the freeze dryer front box and ensure a sterile environment.

[0049] The vacuum degree of the silicone oil detection chamber 14 is not higher than 0.1 Pa because the vacuum degree of the detection device in the silicone oil detection chamber 14 cannot be higher than 0.1 Pa. The vacuum degree of the freeze dryer front box 5 is not higher than 50 Pa because when the vacuum degree of the freeze dryer front box 5 is higher than 50 Pa, the silicone oil detection chamber 14 does not meet the vacuum degree lower than 0.1 Pa.

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

[0051] In the connection diagram of the device for judging the leakage and residue of silicone oil in the front box of the freeze dryer, codes 7, 5, and 51 do not belong to the components of the device for judging the leakage and residue of silicone oil in the front box of the freeze dryer. 7, 5, and 51 are the components of the freeze dryer being tested.

[0052] Figure 1 The silicone oil detection device 1 includes a main unit 11, a second solenoid valve 12, a first solenoid valve 13, a silicone oil detection chamber 14, a second vacuum gauge 15, an alarm device 16, a molecular pump 17, and a diaphragm pump 18. The outer 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 chamber 14 through fasteners, and the diaphragm pump 18 is connected to the molecular pump 17 through an air pipe. The diaphragm pump 18 extracts a first-level vacuum for the silicone oil detection chamber 14, and the molecular pump 17 extracts a second-level vacuum for the silicone oil detection chamber 14; the second vacuum gauge 15 is connected to the silicone oil detection chamber 14 through a KF16 clamp to measure the vacuum value of the silicone oil detection chamber 14; the first solenoid valve 13 is connected to the silicone oil detection chamber 14 through a stainless steel straight pipe, and the opening and closing of the first solenoid valve 13 is controlled by the main unit 11 during the detection process. When the silicone oil detection chamber 14 is opened, the silicone oil molecules enter the silicone oil detection chamber 14 for detection. At the same time, when the vacuum degree of the silicone oil detection chamber 14 is greater than 0.1Pa, the host closes the first solenoid valve 13 to protect the detection device in the silicone oil detection chamber 14; one end of the pneumatic diaphragm valve 4 is fixed to the verification hole of the freeze dryer front box through an ISO38 clamp, and the other end of the pneumatic diaphragm valve 4 is connected to the first solenoid valve 13 through a KF16 stainless steel bellows to form a detection sample injection channel. The pneumatic diaphragm valve 4 can prevent the freeze dryer front box from being affected by the external environment and ensure the freeze dryer The original sterile environment of the front box of the dryer; one end of the second solenoid valve 12 is connected to the compressed air source of the freeze dryer through a 6mm air pipe, and the other end of the second solenoid valve 12 is connected to the pneumatic diaphragm valve 4 through a 6mm air pipe. The second solenoid 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 11 issues a command to open the second solenoid valve 12, and the pneumatic diaphragm valve 4 is opened to perform silicone oil detection. During the detection process, when the vacuum degree of the silicone oil detection cavity 14 is greater than 0.1Pa, the host issues a command to close the second solenoid valve 1 2 and close the first solenoid valve 13, the second solenoid valve 12 is closed, and at the same time the pneumatic diaphragm valve 4 is closed, and the first solenoid valve 13 is closed, so as to protect the detection device in the silicone oil detection cavity 14 and prevent 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; during the silicone oil detection process, when the vacuum value of the first vacuum gauge 6 is greater than 50Pa, the host sends a command to close the second solenoid valve 12 and the first solenoid valve 13, so as to detect the detection device in the silicone oil detection cavity 14;

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

[0054] The present invention provides a method for judging the leakage and residue of silicone oil in the front box of a freeze dryer, which comprises the following steps:

[0055] After the freeze dryer has completed freeze drying of a batch of products, a device for judging the leakage and residue of silicone oil in the front box of the freeze dryer is connected, the freeze dryer starts the vacuum program, sets the vacuum degree to 20Pa, and starts a device for judging the leakage and residue of silicone oil in the front box of the freeze dryer with one button. When the vacuum degree of the front box of the freeze dryer reaches 20Pa, the pneumatic diaphragm valve 4 is opened to perform silicone oil detection after the silicone oil detection trend chart of the detection device is stable; when the silicone oil component is detected, a second silicone oil detection is performed under the same conditions after the freeze dryer is cleaned. At 20Pa, there are relatively more silicone oil molecules volatilized in the front box of the freeze dryer, and at the same time, the requirement that the air pressure of the silicone oil detection chamber 14 is lower than 0.1Pa can be met, and the silicone oil detection response is high; the freeze dryer consumes less energy when the vacuum reaches 20Pa.

[0056] 10m 2 The following freeze dryers are directly tested, 10m 2 The above freeze dryers need to be heated and pressurized to accelerate the volatilization of silicone oil molecules. 2 As the limit, according to the volume of the freeze dryer front box and the test results of adding 1ml silicone oil, 10m 2 The following freeze dryers can directly detect silicone oil molecules by putting 1ml of silicone oil into them. 2 Freeze dryers with specifications above 10m can not be detected directly, and need to be heated and pressurized to detect. 2 The volume of the front box of the above freeze dryers is relatively large, and the mass-to-nuclear ratio of silicone oil molecules is much larger than that of air components. Heating and pressurizing accelerate the volatilization movement of silicone oil, so that the silicone oil molecules fill the entire front box space in a shorter time, which is conducive to detection.

[0057] Given that the personnel using a device to determine the leakage and residue of silicone oil in the front box of the freeze dryer lack relevant professional knowledge, the control software uses a machine learning algorithm training model to conduct an in-depth analysis of the two test data. It can more accurately determine the leakage and residue of silicone oil based on different freeze dryer models, working conditions and historical data.

[0058] The in-depth analysis of the two test data using the machine learning algorithm training model includes: first, establishing a test formula, the formula includes the freeze dryer model, the freeze dryer working conditions include vacuum value, temperature, silicone oil leakage detection warning value, silicone oil residue detection warning value and threshold, and the background test data without silicone oil residue and leakage under the formula is used as comparison data. When performing subsequent silicone oil detection, the software performs intelligent comparison based on historical data and test data to determine silicone oil residue and silicone oil leakage.

[0059] Example 2

[0060] A domestic large freeze dryer manufacturer provides freeze dryer (5m 2) is used in conjunction with the device for judging the leakage and residue of silicone oil in the front box of the freeze dryer in the present invention to simulate the detection of silicone oil in the front box of the freeze dryer.

[0061] First, the freeze dryer front box background test is carried out. The freeze dryer front box background test is shown in the figure below. Figure 2 As shown, no silicone oil component was detected.

[0062] Silicone oil was taken out from the silicone oil tube loaded in the freeze dryer, and 0.5 ml of silicone oil sample was put into a standard vial. The vial containing 0.5 ml of silicone oil was placed on the front box layer of the freeze dryer, and the vacuum program of the freeze dryer was started, set to 20 Pa, and the silicone oil detection device of the present invention was started to perform silicone oil detection. The silicone oil detection trend diagram is shown as follows: Figure 3 As shown, after the pneumatic diaphragm valve was opened, the silicone oil content was detected to rise sharply, and the silicone oil detection intensity increased with time, and the silicone oil component was detected.

[0063] Example 3

[0064] A domestic large freeze dryer manufacturer provides freeze dryer (35m 2 ) is used in conjunction with the device for judging the leakage and residue of silicone oil in the front box of the freeze dryer in the present invention to simulate the detection of silicone oil in the front box of the freeze dryer.

[0065] First, the freeze dryer front box background test is carried out. The freeze dryer front box silicone oil background test is shown in the figure below. Figure 4 As shown, no silicone oil component was detected.

[0066] Silicone oil is taken out from the silicone oil tube loaded in the freeze dryer, and 1 ml of silicone oil sample is loaded into a standard vial. The vial containing 1 ml of silicone oil is placed on the front box plate layer of the freeze dryer, and the freeze dryer vacuum program is started, set to 20Pa, and the freeze dryer heating program is started. After the vacuum degree and plate temperature of the front box of the freeze dryer reach the set value, the pressure is maintained, and the silicone oil detection device of the present invention is started to perform silicone oil detection. The detection trend diagram is as shown in FIG. Figure 5 As shown, the silicone oil detection content increased sharply, and the silicone oil detection intensity trend graph showed an upward trend over time, and the silicone oil component was detected.

[0067] In the description of the present application, it should be understood that the terms "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not 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 its various modules provided by the present invention in a purely computer-readable program code, it is entirely possible to implement the same program 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 its various modules provided by the present invention 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 the method and structures within the hardware component.

[0069] The above describes the specific embodiments of the present invention. It should be understood that the present invention is not limited to the above specific embodiments, and those skilled in the art can make various changes or modifications within the scope of the claims, which does not affect the essence of the present invention. In the absence of conflict, the embodiments of the present application and the features in the embodiments can be combined with each other arbitrarily.

Claims

1. A device for judging the leakage and residue of silicone oil in the front box of a freeze dryer, characterized in that: include: Silicone oil detection device (1), air pipe (2), stainless steel hose (3), pneumatic diaphragm valve (4), freeze dryer front box (5), first vacuum gauge (6), freeze dryer high pressure gas source (7), host (11), second solenoid valve (12), first solenoid valve (13), silicone oil detection chamber (14), second vacuum gauge (15), alarm device (16), molecular pump (17), diaphragm pump (18) and verification hole (51); The silicone oil detection cavity (14) is connected to a molecular pump (17), the molecular pump (17) is connected to a 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) to display the vacuum degree of the silicone oil detection cavity (14); One end of the first solenoid valve (13) is connected to the silicone oil detection chamber (14) through a stainless steel straight pipe, and the other end of the first solenoid valve (13) is connected to the pneumatic diaphragm valve (4) through a 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 (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 solenoid valve (13) and the second solenoid valve (12); One end of the second solenoid valve (12) is connected to the high-pressure gas source (7) of the freeze dryer through the air pipe (2), and the other end of the second solenoid valve (12) is connected to the air circuit control interface of the pneumatic diaphragm valve (4) through the air pipe (2), and the second solenoid valve (12) controls the opening and closing of the pneumatic diaphragm valve (4); The first vacuum gauge (6) is connected to the front box (5) of the freeze dryer to display the vacuum degree in the front box (5) of the freeze dryer; The alarm device (16) is connected to the host (11), and when the silicone oil detection value exceeds a set warning value, the alarm device (16) sounds an alarm.

2. The device for judging the leakage and residue of silicone oil in the front box of the freeze dryer according to claim 1, characterized in that: The second solenoid valve (12) and the first solenoid valve (13) have an interlocking function. When the vacuum degree of the freeze dryer front box (5) is higher than 50 Pa during the silicone oil detection process, the host (11) issues a command to close the second solenoid valve (12) to protect the silicone oil detection device (1); when the vacuum degree of the silicone oil detection chamber (14) is higher than 0.1 Pa during the silicone oil detection process, the host (11) issues a command to close the second solenoid valve (12) and the first solenoid valve (13) to prevent external gas from contaminating the freeze dryer front box.

3. The device for judging the leakage and residue of silicone oil in the front box of the freeze dryer according to claim 1, characterized in that: The molecular pump (17) is mounted on the silicone oil detection cavity (14) via a fastener, and the diaphragm pump (18) is connected to the molecular pump (17) via an air pipe. The diaphragm pump (18) extracts a primary vacuum for the silicone oil detection cavity (14), and the molecular pump (17) extracts a secondary vacuum for the silicone oil detection cavity (14).

4. The device for judging the leakage and residue of silicone oil in the front box of the freeze dryer according to claim 1, characterized in that: The second vacuum gauge (15) is connected to the silicone oil detection cavity (14) via a KF16 clamp to measure the vacuum value of the silicone oil detection cavity (14).

5. The device for judging the leakage and residue of silicone oil in the front box of the freeze dryer according to claim 1, characterized in that: The first solenoid valve (13) is connected to the silicone oil detection cavity (14) via a stainless steel straight pipe. The opening and closing of the first solenoid valve (13) is controlled by the host (11). During the detection process, the first solenoid valve (13) is opened, and silicone oil molecules enter the silicone oil detection cavity (14) for detection.

6. The device for judging the leakage and residue of silicone oil in the front box of a freeze dryer according to claim 1, characterized in that: One end of the pneumatic diaphragm valve (4) is fixed to the verification hole (51) of the freeze dryer front box (5) through an ISO38 clamp, and the other end of the pneumatic diaphragm valve (4) is connected to the first solenoid valve (13) through a KF16 stainless steel bellows to form a test sample injection channel.

7. The device for judging the leakage and residue of silicone oil in the front box of a freeze dryer according to claim 1, characterized in that: One end of the second solenoid valve (12) is connected to the high-pressure gas source (7) of the freeze dryer through a 6mm air pipe, and the other end of the second solenoid valve (12) is connected to the pneumatic diaphragm valve (4) through a 6mm air pipe. The second solenoid valve (12) and the pneumatic diaphragm valve (4) are opened and closed synchronously. When the vacuum degree of the silicone oil detection chamber (14) is lower than 0.09Pa, the host (11) issues a command to open the second solenoid valve (12), and the pneumatic diaphragm valve (4) is opened to perform silicone oil detection.

8. The device for judging the leakage and residue of silicone oil in the front box of a freeze dryer according to claim 1, characterized in that: The first vacuum gauge (6) is installed on the front box (5) of the freeze dryer through a clamp to detect the vacuum degree of the front box (5) of the freeze dryer; when the vacuum degree value of the first vacuum gauge (6) is greater than 50Pa during the silicone oil detection process, the host (11) issues an instruction to close the second solenoid valve (12) and the first solenoid valve (13), thereby detecting the detection device in the silicone oil detection cavity (14).

9. The device for judging the leakage and residue of silicone oil in the front box of a freeze dryer according to claim 1, characterized in that: During the silicone oil detection process, the alarm device (16) issues an alarm when the vacuum value of the silicone oil detection cavity (14) is greater than 0.1 Pa, and issues an alarm when the vacuum value of the first vacuum gauge (6) is greater than 50 Pa.

10. A method for judging the leakage and residue of silicone oil in the front box of a freeze dryer, characterized in that: The device for judging the leakage and residue of silicone oil in the front box of a freeze dryer according to any one of claims 1 to 9 comprises the following steps: Connect the device for detecting silicone oil leakage and residue in the front box of the freeze dryer, open the silicone oil detection control software, and control the host to open the first solenoid valve and start the vacuum pumping program of the freeze dryer; When the vacuum degree of the silicone oil detection chamber is less than 0.05Pa and the vacuum degree of the freeze dryer front box is less than 50Pa, the host controls to open the second solenoid valve to perform silicone oil detection; The freeze dryer with a freeze drying area of ​​10 square meters or less will not start the heating program, and the freeze dryer with a freeze drying area of ​​more than 10 square meters will heat and maintain pressure; After the freeze dryer completes a batch of freeze-drying tasks, a device for judging the leakage and residue of silicone oil in the front box of the freeze dryer is used to perform a silicone oil background test. The silicone oil background detects the silicone oil component, and the front box of the freeze dryer is cleaned according to the production procedure. After cleaning, a second silicone oil component test is performed during the pressure holding stage. The two silicone oil test data are imported into the preset machine learning algorithm training model. The control software judges the silicone oil leakage and residue according to different freeze dryer models, working conditions and historical data.

Citation Information

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