High-purity gas small-scale test filling device and filling process

Abstract

The invention relates to the technical field of high-purity gas / liquid filling, in particular to a high-purity gas small-scale test filling device and process. The device comprises a fine product tank for storing high-purity fine product gas, an automatic regulating valve, a filling pump, a film pressing machine and a low-temperature filling cabinet, after the automatic regulating valve, the filling pump and the film press are connected in parallel, one end is communicated with an outlet of the high-quality product tank through a pipeline, and the other end is communicated with an inlet of the low-temperature filling cabinet through a pipeline. The process comprises at least one of the following filling processes: a film press pressurizing filling process, a temperature difference filling process or a pump conveying filling process. The overall structural design of the device is compact, switching of all filling paths can be achieved through valve control, and operation is easy and convenient. Compared with a traditional single-function filling device, frequent equipment replacement or complex process adjustment is not needed, and the efficiency of filling small-scale test operation is greatly improved.

Description

Technical Field

[0001] This application relates to the field of high-purity gas / liquid filling technology, specifically to a high-purity gas pilot filling device and filling process. Background Technology

[0002] High-purity gases and specialty electronic gases are the cornerstone of modern industries such as semiconductors, photovoltaics, medical devices, and fine chemicals. Their quality directly affects the performance and yield of end products. In the research and development, quality control, and small-batch supply of these high-purity gases, pilot filling (i.e., laboratory-scale or small-scale filling operations) is a crucial step. This process requires filling equipment that not only ensures the purity of the gas is not compromised during transfer but also possesses high flexibility and precision to adapt to the physicochemical properties of different types of gases (or liquefied gases) and diverse experimental needs.

[0003] However, current high-purity gas filling technologies and equipment on the market have certain limitations in meeting the specific needs of scientific research and small-batch production. Existing technologies are typically single-function and specialized. Filling equipment is often designed to support only one specific filling mode. For example, for high-purity gases with low boiling points and gaseous state at room temperature, the industry generally uses compressor pressurization for filling. These devices increase the pressure of the source gas cylinder through mechanical compression, thereby filling it into the target cylinder. However, this method is inefficient or even unsuitable for gases that are liquid or easily liquefied at room temperature and pressure. On the other hand, for liquefied gases, cryogenic liquid pumps are usually used for delivery and filling. Announcement No. CN205896688U discloses a device to reduce waste in high-purity gas filling, the core of which is to use a high-purity liquid plunger pump for filling, replacing the traditional differential pressure filling method. However, the applicability of this solution is limited to filling insulated gas cylinders and cannot be directly used for filling ordinary high-purity gas cylinders, and its structural design may pose certain safety risks under certain operating conditions.

[0004] In addition, pressure difference filling is also a common technique. CN103775822A discloses a fully automated high-precision filling system for ultrapure gases. This system achieves filling by cooling the target container and controlling the pressure difference between the source and the target. Although this system achieves high-precision automation, it is not suitable for filling high-purity gases that are liquid at room temperature, essentially remaining a single-modal filling solution. In existing technologies, while temperature difference is an important physical means of generating pressure difference, it is largely a passive factor. This may lead research institutions or production units to purchase and maintain multiple independent filling systems when facing diverse filling tasks. This not only increases equipment procurement costs and laboratory space occupancy but may also result in cumbersome switching procedures between different devices, reducing the efficiency of small-scale work. Although some devices exist on the market for small-scale experiments, such as portable gas pressurization test benches or miniaturized chemical reaction devices, these devices are either too simple in function or designed for specific chemical synthesis and are not designed to solve the technical problem of multimodal filling of high-purity substances.

[0005] In summary, existing high-purity gas filling technologies have significant shortcomings: 1) The equipment has limited functionality and cannot flexibly adapt to the filling needs of materials with different physical properties, such as gaseous and liquid substances, using a single device; 2) There is a lack of highly integrated, compact, and easy-to-operate multi-functional filling platforms specifically designed for scientific research and small-batch production, resulting in low efficiency and high costs; 3) Existing filling technology fields have not yet provided mature and effective solutions to the core technical challenges of cross-contamination and pressure balance during path switching, which are inevitable challenges faced by integrated multi-path filling systems.

[0006] Therefore, it is necessary to develop a process and device that integrates multiple filling modes, can flexibly switch between them, and effectively control cross-contamination, so as to meet the needs of precise, efficient and diversified pilot filling of high-purity gases / liquids in scientific research and small-batch production, and solve the problems existing in the current technology. Summary of the Invention

[0007] To address the shortcomings of existing high-purity gas filling technologies, such as limited equipment functionality making them unsuitable for materials with diverse properties and a lack of highly integrated platforms for research and small-batch production, this application proposes a high-purity gas pilot-scale filling device and process to resolve these issues.

[0008] The technical solution of this application is as follows: On the one hand, this application provides a high-purity gas pilot filling device, including: a high-purity gas storage tank, an automatic regulating valve, a filling pump, a membrane press, and a cryogenic filling cabinet; The automatic regulating valve, filling pump, and membrane press are connected in parallel. One end of the valve is connected to the outlet of the premium tank through a pipeline, and the other end is connected to the inlet of the cryogenic filling cabinet through a pipeline.

[0009] Preferably, the high-purity container is used to store gaseous or liquid high-purity gases.

[0010] Preferably, the membrane press has a diaphragm inside.

[0011] Preferably, the membrane is made of polytetrafluoroethylene.

[0012] Preferably, the filling pump is used for conveying high-purity liquid media, and the automatic regulating valve and diaphragm press are used for conveying high-purity gas media.

[0013] On the other hand, this application provides a high-purity gas pilot filling process, including at least one of the following filling processes: membrane press pressurization filling process, temperature difference filling process, or pump delivery filling process; Membrane press press filling process: High-purity gas enters the membrane press from the concentrate tank, and is then transported to the cryogenic filling cabinet by the membrane press; Temperature difference filling process: A temperature difference is created between the premium tank and the cryogenic filling cabinet. The pressure difference during the temperature difference stroke is used to make the high-purity gas flow from the premium tank to the cryogenic filling cabinet through the automatic regulating valve. Pump delivery and filling process: For high-purity liquid substances, the high-purity liquid gas in the premium tank is delivered to the cryogenic filling cabinet by a filling pump.

[0014] Preferably, for gaseous media, a membrane press pressurization filling process or a temperature difference filling process is used; for liquid media, a pump delivery filling process is used.

[0015] Preferably, the temperature difference is 10~30℃.

[0016] The beneficial effects of this application are as follows: the overall structure of the device is compact, and the switching of each filling path can be achieved through valve control, making operation simple and convenient. Compared with traditional single-function filling devices, it eliminates the need for frequent equipment replacement or complex process adjustments, greatly improving the efficiency of small-scale filling operations. Attached Figure Description

[0017] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings of the embodiments will be briefly described below.

[0018] The accompanying drawings described below are only related to some embodiments of this application and are not intended to limit the scope of this application.

[0019] In the attached diagram: Figure 1 This is a diagram of the high-purity gas pilot filling device for this application.

[0020] 1. Premium filling tank; 2. Filling pump; 3. Automatic regulating valve; 4. Membrane press; 5. Cryogenic filling cabinet. Detailed Implementation

[0021] To further illustrate the technical means and effects adopted by this application in order to achieve the intended purpose of the invention, the following detailed description of the specific implementation methods, structures, features and effects of this application is provided in conjunction with the accompanying drawings and preferred embodiments.

[0022] Device Examples This embodiment provides a high-purity gas pilot filling device; see [link / reference]. Figure 1 It includes: a high-purity gas storage tank 1, an automatic regulating valve 3, a filling pump 2, a membrane press 4, and a cryogenic filling cabinet 5; The automatic regulating valve 3, filling pump 2, and membrane press 4 are connected in parallel. One end of them is connected to the outlet of the premium tank 1 through a pipeline, and the other end is connected to the inlet of the low-temperature filling cabinet 5 through a pipeline.

[0023] Premium tank 1 can store high-purity gases in different media, which can be in gaseous or liquid form.

[0024] Control valves, pressure detection elements, and temperature monitoring elements are installed on the pipelines.

[0025] The diaphragm inside the membrane press 4 is made of polytetrafluoroethylene.

[0026] The required temperature difference is formed between the low-temperature filling cabinet 5 and the premium tank 1.

[0027] The filling pump 2 is used for conveying high-purity liquid media, and the automatic regulating valve 3 and the diaphragm press 4 are used for conveying high-purity gas media.

[0028] Implementation principle of the device: Membrane press 4 pressurization and filling process: This process is suitable for high-purity gas media, relying on membrane press 4 to achieve gas pressurization and filling. Before operation, check the pipeline sealing. Then, open the outlet valve of the high-purity tank 1 to allow high-purity gas to enter the membrane press 4. After the membrane press 4 starts, its corrosion-resistant diaphragm, made of polytetrafluoroethylene (PTFE), begins to reciprocate, pressurizing the gas to the set pressure. During the pressurization process, the diaphragm material prevents gas contamination. After the gas is output from the membrane press 4, it is transported to the cryogenic filling cabinet 5 through pipeline. The pressure monitoring element tracks the filling pressure in real time to ensure that it does not exceed the cylinder's pressure limit. After filling is completed, first shut down the membrane press 4, then close the valve of the high-purity tank 1, and finally discharge the residual gas to prevent cross-contamination. This process has high pressurization efficiency and is suitable for low-boiling-point gases.

[0029] Thermostatic Filling Process: This process utilizes the temperature difference between the high-purity gas tank 1 and the cryogenic filling chamber 5 to create a pressure difference, driving the spontaneous flow of gas. It is suitable for heat-sensitive high-purity gases. Before operation, the system is regulated by temperature monitoring elements: the high-purity gas tank 1 is first heated or kept at a relatively high temperature, while the cryogenic filling chamber 5 is cooled to the required temperature, creating a temperature gradient of 10-30℃. This temperature difference causes the gas pressure in the high-purity gas tank 1 to be higher than that in the cryogenic filling chamber 5, generating a pressure difference. Subsequently, the automatic regulating valve 3 is opened, and the gas flows from the high-purity gas tank 1 to the cryogenic filling chamber 5 under the action of the pressure difference. The automatic regulating valve 3 dynamically adjusts its opening based on real-time flow data to ensure smooth flow; the pressure detection element monitors changes in the pressure difference to maintain the flow rate. After the process is completed, the automatic regulating valve 3 is closed first, and then the system temperature is balanced to prevent thermal stress damage to the pipeline. This process has low energy consumption and requires no mechanical power.

[0030] Pump-based filling process: This process is specifically designed for high-purity liquid media, using filling pump 2 for liquid transfer. The inlet valve of filling pump 2 is opened, allowing the liquid to enter the pump body under gravity or differential pressure. After pump 2 starts, the liquid flows directly to the cryogenic filling cabinet 5 via pipeline. During pumping, pressure detection elements ensure the pipeline pressure remains within a safe range to prevent cavitation or liquid hammer. After filling is complete, filling pump 2 is stopped first, then the inlet and outlet valves are closed, and the pipeline is purged to reduce residue. This process is highly efficient and suitable for batch filling.

[0031] Examples 1-3 are based on the devices provided in the device embodiments, and their specific operations are as follows: Example 1 This embodiment provides a small-scale test of argon gas pressurization and filling, based on a membrane pressurization and filling process, as detailed below: A small-scale argon pressurization and filling test was conducted to pressurize and fill high-purity 5N argon gas, providing data support for industrial-scale design. The goal was to achieve a post-filling argon pressure of 15 MPa and obtain filling times under different membrane press exhaust rates. The outlet valve of the high-purity tank, and the inlet and outlet valves of the membrane press were opened to ensure smooth entry of argon gas into the press. The membrane press was started, and the outlet pressure was set to 15 MPa. The exhaust rates were sequentially set to 50 Nm³ / h, 100 Nm³ / h, and 150 Nm³ / h. The diaphragm began reciprocating to pressurize the argon gas. This filling operation involved 6 cylinders, requiring the filling of 48 47mm steel cylinders. Pressure changes were monitored in real-time using the pressure monitoring element at the membrane press outlet. Once the pressure reached the required high pressure of 15 MPa, the membrane press was kept running stably, continuously filling the high-pressure cylinders. During the filling process, pressure changes were closely monitored, and the membrane press operating parameters were adjusted promptly if pressure fluctuations occurred. After filling, the membrane press was shut down first, followed by the sequential closing of each valve. The final experiment, based on the purity of 5N argon gas, showed that filling 48 cylinders at membrane press rates of 50Nm³ / h, 100Nm³ / h, and 150Nm³ / h required 2.7, 2.4, and 2.2 hours, respectively. The argon gas was tested and found to be of acceptable quality, providing reliable experimental data for industrialization.

[0032] Example 2 This embodiment provides a small-scale liquid nitrogen filling operation based on a pump delivery filling process, as detailed below: A chemical company conducted a small-scale liquid nitrogen filling test. To meet the requirements of small-batch, high-precision filling, the pump delivery path of this device was tested. Liquid nitrogen, as a high-purity gas, was stored in a purification tank. When filling began, the pump delivered the liquid nitrogen to the cylinders in the filling cabinet according to a set flow rate. Reliable experimental data was obtained by adjusting the pump parameters. Delivery equipment: cryogenic centrifugal pump, maximum flow rate: 100 L / min, maximum head: 150 m.

[0033] The experimental results are shown in Table 1: Table 1 Serial number Pump speed Outlet flow rate (L / min) Filling pressure (MPa) Target filling amount (kg) Actual filling amount (kg) Filling error (kg) Completion time (s) Note 1 30% 12 0.5 30.00 30.05 +0.05 188 Flow rate is stable, process is smooth 2 50% 20 0.7 30.00 29.91 -0.09 113 Process is stable, high efficiency 3 70% 28 0.9 30.00 30.15 +0.15 81 Large error, slight cavitation noise 4 40% 16 0.6 15.00 14.97 -0.03 56 Small batch filling, good precision 5 40% 16 0.6 45.00 44.78 -0.22 169 Close to the safe volume of the cylinder, precision still meets the standard Example 3 This embodiment provides a small-scale test experiment of high-purity nitrogen temperature difference filling, based on a temperature difference filling process, and optimizes the filling of heat-sensitive high-purity gases. The purpose of the experiment is to verify the efficiency, stability, and gas purity maintenance capability of the temperature difference driven filling mode, providing experimental basis for high-purity gas delivery in semiconductor material processing.

[0034] The experiment used the aforementioned high-purity gas pilot-scale filling device, with the following specific equipment parameters: a 50L high-purity gas tank with a design pressure of 20MPa, containing high-purity 5N nitrogen; a cryogenic filling cabinet equipped with a refrigeration unit, with a temperature control range of -50℃ to room temperature; an automatic regulating valve with a flow rate adjustment accuracy of ±1%; and a piping system equipped with a pressure sensor and a platinum resistance thermometer. Before the experiment, all pipelines were purged three times with high-purity nitrogen to ensure no cross-contamination.

[0035] The specific experiment is as follows: First, the temperature control system stabilized the premium gas tank at 25℃, while simultaneously activating the cooling module of the cryogenic filling cabinet to lower its internal temperature to 5℃, creating a 20℃ temperature gradient. This temperature difference resulted in a higher gas pressure inside the premium gas tank compared to the cryogenic filling cabinet, generating a driving pressure difference of approximately 11.9 MPa. Subsequently, the automatic regulating valve was opened, with an initial opening of 30%, allowing the gas to flow under the pressure difference. During the filling process, a pressure sensor monitored the pressure difference in real time, and the automatic regulating valve dynamically adjusted its opening based on the pressure difference changes, maintaining a stable flow rate of 5-10 L / min. The filling objective was to transfer 20 kg of high-purity nitrogen gas into the 47 L storage tank of the cryogenic filling cabinet, with the final filling pressure set at 10 MPa. Experimental data are shown in Table 2. The results analysis indicates that the temperature difference filling process effectively maintains gas purity, and the filling efficiency is positively correlated with the temperature difference. When the temperature difference is 20℃, the pressure fluctuation during the filling process is minimal, demonstrating the precise control capability of the automatic regulating valve. Table 2 Experimental group Temperature difference (°C) Initial pressure difference (MPa) Average flow rate (L / min) Filling time (min) Final gas purity Pressure fluctuation range (MPa) 1 10 6.2 3.5 38.2 99.998% ±0.15 2 20 11.9 7.8 17.1 99.999% ±0.08 3 30 17.3 12.4 10.8 99.997% ±0.21 The above description is merely a preferred embodiment of this application and is not intended to limit this application in any way. Although this application has been disclosed above with reference to preferred embodiments, it is not intended to limit this application. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the technical solution of this application. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of this application without departing from the scope of the technical solution of this application shall still fall within the scope of the technical solution of this application.

Claims

1. A high-purity gas pilot-scale filling device, characterized in that, include: The high-purity gas storage tank (1), automatic regulating valve (3), filling pump (2), membrane press (4) and cryogenic filling cabinet (5) are used for storing high-purity gases. The automatic regulating valve (3), filling pump (2), and membrane press (4) are connected in parallel. One end of the valve is connected to the outlet of the premium tank (1) through a pipeline, and the other end is connected to the inlet of the low-temperature filling cabinet (5) through a pipeline.

2. The high-purity gas pilot filling device according to claim 1, characterized in that, The high-purity tank (1) is used to store gaseous or liquid high-purity gases.

3. The high-purity gas pilot-scale filling device according to claim 1, characterized in that, The membrane press (4) has a diaphragm inside.

4. The high-purity gas pilot filling device according to claim 3, characterized in that, The diaphragm is made of polytetrafluoroethylene.

5. The high-purity gas pilot filling device according to claim 1, characterized in that, The filling pump (2) is used for conveying high-purity liquid media, and the automatic regulating valve (3) and the diaphragm press (4) are used for conveying high-purity gas media.

6. A high-purity gas pilot-scale filling process, based on the high-purity gas pilot-scale filling device according to claim 1, characterized in that, Including at least one of the following filling processes: membrane press (4) pressurization filling process, temperature difference filling process or pump delivery filling process; Membrane press (4) pressurization and filling process: High-purity gas enters the membrane press (4) from the fine product tank (1), and the high-purity gas is transported to the low-temperature filling cabinet (5) through the membrane press (4). Temperature difference filling process: A temperature difference is formed between the premium tank (1) and the low temperature filling cabinet (5). The pressure difference formed by the temperature difference is used to make the high-purity gas flow from the premium tank (1) to the low temperature filling cabinet (5) through the automatic regulating valve (3). Pump delivery and filling process: For liquid high-purity substances, the liquid high-purity gas in the fine tank (1) is delivered to the cryogenic filling cabinet (5) by the filling pump (2).

7. The high-purity gas pilot filling process according to claim 6, characterized in that, For gaseous media, a membrane press (4) is used for pressurization and filling or a temperature difference filling process; for liquid media, a pump is used for delivery and filling.

8. The high-purity gas pilot filling process according to claim 6, characterized in that, The temperature difference is 10~30℃.

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