A method and apparatus for full-process safety control of silane filling

Abstract

The application discloses a kind of silane filling whole-process safety control method and device, belong to silane filling technical field, it is pre-recorded by PLC system filling pressure, filling weight, replacement frequency, helium leak detection index etc. Safety parameters, tank car is positioned after distinguishing new, old tank car executes different pre-treatment sequence control: new tank car is completed nitrogen purging, vacuumizing, silane passivation, old tank car carries out residual gas replacement and helium leak detection; After pre-treatment, unqualified is forced to return to replace, and qualified silane is filled after two-stage gradient pressurization by diaphragm compressor, whole process monitors pressure, weight, overpressure, excess, equipment failure triggers interlock protection, automatically cuts material or switches standby station, and pipeline residual gas is recycled to disproportionation system after filling is finished, and then purging is disassembled.The application realizes whole-process automatic closed-loop control, eliminates artificial misoperation hidden danger, and considers tank car differentiating management and control as well as high-purity medium guarantee and residual gas recycling.

Description

Technical Field

[0001] This invention relates to the field of silane filling technology, and more specifically, to a method and apparatus for full-process safety control of silane filling. Background Technology

[0002] Silane is a key gas in the electronics, photovoltaic, and special alloy manufacturing industries, and its filling operations involve high-risk characteristics such as high pressure, flammability, and explosiveness. Currently, silane tanker filling in the industry mainly relies on manual operation and conventional instrument control, which has significant drawbacks: the filling process has a low degree of standardization, each step is independent and decentralized, and there is a lack of integrated control throughout the entire process. Operators need to manually switch valves, record data, and judge operating conditions, which can easily lead to leakage or overpressure accidents due to misoperation. At the same time, the existing process fails to perform differentiated pretreatment based on the risk characteristics of new and old tankers. New tankers require thorough purging, replacement, and passivation treatment, while old tankers focus on residual gas replacement and leak detection. However, the "one-size-fits-all" operation mode results in incomplete passivation or insufficient residual treatment, and there is a lack of standardized mandatory return verification mechanisms, making it easy for unqualified products to flow into the next process.

[0003] Furthermore, if the residual high-pressure silane gas in the pipeline is directly vented after filling, it will not only waste materials but also increase safety risks. Existing technologies lack a specific control process for safely recovering residual silane to the disproportionation system. Therefore, in order to address the above issues, there is an urgent need for a standardized control method and device that covers the entire filling process and integrates differentiated pretreatment and safe recovery functions. Summary of the Invention

[0004] The purpose of this invention is to provide a method and apparatus for full-process safety control of silane filling, so as to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a method for full-process safety control of silane filling, comprising the following steps: S1. Pre-filling parameter preset: The safety parameters for silane filling are preset through the PLC system. The safety parameters include the upper limit of filling pressure, the target value of filling weight, the number of replacements and the helium leak detection qualification index. S2. Tank Car Entry and Pre-treatment: After the tank car enters the filling position, differentiated pre-treatment sequential control is performed according to the tank car type. Among them, new tank cars are subject to initial purging and replacement sequential control and silane passivation sequential control, while old tank cars are subject to residual silane replacement sequential control and leak detection analysis sequential control. S3. Pre-filling analysis and judgment: Silane purity analysis is performed on the pre-treated tank truck. If the analysis is qualified, the filling sequence control is entered. If the analysis is unqualified, the truck is forced to return to the pre-treatment step and replace it again until it is qualified. S4. Filling and Interlock Protection: After the compressor is started to pressurize the silane gas, the filling sequence control is executed to fill the silane gas into the tank truck. During the filling process, the filling pressure and filling weight are monitored in real time. When an abnormality is detected, the interlock protection action is triggered. S5. Post-filling treatment: After filling is completed, post-treatment sequential control is performed to recover the residual silane gas in the pipeline to the disproportionation system. After purging and replacement, the pipeline is disassembled and sealed.

[0006] Preferably, in step S2, the initial purging and displacement sequential control and silane passivation sequential control performed on the new tanker specifically include: S201. Detect dew point and micro-oxygen content; S202. Use nitrogen to purge and replace the tank truck; S203, Evacuate to -90KPa; S204. Introduce silane gas into the tank truck and pressurize it to 0.3 MPa. Let it stand for 8 hours for silane passivation. S205. Analyze and check whether the purity of silane gas is up to standard; S206. If the test fails, the tank truck shall be depressurized, evacuated, and then replaced with silane gas again until the analysis is satisfactory.

[0007] Preferably, in step S2, the residual silane replacement sequence control and leak detection analysis sequence control performed on the old tanker specifically includes: S211, Perform residual silane replacement cis-control; S212, Perform positive and negative pressure tests and helium leak detection; S213. Open the tank truck valve to sample and analyze residual gas. S214. If the analysis fails, repeat the analysis after depressurization and replacement, or force a return to the residual silane replacement sequential control until the analysis passes.

[0008] Preferably, in step S1, the number of replacements is preset to be ≥30.

[0009] Preferably, in step S3, the silane gas is heated to 20°C by a preheater from the tank area and then enters the full high-pressure analysis panel for analysis. Qualified products are sent to the silane gas buffer tank for pressure stabilization, and unqualified products are sent to the disproportionation tower for recovery.

[0010] Preferably, in step S4, the compressor performs gradient filling, and the interlock protection action includes: When the filling pressure exceeds the preset threshold, the filling feed is immediately shut off. Filling will automatically stop when the preset target weight is reached. When the filling weight deviates from the preset range, the system will alarm and stop filling; When the equipment malfunctions, it automatically switches to the backup filling station.

[0011] Preferably, in step S5, recovering the residual silane gas in the pipeline to the disproportionation system specifically involves: opening the shut-off valve on the filling panel for recovery to disproportionation and the shut-off valve on the main disproportionation pipe for recovery, sending the residual silane gas to the disproportionation tower for recovery, and reducing the panel pressure to 4-5 kg.

[0012] Preferably, in step S4, before starting the compressor, the method further includes: opening the compressor's second pressure equalization shut-off valve to equalize the pressure until the filling panel pressure is stable.

[0013] Preferably, in step S4, the silane gas is pressurized to 12.5 MPag and 40°C after being compressed and cooled in two stages by a diaphragm compressor, and then filled into the tank truck through the filling panel.

[0014] The present invention also provides a full-process safety control device for silane filling, comprising: The silane buffer section includes a silane gas preheater, a full high-pressure analysis panel, a silane gas buffer tank, and a silane gas recovery pipeline. The outlet of the silane gas preheater is connected to the inlet of the full high-pressure analysis panel, the qualified product outlet of the full high-pressure analysis panel is connected to the inlet of the silane gas buffer tank, and the unqualified product outlet of the full high-pressure analysis panel is connected to the recovery pipeline. The silane compression section includes multiple diaphragm compressors, the inlet of which is connected to the outlet of the silane gas buffer tank; The product filling section includes multiple filling positions, each of which is equipped with a filling panel. The inlet of the filling panel is connected to the outlet of the diaphragm compressor. The filling panel integrates filling pipeline, purging and replacement pipeline, sampling and analysis pipeline, residual gas venting pipeline and vacuum pipeline. The PLC / DCS control system is communicatively connected to the valves and sensors of the silane buffer section, silane compression section and product filling section, and is used to execute the full-process safety control method for silane filling as described above.

[0015] Compared with the prior art, the beneficial effects of the present invention are: I. This invention integrates the entire process sequential control logic through a PLC / DCS system to achieve standardized automatic control of silane filling from parameter preset, pre-processing, analysis and judgment, filling interlocking to post-processing and recycling. Combined with the valve interlocking mechanism, it effectively eliminates human error and greatly improves operational safety. 2. Different pretreatment sequential control and forced cycle verification processes are designed for new tank cars and old tank cars respectively. New tank cars undergo purging and replacement, vacuuming, pressurization and static passivation and purity analysis closed-loop verification. Old tank cars undergo residual replacement, positive and negative pressure testing, helium leak detection and residual gas analysis to ensure the thoroughness of treatment and product purity under different scenarios, and fundamentally prevent unqualified products from flowing into the filling process. Third, by establishing a real-time monitoring and multi-level interlocking protection mechanism for the entire filling process, emergency cut-off, filling stop and backup station switching are automatically executed when pressure exceeds the limit, weight is abnormal or equipment fails. At the same time, residual silane gas after filling is safely recovered to the disproportionation system through a dedicated pipeline, which reduces material waste and eliminates the risk of venting, thus comprehensively improving the inherent safety level and resource utilization rate of silane filling. Attached Figure Description

[0016] Figure 1 This is a flowchart illustrating the full-process safety control method for silane filling according to an embodiment of the present invention. Figure 2 This is a structural block diagram of the safety control device for the entire process of silane filling according to an embodiment of the present invention. Detailed Implementation

[0017] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0018] Please see Figure 1 The present invention provides a method for full-process safety control of silane filling, comprising the following steps: S1. Preset the safety parameters for silane filling through the PLC system. The safety parameters include the upper limit of filling pressure, the target value of filling weight, the number of replacements, and the helium leak detection qualification index.

[0019] The PLC inputs the aforementioned safety parameters based on the tanker type, volume, and process requirements, stores these parameters in its memory, and uses them as the basis for judgment in subsequent steps. The upper limit of the filling pressure is preferably set to 12.5 MPa based on the tanker's design pressure and the physical properties of silane. The target filling weight is set based on the tanker's rated load capacity. The preset replacement number is preferably ≥30 times to ensure that the air in the pipeline and tanker is fully replaced. The helium leak detection qualification index is set to a leakage rate preferably not exceeding 1×10⁻⁶. -6 Pa·m 3 / s, to ensure the system's sealing meets safety requirements.

[0020] S2. When the tank truck enters the filling position, differentiated pretreatment sequential control is performed according to the tank truck type. New tank trucks are subject to initial purging and replacement sequential control and silane passivation sequential control, while old tank trucks are subject to residual silane replacement sequential control and leak detection analysis sequential control.

[0021] Specifically, after the tanker truck enters the designated filling position, the operator eliminates static electricity by connecting the ground wire and connects the tanker truck's gas phase interface to the corresponding interface on the filling panel. The operator then uses a human-machine interface or barcode scanning to identify the tanker truck number and automatically determines whether the tanker truck is new or old, and then calls the corresponding pre-processing sequential control program.

[0022] New tank trucks contain air and moisture, so they need to undergo nitrogen purging, vacuuming, and silane passivation treatment in sequence to form a stable silane passivation layer on their inner walls to prevent silane from reacting with the metal substrate during subsequent filling. Old tank trucks contain residual silane gas from the previous filling, so residual silane replacement and leak testing are required to prevent residual gas from contaminating the product being filled or causing leakage risks.

[0023] The initial purging and replacement sequential control and silane passivation sequential control performed on the new tank truck specifically include: S201. Detect dew point and trace oxygen content. After the new tank truck is connected to the filling panel, first use a dew point meter and a trace oxygen analyzer to detect the dew point temperature and trace oxygen content of the gas inside the tank truck in order to assess the dryness and residual air volume inside the tank truck. The dew point is usually required to be below -60℃ and the trace oxygen content is required to be below 1ppm. If the initial value does not meet the requirements, the subsequent purging time needs to be extended.

[0024] S202. Use nitrogen to purge and replace the tank truck. The system opens the nitrogen inlet valve to introduce high-purity nitrogen (purity ≥99.999%) into the tank truck. At the same time, the exhaust valve is opened to use nitrogen to drive out the original air and moisture in the tank truck. This purging process is repeated. After each purging, the oxygen content and dew point at the outlet are measured until both reach the set indicators.

[0025] S203. After evacuating to -90KPa and passing the purging and replacement, the system closes the nitrogen valve and the exhaust valve, and turns on the vacuum pump to evacuate the tank truck, reducing the internal pressure of the tank truck to -90KPa, in order to further remove the residual moisture and gas molecules adsorbed on the inner wall of the tank truck, creating a clean substrate environment for subsequent silane passivation.

[0026] S204. Introduce silane gas into the tank truck and pressurize it to 0.3 MPa. Let it stand for 8 hours for silane passivation. Slowly open the silane inlet valve to introduce silane gas from the buffer tank into the tank truck, so that the tank truck pressure rises steadily to 0.3 MPa. Then close the inlet valve and keep it at this pressure for 8 hours.

[0027] S205. Analyze and check whether the purity of silane gas is qualified. Specifically, after the passivation and settling are completed, the system opens the sampling valve and introduces the silane gas in the tank truck into the online gas chromatograph for purity analysis to detect the main content of silane and the content of key impurities (such as hydrogen, oxygen, nitrogen, moisture, etc.).

[0028] S206. If the result is not satisfactory, the tank truck shall be depressurized and evacuated, and then replaced with silane gas again until the analysis is satisfactory. If the analysis result shows that the purity is not up to standard, the system will automatically determine that the passivation replacement is insufficient, open the depressurization valve to discharge the silane gas in the tank truck to the recovery system, and then repeat the vacuuming step of S203 and the silane replacement and analysis steps of S204-S205 until the analysis is satisfactory.

[0029] In addition, the follow-up control for residual silane replacement and leak detection performed on old tank trucks specifically includes: S211. Perform residual silane replacement sequential control. After the previous round of filling, the old tank truck usually has high-pressure silane gas remaining inside. The system first opens the tank truck exhaust valve to guide the residual silane gas to the recovery system for recovery. Then, nitrogen is introduced for replacement to further remove the residual silane gas in the pipeline and tank truck, preventing it from mixing with the air that enters later to form an explosive atmosphere.

[0030] S212. Perform positive and negative pressure tests and helium leak detection. The system sequentially performs positive pressure holding tests and negative pressure holding tests on the tank truck and connecting pipelines to verify the sealing integrity of the entire filling circuit.

[0031] During the positive pressure test, nitrogen gas is introduced into the system to the set pressure and the valve is closed. The pressure is observed to see if it decreases within the holding time. During the negative pressure test, the vacuum pump is started and evacuated to the set negative pressure, then shut off. The vacuum level is observed to be maintained. After both tests pass, a helium mass spectrometer leak detector is used to perform helium leak testing on key sealing points such as tank truck valves, flange connections, and welds. The leakage rate is not to exceed 1×10⁻⁶. -6 Pa·m 3 / s means it is qualified.

[0032] S213. Open the tank truck valve to sample and analyze residual gas. After the leak test is qualified, the system opens the tank truck sampling valve to introduce the residual gas in the tank truck into the analysis instrument to detect the content of residual silane and other impurities, so as to assess whether the atmosphere in the tank truck meets the filling requirements.

[0033] S214. If the analysis fails, the system will perform pressure relief and replacement and repeat the analysis, or force a return to the residual silane replacement sequence control until the analysis is qualified. Specifically, if the analysis results show that the purity of the residual silane is insufficient or the impurity content exceeds the standard, the system will automatically select to perform partial pressure relief and replacement and resample for analysis according to the degree of deviation, or directly force a return to the residual silane replacement sequence control in S211 to start from the beginning until all analysis results are qualified before entering the filling process.

[0034] S3. Perform silane purity analysis on the pretreated tank truck. If the analysis is qualified, proceed to the filling sequence control. If the analysis is unqualified, force return to the pretreatment step to replace the silane until it is qualified.

[0035] When executing S3, the system automatically opens the sampling valve of the tank truck, introduces the gas in the tank truck into the analytical instrument for silane purity detection. If the purity is ≥99.99%, it is judged as qualified, and the system automatically proceeds to the next step of the charging sequence control; if the purity does not reach the standard, the system issues an alarm prompt and automatically switches the valve, discharges the unqualified gas in the tank truck and re-executes the nitrogen replacement and vacuum pumping steps until the analysis is qualified before release.

[0036] Among them, the silane gas is heated to 20°C by the preheater from the tank farm and then enters the full-pressure analysis panel for analysis. Qualified products are sent to the silane gas buffer tank for pressure stabilization, and unqualified products are sent to the disproportionation tower for recovery. The temperature of the liquid silane outside the battery limit after vaporization from the tank farm is about -20°C, and the pressure is about 1.3MPa. If this low-temperature silane gas directly enters the analysis panel, it may cause pipeline freezing blockage and deviation of analysis results.

[0037] Therefore, the silane gas first enters the preheater to be heated to 20°C, so that the silane gas is completely vaporized and reaches a suitable analysis temperature, and then enters the full-pressure analysis panel for on-line purity analysis. The analysis panel has a built-in gas chromatograph and multiple sensors, which can simultaneously detect the purity of silane and the content of multiple impurities. The silane gas judged to be qualified is sent to the silane gas buffer tank for pressure stabilization storage to balance the flow fluctuation between the upstream incoming material and the downstream charging; the silane gas judged to be unqualified is sent to the disproportionation tower through a special recovery pipeline for chemical recovery treatment, so as to prevent unqualified products from entering the downstream to pollute the product pipeline or cause waste.

[0038] S4. After the compressor is started to pressurize the silane gas, the charging sequence control is executed to charge the silane gas into the tank truck. During the charging process, the charging pressure and charging weight are monitored in real time, and the interlock protection action is triggered when an abnormality is detected.

[0039] The compressor extracts the silane gas from the buffer tank and pressurizes it to the set pressure, then sends it to the charging pipeline. The regulating valve on the charging panel automatically adjusts the opening according to the preset charging curve to realize gradient charging. During the charging process, the pressure transmitter collects the pressure signals of the pipeline and the tank truck in real time, and the weighing sensor collects the weight gain signal of the tank truck in real time. Both signals are transmitted to the PLC / DCS control system for real-time comparison. When any parameter exceeds the preset safety threshold, the system does not rely on manual judgment and automatically triggers the corresponding interlock protection action.

[0040] Wherein, before starting the compressor, the method further comprises: opening the second-stage pressure equalizing shut-off valve of the compressor to equalize the pressure until the pressure of the charging panel is stable. In the charging process of the old tank truck, when all the pretreatment and analysis judgments are qualified, the pipeline between the charging panel and the tank truck is connected.

[0041] At this time, the pressure of silane gas in the buffer tank is about 1.3 MPa, while the pressure of the filling panel and tank truck system is in a negative pressure or normal pressure state after vacuuming. If the compressor is started directly, the huge pressure difference will impact the compressor and pipeline, affecting the equipment life and filling stability. Therefore, before starting the compressor, the system first opens the compressor's second pressure equalization shut-off valve, allowing the low-pressure silane gas in the buffer tank to slowly flow into the filling pipeline and tank truck. When the pressure gauge on the filling panel shows that the pressure is stable and basically consistent with the outlet pressure of the buffer tank, the system confirms that the pressure difference has been eliminated before allowing the compressor to start. This effectively protects the compressor from the impact of starting under load, while ensuring a stable flow rate in the initial stage of filling.

[0042] The compressor performs gradient filling, and the interlock protection actions include: When the filling pressure exceeds the preset threshold, the filling feed is immediately shut off. Filling will automatically stop when the preset target weight is reached. When the filling weight deviates from the preset range, the system will alarm and stop filling; When the equipment malfunctions, it automatically switches to the backup filling station.

[0043] In this embodiment, gradient filling refers to the compressor operating at a lower flow rate at the initial stage of filling, and gradually increasing the filling rate after the tank truck pressure stabilizes, to avoid the impact of a sudden pressure rise on the tank truck and pipeline. The interlock protection specifically includes: Regarding pressure monitoring: The system is equipped with high-precision pressure transmitters at the filling pipeline and tank truck inlet. When the monitored pressure exceeds the preset upper limit of filling pressure, such as 12.5MPa, the control system issues a command to close the filling feed shut-off valve and at the same time open the emergency pressure relief valve to release the pipeline pressure to a safe value.

[0044] In terms of weight monitoring: the weighing sensor collects the weight gain data of the tank truck in real time. When the cumulative filling weight reaches the preset target value, the system automatically closes the main filling valve and stops the compressor to achieve accurate quantitative filling. If the actual filling weight deviates from the target value range, such as exceeding the target value ±2%, the system judges it as abnormal and simultaneously triggers an audible and visual alarm and automatically stops filling to prevent underfilling or overfilling.

[0045] Regarding equipment failures: When critical equipment such as compressors, valves, or sensors malfunction, the system automatically switches the filling task to a backup filling station to ensure uninterrupted filling operations. At the same time, it isolates the faulty equipment and notifies maintenance personnel for repair.

[0046] S5. After filling is completed, post-processing sequential control is performed to recover the residual silane gas in the pipeline to the disproportionation system. After purging and replacement, the pipeline is disassembled and sealed. After filling reaches the target weight, the system automatically closes the main filling valve and stops the compressor. Then, the recovery pipeline valve is opened to guide the high-pressure silane gas remaining in the filling panel and connecting pipeline to the disproportionation tower for chemical recovery treatment. After the pipeline pressure drops to a safe range, the system automatically performs nitrogen purging and replacement to completely replace the residual gas in the pipeline.

[0047] Specifically, recovering residual silane gas in the pipeline to the disproportionation system involves opening the shut-off valve on the filling panel for recovery to disproportionation and the shut-off valve on the main disproportionation pipe, sending the residual silane gas to the disproportionation tower for recovery, and reducing the panel pressure to 4-5 kg.

[0048] After filling is completed, there is still high-pressure silane gas with a pressure of about 6-8 MPa in the filling panel and connecting pipeline. The system first confirms that the disproportionation tower is in the receiving state, and then opens the recovery shut-off valve on the filling panel and the shut-off valve on the disproportionation main pipe in sequence. The residual silane gas is sent into the disproportionation tower through the dedicated recovery pipeline by using the pressure difference.

[0049] The disproportionation tower contains a catalyst that chemically converts silane gas, enabling the resource recovery and utilization of the material. As residual gas is continuously discharged, the pressure on the panel and in the pipeline gradually decreases. When the pressure drops to 0.4-0.5 MPa, the system automatically closes the recovery shut-off valve. At this point, the pressure in the pipeline is within a safe range, facilitating subsequent nitrogen purging and pipeline disassembly operations. This also avoids the material waste and environmental risks caused by directly discharging a large amount of high-pressure silane gas into the venting system.

[0050] like Figure 2 As shown, embodiments of the present invention also provide a full-process safety control device for silane filling, comprising: The silane buffer section includes a silane gas preheater, a full high-pressure analysis panel, a silane gas buffer tank, and a silane gas recovery pipeline. The outlet of the silane gas preheater is connected to the inlet of the full high-pressure analysis panel. The qualified product outlet of the full high-pressure analysis panel is connected to the inlet of the silane gas buffer tank, and the unqualified product outlet of the full high-pressure analysis panel is connected to the recovery pipeline.

[0051] The silane gas preheater E0401A / B adopts a shell-and-tube heat exchange structure. The full high-pressure analysis panel integrates an online gas chromatograph, dew point meter, and micro-oxygen analyzer to perform real-time full-component analysis of high-pressure silane gas. The silane gas buffer tank V0401 is a horizontal pressure vessel with a volume designed according to the peak filling flow rate. It is used for pressure stabilization and temporary storage of qualified silane gas. The recovery pipeline is an independent pipeline, which directly guides unqualified products to the disproportionation tower for recovery and treatment, avoiding cross-contamination.

[0052] The silane compression section includes multiple diaphragm compressors, with the inlet of each compressor connected to the outlet of a silane gas buffer tank.

[0053] Specifically, this embodiment is equipped with four diaphragm compressors C0401A-D, each with a rated flow rate of 210 Nm³. 3 The compressors are arranged in parallel and can be flexibly combined to operate according to filling requirements. Each compressor is equipped with a primary compression cylinder, an intercooler, a secondary compression cylinder, and an aftercooler. The outlet pressure can reach 12.5MPa and the outlet temperature is 40℃.

[0054] The product filling section includes multiple filling positions, each equipped with a filling panel. The inlet of the filling panel is connected to the outlet of the diaphragm compressor. The filling panel integrates filling pipeline, purging and replacement pipeline, sampling and analysis pipeline, residual gas venting pipeline and vacuuming pipeline.

[0055] This embodiment has 6 tank truck filling positions and 1 pretreatment replacement and passivation position. It can carry out multiple filling operations simultaneously or individually. Each filling panel is an integrated modular design, which integrates filling pipeline, purging and replacement pipeline, sampling and analysis pipeline, residual gas venting pipeline and vacuum pipeline. The pipelines are connected by valve interlocking logic to achieve safe switching, ensuring that only one functional pipeline is in the conducting state at any time.

[0056] The PLC / DCS control system is communicatively connected to the valves and sensors in the silane buffer section, silane compression section, and product filling section, and is used to execute the method of this embodiment.

[0057] Specifically, the PLC / DCS control system consists of a central control room operator station, field control stations, a communication bus, and various I / O modules, enabling bidirectional communication with pressure transmitters, temperature sensors, load cells, valve actuators, compressor motors, and other equipment in each section.

[0058] The control system has pre-stored the sequential control program logic, safety parameter thresholds and interlocking protection rules of the above embodiments, and can automatically execute the entire process of safety control from parameter preset to post-processing. At the same time, it can display the equipment operating status, process parameter trends and alarm information to the operator in real time through the human-machine interface.

[0059] In addition, the system is equipped with a GDS combustible gas detection system, which deploys multiple combustible gas detectors in the filling area. Once a silane leak is detected, the GDS system will independently trigger an emergency shut-off of the filling feed, providing multiple redundancy protections for safety control.

[0060] In summary, this invention integrates full-process sequential control logic through a PLC / DCS system to achieve standardized automatic control of silane filling from parameter preset, pre-processing, analysis and judgment, filling interlocking to post-processing and recycling. Combined with the valve interlocking mechanism, it effectively eliminates human error and significantly improves operational safety. Differentiated pre-processing sequential control and forced cycle verification processes are designed for new and old tank cars. New tank cars undergo purging and replacement, vacuuming, pressurization and static passivation, and purity analysis closed-loop verification. Old tank cars undergo residual replacement, positive and negative pressure testing, helium leak detection, and residual gas analysis to ensure thorough processing and product purity in different scenarios, fundamentally preventing unqualified products from entering the filling process. By establishing a real-time monitoring and multi-level interlocking protection mechanism for the entire filling process, emergency cut-off, filling stop, and backup station switching are automatically executed when pressure exceeds limits, weight is abnormal, or equipment malfunctions occur. At the same time, residual silane gas after filling is safely recovered to the disproportionation system through a dedicated pipeline, which reduces material waste and eliminates the risk of venting, thus comprehensively improving the inherent safety level and resource utilization rate of silane filling.

[0061] All parts not described in this invention are the same as or can be implemented using existing technology. Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for full-process safety control of silane filling, characterized in that: Includes the following steps: S1. Pre-filling parameter preset: The safety parameters for silane filling are preset through the PLC system. The safety parameters include the upper limit of filling pressure, the target value of filling weight, the number of replacements and the helium leak detection qualification index. S2. Tank Car Entry and Pre-treatment: After the tank car enters the filling position, differentiated pre-treatment sequential control is performed according to the tank car type. Among them, new tank cars are subject to initial purging and replacement sequential control and silane passivation sequential control, while old tank cars are subject to residual silane replacement sequential control and leak detection analysis sequential control. S3. Pre-filling analysis and judgment: Silane purity analysis is performed on the pre-treated tank truck. If the analysis is qualified, the filling sequence control is entered. If the analysis is unqualified, the truck is forced to return to the pre-treatment step and replace it again until it is qualified. S4. Filling and Interlock Protection: After the compressor is started to pressurize the silane gas, the filling sequence control is executed to fill the silane gas into the tank truck. During the filling process, the filling pressure and filling weight are monitored in real time. When an abnormality is detected, the interlock protection action is triggered. S5. Post-filling treatment: After filling is completed, post-treatment sequential control is performed to recover the residual silane gas in the pipeline to the disproportionation system. After purging and replacement, the pipeline is disassembled and sealed.

2. The method for full-process safety control of silane filling according to claim 1, characterized in that: In step S2, the initial purging and displacement sequential control and silane passivation sequential control performed by the new tanker truck specifically include: S201. Detect dew point and micro-oxygen content; S202. Use nitrogen to purge and replace the tank truck; S203, Evacuate to -90KPa; S204. Introduce silane gas into the tank truck and pressurize it to 0.3 MPa. Let it stand for 8 hours for silane passivation. S205. Analyze and check whether the purity of silane gas is up to standard; S206. If the test fails, the tank truck shall be depressurized, evacuated, and then replaced with silane gas again until the analysis is satisfactory.

3. The method for full-process safety control of silane filling according to claim 1, characterized in that: In step S2, the residual silane replacement sequential control and leak detection analysis sequential control performed on the old tanker specifically include: S211, Perform residual silane replacement cis-control; S212, Perform positive and negative pressure tests and helium leak detection; S213. Open the tank truck valve to sample and analyze residual gas. S214. If the analysis fails, repeat the analysis after depressurization and replacement, or force a return to the residual silane replacement sequential control until the analysis passes.

4. The method for full-process safety control of silane filling according to claim 1, characterized in that: In step S1, the number of replacements is preset to be ≥30.

5. The method for full-process safety control of silane filling according to claim 1, characterized in that: In step S3, silane gas is heated to 20°C by a preheater from the tank area and then enters the full high-pressure analysis panel for analysis. Qualified products are sent to the silane gas buffer tank for pressure stabilization, while unqualified products are sent to the disproportionation tower for recovery.

6. The method for full-process safety control of silane filling according to claim 1, characterized in that: In step S4, the compressor performs gradient filling, and the interlock protection action includes: When the filling pressure exceeds the preset threshold, the filling feed is immediately shut off. Filling will automatically stop when the preset target weight is reached. When the filling weight deviates from the preset range, the system will alarm and stop filling; When the equipment malfunctions, it automatically switches to the backup filling station.

7. The method for full-process safety control of silane filling according to claim 1, characterized in that: In step S5, recovering the residual silane gas in the pipeline to the disproportionation system specifically involves: opening the shut-off valve on the filling panel for recovery to disproportionation and the shut-off valve on the main disproportionation pipe for recovery, sending the residual silane gas to the disproportionation tower for recovery, and reducing the panel pressure to 4-5 kg.

8. The method for full-process safety control of silane filling according to claim 6, characterized in that: S4 further includes, before starting the compressor: opening the compressor's second pressure equalization shut-off valve to equalize the pressure until the filling panel pressure is stable.

9. The method for full-process safety control of silane filling according to claim 6, characterized in that: In step S4, the silane gas is pressurized to 12.5 MPa and 40°C after being compressed and cooled in two stages by a diaphragm compressor, and then filled into the tank truck through the filling panel.

10. A full-process safety control device for silane filling, characterized in that, include: The silane buffer section includes a silane gas preheater, a full high-pressure analysis panel, a silane gas buffer tank, and a silane gas recovery pipeline. The outlet of the silane gas preheater is connected to the inlet of the full high-pressure analysis panel, the qualified product outlet of the full high-pressure analysis panel is connected to the inlet of the silane gas buffer tank, and the unqualified product outlet of the full high-pressure analysis panel is connected to the recovery pipeline. The silane compression section includes multiple diaphragm compressors, the inlet of which is connected to the outlet of the silane gas buffer tank; The product filling section includes multiple filling positions, each of which is equipped with a filling panel. The inlet of the filling panel is connected to the outlet of the diaphragm compressor. The filling panel integrates filling pipeline, purging and replacement pipeline, sampling and analysis pipeline, residual gas venting pipeline and vacuum pipeline. The PLC / DCS control system is communicatively connected to the valves and sensors of the silane buffer section, silane compression section and product filling section, and is used to execute the method described in any one of claims 1 to 9.

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