A system and method for filling ultrapure ammonia tank trucks and recovering residual liquid.

Abstract

This invention relates to a system and method for filling ultrapure ammonia tank trucks and recovering residual liquid; it includes an ultrapure ammonia purification device and an ammonia recovery unit, comprising several tank trucks and several filling units corresponding to each tank truck; the filling unit includes a liquid phase filling panel and a gas phase filling panel; the liquid phase filling panel is equipped with an ultrapure ammonia filling pipeline and a liquid phase recovery pipeline section; the gas phase filling panel is equipped with a gas phase recovery pipeline section; the inlet end of the gas phase recovery pipeline section is connected to the gas phase filling valve of the corresponding tank truck, and the outlet end of the gas phase recovery pipeline section is connected to the ammonia recovery unit; it has the characteristics of realizing the fractional recovery and effective tracking and detection of ultrapure ammonia, improving filling efficiency while reducing ultrapure ammonia consumption, and ensuring the quality of ultrapure ammonia products.

Description

Technical Field

[0001] This invention relates to the field of ultrapure ammonia filling technology, specifically to a system and method for filling ultrapure ammonia tank trucks and recovering residual liquid. Background Technology

[0002] Ultra-pure ammonia (purity not less than 99.99999%) is a very important specialty gas, widely used in industries such as semiconductor integrated circuits (ICs), liquid crystal displays (LCDs), semiconductor light-emitting devices (LEDs), and solar photovoltaics. In recent years, my country's solar cell and semiconductor industries have developed rapidly, requiring large quantities of ultra-pure ammonia as a nitrogen source during production. Currently, ultra-pure ammonia is mostly supplied via tank trucks. At the customer's site, the tank truck uses its own electric heating device to vaporize liquid ammonia, supplying it to the user's pipeline through the tank truck's gas phase port. Because ultra-pure ammonia contains trace amounts of moisture, and moisture has a higher boiling point than ammonia, the moisture concentrates at the bottom of the tank truck during vaporization. When the concentrated moisture content exceeds the required value, the tank truck stops supplying gas, and the remaining liquid ammonia is returned to the ultra-pure ammonia production plant for recycling. The tank truck is then treated before refilling. Therefore, tank truck treatment and filling technology are crucial to ensuring the quality of ultra-pure ammonia products.

[0003] Most existing tank truck handling and filling devices use the tank truck's built-in electric heating device to vaporize the liquid ammonia inside the tank truck. During this process, both gaseous and liquid ammonia in the tank truck enter the waste ammonia storage tank. After the tank truck is filled, product quality analysis only analyzes the gas phase indicators in the tank truck. The traditional tank truck handling and filling method has the following defects: 1. The gas and liquid phases in the tank truck are not separated and recovered, resulting in the waste of high-quality ammonia, thereby increasing the cost of ultrapure ammonia; 2. The method of only testing the gas phase of high-purity ammonia after filling cannot guarantee the quality of high-purity ammonia in the tank truck. Summary of the Invention

[0004] The purpose of this invention is to provide a system and method for filling ultrapure ammonia tank trucks and recovering residual liquid, 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:

[0006] A system for filling ultrapure ammonia tank trucks and recovering residual liquid is disclosed. The system includes an ultrapure ammonia purification device and an ammonia recovery unit, as well as several tank trucks and several filling units corresponding to each tank truck. Each filling unit includes a liquid phase filling panel and a gas phase filling panel for filling liquid-phase ultrapure ammonia and for separately recovering residual gas and liquid phases from the tank trucks. The liquid phase filling panel is equipped with at least an ultrapure ammonia filling pipeline with a filling valve, and a liquid phase detection and separation recovery system for the liquid phase inside the tank trucks. The ultrapure ammonia filling pipeline has an inlet connected to an ultrapure ammonia purification unit, and an outlet connected to the corresponding tank truck's liquid phase filling valve via a liquid phase recovery pipeline. The outlet of the liquid phase recovery pipeline is connected to the ammonia recovery unit. The gas phase filling panel contains at least one gas phase recovery pipeline for detecting the gas phase inside the tank truck and for gas phase recovery. The inlet of the gas phase recovery pipeline is connected to the corresponding tank truck's gas phase filling valve, and the outlet of the gas phase recovery pipeline is connected to the ammonia recovery unit.

[0007] The beneficial effects of this invention are as follows: By setting up a liquid phase filling panel and a gas phase filling panel, and by setting up recovery units capable of detecting the gas and liquid phases inside the liquid phase filling panel and the gas phase filling panel respectively, this gas and liquid phase recovery unit can not only be used to detect and recover residual gaseous ammonia and liquid ammonia in the tank truck, but also to detect the quality of gaseous ammonia and liquid ammonia during and after filling, thereby achieving the purpose of reducing costs and ensuring the quality of liquid ammonia after filling the tank truck; furthermore, this invention uses the filling unit as an independent unit and sets it up in parallel, so that it is connected to the corresponding tank truck of the filling unit through an ultrapure ammonia purification device. This method can avoid pipeline contamination during the recovery and filling process, thereby achieving the characteristics of continuous recovery and continuous filling.

[0008] Preferably, the liquid phase recovery pipeline section includes a first ammonia analysis pipeline equipped with a first ammonia purity analyzer, a high-purity ammonia recovery pipeline equipped with a high-purity ammonia valve, and an industrial ammonia recovery pipeline equipped with an industrial ammonia valve.

[0009] Preferably, the liquid phase filling panel further includes a first venting line with a first venting valve, a first vacuum line with a first vacuum valve, a first nitrogen line with a first nitrogen valve, and a first pressure detection line with a first pressure gauge.

[0010] Preferably, the gas phase recovery pipeline section includes a second ammonia analysis pipeline equipped with a second ammonia purity analyzer and a gas ammonia recovery pipeline equipped with a gas ammonia recovery valve.

[0011] Preferably, the gas phase filling panel further includes a second venting line with a second venting valve, a second vacuum line with a second vacuum valve, a second nitrogen line with a second nitrogen valve, and a second pressure detection line with a second pressure gauge.

[0012] Preferably, the ammonia recovery unit includes an industrial ammonia recovery tank and a high-purity ammonia recovery tank; the industrial ammonia recovery tank is connected to the industrial ammonia recovery pipeline in the liquid phase recovery pipeline section and the gaseous ammonia recovery pipeline in the gas phase recovery pipeline section via an industrial ammonia condenser; the high-purity ammonia recovery tank is connected to the high-purity ammonia recovery pipeline via a high-purity ammonia subcooler.

[0013] Preferably, it also includes an ammonia tail gas emission main pipe, which is connected to the first venting line and the second venting line respectively; it also includes a vacuum pumping main pipe connected to the vacuum pumping device, which is connected to the first vacuum pumping line and the second vacuum pumping line respectively; and it also includes a high-purity nitrogen main pipe, which is connected to the first nitrogen line and the second nitrogen line respectively.

[0014] Preferably, an ultrapure ammonia subcooler is provided between the ultrapure ammonia purification device and the liquid phase filling panel; the tank truck is provided with a tank truck liquid phase valve and a tank truck gas phase valve, the tank truck liquid phase valve is connected to the liquid phase filling valve through an arm, and the tank truck gas phase valve is connected to the gas phase filling valve through an arm.

[0015] A method for filling and recovering residual liquid using ultrapure ammonia tank trucks, characterized by the following steps:

[0016] Step 1: Inspect the pipeline sealing between the tank truck and the liquid phase filling panel and the gas phase filling panel;

[0017] Step 2: After the pipeline sealing test is passed, the liquid phase in the tank truck is separated and recovered.

[0018] Step 3: Recover the gas phase inside the tanker truck;

[0019] Step 4: Analyze and test the quality of ultrapure ammonia during the tanker filling process;

[0020] Step 5: When the quality analysis and testing of ultrapure ammonia in Step 4 is qualified, continue filling ultrapure ammonia. After the tanker is filled, perform quality analysis and testing of the ultrapure ammonia in the tanker.

[0021] Step 6: When the quality analysis and testing of ultrapure ammonia in Step 5 is qualified, seal the pipelines between the tank truck and the liquid phase filling panel and the gas phase filling panel.

[0022] Step 7: If the pipeline sealing test in Step 1 fails, reconnect the corresponding pipeline; repeat Step 1 after reconnection.

[0023] Step 8: If the quality analysis of ultrapure ammonia in Step 4 fails, repeat Steps 2-4;

[0024] Step 9: If the quality analysis of ultrapure ammonia in Step 5 fails, repeat Steps 2-5;

[0025] Step 10: The ultrapure ammonia purification unit is connected to a corresponding tank truck through several filling units, and is filled separately through steps 1-9 above.

[0026] A method for filling and recovering residual liquid using ultrapure ammonia tank trucks, the method comprising the following steps:

[0027] Step 1: The liquid phase valve and gas phase valve on the tank truck are connected to the loading arm respectively. The liquid phase port on the loading arm is connected to the pipeline with the liquid phase filling valve, and the gas phase port on the loading arm is connected to the pipeline with the gas phase filling valve.

[0028] Step 2: Open the liquid phase filling valve to close the liquid phase valve of the tank truck. Use a portable leak detector to check for leaks at the liquid phase interface between the tank truck and the loading arm. Open the first vent valve to release the liquid ammonia in the pipeline to the exhaust gas treatment system. When the pressure in the pipeline detected by the first pressure gauge is <50 kPa, close the first vent valve, open the first vacuum valve, and start the vacuum device to vacuum the puncture pipeline between the liquid phase filling valve and the liquid phase valve of the tank truck. When the pressure in the pipeline detected by the first pressure gauge is <0.1 Pa, continue vacuuming for 10 to 30 minutes. Close the first vacuum valve and stop the vacuum device.

[0029] Step 3: When the pressure exceeds the preset threshold, it is determined that the liquid phase pipeline has poor sealing. At this time, replace the sealing gasket at the liquid phase connection of the loading arm and repeat the above steps 1-2.

[0030] When the pressure does not exceed the preset threshold, and the liquid phase pipeline is determined to be in good sealing condition, the industrial ammonia valve and the tank truck liquid phase valve are opened. The liquid phase ultrapure ammonia in the tank truck is transported to the industrial ammonia recovery tank through the industrial ammonia valve and the industrial ammonia condenser. The liquid phase filling pipeline and liquid phase filling panel are replaced. The liquid weight is 30-80 kg. At the same time, the first ammonia purity analyzer tests the pipeline. After ensuring that there are no impurity gases in the pipeline, the industrial ammonia valve, liquid phase filling valve and tank truck liquid phase valve are closed.

[0031] Step 4: Open the tank truck vapor phase valve to close the vapor phase filling valve. Use a portable leak detector to check for leaks at the vapor phase interface between the tank truck and the loading arm. Close the tank truck vapor phase valve and sequentially open the vapor phase filling valve and the second vent valve to release the nitrogen and ammonia in the pipeline to the tail gas treatment system. When the pressure in the pipeline detected by the second pressure gauge is <50 kPa, close the second vent valve, open the second vacuum valve, and start the vacuum pumping device to vacuum the vented pipeline between the vapor phase filling valve and the tank truck vapor phase valve. When the pressure in the pipeline detected by the second pressure gauge is <0.1 Pa, continue vacuuming for 10 to 30 minutes. Close the second vacuum valve, and the vacuum pumping device will stop operating.

[0032] Step 5: When the pressure exceeds the preset threshold, it is determined that the pipeline has poor sealing. At this time, replace the sealing gasket at the gas phase connection of the loading arm and repeat Step 4 above.

[0033] When the pressure does not exceed the preset threshold, and the liquid phase pipeline is determined to be in good sealing condition, the gaseous ammonia recovery valve, gas phase filling valve, and tank truck gas phase valve are opened. The gaseous ultrapure ammonia in the tank truck is transported to the industrial ammonia recovery tank by the gaseous ammonia recovery valve and the industrial ammonia condenser. At the same time, the second ammonia purity analyzer detects the pipeline. After ensuring that there are no impurity gases in the pipeline, the gaseous ammonia recovery valve, gas phase filling valve, and tank truck gas phase valve are closed.

[0034] Step 6: Open the liquid phase valve and liquid phase filling valve of the tank truck. The first ammonia purity analyzer will test the liquid phase in the pipeline. When the analysis result shows that the ammonia purity is >99.9995%, open the high-purity ammonia valve to allow the liquid phase in the tank truck to enter the high-purity ammonia subcooler through the high-purity ammonia valve. After being subcooled by 5-20°C in the high-purity ammonia subcooler, it will be recovered to the high-purity ammonia recovery tank. If the analysis result shows that the ammonia purity is ≤99.9995%, open the industrial ammonia valve. The liquid phase in the tank truck will transport the high-purity nitrogen in the pipeline through the industrial ammonia valve and the industrial ammonia condenser to the industrial ammonia recovery tank.

[0035] Step 7: Open the ammonia recovery valve, the gas phase filling valve, and the tank truck gas phase valve. The gas phase in the tank truck is transported to the industrial ammonia recovery tank through the ammonia recovery valve and the industrial ammonia condenser. When the pressure in the tank truck and the pressure in the industrial ammonia recovery tank are the same, close the ammonia recovery valve and open the second vent valve to allow the gas phase in the tank truck to be vented through the second vent line and the ammonia tail gas discharge main. When the pressure in the pipeline detected by the second pressure gauge is 0.15-0.2 MPa, close the second vent valve and open the second vacuum valve. Start the vacuuming device to vacuum the inside of the tank truck. When the pressure in the pipeline detected by the second pressure gauge is <0.1 Pa, continue vacuuming for 10-30 minutes, close the second vacuum valve, and stop the vacuuming process.

[0036] Step 8: With the ultrapure ammonia subcooler in a stopped state, open the filling valve. The saturated ultrapure ammonia product in the ultrapure ammonia purification unit enters the tank truck through the filling valve. The saturated ultrapure ammonia product vaporizes into cushion gas in the tank truck. Continue to fill the tank truck with saturated ultrapure ammonia product until the pressure in the tank truck reaches 0.5 MPa. Then, close the filling valve and open the gas phase filling valve and the tank truck gas phase valve to allow the second ammonia purity analyzer to detect the gas phase from the tank truck. If the detection meets the purity requirements of the ultrapure ammonia product, the cushion gas is deemed qualified. If the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion gas is deemed unqualified.

[0037] Step 9: If the cushion air is determined to be unqualified, repeat steps 6, 7 and 8 above until the cushion air is found to be qualified.

[0038] When the cushion gas is deemed qualified, the filling valve is opened, allowing the saturated ultrapure ammonia product in the ultrapure ammonia purification unit to enter the tank truck through the filling valve to form cushion liquid. When the weight of the filling cushion liquid is 300-600 kg, the filling valve is closed, and the first ammonia purity analyzer is used to detect the liquid phase in the tank truck. If the detection meets the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed qualified; if the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed unqualified.

[0039] Step 10: If the padding liquid is found to be unqualified, repeat steps 6, 7, 8 and 9 above until the padding liquid is found to be qualified.

[0040] When the padding liquid is deemed qualified, the ultrapure ammonia subcooler is turned on and the filling valve is opened. The saturated ultrapure ammonia product in the ultrapure ammonia purification unit enters the ultrapure ammonia subcooler and is subcooled to 5-20°C. Then, it enters the tank truck through the filling valve for filling. During the filling process, the weight is weighed using a weighbridge. When the weight reaches the corresponding threshold, the filling valve is closed and the filling is completed.

[0041] Step 11: After filling, let stand for 2-3 hours, open the gas phase filling valve and the tank truck gas phase valve, and let the second ammonia purity analyzer detect the gas phase from the tank truck. When the detection meets the purity requirements of ultrapure ammonia products, the product gas is judged to be qualified; when the detection does not meet the purity requirements of ultrapure ammonia products, the product gas is judged to be unqualified.

[0042] Step 12: When the product gas is determined to be unqualified, open the ammonia recovery valve. The gaseous ultrapure ammonia in the tank truck is transported to the industrial ammonia recovery tank through the ammonia recovery valve and the industrial ammonia condenser. 50-100 kg of gaseous phase in the tank truck is discharged. Then, analyze whether it is qualified. If it is still unqualified, repeat the above steps 6, 7, 8, 9, 10 and 11 until the product gas is found to be qualified.

[0043] When the product gas is deemed qualified, the gas phase filling valve and the tank truck gas phase valve are closed, and the tank truck liquid phase valve and the liquid phase filling valve are opened. The first ammonia purity analyzer detects the liquid phase in the pipeline. When the detection meets the purity requirements of ultrapure ammonia products, the product is deemed qualified. When the detection does not meet the purity requirements of ultrapure ammonia products, the product is deemed unqualified.

[0044] Step 13: When a product is determined to be unqualified, repeat steps 6, 7, 8, 9, 10, 11 and 12 above until the product is found to be qualified.

[0045] When the product is deemed qualified, close the liquid phase valve of the tank truck and open the industrial ammonia valve to allow the liquid phase in the pipeline to enter the industrial ammonia recovery tank through the industrial ammonia recovery pipeline and the industrial ammonia condenser. After the liquid phase in the pipeline is emptied, close the industrial ammonia valve, open the first vacuum valve, start the vacuum device, and perform vacuuming. At the same time, close the liquid phase filling valve and the first vacuum valve in sequence, disassemble the loading arm liquid connection pipe, and install a blind flange on the loading arm liquid phase port for sealing and protection.

[0046] Step 14: Close the tank truck vapor phase valve and open the second vacuum valve to perform vacuuming; at the same time, close the tank truck vapor phase valve and the vapor phase filling valve in sequence; close the vacuuming device and at the same time open the second nitrogen valve to allow high-purity nitrogen from the high-purity nitrogen main pipe to enter the pipeline between the vapor phase filling panel and the vapor phase filling valve; when the pressure in the pipeline detected by the second pressure gauge is 0.5-0.8 MPa, close the second nitrogen valve, disassemble the loading arm gas connection pipe, and install a blind flange on the loading arm's vapor phase port for sealing protection.

[0047] A system and method for filling and recovering ultrapure ammonia tank trucks according to the above scheme, by setting up filling units in parallel, can achieve independent ammonia recovery and ultrapure ammonia filling in the tank truck, without mutual interference and without pipeline contamination, thereby achieving the purpose of continuous filling. Furthermore, the invention includes a liquid phase filling panel and a gas phase filling panel, and each panel has a recovery unit capable of detecting the gas and liquid phases. This gas and liquid phase recovery unit can detect gaseous ammonia... The invention detects residual gaseous and liquid ammonia in tank trucks, enabling the separation and recovery of these substances. It also tests the airtightness of corresponding pipelines and detects the gaseous and liquid phases of ultrapure ammonia in the tank truck after filling. This achieves the goal of detecting and recovering residual gaseous and liquid ammonia, reducing costs and ensuring the quality of liquid ammonia after filling. Furthermore, the exhaust gas treatment system and vacuum device work together to test the airtightness of the corresponding gaseous and liquid phase pipelines. This method eliminates the need for gas replacement as in traditional technologies. It also features improved efficiency in airtightness testing and better sealing performance. Furthermore, during the filling process, cushion gas and cushion fluid are added, and their purity is analyzed and tested to track and monitor the quality of ultrapure ammonia during the filling process. This ensures the quality of filled ultrapure ammonia while reducing its loss (analysis of cushion gas and cushion fluid avoids the problem of discovering substandard products in the tanker after filling due to improper tanker handling). This invention also incorporates an ultrapure ammonia subcooler during the filling process to further enhance the ultrapure ammonia's properties. Cooling the ammonia to 5–20°C before filling it into tank trucks overcomes the problem of large-scale vaporization of saturated liquid ammonia entering the tank trucks using existing purification systems or distillation columns. This effectively saves on ultrapure ammonia while improving the smoothness and efficiency of tank truck filling. Furthermore, this invention allows for the detection of both the gaseous and liquid phases of the product in the tank truck after filling, ensuring the quality of the ultrapure ammonia. It features the ability to achieve fractional recovery and effective tracking of ultrapure ammonia, improve filling efficiency while reducing high-purity ammonia consumption, and guarantee the quality of ultrapure ammonia products. Attached Figure Description

[0048] Figure 1 This is a schematic diagram of the structure of the present invention.

[0049] Figure 2 This is a schematic diagram of the liquid phase filling panel of the present invention.

[0050] Figure 3 This is a schematic diagram of the structure of the vapor phase filling panel of the present invention.

[0051] In the diagram: 1. Tank truck; 2. Ultra-pure ammonia purification unit; 3. Liquid phase filling panel; 4. Gas phase filling panel; 5. Industrial ammonia recovery tank; 6. High-purity ammonia recovery tank; 7. Industrial ammonia condenser; 8. High-purity ammonia subcooler; 9. Ammonia tail gas exhaust manifold; 10. Vacuum pumping device; 11. Vacuum pumping manifold; 12. High-purity nitrogen manifold; 13. Ultra-pure ammonia subcooler; 14. Loading arm; 15. Tank truck liquid phase valve; 16. Tank truck gas phase valve; 17. Liquid phase filling... 18. Gas phase filling valve; 19. Filling valve; 20. First ammonia purity analyzer; 21. High-purity ammonia valve; 22. Industrial ammonia valve; 23. First vent valve; 24. First vacuum valve; 25. First nitrogen valve; 26. First pressure gauge; 27. Second ammonia purity analyzer; 28. Gaseous ammonia recovery valve; 29. ​​Second vent valve; 30. Second vacuum valve; 31. Second nitrogen valve; 32. Second pressure gauge. Detailed Implementation

[0052] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.

[0053] Reference Figure 1-3As shown, a system and method for filling ultrapure ammonia tank trucks and recovering residual liquid is disclosed. The system includes an ultrapure ammonia purification device 2 and an ammonia recovery unit, as well as several tank trucks 1 and several filling units corresponding to each tank truck 1. The filling unit includes a liquid phase filling panel 3 and a gas phase filling panel 4 for filling liquid-phase ultrapure ammonia and recovering residual gas and liquid phases in the tank truck 1 respectively. The liquid phase filling panel 3 is equipped with at least an ultrapure ammonia filling pipeline with a filling valve 19, and a liquid phase detection and separation recovery system for the tank truck 1. The liquid phase recovery pipeline section; the inlet end of the ultrapure ammonia filling pipeline is connected to the ultrapure ammonia purification device 2, and the outlet end of the ultrapure ammonia filling pipeline is connected to the liquid phase filling valve 17 of the corresponding tank truck 1 through the liquid phase recovery pipeline section, and the outlet end of the liquid phase recovery pipeline section is connected to the ammonia recovery unit; the gas phase filling panel 4 is provided with at least a gas phase recovery pipeline section for gas phase detection inside the tank truck 1 and for gas phase recovery; the inlet end of the gas phase recovery pipeline section is connected to the gas phase filling valve 18 of the corresponding tank truck 1, and the outlet end of the gas phase recovery pipeline section is connected to the ammonia recovery unit. This invention features a parallel and independently configured filling unit between the ultrapure ammonia purification device 2 and several tank trucks 1. This avoids mutual interference during the discharge of residual liquid from the tank trucks 1 and the filling process, thereby improving filling efficiency and enabling continuous filling. The filling unit includes a liquid phase filling panel 3 and a gas phase filling panel 4, with gas phase and liquid phase detection recovery sections inside the liquid phase filling panel 3 and gas phase filling panel 4. These detections not only enable the separation and recovery of residual gaseous and liquid ammonia in the tank trucks, but also allow for airtightness testing of the corresponding pipelines and detection of the gaseous and liquid phases of ultrapure ammonia in the tank trucks after filling. This achieves the goal of detecting and recovering residual gaseous and liquid ammonia in the tank trucks, reducing costs and ensuring the quality of liquid ammonia after filling.

[0054] Furthermore, the liquid phase recovery pipeline section includes a first ammonia analysis pipeline equipped with a first ammonia purity analyzer 20, a high-purity ammonia recovery pipeline equipped with a high-purity ammonia valve 21, and an industrial ammonia recovery pipeline equipped with an industrial ammonia valve 22. The first ammonia purity analyzer 20 described in this invention is used to detect the purity of the liquid phase entering the liquid phase filling panel 3. By cooperating with the first ammonia purity analyzer 20 and the high-purity ammonia valve 21 or the industrial ammonia valve 22, the residual liquid in the tank truck 1 can be analyzed and detected, and its recovery can be performed in stages.

[0055] Furthermore, the liquid phase filling panel 3 also includes a first venting line with a first venting valve 23, a first vacuum line with a first vacuum valve 24, a first nitrogen line with a first nitrogen valve 25, and a first pressure detection line with a first pressure gauge 26. By setting the first venting valve 23 and the first vacuum valve 24, the corresponding lines can be vented; the first nitrogen line with the first nitrogen valve 25 in this invention is used for nitrogen pressure maintenance of the corresponding lines.

[0056] Furthermore, the gas phase recovery pipeline includes a second ammonia analysis pipeline equipped with a second ammonia purity analyzer 27 and a gas ammonia recovery pipeline equipped with a gas ammonia recovery valve 28. By installing the second ammonia purity analyzer 27 and cooperating with the gas ammonia recovery valve 28, the gas ammonia can be recovered in different phases.

[0057] Furthermore, the vapor phase filling panel 4 also includes a second venting line with a second venting valve 29, a second vacuum line with a second vacuum valve 30, a second nitrogen line with a second nitrogen valve 31, and a second pressure detection line with a second pressure gauge 32. The two venting valves 29 and the second vacuum valve 30 enable the venting of the corresponding lines; the second nitrogen line with the second nitrogen valve 31 is used for nitrogen pressure maintenance of the corresponding lines.

[0058] Furthermore, the ammonia recovery unit includes an industrial ammonia recovery tank 5 and a high-purity ammonia recovery tank 6. The industrial ammonia recovery tank 5 is connected to the industrial ammonia recovery pipeline in the liquid phase recovery pipeline section and the gaseous ammonia recovery pipeline in the gas phase recovery pipeline section via an industrial ammonia condenser 7. The high-purity ammonia recovery tank 6 is connected to the high-purity ammonia recovery pipeline via a high-purity ammonia subcooler 8. This configuration enables the effective recovery and reuse of the liquid and gaseous phases within the tank truck, thereby reducing costs.

[0059] Furthermore, the system also includes an ammonia tail gas emission main pipe 9, which is connected to the first venting line and the second venting line respectively; it also includes a vacuum pumping main pipe 11 connected to the vacuum pumping device 10, which is connected to the first vacuum pumping line and the second vacuum pumping line respectively; and it also includes a high-purity nitrogen main pipe 12, which is connected to the first nitrogen line and the second nitrogen line respectively. This invention, by providing the vacuum pumping device 10 and the vacuum pumping main pipe 11, can improve the efficiency of tank truck handling and pipeline replacement.

[0060] Furthermore, an ultrapure ammonia supercooler 13 is provided between the ultrapure ammonia purification device 2 and the liquid phase filling panel 3; the tank truck 1 is provided with a tank truck liquid phase valve 15 and a tank truck gas phase valve 16, the tank truck liquid phase valve 15 is connected to the liquid phase filling valve 17 through the loading arm 14, and the tank truck gas phase valve 16 is connected to the gas phase filling valve 18 through the loading arm 14.

[0061] A method for filling and recovering residual liquid using ultrapure ammonia tank trucks, the method comprising the following steps:

[0062] Step 1: Inspect the pipeline sealing between tank truck 1 and liquid phase filling panel 3 and gas phase filling panel 4;

[0063] Step 2: After the pipeline sealing test is passed, the liquid phase in tank truck 1 is separated and recovered.

[0064] Step 3: Recover the gas phase inside tanker 1;

[0065] Step 4: The quality of ultrapure ammonia is analyzed and tested during the filling process of tanker truck 1;

[0066] Step 5: When the quality analysis and testing of ultrapure ammonia in Step 4 is qualified, continue filling ultrapure ammonia. After the filling of tank truck 1 is completed, perform quality analysis and testing of ultrapure ammonia in tank truck 1.

[0067] Step 6: When the quality analysis and testing of ultrapure ammonia in Step 5 is qualified, seal the pipeline between tank truck 1 and liquid phase filling panel 3 and gas phase filling panel 4.

[0068] Step 7: If the pipeline sealing test in Step 1 fails, reconnect the corresponding pipeline; repeat Step 1 after reconnection.

[0069] Step 8: If the quality analysis of ultrapure ammonia in Step 4 fails, repeat Steps 2-4;

[0070] Step 9: If the quality analysis of ultrapure ammonia in Step 5 fails, repeat Steps 2-5;

[0071] Step 10: The ultrapure ammonia purification device 2 is connected to the corresponding tank truck 1 through several filling units, and is filled separately through steps 1-9 above.

[0072] A method for filling and recovering residual liquid using ultrapure ammonia tank trucks, the method comprising the following steps:

[0073] Step 1: The liquid phase valve 15 and the gas phase valve 16 on the tank truck 1 are connected to the loading arm 14 respectively. The liquid phase port on the loading arm 14 is connected to the pipeline with the liquid phase filling valve 17, and the gas phase port on the loading arm 14 is connected to the pipeline with the gas phase filling valve 18.

[0074] Step 2: Open the liquid phase filling valve 17 to close the tank truck liquid phase valve 15. Use a portable leak detector to check for leaks at the liquid phase interface between the tank truck and the loading arm. Open the first vent valve 23 to release the liquid ammonia in the pipeline to the tail gas treatment system 9. When the pressure in the pipeline detected by the first pressure gauge 26 is <50 kPa, close the first vent valve 23, open the first vacuum valve 24, and start the vacuum device 10 to vacuum the puncture pipeline between the liquid phase filling valve 17 and the tank truck liquid phase valve 15. When the pressure in the pipeline detected by the first pressure gauge 26 is <0.1 Pa, continue vacuuming for 10 min to 30 min. Close the first vacuum valve 24, and the vacuum device 10 stops operating.

[0075] Step 3: When the pressure exceeds the preset threshold, it is determined that the liquid phase pipeline has poor sealing. At this time, replace the sealing gasket at the liquid phase connection of the loading arm and repeat the above steps 1-2.

[0076] When the pressure does not exceed the preset threshold, and the liquid phase pipeline is determined to be in good sealing condition, the industrial ammonia valve 22 and the tank truck liquid phase valve 15 are opened. The liquid phase ultrapure ammonia in the tank truck 1 is transported to the industrial ammonia recovery tank 5 through the industrial ammonia valve 22 and the industrial ammonia condenser 7. The liquid phase filling pipeline and the liquid phase filling panel are replaced. The liquid weight is 30-80Kg. At the same time, the first ammonia purity analyzer 20 tests the pipeline. After ensuring that there are no impurity gases in the pipeline, the industrial ammonia valve 22, the liquid phase filling valve 17 and the tank truck liquid phase valve 15 are closed.

[0077] Step 4: Open the tank truck vapor phase valve 16, and close the vapor phase filling valve 18. Use a portable leak detector to check for leaks at the vapor phase interface between the tank truck and the loading arm. Close the tank truck vapor phase valve 16, and then open the vapor phase filling valve 18 and the second vent valve 29 in sequence to release the nitrogen and ammonia in the pipeline to the tail gas treatment system 9. When the pressure in the pipeline detected by the second pressure gauge 32 is <50 kPa, close the second vent valve 29, open the second vacuum valve 30, and start the vacuum device 10 to perform vacuuming on the vented pipeline between the vapor phase filling valve 18 and the tank truck vapor phase valve 16. When the pressure in the pipeline detected by the second pressure gauge 32 is <0.1 Pa, continue vacuuming for 10 min to 30 min, close the second vacuum valve 30, and stop the vacuum device 10.

[0078] Step 5: When the pressure exceeds the preset threshold, it is determined that the pipeline has poor sealing. At this time, replace the sealing gasket at the gas phase connection of the loading arm and repeat Step 4 above.

[0079] When the pressure does not exceed the preset threshold, and the liquid phase pipeline is determined to be in good sealing condition, the gaseous ammonia recovery valve 28, the gas phase filling valve 18, and the tank truck gas phase valve 16 are opened. The gaseous ultrapure ammonia in the tank truck 1 is transported to the industrial ammonia recovery tank 5 by the gaseous ammonia recovery valve 28 and the industrial ammonia condenser 7. At the same time, the second ammonia purity analyzer 27 detects the pipeline. After ensuring that there are no impurity gases in the pipeline, the gaseous ammonia recovery valve 28, the gas phase filling valve 18, and the tank truck gas phase valve 16 are closed.

[0080] Step 6: Open the liquid phase valve 15 and liquid phase filling valve 17 of the tank truck. The first ammonia purity analyzer 20 detects the liquid phase in the pipeline. When the analysis result shows that the ammonia purity is >99.9995%, open the high-purity ammonia valve 21, allowing the liquid phase in the tank truck 1 to enter the high-purity ammonia subcooler 8 through the high-purity ammonia valve 21. After being subcooled by 5-20°C in the high-purity ammonia subcooler 8, it is recovered to the high-purity ammonia recovery tank 6. If the analysis result shows that the ammonia purity is ≤99.9995%, open the industrial ammonia valve 22. The liquid phase in the tank truck 1 will transport the high-purity nitrogen gas in the pipeline to the industrial ammonia recovery tank 5 through the industrial ammonia valve 22 and the industrial ammonia condenser 7.

[0081] Step 7: Open the ammonia recovery valve 28, the gas phase filling valve 18, and the tank truck gas phase valve 16. The gas phase in the tank truck 1 is transported to the industrial ammonia recovery tank 5 through the ammonia recovery valve 28 and the industrial ammonia condenser 7. When the pressure in the tank truck 1 and the pressure in the industrial ammonia recovery tank 5 are the same, close the ammonia recovery valve 28 and open the second vent valve 29 to allow the gas phase in the tank truck 1 to be vented through the second vent pipeline and the ammonia tail gas discharge main pipe 9. When the pressure in the pipeline detected by the second pressure gauge 32 is 0.15~0.2MPa, close the second vent valve 29 and open the second vacuum valve 30. Start the vacuum device 10 to perform vacuuming treatment inside the tank truck 1. When the pressure in the pipeline detected by the second pressure gauge 32 is <0.1Pa, continue vacuuming for 10min~30min, close the second vacuum valve 30, and stop the vacuuming treatment.

[0082] Step 8: With the ultrapure ammonia subcooler 13 in a stopped state, open the filling valve 19. The saturated ultrapure ammonia product in the ultrapure ammonia purification unit 2 enters the tank truck 1 through the filling valve 19. The saturated ultrapure ammonia product vaporizes into cushion gas in the tank truck 1. Continue to fill the tank truck 1 with saturated ultrapure ammonia product until the pressure in the tank truck 1 reaches 0.5 MPa. Then close the filling valve 19 and open the gas phase filling valve 18 and the tank truck gas phase valve 16. The second ammonia purity analyzer 27 will detect the gas phase from the tank truck 1. If the detection meets the purity requirements of the ultrapure ammonia product, the cushion gas is deemed qualified. If the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion gas is deemed unqualified.

[0083] Step 9: If the cushion air is determined to be unqualified, repeat steps 6, 7 and 8 above until the cushion air is found to be qualified.

[0084] When the cushion gas is deemed qualified, the filling valve 19 is opened, allowing the saturated ultrapure ammonia product in the ultrapure ammonia purification device 2 to enter the tank truck 1 through the filling valve 19 to form a cushion liquid. When the weight of the filling cushion liquid is 300-600 kg, the filling valve 19 is closed, and the first ammonia purity analyzer 20 is used to detect the liquid phase in the tank truck 1. If the detection meets the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed qualified; if the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed unqualified.

[0085] Step 10: If the padding liquid is found to be unqualified, repeat steps 6, 7, 8 and 9 above until the padding liquid is found to be qualified.

[0086] When the padding liquid is deemed qualified, the ultrapure ammonia subcooler 13 is turned on and the filling valve 19 is opened. The saturated ultrapure ammonia product in the ultrapure ammonia purification device 2 enters the ultrapure ammonia subcooler 13 and is subcooled to 5-20°C. Then it enters the tank truck 1 through the filling valve 19 for filling. During the filling process, the weight is weighed by a weighbridge. When the weight reaches the corresponding threshold, the filling valve 19 is closed and the filling is completed.

[0087] Step 11: After filling, let stand for 2-3 hours, open the gas phase filling valve 18 and the tank truck gas phase valve 16, so that the second ammonia purity analyzer 27 can detect the gas phase from the tank truck 1. When the detection meets the purity requirements of ultrapure ammonia products, the product gas is judged to be qualified; when the detection does not meet the purity requirements of ultrapure ammonia products, the product gas is judged to be unqualified.

[0088] Step 12: When the product gas is determined to be unqualified, open the ammonia recovery valve 28. The gaseous ultrapure ammonia in tank truck 1 is transported to the industrial ammonia recovery tank 5 through the ammonia recovery valve 28 and the industrial ammonia condenser 7. 50-100 kg of gaseous phase in tank truck 1 is discharged, and then the product gas is analyzed to see if it is qualified. If it is still unqualified, repeat steps 6, 7, 8, 9, 10 and 11 above until the product gas is found to be qualified.

[0089] When the product gas is deemed qualified, the gas phase filling valve 18 and the tank truck gas phase valve 16 are closed, and the tank truck liquid phase valve 15 and the liquid phase filling valve 17 are opened. The first ammonia purity analyzer 20 detects the liquid phase in the pipeline. When the detection meets the purity requirements of ultrapure ammonia products, the product is deemed qualified. When the detection does not meet the purity requirements of ultrapure ammonia products, the product is deemed unqualified.

[0090] Step 13: When a product is determined to be unqualified, repeat steps 6, 7, 8, 9, 10, 11 and 12 above until the product is found to be qualified.

[0091] When the product is deemed qualified, close the liquid phase valve 15 of the tank truck and open the industrial ammonia valve 22 to allow the liquid phase in the pipeline to enter the industrial ammonia recovery tank 5 through the industrial ammonia recovery pipeline and the industrial ammonia condenser 7. After the liquid phase in the pipeline is emptied, close the industrial ammonia valve 22, open the first vacuum valve 24, start the vacuum device 10, and perform vacuuming. At the same time, close the liquid phase filling valve 17 and the first vacuum valve 24 in sequence, disassemble the loading arm liquid connection pipe, and install a blind flange on the liquid phase port of the loading arm 14 for sealing and protection.

[0092] Step 14: Close the tank truck vapor phase valve 16, open the second vacuum valve 30, and perform vacuuming; at the same time, close the tank truck vapor phase valve 16 and the vapor phase filling valve 18 in sequence; close the vacuuming device 10, and at the same time open the second nitrogen valve 31 to allow high-purity nitrogen from the high-purity nitrogen main pipe 12 to enter the pipeline between the vapor phase filling panel 4 and the vapor phase filling valve 18; when the second pressure gauge 32 detects that the pressure in the pipeline is 0.5-0.8 MPa, close the second nitrogen valve 31, disassemble the loading arm gas connection pipe, and install a blind flange on the vapor phase port of the loading arm 14 for sealing and protection.

[0093] To more clearly explain the present invention, it will now be further described in conjunction with specific embodiments. The specific embodiments are as follows:

[0094] Example 1

[0095] A system for filling and recovering residual liquid from ultrapure ammonia tank trucks is disclosed. The system includes an ultrapure ammonia purification unit 2 and an ammonia recovery unit, as well as several tank trucks 1 and several filling units corresponding to each tank truck 1. Each filling unit includes a liquid phase filling panel 3 and a gas phase filling panel 4 for filling liquid-phase ultrapure ammonia and separately recovering residual gas and liquid phases from the tank trucks 1. The liquid phase filling panel 3 is internally equipped with at least an ultrapure ammonia filling pipeline with a filling valve 19, and a liquid phase detection and separation recovery system for the liquid phase inside the tank trucks 1. The system includes a recovery pipeline section; the inlet end of the ultrapure ammonia filling pipeline is connected to the ultrapure ammonia purification device 2, and the outlet end of the ultrapure ammonia filling pipeline is connected to the liquid phase filling valve 17 of the corresponding tank truck 1 via a liquid phase recovery pipeline section. The outlet end of the liquid phase recovery pipeline section is connected to the ammonia recovery unit. The gas phase filling panel 4 is equipped with at least one gas phase recovery pipeline section for gas phase detection inside the tank truck 1 and for gas phase recovery. The inlet end of the gas phase recovery pipeline section is connected to the gas phase filling valve 18 of the corresponding tank truck 1, and the outlet end of the gas phase recovery pipeline section is connected to the ammonia recovery unit. The liquid phase recovery pipeline section includes a first ammonia analysis pipeline equipped with a first ammonia purity analyzer 20, a high-purity ammonia recovery pipeline equipped with a high-purity ammonia valve 21, and an industrial ammonia recovery pipeline equipped with an industrial ammonia valve 22. The liquid phase filling panel 3 further includes a first venting line with a first vent valve 23, a first vacuum line with a first vacuum valve 24, a first nitrogen line with a first nitrogen valve 25, and a first pressure detection line with a first pressure gauge 26. The gas phase recovery line section includes a second ammonia analysis line with a second ammonia purity analyzer 27 and a gas ammonia recovery line with a gas ammonia recovery valve 28. The gas phase filling panel 4 further includes a second venting line with a second vent valve 29, a second vacuum line with a second vacuum valve 30, a second nitrogen line with a second nitrogen valve 31, and a second pressure detection line with a second pressure gauge 32. The ammonia recovery unit includes an industrial ammonia recovery tank 5 and a high-purity ammonia recovery tank 6; the industrial ammonia recovery tank 5 is connected to the industrial ammonia recovery line in the liquid phase recovery line section and the gas ammonia recovery line in the gas phase recovery line section via an industrial ammonia condenser 7; the high-purity ammonia recovery tank 6 is connected to the high-purity ammonia recovery line via a high-purity ammonia subcooler 8. It also includes an ammonia tail gas discharge main pipe 9, which is connected to the first venting line and the second venting line respectively; it also includes a vacuum pumping main pipe 11 connected to the vacuum pumping device 10, which is connected to the first vacuum pumping line and the second vacuum pumping line respectively; it also includes a high-purity nitrogen main pipe 12, which is connected to the first nitrogen line and the second nitrogen line respectively.An ultrapure ammonia supercooler 13 is provided between the ultrapure ammonia purification device 2 and the liquid phase filling panel 3; the tank truck 1 is provided with a tank truck liquid phase valve 15 and a tank truck gas phase valve 16. The tank truck liquid phase valve 15 is connected to the liquid phase filling valve 17 through the loading arm 14, and the tank truck gas phase valve 16 is connected to the gas phase filling valve 18 through the loading arm 14.

[0096] A method for filling and recovering residual liquid using ultrapure ammonia tank trucks, the method comprising the following steps:

[0097] Step 1: Inspect the pipeline sealing between tank truck 1 and liquid phase filling panel 3 and gas phase filling panel 4;

[0098] Step 2: After the pipeline sealing test is passed, the liquid phase in tank truck 1 is separated and recovered.

[0099] Step 3: Recover the gas phase inside tanker 1;

[0100] Step 4: The quality of ultrapure ammonia is analyzed and tested during the filling process of tanker truck 1;

[0101] Step 5: When the quality analysis and testing of ultrapure ammonia in Step 4 is qualified, continue filling ultrapure ammonia. After the filling of tank truck 1 is completed, perform quality analysis and testing of ultrapure ammonia in tank truck 1.

[0102] Step 6: When the quality analysis and testing of ultrapure ammonia in Step 5 is qualified, seal the pipeline between tank truck 1 and liquid phase filling panel 3 and gas phase filling panel 4.

[0103] Step 7: If the pipeline sealing test in Step 1 fails, reconnect the corresponding pipeline; repeat Step 1 after reconnection.

[0104] Step 8: If the quality analysis of ultrapure ammonia in Step 4 fails, repeat Steps 2-4;

[0105] Step 9: If the quality analysis of ultrapure ammonia in Step 5 fails, repeat Steps 2-5;

[0106] Step 10: The ultrapure ammonia purification device 2 is connected to the corresponding tank truck 1 through several filling units, and is filled separately through steps 1-9 above.

[0107] Example 2

[0108] A system for filling ultrapure ammonia tank trucks and recovering residual liquid is provided. This system is the same as that in Example 1, so it will not be described again.

[0109] A method for filling and recovering residual liquid using ultrapure ammonia tank trucks, the method comprising the following steps:

[0110] Step 1: The liquid phase valve 15 and the gas phase valve 16 on the tank truck 1 are connected to the loading arm 14 respectively. The liquid phase port on the loading arm 14 is connected to the pipeline with the liquid phase filling valve 17, and the gas phase port on the loading arm 14 is connected to the pipeline with the gas phase filling valve 18.

[0111] Step 2: Open the liquid phase filling valve 17 to close the tank truck liquid phase valve 15. Use a portable leak detector to check for leaks at the liquid phase interface between the tank truck and the loading arm. Open the first vent valve 23 to release the liquid ammonia in the pipeline to the tail gas treatment system 9. When the pressure in the pipeline detected by the first pressure gauge 26 is <50 kPa, close the first vent valve 23, open the first vacuum valve 24, and start the vacuum device 10 to vacuum the puncture pipeline between the liquid phase filling valve 17 and the tank truck liquid phase valve 15. When the pressure in the pipeline detected by the first pressure gauge 26 is <0.1 Pa, continue vacuuming for 10 min to 30 min. Close the first vacuum valve 24, and the vacuum device 10 stops operating.

[0112] Step 3: When the pressure exceeds the preset threshold, it is determined that the liquid phase pipeline has poor sealing. At this time, replace the sealing gasket at the liquid phase connection of the loading arm and repeat the above steps 1-2.

[0113] When the pressure does not exceed the preset threshold, and the liquid phase pipeline is determined to be in good sealing condition, the industrial ammonia valve 22 and the tank truck liquid phase valve 15 are opened. The liquid phase ultrapure ammonia in the tank truck 1 is transported to the industrial ammonia recovery tank 5 through the industrial ammonia valve 22 and the industrial ammonia condenser 7. The liquid phase filling pipeline and the liquid phase filling panel are replaced. The liquid weight is 30-80Kg. At the same time, the first ammonia purity analyzer 20 tests the pipeline. After ensuring that there are no impurity gases in the pipeline, the industrial ammonia valve 22, the liquid phase filling valve 17 and the tank truck liquid phase valve 15 are closed.

[0114] Step 4: Open the tank truck vapor phase valve 16, and close the vapor phase filling valve 18. Use a portable leak detector to check for leaks at the vapor phase interface between the tank truck and the loading arm. Close the tank truck vapor phase valve 16, and then open the vapor phase filling valve 18 and the second vent valve 29 in sequence to release the nitrogen and ammonia in the pipeline to the tail gas treatment system 9. When the pressure in the pipeline detected by the second pressure gauge 32 is <50 kPa, close the second vent valve 29, open the second vacuum valve 30, and start the vacuum device 10 to perform vacuuming on the vented pipeline between the vapor phase filling valve 18 and the tank truck vapor phase valve 16. When the pressure in the pipeline detected by the second pressure gauge 32 is <0.1 Pa, continue vacuuming for 10 min to 30 min, close the second vacuum valve 30, and stop the vacuum device 10.

[0115] Step 5: When the pressure exceeds the preset threshold, it is determined that the pipeline has poor sealing. At this time, replace the sealing gasket at the gas phase connection of the loading arm and repeat Step 4 above.

[0116] When the pressure does not exceed the preset threshold, and the liquid phase pipeline is determined to be in good sealing condition, the gaseous ammonia recovery valve 28, the gas phase filling valve 18, and the tank truck gas phase valve 16 are opened. The gaseous ultrapure ammonia in the tank truck 1 is transported to the industrial ammonia recovery tank 5 by the gaseous ammonia recovery valve 28 and the industrial ammonia condenser 7. At the same time, the second ammonia purity analyzer 27 detects the pipeline. After ensuring that there are no impurity gases in the pipeline, the gaseous ammonia recovery valve 28, the gas phase filling valve 18, and the tank truck gas phase valve 16 are closed.

[0117] Step 6: Open the liquid phase valve 15 and liquid phase filling valve 17 of the tank truck. The first ammonia purity analyzer 20 detects the liquid phase in the pipeline. When the analysis result shows that the ammonia purity is >99.9995%, open the high-purity ammonia valve 21 to allow the liquid phase in the tank truck 1 to enter the high-purity ammonia subcooler 8 through the high-purity ammonia valve 21. After being subcooled by 5-20°C in the high-purity ammonia subcooler 8, it is recovered to the high-purity ammonia recovery tank 6.

[0118] Step 7: Open the ammonia recovery valve 28, the gas phase filling valve 18, and the tank truck gas phase valve 16. The gas phase in the tank truck 1 is transported to the industrial ammonia recovery tank 5 through the ammonia recovery valve 28 and the industrial ammonia condenser 7. When the pressure in the tank truck 1 and the pressure in the industrial ammonia recovery tank 5 are the same, close the ammonia recovery valve 28 and open the second vent valve 29 to allow the gas phase in the tank truck 1 to be vented through the second vent pipeline and the ammonia tail gas discharge main pipe 9. When the pressure in the pipeline detected by the second pressure gauge 32 is 0.15~0.2MPa, close the second vent valve 29 and open the second vacuum valve 30. Start the vacuum device 10 to perform vacuuming treatment inside the tank truck 1. When the pressure in the pipeline detected by the second pressure gauge 32 is <0.1Pa, continue vacuuming for 10min~30min, close the second vacuum valve 30, and stop the vacuuming treatment.

[0119] Step 8: With the ultrapure ammonia subcooler 13 in a stopped state, open the filling valve 19. The saturated ultrapure ammonia product in the ultrapure ammonia purification unit 2 enters the tank truck 1 through the filling valve 19. The saturated ultrapure ammonia product vaporizes into cushion gas in the tank truck 1. Continue to fill the tank truck 1 with saturated ultrapure ammonia product until the pressure in the tank truck 1 reaches 0.5 MPa. Then close the filling valve 19 and open the gas phase filling valve 18 and the tank truck gas phase valve 16. The second ammonia purity analyzer 27 will detect the gas phase from the tank truck 1. If the detection meets the purity requirements of the ultrapure ammonia product, the cushion gas is deemed qualified. If the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion gas is deemed unqualified.

[0120] Step 9: If the cushion air is determined to be unqualified, repeat steps 6, 7 and 8 above until the cushion air is found to be qualified.

[0121] When the cushion gas is deemed qualified, the filling valve 19 is opened, allowing the saturated ultrapure ammonia product in the ultrapure ammonia purification device 2 to enter the tank truck 1 through the filling valve 19 to form a cushion liquid. When the weight of the filling cushion liquid is 300-600 kg, the filling valve 19 is closed, and the first ammonia purity analyzer 20 is used to detect the liquid phase in the tank truck 1. If the detection meets the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed qualified; if the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed unqualified.

[0122] Step 10: If the padding liquid is found to be unqualified, repeat steps 6, 7, 8 and 9 above until the padding liquid is found to be qualified.

[0123] When the padding liquid is deemed qualified, the ultrapure ammonia subcooler 13 is turned on and the filling valve 19 is opened. The saturated ultrapure ammonia product in the ultrapure ammonia purification device 2 enters the ultrapure ammonia subcooler 13 and is subcooled to 5-20°C. Then it enters the tank truck 1 through the filling valve 19 for filling. During the filling process, the weight is weighed by a weighbridge. When the weight reaches the corresponding threshold, the filling valve 19 is closed and the filling is completed.

[0124] Step 11: After filling, let stand for 2-3 hours, open the gas phase filling valve 18 and the tank truck gas phase valve 16, so that the second ammonia purity analyzer 27 can detect the gas phase from the tank truck 1. When the detection meets the purity requirements of ultrapure ammonia products, the product gas is judged to be qualified; when the detection does not meet the purity requirements of ultrapure ammonia products, the product gas is judged to be unqualified.

[0125] Step 12: When the product gas is determined to be unqualified, open the ammonia recovery valve 28. The gaseous ultrapure ammonia in tank truck 1 is transported to the industrial ammonia recovery tank 5 through the ammonia recovery valve 28 and the industrial ammonia condenser 7. 50-100 kg of gaseous phase in tank truck 1 is discharged, and then the product gas is analyzed to see if it is qualified. If it is still unqualified, repeat steps 6, 7, 8, 9, 10 and 11 above until the product gas is found to be qualified.

[0126] When the product gas is deemed qualified, the gas phase filling valve 18 and the tank truck gas phase valve 16 are closed, and the tank truck liquid phase valve 15 and the liquid phase filling valve 17 are opened. The first ammonia purity analyzer 20 detects the liquid phase in the pipeline. When the detection meets the purity requirements of ultrapure ammonia products, the product is deemed qualified. When the detection does not meet the purity requirements of ultrapure ammonia products, the product is deemed unqualified.

[0127] Step 13: When a product is determined to be unqualified, repeat steps 6, 7, 8, 9, 10, 11 and 12 above until the product is found to be qualified.

[0128] When the product is deemed qualified, close the liquid phase valve 15 of the tank truck and open the industrial ammonia valve 22 to allow the liquid phase in the pipeline to enter the industrial ammonia recovery tank 5 through the industrial ammonia recovery pipeline and the industrial ammonia condenser 7. After the liquid phase in the pipeline is emptied, close the industrial ammonia valve 22, open the first vacuum valve 24, start the vacuum device 10, and perform vacuuming. At the same time, close the liquid phase filling valve 17 and the first vacuum valve 24 in sequence, disassemble the loading arm liquid connection pipe, and install a blind flange on the liquid phase port of the loading arm 14 for sealing and protection.

[0129] Step 14: Close the tank truck vapor phase valve 16, open the second vacuum valve 30, and perform vacuuming; at the same time, close the tank truck vapor phase valve 16 and the vapor phase filling valve 18 in sequence; close the vacuuming device 10, and at the same time open the second nitrogen valve 31 to allow high-purity nitrogen from the high-purity nitrogen main pipe 12 to enter the pipeline between the vapor phase filling panel 4 and the vapor phase filling valve 18; when the second pressure gauge 32 detects that the pressure in the pipeline is 0.5-0.8 MPa, close the second nitrogen valve 31, disassemble the loading arm gas connection pipe, and install a blind flange on the vapor phase port of the loading arm 14 for sealing and protection.

[0130] Example 3

[0131] A system for filling ultrapure ammonia tank trucks and recovering residual liquid is provided. This system is the same as that in Example 1, so it will not be described again.

[0132] A method for filling and recovering residual liquid using ultrapure ammonia tank trucks, the method comprising the following steps:

[0133] Step 1: The liquid phase valve 15 and the gas phase valve 16 on the tank truck 1 are connected to the loading arm 14 respectively. The liquid phase port on the loading arm 14 is connected to the pipeline with the liquid phase filling valve 17, and the gas phase port on the loading arm 14 is connected to the pipeline with the gas phase filling valve 18.

[0134] Step 2: Open the liquid phase filling valve 17 to close the tank truck liquid phase valve 15. Use a portable leak detector to check for leaks at the liquid phase interface between the tank truck and the loading arm. Open the first vent valve 23 to release the liquid ammonia in the pipeline to the tail gas treatment system 9. When the pressure in the pipeline detected by the first pressure gauge 26 is <50 kPa, close the first vent valve 23, open the first vacuum valve 24, and start the vacuum device 10 to vacuum the puncture pipeline between the liquid phase filling valve 17 and the tank truck liquid phase valve 15. When the pressure in the pipeline detected by the first pressure gauge 26 is <0.1 Pa, continue vacuuming for 10 min to 30 min. Close the first vacuum valve 24, and the vacuum device 10 stops operating.

[0135] Step 3: When the pressure exceeds the preset threshold, it is determined that the liquid phase pipeline has poor sealing. At this time, replace the sealing gasket at the liquid phase connection of the loading arm and repeat the above steps 1-2.

[0136] When the pressure does not exceed the preset threshold, and the liquid phase pipeline is determined to be in good sealing condition, the industrial ammonia valve 22 and the tank truck liquid phase valve 15 are opened. The liquid phase ultrapure ammonia in the tank truck 1 is transported to the industrial ammonia recovery tank 5 through the industrial ammonia valve 22 and the industrial ammonia condenser 7. The liquid phase filling pipeline and the liquid phase filling panel are replaced. The liquid weight is 30-80Kg. At the same time, the first ammonia purity analyzer 20 tests the pipeline. After ensuring that there are no impurity gases in the pipeline, the industrial ammonia valve 22, the liquid phase filling valve 17 and the tank truck liquid phase valve 15 are closed.

[0137] Step 4: Open the tank truck vapor phase valve 16, and close the vapor phase filling valve 18. Use a portable leak detector to check for leaks at the vapor phase interface between the tank truck and the loading arm. Close the tank truck vapor phase valve 16, and then open the vapor phase filling valve 18 and the second vent valve 29 in sequence to release the nitrogen and ammonia in the pipeline to the tail gas treatment system 9. When the pressure in the pipeline detected by the second pressure gauge 32 is <50 kPa, close the second vent valve 29, open the second vacuum valve 30, and start the vacuum device 10 to perform vacuuming on the vented pipeline between the vapor phase filling valve 18 and the tank truck vapor phase valve 16. When the pressure in the pipeline detected by the second pressure gauge 32 is <0.1 Pa, continue vacuuming for 10 min to 30 min, close the second vacuum valve 30, and stop the vacuum device 10.

[0138] Step 5: When the pressure exceeds the preset threshold, it is determined that the pipeline has poor sealing. At this time, replace the sealing gasket at the gas phase connection of the loading arm and repeat Step 4 above.

[0139] When the pressure does not exceed the preset threshold, and the liquid phase pipeline is determined to be in good sealing condition, the gaseous ammonia recovery valve 28, the gas phase filling valve 18, and the tank truck gas phase valve 16 are opened. The gaseous ultrapure ammonia in the tank truck 1 is transported to the industrial ammonia recovery tank 5 by the gaseous ammonia recovery valve 28 and the industrial ammonia condenser 7. At the same time, the second ammonia purity analyzer 27 detects the pipeline. After ensuring that there are no impurity gases in the pipeline, the gaseous ammonia recovery valve 28, the gas phase filling valve 18, and the tank truck gas phase valve 16 are closed.

[0140] Step 6: Open the liquid phase valve 15 and liquid phase filling valve 17 of the tank truck. The first ammonia purity analyzer 20 detects the liquid phase in the pipeline. When the analysis result shows that the ammonia purity is ≤99.9995%, the industrial ammonia valve 22 is opened. The liquid phase in the tank truck 1 transports the high-purity nitrogen gas in the pipeline to the industrial ammonia recovery tank 5 through the industrial ammonia valve 22 and the industrial ammonia condenser 7.

[0141] Step 7: Open the ammonia recovery valve 28, the gas phase filling valve 18, and the tank truck gas phase valve 16. The gas phase in the tank truck 1 is transported to the industrial ammonia recovery tank 5 through the ammonia recovery valve 28 and the industrial ammonia condenser 7. When the pressure in the tank truck 1 and the pressure in the industrial ammonia recovery tank 5 are the same, close the ammonia recovery valve 28 and open the second vent valve 29 to allow the gas phase in the tank truck 1 to be vented through the second vent pipeline and the ammonia tail gas discharge main pipe 9. When the pressure in the pipeline detected by the second pressure gauge 32 is 0.15~0.2MPa, close the second vent valve 29 and open the second vacuum valve 30. Start the vacuum device 10 to perform vacuuming treatment inside the tank truck 1. When the pressure in the pipeline detected by the second pressure gauge 32 is <0.1Pa, continue vacuuming for 10min~30min, close the second vacuum valve 30, and stop the vacuuming treatment.

[0142] Step 8: With the ultrapure ammonia subcooler 13 in a stopped state, open the filling valve 19. The saturated ultrapure ammonia product in the ultrapure ammonia purification unit 2 enters the tank truck 1 through the filling valve 19. The saturated ultrapure ammonia product vaporizes into cushion gas in the tank truck 1. Continue to fill the tank truck 1 with saturated ultrapure ammonia product until the pressure in the tank truck 1 reaches 0.5 MPa. Then close the filling valve 19 and open the gas phase filling valve 18 and the tank truck gas phase valve 16. The second ammonia purity analyzer 27 will detect the gas phase from the tank truck 1. If the detection meets the purity requirements of the ultrapure ammonia product, the cushion gas is deemed qualified. If the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion gas is deemed unqualified.

[0143] Step 9: If the cushion air is determined to be unqualified, repeat steps 6, 7 and 8 above until the cushion air is found to be qualified.

[0144] When the cushion gas is deemed qualified, the filling valve 19 is opened, allowing the saturated ultrapure ammonia product in the ultrapure ammonia purification device 2 to enter the tank truck 1 through the filling valve 19 to form a cushion liquid. When the weight of the filling cushion liquid is 300-600 kg, the filling valve 19 is closed, and the first ammonia purity analyzer 20 is used to detect the liquid phase in the tank truck 1. If the detection meets the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed qualified; if the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed unqualified.

[0145] Step 10: If the padding liquid is found to be unqualified, repeat steps 6, 7, 8 and 9 above until the padding liquid is found to be qualified.

[0146] When the padding liquid is deemed qualified, the ultrapure ammonia subcooler 13 is turned on and the filling valve 19 is opened. The saturated ultrapure ammonia product in the ultrapure ammonia purification device 2 enters the ultrapure ammonia subcooler 13 and is subcooled to 5-20°C. Then it enters the tank truck 1 through the filling valve 19 for filling. During the filling process, the weight is weighed by a weighbridge. When the weight reaches the corresponding threshold, the filling valve 19 is closed and the filling is completed.

[0147] Step 11: After filling, let stand for 2-3 hours, open the gas phase filling valve 18 and the tank truck gas phase valve 16, so that the second ammonia purity analyzer 27 can detect the gas phase from the tank truck 1. When the detection meets the purity requirements of ultrapure ammonia products, the product gas is judged to be qualified; when the detection does not meet the purity requirements of ultrapure ammonia products, the product gas is judged to be unqualified.

[0148] Step 12: When the product gas is determined to be unqualified, open the ammonia recovery valve 28. The gaseous ultrapure ammonia in tank truck 1 is transported to the industrial ammonia recovery tank 5 through the ammonia recovery valve 28 and the industrial ammonia condenser 7. 50-100 kg of gaseous phase in tank truck 1 is discharged, and then the product gas is analyzed to see if it is qualified. If it is still unqualified, repeat steps 6, 7, 8, 9, 10 and 11 above until the product gas is found to be qualified.

[0149] When the product gas is deemed qualified, the gas phase filling valve 18 and the tank truck gas phase valve 16 are closed, and the tank truck liquid phase valve 15 and the liquid phase filling valve 17 are opened. The first ammonia purity analyzer 20 detects the liquid phase in the pipeline. When the detection meets the purity requirements of ultrapure ammonia products, the product is deemed qualified. When the detection does not meet the purity requirements of ultrapure ammonia products, the product is deemed unqualified.

[0150] Step 13: When a product is determined to be unqualified, repeat steps 6, 7, 8, 9, 10, 11 and 12 above until the product is found to be qualified.

[0151] When the product is deemed qualified, close the liquid phase valve 15 of the tank truck and open the industrial ammonia valve 22 to allow the liquid phase in the pipeline to enter the industrial ammonia recovery tank 5 through the industrial ammonia recovery pipeline and the industrial ammonia condenser 7. After the liquid phase in the pipeline is emptied, close the industrial ammonia valve 22, open the first vacuum valve 24, start the vacuum device 10, and perform vacuuming. At the same time, close the liquid phase filling valve 17 and the first vacuum valve 24 in sequence, disassemble the loading arm liquid connection pipe, and install a blind flange on the liquid phase port of the loading arm 14 for sealing and protection.

[0152] Step 14: Close the tank truck vapor phase valve 16, open the second vacuum valve 30, and perform vacuuming; at the same time, close the tank truck vapor phase valve 16 and the vapor phase filling valve 18 in sequence; close the vacuuming device 10, and at the same time open the second nitrogen valve 31 to allow high-purity nitrogen from the high-purity nitrogen main pipe 12 to enter the pipeline between the vapor phase filling panel 4 and the vapor phase filling valve 18; when the second pressure gauge 32 detects that the pressure in the pipeline is 0.5-0.8 MPa, close the second nitrogen valve 31, disassemble the loading arm gas connection pipe, and install a blind flange on the vapor phase port of the loading arm 14 for sealing and protection.

[0153] 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 alterations 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 system for filling and recovering residual liquid from ultrapure ammonia tank trucks, the system comprising an ultrapure ammonia purification device (2) and an ammonia recovery unit, characterized in that: It also includes several tank cars (1) and several filling units that correspond one-to-one with the tank cars (1); The filling unit includes a liquid phase filling panel (3) for filling liquid ultrapure ammonia and for separately recovering the gas and liquid phases remaining in the tank truck (1) and a gas phase filling panel (4). The liquid phase filling panel (3) is provided with at least an ultrapure ammonia filling pipeline with a filling valve (19) and a liquid phase recovery pipeline for liquid phase detection and fractional recovery inside the tank truck (1); the inlet end of the ultrapure ammonia filling pipeline is connected to the ultrapure ammonia purification device (2), the outlet end of the ultrapure ammonia filling pipeline is connected to the liquid phase filling valve (17) of the corresponding tank truck (1) through the liquid phase recovery pipeline, and the outlet end of the liquid phase recovery pipeline is connected to the ammonia recovery unit. The gas phase filling panel (4) is provided with at least a gas phase recovery pipeline for gas phase detection inside the tank truck (1) and for gas phase recovery; the inlet end of the gas phase recovery pipeline is connected to the gas phase filling valve (18) of the corresponding tank truck (1), and the outlet end of the gas phase recovery pipeline is connected to the ammonia recovery unit.

2. The system for filling ultrapure ammonia tank trucks and recovering residual liquid according to claim 1, characterized in that: The liquid phase recovery pipeline section includes a first ammonia analysis pipeline with a first ammonia purity analyzer (20), a high-purity ammonia recovery pipeline with a high-purity ammonia valve (21), and an industrial ammonia recovery pipeline with an industrial ammonia valve (22).

3. The system for filling ultrapure ammonia tank trucks and recovering residual liquid according to claim 1, characterized in that: The liquid phase filling panel (3) also includes a first venting line with a first venting valve (23), a first vacuum line with a first vacuum valve (24), a first nitrogen line with a first nitrogen valve (25), and a first pressure detection line with a first pressure gauge (26).

4. The system for filling ultrapure ammonia tank trucks and recovering residual liquid according to claim 1, characterized in that: The gas phase recovery pipeline section includes a second ammonia analysis pipeline with a second ammonia purity analyzer (27) and a gas ammonia recovery pipeline with a gas ammonia recovery valve (28).

5. The system for filling ultrapure ammonia tank trucks and recovering residual liquid according to claim 1, characterized in that: The gas phase filling panel (4) also includes a second venting line with a second venting valve (29), a second vacuum line with a second vacuum valve (30), a second nitrogen line with a second nitrogen valve (31), and a second pressure detection line with a second pressure gauge (32).

6. The system for filling ultrapure ammonia tank trucks and recovering residual liquid according to claim 1, characterized in that: The ammonia recovery unit includes an industrial ammonia recovery tank (5) and a high-purity ammonia recovery tank (6); The industrial ammonia recovery tank (5) is connected to the industrial ammonia recovery pipeline in the liquid phase recovery pipeline section and the gaseous ammonia recovery pipeline in the gas phase recovery pipeline section through the industrial ammonia condenser (7). The high-purity ammonia recovery tank (6) is connected to the high-purity ammonia recovery pipeline via a high-purity ammonia subcooler (8).

7. The system for filling ultrapure ammonia tank trucks and recovering residual liquid according to claim 1, characterized in that: It also includes an ammonia tail gas discharge main pipe (9), which is connected to the first venting pipeline and the second venting pipeline respectively; It also includes a vacuum manifold (11) connected to the vacuum device (10), which is connected to the first vacuum line and the second vacuum line respectively. It also includes a high-purity nitrogen main pipe (12), which is connected to the first nitrogen pipeline and the second nitrogen pipeline respectively.

8. The system for filling ultrapure ammonia tank trucks and recovering residual liquid according to claim 1, characterized in that: An ultrapure ammonia subcooler (13) is provided between the ultrapure ammonia purification device (2) and the liquid phase filling panel (3). The tank truck (1) is equipped with a liquid phase valve (15) and a gas phase valve (16). The liquid phase valve (15) is connected to the liquid phase filling valve (17) through the loading arm (14), and the gas phase valve (16) is connected to the gas phase filling valve (18) through the loading arm (14).

9. A method for filling and recovering residual liquid from ultrapure ammonia tank trucks using the system described in any one of claims 1-8, characterized in that: The method includes the following steps: Step 1: Inspect the pipeline sealing between the tank truck (1) and the liquid phase filling panel (3) and the gas phase filling panel (4); Step 2: After the pipeline sealing test is qualified, the liquid phase in the tank truck (1) is separated and recovered. Step 3: Recover the gas phase inside the tanker (1); Step 4: The quality of ultrapure ammonia is analyzed and tested during the tanker filling process (1); Step 5: When the quality analysis and testing of ultrapure ammonia in step 4 is qualified, continue filling ultrapure ammonia. After the filling of tank truck (1) is completed, perform quality analysis and testing of ultrapure ammonia in tank truck (1). Step 6: When the quality analysis and testing of ultrapure ammonia in step 5 is qualified, the pipeline between the tank truck (1) and the liquid phase filling panel (3) and the gas phase filling panel (4) shall be sealed. Step 7: If the pipeline sealing test in Step 1 fails, reconnect the corresponding pipeline; repeat Step 1 after reconnection. Step 8: If the quality analysis of ultrapure ammonia in Step 4 fails, repeat Steps 2-4; Step 9: If the quality of the ultrapure ammonia analyzed in Step 5 fails to meet the standard, repeat Steps 2-5. Step 10: The ultrapure ammonia purification device (2) is connected to the corresponding tank truck (1) through several filling units, and is filled separately through the above steps 1-9.

10. A method for filling and recovering residual liquid using ultrapure ammonia tank trucks according to claim 9, characterized in that: The method includes the following steps: Step 1: The liquid phase valve (15) and gas phase valve (16) on the tank truck (1) are connected to the loading arm (14) respectively. The liquid phase port on the loading arm (14) is connected to the pipeline with the liquid phase filling valve (17), and the gas phase port on the loading arm (14) is connected to the pipeline with the gas phase filling valve (18). Step 2: Open the liquid phase filling valve (17) and close the tank truck liquid phase valve (15). Use a portable leak detector to check for leaks at the liquid phase interface between the tank truck and the loading arm. Open the first vent valve (23) to release the liquid ammonia in the pipeline to the ammonia tail gas discharge main pipe (9). When the pressure in the pipeline detected by the first pressure gauge (26) is <50 kPa, close the first vent valve (23), open the first vacuum valve (24), start the vacuum device (10), and vacuum the puncture pipeline between the liquid phase filling valve (17) and the tank truck liquid phase valve (15). When the pressure in the pipeline detected by the first pressure gauge (26) is <0.1 Pa, continue vacuuming for 10 min to 30 min, close the first vacuum valve (24), and stop the operation of the vacuum device (10). Step 3: When the pressure exceeds the preset threshold, it is determined that the liquid phase pipeline has poor sealing. At this time, replace the sealing gasket at the liquid phase connection of the loading arm and repeat the above steps 1-2. When the pressure does not exceed the preset threshold, the liquid phase pipeline is determined to be in good sealing condition. At this time, the industrial ammonia valve (22) and the tank truck liquid phase valve (15) are opened, and the liquid phase ultrapure ammonia in the tank truck (1) is transported to the industrial ammonia recovery tank (5) through the industrial ammonia valve (22) and the industrial ammonia condenser (7). The liquid phase filling pipeline and the liquid phase filling panel are replaced, and the liquid pressure weight is 30-80Kg. At the same time, the first ammonia purity analyzer (20) tests the pipeline. After ensuring that there are no impurity gases in the pipeline, the industrial ammonia valve (22), the liquid phase filling valve (17) and the tank truck liquid phase valve (15) are closed. Step 4: Open the tank truck vapor phase valve (16) and close the vapor phase filling valve (18). Use a portable leak detector to check for leaks at the vapor phase interface between the tank truck and the loading arm. Close the tank truck vapor phase valve (16), and open the vapor phase filling valve (18) and the second vent valve (29) in sequence to release the nitrogen and ammonia in the pipeline to the ammonia tail gas discharge main pipe (9). When the pressure in the pipeline detected by the second pressure gauge (32) is <50 kPa, close the second vent valve (29), open the second vacuum valve (30), start the vacuum device (10), and vacuum the puncture pipeline between the vapor phase filling valve (18) and the tank truck vapor phase valve (16). When the pressure in the pipeline detected by the second pressure gauge (32) is <0.1 Pa, continue vacuuming for 10 min to 30 min, close the second vacuum valve (30), and stop the operation of the vacuum device (10). Step 5: When the pressure exceeds the preset threshold, it is determined that the pipeline has poor sealing. At this time, replace the sealing gasket at the gas phase connection of the loading arm and repeat Step 4 above. When the pressure does not exceed the preset threshold, the gas phase pipeline is determined to be in good sealing condition. At this time, the gas ammonia recovery valve (28), the gas phase filling valve (18), and the tank truck gas phase valve (16) are opened. The gas phase ultrapure ammonia in the tank truck (1) is transported to the industrial ammonia recovery tank (5) by the gas ammonia recovery valve (28) and the industrial ammonia condenser (7). At the same time, the second ammonia purity analyzer (27) detects the pipeline. After ensuring that there are no impurity gases in the pipeline, the gas ammonia recovery valve (28), the gas phase filling valve (18), and the tank truck gas phase valve (16) are closed. Step 6: Open the liquid phase valve (15) and liquid phase filling valve (17) of the tank truck, and the first ammonia purity analyzer (20) detects the liquid phase in the pipeline; when the analysis result shows that the ammonia purity is >99.9995%, open the high-purity ammonia valve (21) so that the liquid phase in the tank truck (1) enters the high-purity ammonia subcooler (8) through the high-purity ammonia valve (21), and is subcooled in the high-purity ammonia subcooler (8) for 5-20°C and then recovered to the high-purity ammonia recovery tank (6); when the analysis result shows that the ammonia purity is ≤99.9995%, open the industrial ammonia valve (22), and the liquid phase in the tank truck (1) transports the high-purity nitrogen in the pipeline to the industrial ammonia recovery tank (5) through the industrial ammonia valve (22) and the industrial ammonia condenser (7); Step 7: Open the ammonia recovery valve (28), the gas phase filling valve (18), and the tank truck gas phase valve (16). The gas phase in the tank truck (1) is transported to the industrial ammonia recovery tank (5) through the ammonia recovery valve (28) and the industrial ammonia condenser (7). When the pressure in the tank truck (1) is the same as the pressure in the industrial ammonia recovery tank (5), close the ammonia recovery valve (28) and open the second vent valve (29) to allow the gas phase in the tank truck (1) to be vented through the second vent pipeline and the ammonia tail gas discharge main pipe (9). When the pressure in the pipeline detected by the second pressure gauge (32) is 0.15~0.2MPa, close the second vent valve (29) and open the second vacuum valve (30). Start the vacuum device (10) to vacuum the inside of the tank truck (1). When the pressure in the pipeline detected by the second pressure gauge (32) is <0.1Pa, continue vacuuming for 10min~30min, close the second vacuum valve (30), and stop the vacuuming process. Step 8: The ultrapure ammonia subcooler (13) is in a stopped state. Open the filling valve (19). The saturated ultrapure ammonia product in the ultrapure ammonia purification device (2) enters the tank truck (1) through the filling valve (19). The saturated ultrapure ammonia product vaporizes into cushion gas in the tank truck (1). Continue to fill the tank truck (1) with saturated ultrapure ammonia product until the pressure in the tank truck (1) is 0.5MPa. Then close the filling valve (19), open the gas phase filling valve (18) and the tank truck gas phase valve (16), so that the second ammonia purity analyzer (27) can detect the gas phase from the tank truck (1). When the detection meets the purity requirements of the ultrapure ammonia product, the cushion gas is judged to be qualified. When the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion gas is judged to be unqualified. Step 9: If the cushion air is determined to be unqualified, repeat steps 6, 7 and 8 above until the cushion air is found to be qualified. When the cushion gas is deemed qualified, the filling valve (19) is opened, allowing the saturated ultrapure ammonia product in the ultrapure ammonia purification device (2) to enter the tank truck (1) through the filling valve (19) to form a cushion liquid. When the weight of the filling cushion liquid is 300-600 kg, the filling valve (19) is closed, and the first ammonia purity analyzer (20) is used to detect the liquid phase in the tank truck (1). When the detection meets the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed qualified; when the detection does not meet the purity requirements of the ultrapure ammonia product, the cushion liquid is deemed unqualified. Step 10: If the padding liquid is found to be unqualified, repeat steps 6, 7, 8 and 9 above until the padding liquid is found to be qualified. When the padding liquid is deemed qualified, the ultrapure ammonia subcooler (13) is turned on and the filling valve (19) is opened. The saturated ultrapure ammonia product in the ultrapure ammonia purification device (2) enters the ultrapure ammonia subcooler (13), and after being subcooled to 5-20°C, it enters the tank truck (1) through the filling valve (19) for filling. During the filling process, the weight is weighed by a weighbridge. When the weight reaches the corresponding threshold, the filling valve (19) is closed and the filling is completed. Step 11: After filling, let stand for 2-3 hours, open the gas phase filling valve (18) and the tank truck gas phase valve (16) so that the second ammonia purity analyzer (27) can detect the gas phase from the tank truck (1). When the detection meets the purity requirements of ultrapure ammonia products, the product gas is judged to be qualified. When the detection does not meet the purity requirements of ultrapure ammonia products, the product gas is judged to be unqualified. Step 12: When the product gas is determined to be unqualified, open the ammonia recovery valve (28). The gaseous ultrapure ammonia in the tank truck (1) is transported to the industrial ammonia recovery tank (5) through the ammonia recovery valve (28) and the industrial ammonia condenser (7). 50-100 kg of gaseous phase in the tank truck (1) is discharged. Then, analyze whether it is qualified. If it is still unqualified, repeat the above steps 6, 7, 8, 9, 10 and 11 until the product gas is found to be qualified. When the product gas is deemed qualified, the gas phase filling valve (18) and the tank truck gas phase valve (16) are closed, and the tank truck liquid phase valve (15) and the liquid phase filling valve (17) are opened. The first ammonia purity analyzer (20) detects the liquid phase in the pipeline. When the detection meets the purity requirements of ultrapure ammonia products, the product is deemed qualified. When the detection does not meet the purity requirements of ultrapure ammonia products, the product is deemed unqualified. Step 13: When a product is determined to be unqualified, repeat steps 6, 7, 8, 9, 10, 11 and 12 above until the product is found to be qualified. When the product is deemed qualified, close the tank truck liquid phase valve (15), open the industrial ammonia valve (22), and allow the liquid phase in the pipeline to enter the industrial ammonia recovery tank (5) through the industrial ammonia recovery pipeline and the industrial ammonia condenser (7); after the liquid phase in the pipeline is emptied, close the industrial ammonia valve (22), open the first vacuum valve (24), start the vacuum device (10), and perform vacuum treatment; at the same time, close the liquid phase filling valve (17) and the first vacuum valve (24) in sequence, disassemble the loading arm liquid connection pipe, and install a blind flange on the liquid phase port of the loading arm (14) for sealing and protection; Step 14: Close the tank truck gas phase valve (16), open the second vacuum valve (30) to perform vacuuming; at the same time, close the gas phase filling valve (18); close the vacuum device (10), and at the same time open the second nitrogen valve (31) to allow the high-purity nitrogen from the high-purity nitrogen main pipe (12) to enter the pipeline between the gas phase filling panel (4) and the gas phase filling valve (18); when the second pressure gauge (32) detects that the pressure in the pipeline is 0.5 to 0.8 MPa, close the second nitrogen valve (31), disassemble the loading arm gas connection pipe, and install a blind flange on the gas phase port of the loading arm (14) for sealing protection.

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