An apparatus for drying ruthenium trichloride
By combining the jacketed vessel with a temperature-controlled heater, nitrogen purging, and cryogenic collection unit, the high-temperature decomposition and oxidation problems of ruthenium trichloride drying equipment are solved, achieving a highly efficient and environmentally friendly ruthenium trichloride drying process and avoiding material loss and equipment corrosion.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- DEZHOU LUEN NEW MATERIALS TECHNOLOGY CO LTD
- Filing Date
- 2025-07-14
- Publication Date
- 2026-06-23
AI Technical Summary
Existing ruthenium trichloride drying equipment is prone to decomposition and oxidation at high temperatures and has low heat transfer efficiency, resulting in material loss and environmental pollution, as well as equipment corrosion problems.
The design incorporates a jacketed vessel, a temperature-controlled heater, a nitrogen purging unit, a cryogenic collection unit, and a discharge unit. Through vacuum low-temperature heating, nitrogen replacement, and cryogenic collection, high-temperature oxidation and material agglomeration are avoided. Corrosion-resistant materials and a dispersing paddle are used for stirring to ensure uniform heating.
This method achieves efficient low-temperature drying of ruthenium trichloride, avoiding material loss and environmental pollution, improving heat transfer efficiency, and preventing equipment corrosion.
Smart Images
Figure CN224398196U_ABST
Abstract
Description
Technical Field
[0001] This utility model specifically relates to a device for drying ruthenium trichloride, belonging to the technical field of ruthenium trichloride processing equipment. Background Technology
[0002] After the synthesis of ruthenium trichloride is completed, it needs to be dried. Existing drying equipment, such as the drying and stirring device for ruthenium trichloride preparation disclosed in Chinese Patent Publication No. CN222978498U, uses a heating plate to heat and dry the ruthenium trichloride raw material introduced into the drying and stirring chamber. A stirring motor drives the stirring shaft and rotating plate to rotate, causing two sets of mixing plates to rotate, and corresponding multiple sets of stirring racks to rotate circumferentially within the drying and stirring chamber. This allows for the stirring and mixing of the ruthenium trichloride in the drying and stirring chamber. This process ensures full contact between ruthenium trichloride and the heat source, thereby improving heat transfer efficiency and accelerating the drying speed. However, due to its strong hygroscopicity, thermosensitivity, strong oxidizing properties, and high added value, ruthenium trichloride is prone to decomposition into RuO2 and Cl2 when dried in the aforementioned drying device or existing oven due to uneven temperature leading to local temperatures exceeding 120°C. This results in material loss. Furthermore, oven drying causes ruthenium trichloride to easily oxidize upon contact with air, and also leads to problems such as material agglomeration, low heat transfer efficiency, and severe equipment corrosion. Utility Model Content
[0003] To address the aforementioned problems, this invention proposes a device for drying ruthenium trichloride, which can ensure the drying quality of ruthenium trichloride and avoid material loss and environmental pollution.
[0004] The apparatus of this invention for drying ruthenium trichloride includes:
[0005] A jacketed vessel body, the top of which is provided with a vessel lid, and a dispersing paddle rotatably disposed inside the jacketed vessel body; the dispersing paddle is connected to a stirring motor at the top of the vessel lid; and a gate valve is provided at the bottom of the jacketed vessel body.
[0006] A temperature-controlled heater, wherein the temperature-controlled heater is disposed on the inner side of the jacket of the jacketed vessel;
[0007] A nitrogen purging unit is provided, wherein a nitrogen purging pipeline is installed on the upper inner side of the inner liner of the jacketed vessel; the nitrogen purging pipeline is connected to a nitrogen pressure source.
[0008] The cryogenic trapping unit includes an exhaust pipe connected to the upper inner side of the inner liner of the jacketed vessel, the exhaust pipe being connected to an exhaust pump; the exhaust pump being connected to the lower part of the cryogenic trap; an vent pipe being provided at the upper part of the cryogenic trap; and a dual-valve assembly being provided at the bottom of the cryogenic trap.
[0009] A discharge unit, the discharge unit including a gate valve.
[0010] In use, wet ruthenium trichloride is added to the jacketed vessel and sealed. Then, nitrogen is purged into the jacketed vessel through a nitrogen pressure source and its purging pipeline, and the exhaust pump is used to vent the gas, achieving 2-3 nitrogen replacements inside the jacketed vessel. After replacement, the temperature control heater and the exhaust pump are turned on to create a vacuum inside the jacketed vessel, and the temperature control heater is controlled to not exceed 80°C. The gas discharged by the exhaust pump enters the lower part of the cryogenic trap, is deeply cooled by the cryogenic trap, and the liquefied liquid is discharged by alternating opening of the dual valve group. After drying, the gate valve is opened, and the dried ruthenium trichloride material is discharged through the discharge unit.
[0011] Furthermore, the deep cold trap includes a vertical tube, the bottom of which is integrally formed with a reduced diameter section, and the dual valve assembly is connected to the reduced diameter section; a sealing plate is fixed to the top of the vertical tube by a flange; a heat exchange tube column is fixed inside the sealing plate; an exhaust gap is provided between the heat exchange tube column and the vertical tube; and a cold medium flow flange is provided at the top of the heat exchange tube column.
[0012] During the ruthenium trichloride drying process, an exhaust pump introduces hot gas into the vertical tube. The hot gas then enters the vertical tube and forms a slow flow. The hot gas then comes into full contact with the heat exchange tube column, where the cold medium in the heat exchange tube column deeply cools the hot gas, forming droplets. The droplets enter the bottom of the vertical tube, and the dual valve group alternately opens to ensure the sealing of the vertical tube while simultaneously discharging the accumulated droplets, thus completing the exhaust of the deeply cooled hot gas.
[0013] Furthermore, the inner wall of the vertical tube is provided with multiple rings of guide rings at intervals, and an exhaust gap is provided between the guide rings and the heat exchange tube column; the top surface of the guide ring is a downward-guiding slope structure; the guide ring can guide the direction of the interfering airflow, so that the exhaust is guided to the heat exchange tube column, and the airflow is cooled by the heat exchange tube column to form droplets; the droplets are guided to the bottom of the vertical tube through the guide ring.
[0014] Furthermore, the discharge unit is a screw conveyor or a discharge belt.
[0015] Furthermore, the reactor lid is provided with a feeding port or a screw feeder, and the feeding port is provided with a feeding gate valve; the wet ruthenium trichloride is fed into the jacketed reactor body through the feeding port or the screw feeder, and the feeding port is sealed after feeding is completed.
[0016] Furthermore, the temperature-controlled heater is a carbon fiber infrared film heater or a heat exchanger heater; when using a carbon fiber infrared film heater, the flexible carbon fiber infrared heating film of the carbon fiber infrared film heater is attached to the outer wall of the inner liner, controlling uniform radiant heating below 70±5℃; when using a heat exchanger heater, the heat exchanger heater continuously heats and controls the heat medium temperature below 70±5℃, providing circulating heat medium. The heat exchanger heater and the jacketed vessel form a closed loop through the heat medium circulation pipe, and the heat medium flows in the jacket of the jacketed vessel, continuously heating and drying ruthenium trichloride at low temperature.
[0017] Furthermore, the inner liner of the jacketed vessel is a Hastelloy alloy liner, which is resistant to chloride corrosion; the dispersion paddle is externally coated with a polytetrafluoroethylene (PTFE) layer; the PTFE layer can prevent material adhesion and has good corrosion resistance.
[0018] Compared with existing technologies, the equipment for drying ruthenium trichloride of this invention has good corrosion resistance. It uses a temperature-controlled heater for constant temperature heating and a dispersing paddle to intermittently disperse ruthenium trichloride, which can fully dry ruthenium trichloride and avoid agglomeration during the drying process. Vacuum low-temperature drying is used to prevent pyrolysis and oxidation during the drying process, and RuO4 in the hot air is captured by deep cooling. The entire drying process can avoid material loss and environmental pollution. Attached Figure Description
[0019] Figure 1 This is a schematic diagram of the overall structure of the ruthenium trichloride drying equipment of this utility model.
[0020] Figure 2 This is a schematic diagram of one embodiment of the jacketed vessel body of this utility model.
[0021] Figure 3 This is a schematic diagram of another embodiment of the jacketed vessel of this utility model.
[0022] Figure 4 This is a schematic diagram of the overall structure of the cryogenic trap of this utility model.
[0023] Figure 5 For the present utility model Figure 4 A magnified schematic diagram of the structure at point A in the middle.
[0024] Reference numerals: 1. Jacketed vessel body, 2. Vessel cover, 3. Dispersion paddle, 4. Stirring motor, 5. Gate valve, 6. Nitrogen purging line, 7. Exhaust pipe, 8. Exhaust pump, 9. Deep cold trap, 10. Drain pipe, 11. Dual valve assembly, 12. Vertical pipe, 13. Reduction section, 14. Sealing plate, 15. Heat exchange tube column, 16. Cold medium flow flange, 17. Guide ring, 18. Screw discharge device, 19. Feed port, 20. Carbon fiber infrared film heater, 21. Hot medium circulation pipe. Detailed Implementation
[0025] Example:
[0026] like Figures 1 to 5 The apparatus shown for drying ruthenium trichloride includes:
[0027] A jacketed vessel body 1 is provided with a vessel cover 2 on the top of the jacketed vessel body 1, and a dispersing paddle 3 is rotatably provided on the inner side of the jacketed vessel body 1; the dispersing paddle 3 is connected to a stirring motor 4 on the top of the vessel cover 2; and a gate valve 5 is provided at the bottom of the jacketed vessel body 1.
[0028] A temperature-controlled heater is disposed inside the jacket of the jacketed vessel 1;
[0029] A nitrogen purging unit is provided, wherein a nitrogen purging pipeline 6 is installed on the upper inner side of the inner liner of the jacketed vessel 1; the nitrogen purging pipeline 6 is connected to a nitrogen pressure source.
[0030] The cryogenic trapping unit includes an exhaust pipe 7 connected to the upper inner side of the inner liner of the jacketed vessel 1, the exhaust pipe 7 being connected to an exhaust pump 8; the exhaust pump 8 being connected to the lower part of the cryogenic trap 9; an vent pipe 10 being provided on the upper part of the cryogenic trap 9; and a double valve group 11 being provided at the bottom of the cryogenic trap 9.
[0031] The discharge unit includes a valve 5 connected to the gate valve.
[0032] In use, wet ruthenium trichloride is added into the jacketed vessel 1 and sealed. Then, nitrogen is purged into the jacketed vessel 1 through a nitrogen pressure source and its purging pipeline, and exhaust is carried out by the exhaust pump 8, achieving 2-3 nitrogen replacements inside the jacketed vessel 1. After replacement, the temperature control heater and the exhaust pump 8 are turned on to maintain the reaction vessel at -0.06~-0.09 MPa, so that the jacketed vessel 1 is in a vacuum state, and the temperature control heater is controlled not to exceed 80°C. During heating, the stirring motor 4 is controlled to operate, so that the dispersion paddle 3 is intermittently stirred, rotating 2 revolutions every 5 minutes. The gas discharged by the exhaust pump 8 enters the lower part of the deep cold trap 9, is deeply cooled by the deep cold trap 9, and the deeply liquefied liquid is discharged by the alternating opening of the double valve group 11. After drying is completed, the gate valve 5 is opened, and the dried ruthenium trichloride material is discharged through the discharge unit.
[0033] The deep cold trap 9 includes a vertical tube 12, the bottom of which is integrally formed with a reduced diameter section 13, and the dual valve group 11 is connected to the reduced diameter section 13; a sealing plate 14 is fixed to the top of the vertical tube 12 by a flange; a heat exchange tube column 15 is fixed inside the sealing plate 14; an exhaust gap is provided between the heat exchange tube column 15 and the vertical tube 12; and a cold medium flow flange 16 is provided at the top of the heat exchange tube column 15.
[0034] During the ruthenium trichloride drying process, the exhaust pump 8 introduces hot gas into the vertical pipe 12. The hot gas then enters the vertical pipe 12 and forms a slow flow. The hot gas then comes into full contact with the heat exchange column 15. The cold medium in the heat exchange column 15 deeply cools the hot gas to a temperature of -40°C, capturing volatile RuO4 vapor to prevent material loss and environmental pollution. The RuO4 vapor liquefies to form droplets, which enter the bottom of the vertical pipe 12. The droplets are alternately opened by the dual valve group 11, which ensures the sealing of the vertical pipe 12 and discharges the accumulated droplets, thus completing the discharge of the deeply cooled hot gas.
[0035] The inner wall of the vertical tube 12 is provided with multiple rings of guide rings 17 at intervals, and an exhaust gap is provided between the guide rings 17 and the heat exchange tube column 15; the top surface of the guide rings 17 is a downward-sloping structure; the guide rings 17 can guide the direction of the airflow, causing the exhaust to be guided to the heat exchange tube column 15, and the airflow is cooled by the heat exchange tube column 15 to form droplets; the droplets are guided to the bottom of the vertical tube 12 through the guide rings 17.
[0036] The discharge unit is a screw conveyor 18 or a discharge belt.
[0037] The reactor lid 2 is provided with a feeding port 19 or a screw feeder, and the feeding port 19 is provided with a feeding gate valve; wet ruthenium trichloride is fed into the jacketed reactor body 1 through the feeding port 19 or the screw feeder, and the feeding port 19 is sealed after feeding is completed.
[0038] The temperature-controlled heater is either a carbon fiber infrared film heater 20 or a heat exchanger heater. When using a carbon fiber infrared film heater 20, the flexible carbon fiber infrared heating film of the carbon fiber infrared film heater 20 is attached to the outer wall of the inner liner to control uniform radiant heating below 70±5℃. When using a heat exchanger heater, the heat exchanger heater continuously heats and controls the temperature of the heat medium below 70±5℃, providing circulating heat medium. The heat exchanger heater and the jacketed vessel 1 form a closed loop through the heat medium circulation pipe 21. The heat medium flows in the jacket of the jacketed vessel 1 to continuously heat and dry ruthenium trichloride at a low temperature.
[0039] The inner liner of the jacketed vessel 1 is made of Hastelloy alloy and is resistant to chloride corrosion. The dispersion paddle 3 is covered with a polytetrafluoroethylene (PTFE) layer. The PTFE layer can prevent material adhesion and has good corrosion resistance.
[0040] The above embodiments are merely preferred embodiments of the present utility model. Therefore, all equivalent changes or modifications made to the structure, features and principles described in the claims of the present utility model are included within the scope of the present utility model.
Claims
1. An apparatus for drying ruthenium trichloride, characterized by: include: A jacketed vessel body, the top of which is provided with a vessel lid, and a dispersing paddle rotatably disposed inside the jacketed vessel body; the dispersing paddle is connected to a stirring motor at the top of the vessel lid; and a gate valve is provided at the bottom of the jacketed vessel body. A temperature-controlled heater, wherein the temperature-controlled heater is disposed on the inner side of the jacket of the jacketed vessel; A nitrogen purging unit is provided, wherein a nitrogen purging pipeline is installed on the upper inner side of the inner liner of the jacketed vessel; the nitrogen purging pipeline is connected to a nitrogen pressure source. A cryogenic trapping unit, the cryogenic trapping unit including an exhaust pipe connected to the upper inner side of the inner liner of the jacketed vessel, the exhaust pipe being connected to an exhaust pump; The exhaust pump is connected to the lower part of the cryogenic trap; an vent pipe is provided at the upper part of the cryogenic trap; a dual-valve assembly is provided at the bottom of the cryogenic trap; A discharge unit, the discharge unit including a gate valve.
2. The apparatus for drying ruthenium trichloride according to claim 1, characterized in that: The deep cold trap includes a vertical tube, the bottom of which is integrally formed with a reduced diameter section, and the dual valve assembly is connected to the reduced diameter section; a sealing plate is fixed to the top of the vertical tube by a flange; a heat exchange tube column is fixed inside the sealing plate; an exhaust gap is provided between the heat exchange tube column and the vertical tube; and a cold medium flow flange is provided at the top of the heat exchange tube column.
3. The apparatus for drying ruthenium trichloride according to claim 2, characterized in that: The inner wall of the vertical tube is provided with multiple guide rings at intervals, and an exhaust gap is provided between the guide rings and the heat exchange tube column; the top surface of the guide rings is a downward guiding slope structure.
4. The apparatus for drying ruthenium trichloride according to claim 1, characterized in that: The discharge unit is a screw conveyor or a discharge belt.
5. The apparatus for drying ruthenium trichloride according to claim 1, characterized in that: The reactor lid is equipped with a feeding port or a screw feeder, and the feeding port is equipped with a feeding gate valve.
6. The apparatus for drying ruthenium trichloride according to claim 1, characterized in that: The temperature-controlled heater is a carbon fiber infrared film heater or a heat exchanger heater.
7. The apparatus for drying ruthenium trichloride according to claim 1, characterized in that: The inner liner of the jacketed vessel is made of Hastelloy alloy; the dispersion paddle is covered with a polytetrafluoroethylene layer.