Vacuum distillation equipment
By using a split-type temperature-controlled vacuum distillation equipment, the problems of impurity introduction, high energy consumption, and low production capacity in SiO preparation have been solved, achieving efficient and stable preparation of SiO anode materials and improving product consistency and quality.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- SHENYANG VACUUM TECH INST
- Filing Date
- 2025-07-29
- Publication Date
- 2026-05-19
AI Technical Summary
Existing vacuum distillation equipment for SiO preparation suffers from problems such as impurity introduction, high energy consumption, low production capacity, and poor product performance consistency. In particular, the high content of magnetic impurities and poor product consistency are caused by the inability to control the temperature during the condensation process.
The equipment employs a split-type temperature-controlled vacuum distillation system, which includes a high-temperature reaction chamber, a vapor transition zone, and a constant-temperature condensation chamber. Through independent temperature control and vacuum systems, it achieves temperature and vacuum control during the volatilization, transport, and condensation stages. Non-magnetic materials and high-temperature insulation layers are used to avoid the introduction of impurities and maintain the temperature gradient.
This technology enables the efficient preparation of 400 kg/furnace of SiO anode material, improving material performance and consistency, reducing impurity content, minimizing equipment wear, and enhancing production capacity and product quality.
Smart Images
Figure CN224252121U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the field of vacuum equipment technology, and particularly relates to a vacuum distillation equipment, especially a split-type temperature-controlled vacuum distillation equipment for preparing SiO anode materials based on silicon self-reduction reaction. Background Technology
[0002] Silicon suboxide (SiO), as a silicon-based anode, has the advantages of high energy density and good cycle performance, and has become an important component of lithium-ion battery anode materials. However, existing vacuum distillation equipment for SiO preparation has the following drawbacks:
[0003] 1. Impurity introduction: Excessive temperature at the collection end leads to a high content of magnetic impurities in the product.
[0004] 2. High energy consumption: The reaction requires a high temperature of >1600℃, resulting in significant equipment wear and tear.
[0005] 3. Low production capacity: usually below 100 kg / furnace.
[0006] 4. Poor product performance consistency: Due to the heat release during the SiO condensation process, the temperature at the collection end cannot be controlled, making it impossible to achieve constant temperature collection, resulting in poor consistency of the collected products. Summary of the Invention
[0007] This utility model addresses the shortcomings of existing technologies by providing a vacuum distillation apparatus.
[0008] To achieve the above objectives, the present invention adopts the following technical solution: a vacuum distillation equipment, comprising a high-temperature reaction chamber, a vapor transition zone, a constant-temperature condensation chamber, and a vacuum system.
[0009] The high-temperature reaction chamber includes a vacuum chamber and a heating chamber located inside it. The heating chamber is wrapped by a heating chamber insulation layer and contains a reaction crucible and a heating chamber heater.
[0010] The vapor transition zone includes a transition pipe and a two-stage heating chamber. The two-stage heating chamber is wrapped by a two-stage heating chamber insulation layer and contains a transition pipe and a two-stage heating chamber heater. One end of the transition pipe is connected to the vapor outlet of the reaction crucible, and the other end extends to the constant temperature condensation chamber.
[0011] The constant temperature condensing chamber includes two vacuum chambers and three heating chambers disposed inside them. The three heating chambers are wrapped by a three-section heating chamber insulation layer and have a muffle isolation chamber and a three-section heating chamber heater inside.
[0012] The two-stage vacuum chamber is connected to the vacuum system.
[0013] Furthermore, the vacuum system includes a slide valve vacuum pump, a Roots vacuum pump, a filtration system, and a vacuum valve; wherein, the filtration system is located on the pipeline between the vacuum valve and the slide valve vacuum pump / Roots vacuum pump, and is used to filter dust particles carried by the gas during the vacuuming process.
[0014] Furthermore, the vacuum valve is connected to the pipeline between the second-stage vacuum chamber and the filtration system, and is used to control the connection and disconnection between the vacuum system and the second-stage vacuum chamber.
[0015] Furthermore, the vacuum valve includes a slow-release valve and a fast-evacuation valve arranged in parallel. The slow-release valve is used to open in the initial stage of vacuuming to prevent material from being carried out, and the fast-evacuation valve is used to maintain a high vacuum environment during the reaction stage.
[0016] Furthermore, the first vacuum chamber and the second vacuum chamber have a double-layer water-cooled wall structure, and the two vacuum chambers are sealed together.
[0017] Furthermore, the reaction crucible is a closed isostatic graphite barrel with a loading hole at the top and a vapor outlet connected to a transition pipe on the upper side.
[0018] Furthermore, the first-stage heating chamber heater, the second-stage heating chamber heater, and the third-stage heating chamber heater are each independently connected to a PID temperature control module. Each heater and the thermocouple in the corresponding heating chamber form a closed-loop temperature control system to achieve independent temperature gradient control of the high-temperature reaction chamber, the steam transition zone, and the constant-temperature condensing chamber.
[0019] Furthermore, the muffle isolation chamber is made of non-magnetic metal material.
[0020] Furthermore, the two ends of the transition tube are respectively connected to the reaction crucible and the constant temperature condensation chamber in a non-magnetic isolation manner.
[0021] Furthermore, the transition tube has a density greater than 1.82 g / cm³. 3 Isostatic graphite tubes.
[0022] Compared with the prior art, this utility model has the following advantages.
[0023] This invention relates to a split-type temperature-controlled vacuum distillation furnace, which solves the temperature fluctuation problem caused by condensation heat accumulation in traditional processes by controlling the temperature and vacuum during the volatilization, transport, and condensation stages. Attached Figure Description
[0024] The present invention will be further described below with reference to the accompanying drawings and specific embodiments. The scope of protection of the present invention is not limited to the following description.
[0025] Figure 1 This is a schematic diagram of the overall structure of the vacuum distillation equipment in a specific embodiment.
[0026] Figure 2 This is a schematic diagram of the high-temperature reaction chamber structure in a specific embodiment.
[0027] Figure 3 This is a schematic diagram of the vapor transition zone structure in a specific embodiment.
[0028] Figure 4 This is a schematic diagram of the constant temperature condenser structure in a specific embodiment.
[0029] Figure 5 This is a schematic diagram of the vacuum system structure in a specific embodiment.
[0030] In the diagram, 1. Vacuum system; 2. Filtration system; 3. Two-stage vacuum chamber; 4. Rotary water-cooled cylinder with water cooling function; 6. Three-stage heating chamber insulation layer; 7. Three-stage heating chamber heater; 8. Two-stage heating chamber insulation layer; 9. Two-stage heating chamber heater; 10. Transition pipe; 11. One-stage heating chamber insulation layer; 12. Reaction crucible; 13. One-stage vacuum chamber; 14. One-stage heating chamber heater. Detailed Implementation
[0031] The technical solutions of the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this disclosure, and not all embodiments. Based on the embodiments of this disclosure, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this disclosure.
[0032] The terminology used in the embodiments of this disclosure is for the purpose of describing particular embodiments only and is not intended to be limiting of this disclosure. The singular forms “a,” “the,” and “the” as used in the embodiments of this disclosure and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise.
[0033] Depending on the context, words such as “if” or “suppose” used here can be interpreted as “when”, “in response to determination”, or “in response to detection”.
[0034] For ease of understanding, the embodiments of this disclosure will be described in detail first.
[0035] like Figure 1-5As shown in the specific embodiment: The vacuum distillation equipment includes a high-temperature reaction chamber, a vapor transition zone, a constant-temperature condensing chamber, and a vacuum system; the high-temperature reaction chamber includes a vacuum chamber 13 and a heating chamber disposed inside it, which is wrapped by a heating chamber insulation layer 11, and contains a reaction crucible 12 and a heating chamber heater 14; the vapor transition zone includes a transition pipe 10 and a second heating chamber, which is wrapped by a second heating chamber insulation layer 8, and contains a transition pipe 10 and a second heating chamber heater 9. One end of the transition pipe 10 is connected to the vapor outlet of the reaction crucible 12, and the other end extends to the constant-temperature condensing chamber; the constant-temperature condensing chamber includes a second vacuum chamber 3 and a third heating chamber disposed inside it, which is wrapped by a third heating chamber insulation layer 6, and contains a muffle isolation chamber and a third heating chamber heater 7; the second vacuum chamber 3 is connected to the vacuum system.
[0036] Preferably, the vacuum system includes a slide valve vacuum pump, a Roots vacuum pump, a filter system 2, and a vacuum valve; wherein, the filter system 2 is located on the pipeline between the vacuum valve and the slide valve vacuum pump / Roots vacuum pump, and is used to filter dust particles carried by the gas during the vacuuming process. The vacuum valve is connected to the pipeline between the secondary vacuum chamber 3 and the filter system 2, and is used to control the opening and closing of the vacuum system and the secondary vacuum chamber 3.
[0037] Preferably, the vacuum valve includes a slow-release valve and a fast-evacuation valve arranged in parallel. The slow-release valve is used to open in the initial stage of vacuuming to prevent material from being carried out, and the fast-evacuation valve is used to maintain a high vacuum environment during the reaction stage.
[0038] Preferably, the first vacuum chamber 13 and the second vacuum chamber 3 have a double-layer water-cooled wall structure, and the two vacuum chambers are sealed together.
[0039] Preferably, the reaction crucible 12 is a closed isostatic graphite barrel with a loading hole at the top and a steam outlet connected to the transition pipe 10 on the upper side.
[0040] Preferably, the first-stage heating chamber heater 14, the second-stage heating chamber heater 9, and the third-stage heating chamber heater 7 are each independently connected to a PID temperature control module. Each heater and the thermocouple in the corresponding heating chamber form a closed-loop temperature control system to achieve independent temperature gradient control of the high-temperature reaction chamber, the steam transition zone, and the constant-temperature condensing chamber.
[0041] Preferably, the muffle isolation chamber is made of non-magnetic metal material.
[0042] Preferably, the two ends of the transition tube are isolated from the reaction crucible and the muffle of the isothermal condenser, respectively. Furthermore, the transition tube has a density greater than 1.82 g / cm³. 3 The isostatic graphite tube, with a transition tube capable of maintaining a temperature gradient of 1350℃→1300℃. Muffle-isolated connections refer to connections with non-magnetic foreign object isolation or non-magnetic isolation.
[0043] In one possible preferred embodiment, a rotating water-cooled cylinder 4 is installed within the three-stage heating chamber. The rotating water-cooled cylinder 4 is rotatably connected to the top of the second-stage vacuum chamber 3, and its interior has a cooling water circulation channel to assist in temperature control of the constant-temperature condensation chamber. The rotating water-cooled cylinder 4 employs a dynamic seal to lead the water pipes out of the second-stage vacuum chamber. This dynamic seal can be a magnetohydrodynamic seal. The rotating water-cooled cylinder 4 counteracts the heat release during condensation by adjusting the cooling water flow rate.
[0044] Example and Effect 1:
[0045] 1. Mix SiO2 and Si powder in a 1:1 molar ratio and ball mill until the particle size is <50μm. Then, put the mixture into the reaction crucible in the high-temperature reaction chamber and close the feeding hole. The crucible has a volume of 600L and can hold 400Kg of raw material.
[0046] 2. Using a vacuum system, the vacuum chamber is evacuated to below 5 Pa, and the temperature is increased to 1350℃ at 10℃ / min to start the heat preservation process. During the heat preservation stage, SiO vapor is generated.
[0047] 3. The transition tube can maintain a temperature gradient of 1350℃→1300℃, suppressing steam condensation.
[0048] 4. Dynamic condensation: After the steam enters the constant temperature condensing chamber, the condensing chamber temperature is set to 800℃. When the local temperature is detected to rise to 815℃ due to heat release, the cooling water flow rate in the rotating water-cooled cylinder with water cooling function is automatically increased to 3L / min, and the temperature is restored to 800℃ within 10 minutes.
[0049] Example and Effect 2:
[0050] When the cooling water inside the rotating water-cooled cylinder with water cooling function is turned off, the temperature of the condensation chamber rises to 840°C within 1 hour of being kept at the high temperature reaction chamber, causing 15% of SiO to re-evaporate, and the yield drops to 78%.
[0051] In this embodiment, the reaction crucible 12 has a density greater than 1.82 g / cm³. 3 The isostatic graphite crucible can be used for a long time under a Si atmosphere, and the SiO vapor will not overflow from the crucible during the reaction process.
[0052] In this embodiment, the three heating chambers in the constant temperature condensation chamber are equipped with a rotating water-cooled cylinder 4 with water cooling function and a muffle isolation chamber. The rotating water-cooled cylinder 4 and the muffle isolation chamber with water cooling function are all made of 310S heat-resistant steel to reduce the volatilization of magnetic foreign matter into the final product.
[0053] In this embodiment, the filtration system 2 is used to filter dust particles carried out by the air during the evacuation process.
[0054] This novel vacuum distillation equipment for preparing SiO anode materials with split-section temperature control can achieve a SiO preparation rate of 400 kg / furnace, filling the gap in domestic large-capacity SiO preparation equipment. Furthermore, the equipment adopts a multi-section split-section temperature control structure, which can collect SiO materials condensed at a constant temperature, greatly improving the performance and consistency of the materials.
[0055] This novel vacuum distillation equipment for preparing SiO anode materials with split temperature control ensures that the material does not come into contact with materials containing magnetic substances during the preparation process, thus significantly improving the material quality.
[0056] This novel vacuum distillation equipment for preparing SiO anode materials with split temperature control can achieve a three-stage temperature gradient design (1350℃→1300℃→800℃), and achieve stable cooling of SiO gas through a high-temperature resistant insulation layer and a graphite flow channel.
[0057] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "illustrative embodiment," "preferred embodiment," "detailed description," or "preferred embodiment," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0058] The above embodiments are only used to illustrate the technical solutions of this utility model, and are not intended to limit it. Although this utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Therefore, these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope defined by the claims of this utility model.
Claims
1. A vacuum distillation apparatus, characterized in that, Includes a high-temperature reaction chamber, a vapor transition zone, a constant-temperature condensation chamber, and a vacuum system; The high-temperature reaction chamber includes a vacuum chamber (13) and a heating chamber located inside it. The heating chamber is wrapped by a heating chamber insulation layer (11) and has a reaction crucible (12) and a heating chamber heater (14) inside. The vapor transition zone includes a transition pipe (10) and a second-stage heating chamber. The second-stage heating chamber is wrapped by a second-stage heating chamber insulation layer (8). Inside, there is a transition pipe (10) and a second-stage heating chamber heater (9). One end of the transition pipe (10) is connected to the vapor outlet of the reaction crucible (12), and the other end extends to the constant temperature condensation chamber. The constant temperature condensing chamber includes a two-section vacuum chamber (3) and a three-section heating chamber disposed inside it. The three-section heating chamber is wrapped by a three-section heating chamber insulation layer (6) and has a muffle isolation chamber and a three-section heating chamber heater (7) inside. The second-stage vacuum chamber (3) is connected to the vacuum system.
2. The vacuum distillation equipment according to claim 1, characterized in that, The vacuum system includes a slide valve vacuum pump, a Roots vacuum pump, a filtration system (2), and a vacuum valve; wherein the filtration system (2) is located on the pipeline between the vacuum valve and the slide valve vacuum pump / Roots vacuum pump, and is used to filter dust particles carried by the gas during the vacuuming process.
3. The vacuum distillation equipment according to claim 2, characterized in that, The vacuum valve is connected to the pipeline between the second-stage vacuum chamber (3) and the filter system (2) and is used to control the opening and closing of the vacuum system and the second-stage vacuum chamber (3).
4. The vacuum distillation equipment according to claim 3, characterized in that, The vacuum valve includes a slow-release valve and a fast-evacuation valve arranged in parallel. The slow-release valve is used to open in the initial stage of vacuuming to prevent material from being carried out, and the fast-evacuation valve is used to maintain a high vacuum environment during the reaction stage.
5. The vacuum distillation equipment according to claim 1, characterized in that, The first vacuum chamber (13) and the second vacuum chamber (3) are double-layer water-cooled wall structures, and the two vacuum chambers are sealed together.
6. The vacuum distillation equipment according to claim 1, characterized in that, The reaction crucible (12) is a closed isostatic graphite barrel with a loading hole at the top and a steam outlet connected to the transition pipe (10) on the upper side.
7. The vacuum distillation equipment according to claim 1, characterized in that, The first-stage heating chamber heater (14), the second-stage heating chamber heater (9), and the third-stage heating chamber heater (7) are each independently connected to a PID temperature control module. Each heater and the thermocouple in the corresponding heating chamber form a closed-loop temperature control system to achieve independent temperature gradient control of the high-temperature reaction chamber, the steam transition zone, and the constant-temperature condensing chamber.
8. The vacuum distillation equipment according to claim 1, characterized in that, The muffle isolation chamber is made of non-magnetic metal material.
9. The vacuum distillation equipment according to claim 1, characterized in that, The two ends of the transition tube (10) are respectively connected to the reaction crucible and the constant temperature condenser in a non-magnetic isolation manner.
10. The vacuum distillation equipment according to claim 1, characterized in that, The transition tube (10) has a density greater than 1.82 g / cm³. 3 Isostatic graphite tubes.