An apparatus for metal rubidium cesium reduction reaction

Abstract

The utility model relates to metal thermal reduction technical field, concretely for a kind of device for metal rubidium cesium reduction reaction, including reaction kettle, the bottom of reaction kettle is equipped with several heat conduction columns, the top of reaction kettle is feed pipe, side is discharge pipe, further include metal collecting device, metal collecting device is by calcium vapor baffle and condenser tube constitute, calcium vapor baffle is located inside the reaction kettle, condenser tube is located inside the discharge pipe. In the device for metal rubidium cesium reduction reaction, the heat conduction column installed at the bottom of the reaction kettle extends to 60%-80% of the depth of the material layer thickness, can heat deeply into the material layer, ensure that the temperature in the material layer is evenly distributed, greatly reduce the incomplete reaction phenomenon caused by uneven temperature. Compared with traditional device, the reaction rate can be greatly improved, the reaction time is significantly shortened, and the output of metal rubidium cesium is greatly improved, meeting the growing market demand.

Description

Technical Field

[0001] This utility model relates to the field of metal thermal reduction technology, and more specifically, to an apparatus for the reduction reaction of metal rubidium and cesium. Background Technology

[0002] In the field of metallothermic reduction technology, the preparation of rubidium and cesium has always been a research focus. Rubidium (Rb) and cesium (Cs), as rare and precious metal resources, have demonstrated immense application value in numerous fields since their discovery due to their unique physical and chemical properties, such as new energy, aerospace, defense industry, bioengineering, advanced medicine, electronic technology, special materials and equipment, and other high-precision manufacturing industries. However, factors such as low ore reserves and complex preparation processes result in scarce production and high prices of high-purity metals, greatly limiting their widespread application.

[0003] Currently, the metallothermic reduction method is the mainstream approach for preparing metallic rubidium and cesium. This method uses rubidium or cesium-containing salts as raw materials and strong reducing metals (such as lithium, sodium, calcium, and magnesium) as reducing agents. The reduction reaction is carried out at high temperature and in an inert atmosphere. Subsequently, vacuum distillation is used to transfer rubidium and cesium as vapors from the reaction apparatus, and the metal vapors are collected by condensation. However, in actual production, existing equipment for the reduction reaction of metallic rubidium and cesium has revealed a series of problems. For example, the reaction vessel in some devices is prone to clogging during the cleaning process after the reaction, which not only increases maintenance costs but also reduces production efficiency. At the same time, the design of some devices is overly complex, making it difficult for the reaction to proceed completely, resulting in excessively long reaction times and insufficient yields, failing to meet the growing market demand.

[0004] Taking patent application number CN220771853 as an example, this patent discloses a reaction chamber applied to metal rubidium and cesium production equipment, which solves the sealing problem in metal rubidium and cesium production, but has the problems of inconvenient material collection and low production efficiency. Utility Model Content

[0005] The purpose of this invention is to provide an apparatus for the reduction reaction of rubidium and cesium metals, so as to solve the problem mentioned in the background art that the existing equipment is inconvenient to collect materials, thus affecting production efficiency.

[0006] To achieve the above objectives, this utility model provides an apparatus for the reduction reaction of rubidium and cesium metals, including a reaction vessel, a plurality of heat-conducting columns installed at the bottom of the reaction vessel, a feed pipe at the top of the reaction vessel, a discharge pipe on the side, and also comprising a calcium vapor baffle and a condenser, wherein the calcium vapor baffle is located inside the reaction vessel and the condenser is located inside the discharge pipe.

[0007] This setup uses a reactor as the core reaction vessel, with a heat-conducting column at the bottom for direct heat transfer to the reactants. A top feed pipe adds rubidium or cesium salts and a strong reducing agent, while a side outlet pipe removes the metal vapors generated during the reaction. A calcium vapor baffle, located inside the reactor, extends the vapor travel and utilizes the difference in condensation points between calcium vapor and rubidium / cesium vapor to preferentially condense the calcium vapor. A condenser, placed inside the outlet pipe, cools the removed gaseous metal. The entire apparatus, through the coordinated operation of its components, achieves the reduction reaction and collection of metallic rubidium and cesium.

[0008] Preferably, both the feed pipe and the discharge pipe are fitted with cooling water jackets, the inside of which is provided with a water storage cavity, and the sides are provided with water jacket inlet and outlet ports respectively.

[0009] This device features cooling water jackets fitted onto the feed and discharge pipes. The internal water storage chambers circulate cooling water through the inlet and outlet ports of the jackets. During the reaction, the cooling water absorbs the heat transferred from the feed and discharge pipes due to the high-temperature reaction, reducing the temperature of the pipe sealing components and providing cooling protection.

[0010] Preferably, a temperature probe hole is provided on the top of the reactor.

[0011] This feature includes a temperature probe hole on the top of the reactor for installing a temperature probe. The probe monitors temperature changes inside the reactor in real time and transmits the temperature data to an external temperature control box. The temperature control box adjusts the heating process of the reactor according to preset reaction temperature parameters, achieving precise temperature control.

[0012] Preferably, the extension depth of the heat-conducting pillar is 60%-80% of the material layer thickness.

[0013] This setting allows the heat-conducting column to extend to a depth of 60%-80% of the material layer thickness, enabling it to penetrate deep into the material layer for heat transfer. Because the distance between the upper and lower parts of the material layer and the heating source varies, conventional heating methods often result in uneven temperatures. The heat-conducting column extending deep into the material layer allows for more even heat distribution throughout the entire layer, reducing temperature gradients.

[0014] Preferably, two calcium vapor baffles are arranged alternately, and each calcium vapor baffle is a flat plate structure, covering 2 / 3 to 3 / 4 of the reactor cavity area.

[0015] This design incorporates two staggered, flat calcium vapor baffles covering 2 / 3 to 3 / 4 of the reactor cavity area, extending the vapor's travel path within the reactor. Among the vapors generated by the metallothermic reduction reaction, calcium vapor has a relatively low condensation point; the longer travel path allows it more opportunities to contact the baffles and preferentially condense, thus separating it from the rubidium and cesium vapors.

[0016] Preferably, the condenser tube is provided with a spiral groove inside as a guide channel to extend the metal vapor's travel distance, allowing the metal vapor to cool naturally and liquefy and be discharged at the outlet of the guide channel.

[0017] This design, with its spiral grooves inside the condenser tubes, extends the travel distance of the metal vapor within the tubes, increasing the contact area and time between the metal vapor and the inner wall of the condenser tubes. Simultaneously, as the metal vapor flows within the spiral channels, its velocity and direction constantly change, promoting heat exchange and enabling rapid cooling of the gaseous metal.

[0018] Preferably, the reactor is a hollow cavity made of stainless steel, with an electric heating furnace attached to the outer layer.

[0019] The reactor in this setup features a hollow stainless steel cavity, which possesses excellent high-temperature and corrosion resistance, enabling it to withstand the high temperatures and chemically corrosive environments encountered during the reaction process. The outer-mounted electric heater converts electrical energy into heat energy, providing a uniform and stable heat source to the reactor, ensuring that the reactor reaches the high-temperature conditions required for the metallothermal reduction reaction.

[0020] Preferably, the discharge pipe is connected to the vacuum pump via a branch pipe.

[0021] This setup involves connecting the discharge pipe to a vacuum pump via a branch pipe. When the vacuum pump operates, it extracts air from the reactor, reducing the pressure inside and creating a negative pressure environment. Under negative pressure, the metal vapor generated by the metallothermic reduction reaction is more easily volatilized from the reactants and discharged through the discharge pipe to the metal collection device.

[0022] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0023] In this apparatus for the reduction reaction of metallic rubidium and cesium, the heat-conducting column installed at the bottom of the reactor extends to a depth of 60%-80% of the material layer thickness, enabling deep heat transfer into the material layer and ensuring uniform temperature distribution within the layer. This significantly reduces incomplete reaction caused by uneven temperature distribution. Compared to traditional apparatus, this method greatly increases the reaction rate, significantly shortens the reaction time, and substantially increases the yield of metallic rubidium and cesium, meeting the growing market demand.

[0024] In the uniquely designed metal collection device, two calcium vapor baffles are staggered. Each baffle is a flat plate structure that covers 2 / 3 to 3 / 4 of the reactor cavity area, which can effectively extend the vapor path and allow calcium vapor to condense preferentially at the front end of the device, minimizing the mixing of calcium impurities into the metal product. The spiral groove guide channel set inside the condenser tube can extend the metal vapor path, allowing the gaseous metal to cool rapidly and further separate impurities, significantly improving the purity of rubidium and cesium metals and effectively ensuring product quality.

[0025] This device features a rational structural design, simplifying the overall structure compared to existing complex devices. The cooling water jackets fitted onto the feed and discharge pipes, along with their internal water storage chambers and side-mounted water inlets and outlets, effectively cool the feed inlet, discharge outlet, and sealing components, protecting the sealing parts and extending the device's service life. Simultaneously, the streamlined structure prevents the reactor from clogging after the reaction, simplifies cleaning, reduces maintenance costs and difficulty, and improves production efficiency. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0027] Figure 2 This is a top view of the structure of this utility model;

[0028] The meanings of the labels in the diagram are as follows:

[0029] 1. Feed pipe; 2. Cooling water jacket; 3. Water jacket inlet and outlet; 4. Temperature probe hole; 5. Condenser; 6. Guide channel; 7. Discharge pipe; 8. Calcium vapor baffle; 9. Heat-conducting column; 10. Reactor; 11. Electric heating furnace. Detailed Implementation

[0030] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0031] This invention provides an apparatus for the reduction reaction of rubidium and cesium metals, such as... Figure 1 , Figure 2 As shown, the reactor includes a reactor 9, with several heat-conducting columns 8 installed at the bottom of the reactor 9. The top of the reactor 9 is a feed pipe 1, and the side is a discharge pipe 6. It also includes a calcium vapor baffle 7 and a condenser pipe 5. The calcium vapor baffle 7 is located inside the reactor 9, and the condenser pipe 5 is located inside the discharge pipe 6.

[0032] The reactor 9 serves as the core reaction vessel. A heat-conducting column 8 installed at the bottom directly transfers heat to the reactants. The top feed pipe 1 adds rubidium or cesium salt raw materials and a strong reducing metal agent, while the side discharge pipe 6 removes the metal vapor generated in the reaction. A calcium vapor baffle 7, located inside the reactor 9, extends the vapor travel and utilizes the difference in condensation points between calcium vapor and rubidium / cesium vapor to preferentially condense calcium vapor. A condenser pipe 5, placed inside the discharge pipe 6, cools and liquefies the discharged gaseous metal. The entire device achieves the reduction reaction and collection of rubidium / cesium metals through the coordinated operation of its components. The clear understanding of the basic structural composition and key component layout provides a foundational framework for the rubidium / cesium metal reduction reaction, enabling the reaction to proceed in an orderly manner and initially achieving metal reduction and collection. Compared to traditional devices, this design is more rational and its functions are more clearly defined.

[0033] In this embodiment, as Figure 1 , Figure 2 As shown, both the feed pipe 1 and the discharge pipe 6 are fitted with cooling water jackets 2. The cooling water jacket 2 has a water storage chamber inside, and water jacket inlet and outlet ports 3 are opened on the upper and lower sides respectively.

[0034] Cooling water jackets 2, fitted onto the feed pipe 1 and discharge pipe 6, circulate cooling water through their internal water storage chambers via inlet and outlet ports 3. During the reaction, the cooling water absorbs the heat transferred from the feed pipe 1 and discharge pipe 6 due to the high-temperature reaction, reducing the temperature of the pipes and sealing components, thus providing cooling protection. This effectively protects the sealing components on the feed pipe 1 and discharge pipe 6, preventing damage or seal failure due to high temperatures, extending the service life of the device, and ensuring the sealing of the reaction process, preventing the entry of external impurities and leakage of reaction gases, and ensuring the safe and stable progress of the reaction.

[0035] Specifically, such as Figure 1 , Figure 2 As shown, a temperature probe hole 4 is provided on the top of the reactor 9.

[0036] Temperature probe hole 4 on the top of reactor 9 is used to install a temperature probe. The temperature probe can monitor temperature changes inside reactor 9 in real time and transmit the temperature data to an external temperature control box. The temperature control box adjusts the heating process of reactor 9 according to preset reaction temperature parameters, achieving precise temperature control. This provides a precise temperature monitoring and control method for the reaction, ensuring that the reaction proceeds within a suitable temperature range, guaranteeing reaction efficiency and product quality. It avoids problems such as incomplete reaction and increased side reactions caused by excessively high or low temperatures, improving the stability and reliability of the reaction.

[0037] Furthermore, the extension depth of the heat-conducting pillar 8 is 60%-80% of the material layer thickness.

[0038] The heat-conducting pillar 8 extends to a depth of 60%-80% of the material layer thickness, allowing it to penetrate deep into the material layer for heat transfer. Because the distance between the upper and lower parts of the material layer and the heating source varies, conventional heating methods often result in uneven temperature distribution. The heat-conducting pillar 8, extending deep into the material layer, ensures more even heat distribution throughout the entire layer, reducing temperature gradients. This ensures uniform temperature distribution within the material layer, effectively preventing incomplete reactions caused by uneven temperature, accelerating the reaction rate, improving reaction efficiency, and contributing to increased rubidium and cesium metal yield and product quality.

[0039] Furthermore, such as Figure 1 As shown, two calcium vapor baffles 7 are arranged alternately. Each calcium vapor baffle 7 is a flat plate structure, covering 2 / 3 to 3 / 4 of the cavity area of ​​the reactor 9.

[0040] Two staggered calcium vapor baffles 7, with a flat plate structure, cover 2 / 3 to 3 / 4 of the cavity area of ​​the reactor 9, extending the travel path of the steam within the reactor 9. Among the steam generated by the metallothermic reduction reaction, calcium vapor has a relatively low condensation point. The longer travel path allows the calcium vapor to have more opportunities to contact the calcium vapor baffles 7 and preferentially condense, thus separating it from the rubidium and cesium vapors. This effectively reduces the contamination of calcium impurities into the metal product, improving the purity of the metallic rubidium and cesium. Through this structural design, preliminary separation of impurities is achieved without adding complex separation processes, simplifying the subsequent purification process and reducing production costs.

[0041] Furthermore, the interior of the condenser tube 5 is provided with a spiral groove as a guide channel 51 to extend the metal vapor path, allowing the metal vapor to cool naturally and liquefy and discharge at the outlet.

[0042] The spiral-shaped grooved guide channel 51 inside the condenser tube 5 extends the travel distance of the metal vapor within the tube, increasing the contact area and contact time between the metal vapor and the inner wall of the condenser tube 5. Simultaneously, as the metal vapor flows within the spiral channel, its velocity and direction constantly change, promoting heat exchange and enabling rapid cooling of the gaseous metal. This improves the cooling efficiency of the metal vapor, ensuring that the gaseous metal is fully cooled and condensed and discharged at the outlet, achieving efficient collection. Compared to ordinary condenser tubes, the spiral guide channel 51 design can more quickly and effectively convert metal vapor into liquid, reducing metal vapor loss and improving metal recovery rate and product quality.

[0043] Furthermore, such as Figure 1 As shown, the reactor 9 is a hollow cavity made of stainless steel, with an electric heating furnace 10 attached to the outer layer.

[0044] The reactor 9 features a hollow stainless steel cavity, exhibiting excellent high-temperature and corrosion resistance, enabling it to withstand the high temperatures and chemically corrosive environments encountered during the reaction process. The outer-mounted electric heater 10 converts electrical energy into heat energy, providing a uniform and stable heat source to the reactor 9, ensuring the reactor reaches the high-temperature conditions required for the metallothermic reduction reaction. This provides a safe and reliable reaction environment, guaranteeing the reaction proceeds at a stable high temperature. Furthermore, the stainless steel material and optimized heating design extend the service life of the reactor 9 and reduce equipment maintenance costs.

[0045] Furthermore, the discharge pipe 6 is connected to the vacuum pump via a branch pipe.

[0046] The discharge pipe 6 is connected to a vacuum pump via a branch pipe. When the vacuum pump is working, it extracts air from the reactor 9, reducing the gas pressure inside the reactor 9 and creating a negative pressure environment. Under negative pressure conditions, the metal vapor generated by the metal thermal reduction reaction is more easily volatilized from the reactants and discharged to the metal collection device through the discharge pipe 6. This creates a suitable negative pressure environment for the rubidium-cesium reduction reaction, accelerating the volatilization and discharge of metal vapor, and improving the reaction rate and metal collection efficiency. Simultaneously, the negative pressure environment helps reduce the mixing of impurity gases, further improving product quality.

[0047] When using the apparatus for the reduction reaction of rubidium and cesium metals according to this invention, a comprehensive inspection and preparation work must be carried out before starting the reduction reaction. First, ensure that all components, including the reactor 9, feed pipe 1, discharge pipe 6, and cooling water jacket 2, are intact and leak-free. Add rubidium or cesium salt raw material and a strong reducing metal (such as lithium, sodium, calcium, magnesium, etc.) reducing agent to the reactor 9 through the feed pipe 1, ensuring that the ratio of raw material and reducing agent meets the process requirements. After adding, close the feed pipe 1 to ensure the sealing of the reactor 9. At the same time, install a temperature probe in the temperature probe hole 4 and connect it to an external temperature control box to complete the temperature monitoring system setup; connect a vacuum pump to the discharge pipe 6 through a branch pipe to prepare for the subsequent formation of a negative pressure environment.

[0048] The vacuum pump and electric heating furnace 10 are started. The heat generated by the electric heating furnace 10 is transferred to the interior of the reactor 9 through the outer layer of the reactor 9. At the same time, the heat-conducting column 8 at the bottom of the reactor 9 penetrates to 60%-80% of the material layer thickness, directly transferring heat to the reactants to ensure uniform temperature distribution within the material layer, gradually raising the reaction temperature to the 500-800℃ required for the metallothermic reduction reaction. During this process, the temperature probe monitors the temperature changes inside the reactor 9 in real time and transmits the data to an external temperature control box. The temperature control box precisely adjusts the heating power of the electric heating furnace 10 and the heat-conducting column 8 according to the preset reaction temperature parameters, stabilizing the reaction temperature within a suitable range.

[0049] Simultaneously, the vacuum pump extracts air from the reactor 9 through the discharge pipe 6, controlling the vacuum level inside the reactor 9 to be between 10 Pa and 10⁻³ Pa, creating a negative pressure environment. Under negative pressure and high temperature conditions, the rubidium or cesium salts in the raw materials undergo a thermal reduction reaction with the strongly reducing metals, generating rubidium and cesium metal vapors as well as impurity vapors such as calcium. These vapors mix inside the reactor 9 and move upwards.

[0050] As the mixed vapor moves upward, it first encounters two staggered calcium vapor baffles 7 located inside the reactor 9. Each calcium vapor baffle 7 is a flat plate structure, covering 2 / 3 to 3 / 4 of the reactor 9's cavity area. This structural design significantly extends the vapor's travel path. Due to the relatively low condensation point of calcium vapor, it has more opportunities to contact the calcium vapor baffles 7 and preferentially condense during its longer journey, thus achieving initial separation from rubidium and cesium vapors and reducing the amount of calcium impurities entering the subsequent collection process.

[0051] The rubidium and cesium vapors, after initial separation, continue to flow out of the device through the discharge pipe 6, entering the condenser 5 located inside the discharge pipe 6. The spiral-shaped grooved guide channel 51 inside the condenser 5 further extends the path of the metal vapor, increasing the contact area and contact time between the metal vapor and the inner wall of the condenser 5. Simultaneously, as the metal vapor flows within the spiral channel, its velocity and direction constantly change, promoting heat exchange and enabling the gaseous rubidium and cesium metals to cool rapidly. Finally, the gaseous rubidium and cesium metals are discharged from the outlet of the condenser 5 in liquid form, completing the collection of metallic rubidium and cesium.

[0052] Throughout the reaction and collection process, the cooling water jackets 2 fitted onto the feed pipe 1 and the discharge pipe 6 operate continuously. The water storage chamber inside the cooling water jacket 2 circulates cooling water through the water jacket inlet and outlet ports 3. The cooling water absorbs the heat transferred from the feed pipe 1 and the discharge pipe 6 due to the high-temperature reaction, reducing the temperature of the pipe sealing components, protecting the sealing components, preventing damage to components or seal failure due to high temperature, ensuring the sealing of the reaction process, preventing the entry of external impurities and leakage of reaction gases, and ensuring the safe and stable progress of the reaction.

[0053] Once the reaction has reached the preset time of 2-8 hours, and the reaction is confirmed to be basically completed through temperature monitoring and other detection methods, the operation of the electric heating furnace 10 and the vacuum pump is stopped. After the device cools down, the collected rubidium and cesium metals are further processed, such as further purification and packaging. At the same time, the device is cleaned and maintained to prepare for the next production.

[0054] Finally, it should be noted that the electronic components in the reactor 9, electric heating furnace 10, etc. in this embodiment are all general standard parts or parts known to those skilled in the art. Their structure and principle can be learned by those skilled in the art through technical manuals or conventional experimental methods. In the idle part of this device, all the above-mentioned electrical components are connected by wires. The specific connection method should refer to the working order between each electrical component in the above working principle to complete the electrical connection. All of these are technologies known in the art.

[0055] The foregoing has shown and described the basic principles, main features, and advantages of this utility model. Those skilled in the art should understand that this utility model is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the utility model. Various changes and modifications can be made to this utility model without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed utility model. The scope of protection of this utility model is defined by the appended claims and their equivalents.

Claims

1. An apparatus for the reduction reaction of rubidium and cesium metals, comprising a reaction vessel (9), characterized in that: The bottom of the reactor (9) is equipped with several heat-conducting columns (8), the top of the reactor (9) is a feed pipe (1), the side is a discharge pipe (6), and it also includes a calcium vapor baffle (7) and a condenser (5). The calcium vapor baffle (7) is located inside the reactor (9), and the condenser (5) is located inside the discharge pipe (6).

2. The apparatus for the reduction reaction of rubidium and cesium metals according to claim 1, characterized in that: Cooling water jackets (2) are fitted on both the feed pipe (1) and the discharge pipe (6). The cooling water jacket (2) has a water storage cavity inside and water inlet and outlet (3) are opened on the upper and lower sides respectively.

3. The apparatus for the reduction reaction of rubidium and cesium metals according to claim 1, characterized in that: The top of the reactor (9) is provided with a temperature probe hole (4).

4. The apparatus for the reduction reaction of rubidium and cesium metals according to claim 1, characterized in that: The extension depth of the heat-conducting column (8) is 60%-80% of the material layer thickness.

5. The apparatus for the reduction reaction of metallic rubidium and cesium according to claim 1, characterized in that: Two calcium vapor baffles (7) are staggered, and each calcium vapor baffle (7) is a flat plate structure, covering 2 / 3 to 3 / 4 of the cavity area of ​​the reactor (9).

6. The apparatus for the reduction reaction of rubidium and cesium metals according to claim 1, characterized in that: The condenser tube (5) has a spiral groove inside as a guide channel (51) to extend the metal vapor path, so that the metal vapor can be cooled naturally and liquefied and discharged at the outlet.

7. The apparatus for the reduction reaction of rubidium and cesium metals according to claim 1, characterized in that: The reactor (9) is a hollow cavity made of stainless steel, with an electric heating furnace (10) attached to the outer layer.

8. The apparatus for the reduction reaction of rubidium and cesium metals according to claim 1, characterized in that: The discharge pipe (6) is connected to the vacuum pump via a branch pipe.

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