Production device for preparing anhydrous aluminum trichloride based on low-temperature indirect chlorination method

Abstract

The invention belongs to the technical field of preparation of anhydrous aluminum trichloride, and particularly relates to a production device for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method, which comprises: a reaction furnace body, which is divided into an upper aluminum accommodating cavity and a lower medium accommodating cavity by a pore plate; the external temperature control device is used for regulating and controlling the temperature of the reaction furnace body; the solid aluminum material is placed in the aluminum containing cavity, the molten medium material is placed in the medium containing cavity, and the filling amount of the medium material is larger than the volume of the medium containing cavity, so that part of the molten medium material overflows the pore plate and makes contact with the solid aluminum material, and a micro-reaction area is formed on the upper side of the pore plate; the height ratio of the micro-reaction area to the medium accommodating cavity is (0.1-0.8): 1; the production device for preparing the anhydrous aluminum trichloride based on the low-temperature indirect chlorination method is simple in structure, the reaction process can be well controlled, and the prepared product is high in purity and white.

Description

Technical Field

[0001] This invention belongs to the field of anhydrous aluminum trichloride preparation technology, and particularly relates to a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method. Background Technology

[0002] Anhydrous aluminum trichloride, with the chemical formula AlCl3, is a colorless, odorless, transparent hexagonal flaky crystalline solid. However, its industrial products often contain impurities such as iron, free chlorine, and free aluminum, giving them a pale yellow, yellow, or light gray appearance and a strong hydrochloric acid odor. It is readily soluble in solvents such as water, alcohol, chloroform, and carbon tetrachloride. It has wide industrial applications, including in the pharmaceutical, pesticide, dye, fragrance, metallurgical, plastics, and lubricant industries. It is an important inorganic chemical product, primarily used as a catalyst in organic synthesis, a detergent, a dehydrating agent, and a nucleating agent. It is particularly widely used as a catalyst in the Frederick-Clefford reaction.

[0003] Currently, there are two main methods for industrial production of anhydrous aluminum trichloride. One is the aluminum ingot method, which involves directly passing chlorine gas into molten aluminum to produce aluminum chloride. The aluminum chloride produced in the reaction sublimates and enters a collector, where it is collected to obtain the finished anhydrous aluminum trichloride. The reaction equation is as follows: 2Al + 3Cl₂ → 2AlCl₃; This is currently the most widely used method both domestically and internationally, and almost all aluminum trichloride production in China uses this method. However, this method has the following serious drawbacks: (1) High raw material cost: The core of the aluminum ingot method is the chlorination reaction that occurs when metallic aluminum comes into direct gas-molten contact with chlorine. The reaction temperature is above 800℃. Under such high temperature conditions, the metal impurities such as iron, silicon, magnesium, and calcium commonly found in low-purity industrial aluminum materials, such as aluminum chips, aluminum slag, and waste aluminum materials, have high reactivity with chlorine. They will react with Al to generate chloride impurities such as FeCl3, SiCl4, and MgCl2. Among them, FeCl3 is a yellow-brown solid that is easy to co-sublimate with AlCl3, which directly causes the product to be colored and cannot be separated by simple collection. SiCl4 is a volatile liquid that will mix with AlCl3 in the finished product, which will increase its hygroscopicity. At the same time, various metal chloride impurities will reduce the activity of anhydrous aluminum trichloride as a catalyst, thus losing its industrial use value. Therefore, the aluminum ingot method has rigid requirements on the purity of aluminum raw materials. Low-purity aluminum materials cannot be adapted to this process. Pure aluminum ingots, such as A00 pure aluminum ingots (aluminum content ≥99.7%), must be used as raw materials, resulting in high raw material costs and poor economic benefits.

[0004] (2) Harsh production environment: The temperature of the reactor in the aluminum ingot process needs to be maintained above 800℃. At the same time, the open or semi-open aluminum liquid pool dissipates heat violently, making the workshop production environment temperature high, especially in summer when it is unbearably hot.

[0005] (3) Low product purity: Even when using high-purity A00 aluminum ingots, it still contains ≤0.3% iron impurities. At chlorination reaction temperatures above 800℃, iron reacts rapidly with chlorine to form FeCl3. The sublimation point of FeCl3 is 315℃, far lower than the reactor temperature. Therefore, it will sublimate into the gas phase simultaneously with AlCl3, and eventually co-condense with AlCl3 in the collector, becoming the main impurity in the product. Due to Fe... 3+ Due to the electronic transition optical properties, the co-crystallization dispersion effect of AlCl3 and FeCl3, and the light scattering amplification effect of solid crystals, even if the FeCl3 content is only 0.01%, it will color the white AlCl3 crystals to pale yellow or yellow. If the iron content of the aluminum ingot is too high, or if the reaction furnace body is made of iron, the FeCl3 content will be further increased, resulting in a gray or even brownish-yellow product. In addition, in the aluminum ingot process, in order to ensure the complete reaction of metallic aluminum, chlorine gas must be introduced in excess. In industrial production, the molar ratio of chlorine gas to aluminum is usually 1.6~2.0:1. Excess chlorine gas will enter the collector along with the gaseous AlCl3. The temperature of the collector is usually controlled at 100~150℃. At this temperature, AlCl3 quickly sublimates into a solid, but some chlorine gas cannot be discharged in time and will be physically adsorbed on the surface of AlCl3 crystals, or a small amount will dissolve in the AlCl3 lattice to form free chlorine. Furthermore, excess chlorine can react with trace amounts of moisture on the surface of AlCl3 crystals to produce HCl: Cl2 + H2O → HCl + HClO. HCl is an irritating gas, giving the product a strong hydrochloric acid odor. The presence of free chlorine also enhances the product's chemical activity, making it more hygroscopic, corrosive, and reducing its storage stability. Therefore, anhydrous aluminum trichloride prepared by the aluminum ingot method is rarely a white, high-purity product; it is generally pale yellow, yellow, or light gray, and contains high levels of free chlorine and iron impurities.

[0006] Another process for producing anhydrous aluminum trichloride is the alumina process. Although the raw material alumina is inexpensive, the product has high impurities, requires large equipment investment, and its overall economic benefits are not as good as the aluminum ingot process. Therefore, it is rarely used both domestically and internationally.

[0007] In view of this, there is an urgent need to develop a new type of anhydrous aluminum trichloride preparation device that is economically efficient, produces high-purity products, has a low reaction temperature, low energy consumption, and is safe and environmentally friendly. Summary of the Invention

[0008] The present invention aims to provide a production device for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method, which has good economic benefits, high product purity, low reaction temperature, low energy consumption, safety, and environmental protection, and can achieve precise control of the reaction process, so as to realize the economical, efficient, safe and environmentally friendly production of anhydrous aluminum trichloride.

[0009] In view of this, the present invention provides a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method, comprising: The reactor body has its internal space divided into an upper aluminum receiving cavity and a lower medium receiving cavity by a perforated plate; An external temperature control device is used to regulate the temperature of the reaction furnace body; In use, solid aluminum material is placed in the aluminum receiving cavity, and molten medium material is placed in the medium receiving cavity. The filling amount of the medium material is greater than the volume of the medium receiving cavity, so that part of the molten medium material can overflow the perforated plate and contact the solid aluminum material to form a micro-reaction zone on the upper side of the perforated plate. The height ratio of the micro-reaction zone to the medium receiving cavity is 0.1~0.8:1. And a chlorine gas delivery device for delivering chlorine gas into the medium-containing cavity.

[0010] Furthermore, the height of the microreaction zone is ≥0.5cm.

[0011] Furthermore, the reactor body is equipped with: A gaseous aluminum trichloride discharge port is located at the top of the reactor body and is connected to a collector. The gaseous aluminum trichloride generated in the reactor body can enter the collector through the gaseous aluminum trichloride discharge port and be collected to obtain anhydrous aluminum trichloride product. The waste discharge port is located at the bottom of the reactor body and is connected to the medium receiving cavity, for discharging the waste in the medium receiving cavity.

[0012] Furthermore, the chlorine gas delivery device includes a chlorine gas source and a chlorine gas delivery pipeline, with the outlet end of the chlorine gas delivery pipeline inserted downwards into the medium receiving cavity.

[0013] Furthermore, the external temperature control device includes: A semi-circular coil or cooling jacket is arranged around the outer wall of the reactor body; The heat exchanger is connected to both ends of a semi-circular coil or cooling jacket via pipes, forming a circulating cooling loop.

[0014] Furthermore, the external temperature control device includes: Cooling jacket, which is a closed-chamber heat exchange structure wrapped around the outside of the reactor body; The heat exchanger is connected to the inlet and outlet of the cooling jacket via pipes, forming a circulating cooling loop; And an external auxiliary cooling jacket, which is an open jacketed heat exchange structure arranged around the cooling jacket.

[0015] Furthermore, the external temperature control device includes: Cooling jacket, which is a closed-chamber heat exchange structure wrapped around the outside of the reactor body; An external auxiliary cooling jacket is a jacketed heat exchange structure that surrounds the cooling jacket. And, heat exchangers; The heat exchange medium in the cooling jacket and the external auxiliary cooling jacket is the same; The lower parts of the cooling jacket and the external auxiliary cooling jacket are connected. The outlet of the cooling jacket is connected to the high-temperature medium inlet of the heat exchanger through a pipe. The high-temperature medium outlet of the heat exchanger is connected to the upper part of the external auxiliary cooling jacket. After the heat exchange medium in the cooling jacket is discharged from its outlet, it first flows through the heat exchanger for cooling and temperature reduction. Then it enters the external auxiliary cooling jacket from the upper part, flows from top to bottom to the lower part of the external auxiliary cooling jacket, enters the lower part of the cooling jacket, and then is discharged again from the upper part of the cooling jacket. This cycle is repeated to continuously cool the reactor body.

[0016] Furthermore, the external temperature control device includes: Cooling jacket, which is a closed-chamber heat exchange structure wrapped around the outside of the reactor body; An external auxiliary cooling jacket is a jacketed heat exchange structure that surrounds the cooling jacket. And, heat exchangers; The lower part of the cooling jacket and the outer auxiliary cooling jacket is filled with a first heat exchange medium, and the upper part of the outer auxiliary cooling jacket is filled with a second heat exchange medium. The density of the second heat exchange medium is less than that of the first heat exchange medium, and they are immiscible. The lower parts of the cooling jacket and the external auxiliary cooling jacket are connected. The outlet of the cooling jacket is connected to the high-temperature medium inlet of the heat exchanger through a pipe. A return pipe is provided at the high-temperature medium outlet of the heat exchanger. The end of the return pipe extends into the external auxiliary cooling jacket, so that after the first heat exchange medium in the cooling jacket is discharged from its outlet, it first flows through the heat exchanger for cooling and temperature reduction. Then, it mixes with the first heat exchange medium in the external auxiliary cooling jacket again through the return pipe, and then enters the lower part of the cooling jacket and is discharged again from the upper part of the cooling jacket. This cycle is repeated to continuously cool the reactor body.

[0017] Furthermore, the production apparatus for preparing anhydrous aluminum trichloride also includes an internal temperature control device, which is a cooling and heat dissipation device disposed in the middle of the reaction furnace body. The internal temperature control device includes a cooling chamber and a phase change material filled in the cooling chamber. The cooling chamber is partially located inside the reaction furnace body and partially exposed outside the reaction furnace body.

[0018] Furthermore, an inner furnace body is provided inside the reactor body, which is a cylindrical structure that can be slidably installed inside the reactor body; an internal temperature control device is provided in the inner furnace body, which is a circular cylindrical structure; holes are drilled in the bottom plate of the inner furnace body to form an annular perforated plate, and the inner furnace body and the internal temperature control device are integrated; the height of the inner furnace body relative to the reactor body is adjustable.

[0019] Compared with existing technologies, the production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method described in this invention has the following advantages: (1) Directly use waste aluminum as raw material, such as aluminum foil, aluminum shavings, aluminum shavings and other waste materials. On the one hand, the price of waste aluminum is much lower than that of pure aluminum ingots. On the other hand, some waste aluminum alloys are rich in valuable metals, such as tin, silver, copper, lithium, nickel and so on. This process can easily separate and recycle them, so the economic benefits are high.

[0020] (2) The reactor of this process is completely sealed and the reaction temperature is low. The reaction heat can be utilized and controlled by the added temperature control device, and the temperature and operating environment of the workshop are greatly improved.

[0021] (3) The product quality is better. Since the process is an indirect reaction, chlorine reacts with the medium first, and the residual chlorine will continue to react with the aluminum material. Therefore, the product and tail gas are basically free of chlorine. Moreover, the reaction is carried out at medium and low temperature, and the volatility of impurity chloride is very small, so the impurities in the product are also very low. Therefore, the product prepared by this process has high purity and is white. After testing, the purity of the product prepared by this invention is: AlCl3≧99.2%; while the purity of the product obtained by other existing methods is: AlCl3≧98.5%.

[0022] (4) The space of the reactor is divided into an upper aluminum containment chamber and a lower medium containment chamber by a perforated plate. By utilizing the characteristics of the medium material and solid aluminum material, the solid aluminum material and the molten medium material Me gradually come into contact and react sequentially in a small range, thereby achieving precise control of the violent reaction process. This can well serve the production process of anhydrous aluminum trichloride based on the low-temperature indirect chlorination method. (5) By optimizing and improving the temperature control system, the temperature gradient from the wall to the center of the furnace is significantly reduced, achieving uniform temperature control across the entire radial and axial regions. The improved temperature field uniformity can alleviate the surge in side reactions and the decrease in product selectivity caused by local high temperatures, thereby improving product quality while better controlling the reaction process.

[0023] Therefore, the production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method described in this invention has a simple structure, is easy to implement, and can effectively control the reaction process. It can achieve safe, environmentally friendly, and controllable production of anhydrous aluminum trichloride, and has the advantages of good economic benefits, high product purity, and low reaction temperature. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the production apparatus for preparing anhydrous aluminum trichloride as described in Embodiment 1 of the present invention; Figure 2 yes Figure 1 A magnified view of a portion of region A in the middle; Figure 3 This is a schematic diagram of the production apparatus for preparing anhydrous aluminum trichloride as described in Embodiment 2 of the present invention; Figure 4 This is a schematic diagram of the production apparatus for preparing anhydrous aluminum trichloride as described in Embodiment 3 of the present invention; Figure 5 This is a schematic diagram of the production apparatus for preparing anhydrous aluminum trichloride as described in Embodiment 4 of the present invention; Figure 6 This is a schematic diagram of the production apparatus for preparing anhydrous aluminum trichloride as described in Embodiment 5 of the present invention; Figure 7 This is a schematic diagram of the production apparatus for preparing anhydrous aluminum trichloride as described in Embodiment 6 of the present invention; Figure 8 This is a schematic diagram of the production apparatus for preparing anhydrous aluminum trichloride as described in Embodiment 7 of the present invention; Figure 9 This is a schematic diagram of the production apparatus for preparing anhydrous aluminum trichloride as described in Embodiment 8 of the present invention; Figure 10 This is a schematic diagram of the production apparatus for preparing anhydrous aluminum trichloride as described in Embodiment 9 of the present invention; Figure 11 This is a three-dimensional structural schematic diagram of the reactor body described in Embodiment 10 of the present invention; Figure 12 This is a schematic cross-sectional view of the reactor body described in Embodiment 10 of the present invention; Figure 13 yes Figure 12 A magnified schematic diagram of the local structure of region B in the middle; Figure 14 yes Figure 12 Another enlarged schematic diagram of a local structure in region B; Figure 15 yes Figure 14 A three-dimensional structural diagram of the intermediate elastic element; Figure 16 This is the product of aluminum trichloride prepared by the present invention. Figure 1 ; Figure 17 This is the product of aluminum trichloride prepared by the present invention. Figure 2 ; The markings in the diagram are as follows: 1. Furnace body; 101. Aluminum receiving cavity; 1011. Guide plate; 102. Medium receiving cavity; 103. Orifice plate; 104. Micro-reaction zone; 105. Gaseous aluminum trichloride discharge port; 106. Waste discharge port; 1061. Control valve three; 107. Inner furnace body; 2. Aluminum feeding hopper; 201. Control valve one; 3. Medium feeding hopper; 301. Control valve two; 4. External temperature control device; 401. Semi-circular coil; 402. Heat exchanger; 403. Cooling jacket; 404. External auxiliary cooling jacket; 5. Chlorine gas conveying device; 6. Temperature detector; 601. Liquid phase temperature detector; 602. Gas phase temperature detector; 7. Internal temperature control device; 8. Mechanical lifting arm; 9. Magnet; 10. Adaptive spring-loaded height adjustment mechanism; 1001. Receiving groove; 1002. Elastic element; 1003. Flanged edge; 1004. Snap-fit ​​flange; 1005. Limiting block; 1006. Bolt. Detailed Implementation

[0025] The technical solutions of the embodiments of this application will be clearly described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application are within the scope of protection of this application.

[0026] It should be noted that all directional and positional terms used in this invention, such as "up," "down," "left," "right," "front," "back," "vertical," "horizontal," "inner," "outer," "top," "lower," "lateral," "longitudinal," and "center," are only used to explain the relative positional relationships and connections between components in a specific state (as shown in the accompanying drawings). They are merely for the convenience of describing the invention and do not require the invention to be constructed and operated in a specific orientation; therefore, they should not be construed as limitations on the invention. Furthermore, descriptions involving "first," "second," etc., are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated.

[0027] In the description of this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal communication between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0028] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," 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 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.

[0029] First, through research, the applicant proposed a novel production process for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method. The principle of this process is as follows: Me (liquid) + Cl2 (gas) → MeCl2 (liquid) Gas-liquid reaction; MeCl2 (liquid) + Al (solid) → Me (liquid) + AlCl3 (gas) Liquid-solid reaction; The furnace temperature of the reactor is controlled at 185~650℃. The medium material Me is a metal or alloy with a melting point between 185~650℃, which can react with chlorine to generate liquid chloride, and whose chloride can undergo a displacement reaction with aluminum, such as tin, lead, bismuth, zinc or their alloys.

[0030] The reaction process is as follows: First, chlorine gas is introduced into molten metal Me, so that molten metal Me reacts with chlorine gas to generate liquid chloride MeCl2. Then, gaseous AlCl3 is generated through the displacement between solid Al and liquid chloride MeCl2. The aluminum chloride generated in the reaction sublimates into the collector and is collected to obtain anhydrous aluminum trichloride product.

[0031] The novel process for preparing anhydrous aluminum trichloride described above can directly use waste aluminum as raw material, eliminating the need for high-purity A00 aluminum ingots. Furthermore, the reaction temperature can be controlled at 185~650℃, significantly lower than existing aluminum ingot and alumina methods, thus greatly reducing energy consumption. Simultaneously, the low reaction temperature ensures that impurities other than aluminum are essentially liquid, preventing them from entering the crystallizer with gaseous aluminum trichloride. The resulting anhydrous aluminum trichloride is a white crystalline solid with an AlCl3 purity ≥99.2%, far exceeding existing processes, and it has no hydrochloric acid odor, meeting the requirements of high-end industrial applications.

[0032] However, in the above-mentioned production process, the reaction is a rapid and violent exothermic reaction, making it very difficult to control. To realize this new production process for preparing anhydrous aluminum trichloride based on low-temperature indirect chlorination, a production device that can precisely control the reaction process is required. Therefore, this invention provides a production device for preparing anhydrous aluminum trichloride by low-temperature indirect chlorination. This device achieves precise control of the violent reaction process by controlling the gradual contact and sequential reaction of the reactants, specifically solid aluminum and molten medium material Me, and can well serve the production process for preparing anhydrous aluminum trichloride based on low-temperature indirect chlorination.

[0033] The following specific embodiments illustrate the production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method described in this invention: Example 1 like Figures 1-2 As shown, a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method includes: The reactor body 1 has its internal space divided into an upper aluminum receiving cavity 101 and a lower medium receiving cavity 102 by a perforated plate 103; In use, solid aluminum material is placed in the upper aluminum receiving cavity 101, and molten medium material is placed in the lower medium receiving cavity 102. The filling amount of the medium material is greater than the volume of the medium receiving cavity 102, so that part of the molten medium material can overflow the perforated plate 103 and contact the solid aluminum material on the upper side to form a micro-reaction zone 104 on the upper side of the perforated plate 103. The height ratio of the micro-reaction zone 104 to the medium receiving cavity 102 is (0.1~0.8):1. And a chlorine gas delivery device 5, which is used to deliver chlorine gas into the medium receiving cavity 102.

[0034] It should be noted that the dielectric material can be filled by preheating it to a molten state before injecting it into the dielectric receiving cavity 102, or by directly adding the solid dielectric material into the dielectric receiving cavity 102 and then heating it to a molten state. Preferably, the dielectric material is heated to a molten state before being injected into the dielectric receiving cavity 102.

[0035] As a preferred example of the present invention, the height of the microreaction zone 104 is 0.5 cm or more.

[0036] As a preferred example of the present invention, the height of the medium receiving cavity 102 is 10~30cm.

[0037] As a preferred example of the present invention, the height ratio of the microreaction zone 104 to the medium accommodating cavity 102 is (0.1~0.5):1.

[0038] As a preferred example of the present invention, the aperture of the perforated plate 103 is 5~15mm.

[0039] As some examples of the present invention, the chlorine pipe in the chlorine conveying device 5 is made of alumina ceramic pipe or quartz pipe, and one or more chlorine pipes can be set for each furnace.

[0040] In the production apparatus for preparing anhydrous aluminum trichloride described in this invention, by setting an orifice plate 103 inside the reaction furnace body 1 and setting the filling amount of the medium material to be greater than the volume of the medium receiving cavity 102, the partially molten medium material can overflow the orifice plate 103 and come into contact with the solid aluminum material, thus providing a basis for the molten medium material to come into contact with the solid aluminum material and carry out a displacement reaction. Based on this, chlorine gas is supplied to the medium-containing cavity 102 through the chlorine gas delivery device 5. In this way, the introduced chlorine gas can first come into contact with the molten medium material and undergo a chlorination reaction to generate MeCl2 (liquid). In this process, Me, as the chlorine acceptor, combines with chlorine gas to generate MeCl2 (liquid), transferring chlorine from the gas phase to the liquid phase, realizing the "liquid phase fixation" of gaseous chlorine gas. This avoids the problems of low gas-solid contact efficiency and uneven reaction that exist when gaseous chlorine gas comes into direct contact with solid aluminum material. Then, MeCl2, as the chlorine donor, comes into contact with solid aluminum material again and undergoes a displacement reaction, transferring chlorine to Al to generate gaseous AlCl3. At the same time, Me is reduced and regenerated, returning to its initial state to continue participating in the next round of reaction. Moreover, the reaction temperature required for the above two steps is not high. Finally, Me completes the low-temperature indirect reaction between Cl2 and Al through the cycle of "combining with Cl2 → releasing Cl2", realizing the purpose of preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method.

[0041] More importantly, in the above reaction process, Me, as the reaction carrier / circulating medium, plays a core role in transferring chlorine and realizing the indirect reaction between Cl2 and Al. From the perspective of reaction stoichiometry, the total amount of Me will not decrease in theory. Although in actual production, its total amount will be slightly lost due to the occurrence of a small number of side reactions, the rate of decrease is extremely slow and can be maintained by periodic replenishment. Therefore, the total amount of medium material in the reactor body 1 can remain basically unchanged for a considerable period of time, ensuring the reliable existence of the micro-reaction zone 104 and realizing continuous production.

[0042] Furthermore, since the molten medium material in this invention acts as a carrier for chlorine, and its total amount can remain relatively constant, within the reactor body 1, as the solid aluminum material in the micro-reaction zone 104 is continuously consumed, the aluminum material at the top of the micro-reaction zone 104 will continuously collapse and enter the micro-reaction zone 104, achieving continuous reaction and continuous generation of gaseous aluminum trichloride. That is, in this invention, the micro-reaction zone 104 forms a relatively small micro-reaction area in terms of volume compared to the reaction zone of a traditional solid-liquid reaction. Therefore, although the above-mentioned reaction process proceeds rapidly and is accompanied by intense exothermic reactions, the production apparatus described in this invention can easily control the reaction process within a relatively controllable range.

[0043] As some examples of the present invention, such as Figure 2 As shown, a guide plate 1011 is provided at the lower part of the aluminum receiving cavity 101, forming a cross-section that gradually narrows from top to bottom. The guide plate 1011 prevents the aluminum material from accumulating or bridging at the top, allowing it to slide continuously and stably into the micro-reaction zone 104.

[0044] As some examples of the present invention, the reactor body 1 is provided with: A gaseous aluminum trichloride discharge port 105 is located at the top of the reactor body 1 and is connected to a collector. The gaseous aluminum trichloride generated in the reactor body 1 can enter the collector through the gaseous aluminum trichloride discharge port 105 and be collected to obtain anhydrous aluminum trichloride product. Waste discharge port 106 is located at the bottom of the reactor body 1 and communicates with the medium receiving cavity 102 for discharging waste from the medium receiving cavity 102.

[0045] As some examples of the present invention, the production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method further includes: An aluminum feeding hopper 2 is disposed on the upper side of the reactor body 1 and communicates with the aluminum receiving cavity 101 for feeding aluminum material into the aluminum receiving cavity 101; The medium feeding hopper 3 is connected to the medium receiving cavity 102 and is used to feed molten medium material into the medium receiving cavity 102.

[0046] As a preferred example of the present invention, the installation height of the medium feeding hopper 3 is higher than that of the medium receiving cavity 102, so as to realize the automatic feeding of the medium feeding hopper 3 without power.

[0047] As a preferred example of the present invention, the aluminum feeding hopper 2 has nitrogen purging and preheating functions.

[0048] As a preferred example of the present invention, a control valve 201 is provided between the aluminum feeding hopper 2 and the reactor body 1 to control the feeding of aluminum material; a control valve 301 is provided between the medium feeding hopper 3 and the reactor body 1 to control the feeding of medium material; and a control valve 1061 is provided between the waste discharge port 106 and the reactor body 1 to control the waste discharge process.

[0049] As a preferred example of the present invention, the waste discharge port 106 is used to remove the medium liquid rich in impurity elements, and the medium liquid after the impurity elements are separated can be replenished back into the medium receiving cavity 102.

[0050] As some examples of the present invention, the production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method further includes: The external temperature control device 4 is a coil arranged around the outside of the reactor body 1. A high-temperature medium or a low-temperature medium can be introduced into the coil as needed to control the temperature inside the reactor body 1.

[0051] As a preferred example of the present invention, the coil is a semi-circular coil 401, which can better fit the outer wall of the reactor body 1 and achieve good heat exchange and temperature control.

[0052] As a preferred example of the present invention, the external temperature control device 4 uses cold / hot air as the heat exchange medium. When the reactor body 1 needs to be kept warm, hot air is introduced for heating, and when the reactor body 1 needs to be cooled, cold air is introduced for heat dissipation.

[0053] As some examples of the present invention, the production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method further includes: A plurality of temperature detectors 6, including a liquid phase temperature detector 601 for detecting liquid medium material in a medium containment cavity 102, and a gas phase temperature detector 602 for detecting generated gaseous aluminum trichloride, wherein the temperature detection unit in the liquid phase temperature detector 601 is inserted into the liquid medium material in the medium containment cavity 102, and the temperature detection unit in the gas phase temperature detector 602 is located at the top of the aluminum containment cavity 101.

[0054] As a preferred example of the present invention, the chlorine conveying device 5 may include components such as a chlorine source, a chlorine conveying pipeline, and a flow meter, wherein the outlet end of the chlorine conveying pipeline can be inserted into the medium receiving cavity 102.

[0055] Preferred, such as Figure 2 As shown, the outlet end of the chlorine gas conveying pipeline is inserted into the medium receiving cavity 102 at a downward angle. The present invention does not limit the angle α between the outlet end of the chlorine gas conveying pipeline and the horizontal line, but it is preferable that the medium liquid in the medium receiving cavity 102 will not flow back into the chlorine gas conveying device 5.

[0056] The chlorine gas delivery pipeline is designed to allow chlorine gas to enter at a downward angle. The resulting bubbles do not rise vertically and escape rapidly; instead, they form an oblique trajectory within the reaction liquid, prolonging their residence time in the liquid phase. Simultaneously, the oblique impact makes the bubbles more easily broken into smaller bubbles, significantly increasing the gas-liquid contact surface area. This allows for more complete mass transfer between chlorine and the reaction liquid, fundamentally improving the chlorine reaction conversion rate and reducing the loss of unreacted chlorine. Furthermore, the obliquely introduced chlorine gas flow creates an oblique impact and stirring effect on the reaction liquid, breaking up the static stratification of the liquid phase and eliminating dead zones at the bottom and sidewalls of the reactor body 1. The airflow disturbance also allows the reaction products to quickly detach from the gas-liquid interface and float to the surface, ensuring the continuous progress of the reaction.

[0057] Example 2 It should be noted that in this invention, it is generally only necessary to preheat the reactor body 1 using a heating device before loading. After the furnace temperature rises to the reaction temperature and the reaction starts, the reaction can be sustained by the self-exothermic reaction process. Simultaneously, a temperature control device is required to strictly regulate the temperature inside the furnace to prevent the temperature inside the reactor body 1 from continuously rising and exceeding the set temperature, leading to reaction runaway. Therefore, in practical applications, the heating function of the external temperature control device 4 is not critical. To simplify the structure of the external temperature control device 4 and avoid switching the heat exchange medium, an electric heating device can also be installed on the reactor body 1. In this case, the external temperature control device 4 only needs to perform cooling and heat dissipation functions. The following Example 2 provides an external temperature control device 4 with only cooling and heat dissipation functions for use in the production apparatus for preparing anhydrous aluminum trichloride according to this invention.

[0058] like Figures 1-3 As shown, a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method differs from the production apparatus described in Example 1 above mainly in that: An electric heating device (not shown in the figure) is installed on the reactor body 1 to preheat the reactor body 1 and the materials inside it before the reaction begins. The external temperature control device 4 is used to cool and dissipate heat from the reaction furnace body 1 during the reaction process. The external temperature control device 4 uses water or other refrigerants as the heat exchange medium.

[0059] As some specific examples of the present invention, the external temperature control device 4 includes: A coil, such as a semi-circular coil 401, is arranged around the outer wall of the reactor body 1; The heat exchanger 402 is connected to both ends of the semi-circular coil 401 through pipes, forming a circulating cooling loop.

[0060] As some examples of the present invention, the heat exchanger 402 can perform heat exchange by means of air cooling, water cooling, etc.

[0061] Example 3 The following embodiment 3 provides another external temperature control device 4 that only has cooling and heat dissipation functions.

[0062] Specifically, such as Figure 4 As shown, the external temperature control device 4 includes: Cooling jacket 403 is a closed-chamber heat exchange structure that wraps around the outside of the reactor body 1. It can force heat exchange with the wall of the reactor body 1 through the cooling medium flowing inside the jacket, quickly remove the excess heat generated by the reaction in the furnace, and accurately control the reaction temperature in the furnace. The heat exchanger 402 is connected to the inlet and outlet of the cooling jacket 403 via pipes, forming a circulating cooling loop.

[0063] As some examples of the present invention, the cooling jacket 403 may be a smooth-walled jacket or a flow-guiding jacket with internal flow-guiding components. Preferably, the cooling jacket 403 is a flow-guiding jacket.

[0064] As some examples of the present invention, the heat exchange medium in the cooling jacket 403 and the heat exchanger 402 can be water, heat transfer oil, molten salt, etc.

[0065] As some examples of the present invention, in order to realize the circulating flow of the heat exchange medium, the external temperature control device 4 may also be equipped with components such as a delivery pump.

[0066] Example 4 The above embodiment 3 provides a single-layer jacketed cooling structure. The following embodiment 4 provides another double-layer jacketed cooling structure.

[0067] Specifically, such as Figure 5 As shown, the external temperature control device 4 includes: Cooling jacket 403 is a closed-chamber heat exchange structure that wraps around the outside of the reactor body 1. It can perform forced heat exchange with the wall of the reactor body 1 through the cooling medium flowing inside the jacket. Heat exchanger 402 is connected to the inlet and outlet of cooling jacket 403 via pipes, forming a circulating cooling loop; In addition, there is an external auxiliary cooling jacket 404, which is a jacketed heat exchange structure surrounding the cooling jacket 403. It can perform forced heat exchange with the wall of the cooling jacket 403 through the internal cooling medium to cool and dissipate heat from the cooling jacket 403.

[0068] As a preferred example of the present invention, the cooling medium in the cooling jacket 403 is molten salt, and the cooling medium in the outer auxiliary cooling jacket 404 is heat transfer oil or water. This gradient heat exchange principle, with the inner layer being highly temperature resistant and having strong heat exchange, and the outer layer being an auxiliary temperature control and stable medium, can utilize the graded temperature control and complementary advantages of the double-layer jacket to avoid the medium failure and thermal shock risks of high-temperature heat exchange in a single jacket, thereby improving the overall heat exchange efficiency and system stability.

[0069] As a preferred example of the present invention, the external auxiliary cooling jacket 404 is an open heat exchange structure arranged around the cooling jacket 403.

[0070] As some examples of the present invention, the upper opening of the external auxiliary cooling jacket 404 is provided to facilitate the rapid dissipation of heat from the external auxiliary cooling jacket 404 into the environment.

[0071] As a preferred example of the present invention, the external auxiliary cooling jacket 404 may also be equipped with a heat exchanger and a delivery pump connected to it according to the heat dissipation requirements, so as to achieve forced heat exchange while dissipating heat naturally.

[0072] As some examples of the present invention, the cooling jacket 403 and the external auxiliary cooling jacket 404 can simultaneously adopt a heat exchange medium circulation mode with bottom inlet and top outlet and unidirectional flow.

[0073] Preferably, this double-layered jacketed cooling structure is particularly suitable for the preparation of anhydrous aluminum trichloride in medium to large-sized reaction furnaces or at reaction temperatures >350°C.

[0074] Example 5 like Figure 6 As shown, a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method includes an external temperature control device 4. The difference between the external temperature control device 4 and that in Embodiment 4 above is that the external temperature control device 4 includes: Cooling jacket 403 is a closed-chamber heat exchange structure that wraps around the outside of the reactor body 1. It can perform forced heat exchange with the wall of the reactor body 1 through the cooling medium flowing inside the jacket. External auxiliary cooling jacket 404 is a jacketed heat exchange structure surrounding the cooling jacket 403; And heat exchanger 402; The heat exchange medium in the cooling jacket 403 and the external auxiliary cooling jacket 404 is the same; The lower parts of the cooling jacket 403 and the external auxiliary cooling jacket 404 are connected. The outlet of the cooling jacket 403 is connected to the high-temperature medium inlet of the heat exchanger 402 through a pipe. The outlet of the high-temperature medium of the heat exchanger 402 is connected to the upper part of the external auxiliary cooling jacket 404. This allows the heat exchange medium in the cooling jacket 403 to first flow through the heat exchanger 402 for cooling after being discharged from its outlet. Then, it enters the external auxiliary cooling jacket 404 from the upper part, flows down to the lower part of the external auxiliary cooling jacket 404, enters the lower part of the cooling jacket 403, and is discharged again from the upper part of the cooling jacket 403. This cycle is repeated to achieve continuous cooling of the reactor body 1.

[0075] This double-layer jacketed cooling structure is simple in structure, has a good heat exchange effect, and the temperature of the reactor body 1 is more stable.

[0076] Example 6 like Figure 7 As shown, a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method includes an external temperature control device 4. The difference between the external temperature control device 4 and that in Embodiment 5 above is that the external temperature control device 4 includes: Cooling jacket 403 is a closed-chamber heat exchange structure that wraps around the outside of the reactor body 1. It can perform forced heat exchange with the wall of the reactor body 1 through the cooling medium flowing inside the jacket. External auxiliary cooling jacket 404 is a jacketed heat exchange structure surrounding the cooling jacket 403; And heat exchanger 402; The lower part of the cooling jacket 403 and the outer auxiliary cooling jacket 404 is filled with a first heat exchange medium, and the upper part of the outer auxiliary cooling jacket 404 is filled with a second heat exchange medium. The density of the second heat exchange medium is less than that of the first heat exchange medium, and it is immiscible with the first heat exchange medium. Therefore, the first heat exchange medium and the second heat exchange medium in the outer auxiliary cooling jacket 404 will naturally form layers, with the second heat exchange medium located on the upper layer and the first heat exchange medium located on the lower layer. The lower parts of the cooling jacket 403 and the external auxiliary cooling jacket 404 are connected. The outlet of the cooling jacket 403 is connected to the high-temperature medium inlet of the heat exchanger 402 through a pipe. A return pipe is provided at the high-temperature medium outlet of the heat exchanger 402. The end of the return pipe extends into the external auxiliary cooling jacket 404, so that after the first heat exchange medium in the cooling jacket 403 is discharged from its outlet, it can first flow through the heat exchanger 402 for cooling and cooling. Then, it mixes with the first heat exchange medium in the external auxiliary cooling jacket 404 again through the return pipe, and then enters the lower part of the cooling jacket 403 and is discharged again from the upper part of the cooling jacket 403. This cycle is repeated to achieve continuous cooling of the reactor body 1.

[0077] As a preferred example of the present invention, the end of the return pipe is inserted into the second heat exchange medium. The first heat exchange medium entering the outer auxiliary cooling jacket 404 through the return pipe will first mix and exchange heat with the second heat exchange medium before entering the lower first heat exchange medium layer.

[0078] As some examples of the present invention, the end of the return pipe is inserted into the first heat exchange medium layer in the external auxiliary cooling jacket 404. The first heat exchange medium entering the external auxiliary cooling jacket 404 through the return pipe will directly mix with the lower first heat exchange medium layer. In this way, the second heat exchange medium can be used to dissipate heat and seal the first heat exchange medium, avoiding the rapid reduction of the total amount caused by the large-scale evaporation of the first heat exchange medium.

[0079] As some specific examples of the present invention, the end of the return pipe may be inserted into the upper, middle or lower part of the first heat exchange medium layer in the external auxiliary cooling jacket 404, preferably the upper part.

[0080] Example 7 like Figure 8 As shown, a production apparatus for preparing anhydrous aluminum trichloride based on low-temperature indirect chlorination includes an external temperature control device 4 and an internal temperature control device 7. The structure of the external temperature control device 4 can be any one of the above embodiments 1 to 6, preferably the single-layer heat exchange structure provided in embodiments 1 to 3.

[0081] The internal temperature control device 7 is a cooling and heat dissipation device installed in the middle of the reactor body 1. The internal temperature control device 7 includes a cooling cavity located in the middle of the reactor body 1 and a phase change material filled in the cooling cavity. The cooling cavity is partially located inside the reactor body 1 and partially exposed outside the reactor body 1. In use, heat is absorbed by the internal temperature control device 7 located inside the reactor body 1, and then released by heat transfer and the internal temperature control device 7 located outside the reactor body 1.

[0082] As some examples of the present invention, the phase change material is a liquid-solid phase change material.

[0083] As some examples of the present invention, the phase change temperature of the phase change material is lower than the reaction temperature, preferably, the phase change temperature of the phase change material is 15~25°C lower than the reaction temperature.

[0084] As some specific examples of the present invention, this production apparatus for anhydrous aluminum trichloride, which includes both an external temperature control device 4 and an internal temperature control device 7, is particularly suitable for the preparation of anhydrous aluminum trichloride in large reaction furnaces 1 and at higher reaction temperatures, such as above 450°C.

[0085] Of course, the cooling chamber in the internal temperature control device 7 can also be filled with heat exchange medium, and cooling and heat dissipation can be achieved through the circulation of heat exchange medium. However, relatively speaking, using phase change material for heat dissipation can avoid large temperature changes in the reactor body 1, making the temperature control process more stable and making better use of the stability and continuity of the reaction.

[0086] For the rapid and intense exothermic reaction in the preparation of anhydrous aluminum trichloride, this embodiment addresses the core process challenges of localized thermal runaway, uneven temperature field, and difficulty in controlling the reaction rhythm through spatialized and precise thermal control. As is known to those skilled in the art, the most challenging problem in rapid and intense exothermic reactions is the accumulation of reaction heat from the outside to the center of the furnace. At this point, the furnace wall cooling structure can only remove heat near the wall surface. Due to the long heat transfer path and low mass and heat transfer efficiency, a high-temperature hotspot forms in the center of the furnace, with temperatures far exceeding the process setpoint. In this invention, an internal temperature control device 7 is installed in the central region of the furnace body 1. This device acts as a built-in heat dissipation source for the core heat accumulation area, directly removing heat from the high-temperature reaction zone in the center of the furnace. This significantly reduces the temperature gradient from the wall surface to the center, achieving uniform temperature control across the entire radial and axial domains. The improved temperature field uniformity alleviates the surge in side reactions and decreased product selectivity caused by localized high temperatures, thus improving product quality while better controlling the reaction process.

[0087] Example 8 like Figure 9 As shown, a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method includes: The reactor body 1 has an inner furnace body 107 inside it. The inner furnace body 107 is a cylindrical structure that can be slidably installed inside the reactor body 1. An internal temperature control device 7 is installed in the inner furnace body 107. The internal temperature control device 7 is a circular columnar structure. A perforated plate 103 is formed by drilling holes in the bottom plate of the inner furnace body 107. The inner furnace body 107 and the internal temperature control device 7 are integrated into one unit. The mechanical lifting arm 8 is connected to the inner furnace body 107 and can drive the inner furnace body 107 and the inner temperature control device 7 to rise or fall. Thus, an aluminum receiving cavity 101 is formed in the upper part of the orifice plate 103, and a medium receiving cavity 102 is formed in the lower part of the orifice plate 103; In use, solid aluminum material is placed in the aluminum receiving cavity 101, that is, in the space formed by the cylinder wall of the inner furnace body 107, the perforated plate 103 and the outer wall of the inner temperature control device 7. Molten medium is filled in the medium receiving cavity 102, that is, the bottom of the reaction furnace body 1. The height of the inner furnace body 107 is adjusted by the mechanical lifting arm 8 so that at least part of the molten medium can overflow the perforated plate 103 and contact the solid aluminum material. In this way, a micro-reaction zone 104 can be formed on the upper side of the perforated plate 103. And a chlorine delivery device 5, which is used to deliver chlorine gas 9 into the micro-reaction zone 104 or the medium receiving cavity 102.

[0088] As some examples of the present invention, an external temperature control device 4 is provided on the outside of the reactor body 1.

[0089] The specific composition and working method of the mechanical lifting mechanism have been widely disclosed in the prior art. The present invention does not limit the specific structure of the mechanical lifting arm 8, as long as it can drive the inner furnace body 107 and the inner temperature control device 7 to rise or fall.

[0090] In addition, it should be noted that when implementing this embodiment, attention should also be paid to the sealing problem between the reactor body 1 and the inner furnace body 107. Since the actual lifting range of the inner furnace body 107 is small, mostly <3~5cm, sealing can be achieved by setting a sealing ring at the connection between the two, or by connecting the top surface of the reactor body 1 and the inner furnace body 107 through a retractable corrugated pipe.

[0091] In the production apparatus for anhydrous aluminum trichloride disclosed in this embodiment, by setting up a liftable inner furnace body 107, the area of ​​the micro-reaction zone 104 can be adjusted, thereby adjusting the reaction rate, making it more flexible, safe and controllable.

[0092] Example 9 like Figure 10 As shown, a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method differs from Example 7 above mainly in that: The internal temperature control device 7 is filled with a composite material consisting of a solid-liquid phase change material and a thermosensitive magnetic material. At the same time, a magnet 9 is set below the reaction furnace body 1. The Curie point temperature of the thermosensitive magnetic material is 15~25℃ lower than the reaction temperature, and the temperature of the phase change material is 10~15℃ lower than the reaction temperature. During operation, the phase change material located at the lower part of the internal temperature control device 7 first absorbs heat and becomes liquid. At the same time, the thermistor magnetic material located at the lower part of the internal temperature control device 7 loses its magnetism and is no longer attracted by the magnetic force of the magnet 9 because its temperature has reached above the Curie point. Meanwhile, the composite material located at the upper part of the internal temperature control device 7 remains solid because its temperature is lower. At the same time, the thermistor magnetic material at the upper part still retains its magnetism. Thus, after the lower composite material melts, the composite material at the upper part of the internal temperature control device 7 can move downward under the magnetic attraction of the magnet 9, while squeezing the melted composite material at the lower part to the upper part of the internal temperature control device 7, where it dissipates heat and re-solidifies. This cycle, using magnetic attraction, achieves the non-powered circulation of the phase change material within the internal temperature control device 7, promoting heat dissipation.

[0093] As a preferred example of the present invention, considering the influence of the internal temperature control device 7, the medium in the central area of ​​the reactor body 1 cannot make good contact with the solid aluminum material. Therefore, an upwardly recessed groove can be provided at the bottom of the reactor body 1, and the magnet 9 can be embedded in the groove. In this way, the distance between the magnet 9 and the internal temperature control device 7 can be shortened, the effect of the magnet 9 on the thermosensitive magnetic material can be more fully utilized, and the molten medium can be better distributed in the area corresponding to the solid aluminum material.

[0094] As a preferred example of the present invention, the internal temperature control device 7 is particularly suitable for the production of anhydrous aluminum trichloride with a reaction temperature of <400°C.

[0095] As some examples of the present invention, the content of phase change material in the composite material is 75-90 wt%.

[0096] Example 10 like Figures 10-13 As shown, a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method differs from Example 9 above mainly in that: The anhydrous aluminum trichloride production apparatus further includes an adaptive spring-loaded height adjustment mechanism 10, which is located at the connection between the reactor body 1 and the inner furnace body 107, and is used to automatically adjust the height of the reactor body 1 according to the pressure exerted by the inner furnace body 107 on the reactor body 1.

[0097] Specifically, the adaptive spring-loaded height adjustment mechanism 10 includes: The receiving groove 1001 is an annular groove provided on the top of the side wall of the reactor body 1; An elastic element 1002 is disposed in the receiving groove 1001; Flanged edge 1003 is an annular flange provided on the lower side of the top surface of the inner furnace body 107; After the inner furnace body 107 is installed inside the reaction furnace body 1, the elastic element 1002 is located inside the receiving groove 1001, the top surface of the inner furnace body 107 is pressed against the elastic element 1002, and the flange 1003 surrounds the outside of the receiving groove 1001.

[0098] Thus, the inner furnace body 107 will be installed on the reaction furnace body 1 mainly by the pressure it exerts on the elastic element 1002. The degree of elastic deformation of the elastic element 1002 will be directly determined by the pressure of the inner furnace body 107. That is, when the pressure of the inner furnace body 107 on the elastic element 1002 increases, the height of the elastic element 1002 under pressure decreases, thereby reducing the height of the inner furnace body 107; conversely, the height of the inner furnace body 107 will increase.

[0099] Based on this, the downward force on the inner furnace body 107 mainly consists of two parts: one is its own gravity. During continuous production, solid aluminum material is constantly consumed while new aluminum material is continuously added to the furnace body, thus its own gravity can remain basically constant. The other part is the magnetic attraction force generated by the magnet 9 on the composite material in the inner temperature control device 7. During the reaction process, when the reaction temperature rises, a large amount of phase change material in the lower part of the inner temperature control device 7 melts, and at the same time, a large amount of thermistor magnetic material loses its magnetism. At this time, the magnetic attraction force generated by the magnet 9 on the composite material in the inner temperature control device 7... The total amount of solid composite material that is magnetically attracted within the internal temperature control device 7 is small and far from the magnet 9. Therefore, the magnetic attraction force from the magnet 9 on the internal temperature control device 7 is small, and consequently, the pressure exerted by the inner furnace body 107 on the elastic member 1002 is also small. At this time, the elastic member 1002 recovers its deformation and increases in height, which will drive the inner furnace body 107 to move upward, so that less solid aluminum material comes into contact with the molten medium, the volume of the micro-reaction zone 104 decreases, the reaction rate slows down, and the released reaction heat decreases. Conversely, when the reaction temperature decreases, the smaller amount of phase change material in the lower part of the internal temperature control device 7 melts, and simultaneously, a smaller amount of thermistor magnetic material loses its magnetism. At this time, because the total amount of solid composite material that can be magnetically attracted within the internal temperature control device 7 is large and close to the magnet 9, the overall magnetic attraction force from the magnet 9 on the internal temperature control device 7 increases. Consequently, the pressure exerted by the inner furnace body 107 on the elastic element 1002 also increases. At this time, the elastic element 1002 is compressed and its height decreases, which can drive the inner furnace body 107 to move downward, allowing more solid aluminum material to come into contact with the molten medium. This increases the volume of the micro-reaction zone 104, improves the reaction rate, and increases the released heat of reaction. Thus, the adaptive spring-loaded height adjustment mechanism 10 achieves automatic adjustment of the height of the inner furnace body 107 and the reaction rate based on changes in the reaction temperature.

[0100] As some examples of the present invention, at room temperature, the magnetic attraction force on the internal temperature control device 7 is 0.5 to 3 times its own weight.

[0101] It should be noted that, in this invention, the height variation of the inner furnace body 107 is generally less than 5cm, mostly less than 3cm. The change in height leading to a change in the distance between the inner furnace body 107 and the magnet 9, and consequently a weakening of the magnetic force of the magnet 9 on the same object, is very small and can be essentially ignored. Therefore, the magnetic force affecting the inner temperature control device 7 is mainly determined by the change in reaction temperature.

[0102] As some examples of the present invention, the elastic deformation capability of the elastic element 1002 is set according to the adjustment stroke of the inner furnace body 107. Specifically, it is preferable that the height of the micro-reaction zone 104 formed by the contact between the solid aluminum material and the molten medium material when the inner furnace body 107 is in its highest and lowest positions meets the set value. In addition, the magnitude of the magnetic force generated by the magnet 9 on the inner temperature control device 7, as well as the type and content of the phase change material and thermistor magnetic material in the inner temperature control device 7, can also be set as needed. Specifically, it is preferable that at the set reaction temperature, the adaptive spring-loaded height adjustment mechanism 10 can achieve height adjustment of the inner furnace body 107 to the set stroke.

[0103] As a preferred example of the present invention, such as Figure 13 As shown, the elastic element 1002 is an elastic structure with a circular or elliptical cross-section, such as an internally inflated industrial air spring. Thus, while achieving height adjustment, the elastic element 1002 can also maintain close contact with the top surface of the inner furnace body 107, achieving a good seal.

[0104] As a preferred example of the present invention, such as Figure 13 As shown, the adaptive spring-loaded height adjustment mechanism 10 further includes: The snap-fit ​​flange 1004 is an inwardly extending protrusion that is circumferentially spaced on the underside of the flange 1003; A notch is provided on the receiving groove 1001 to allow the snap-fit ​​flange 1004 to pass through. After the snap-fit ​​flange 1004 passes through the notch, the top surface of the inner furnace body 107 is rotated so that the snap-fit ​​flange 1004 is misaligned with the notch and located on the lower side of the receiving groove 1001. A gap is reserved between the snap-fit ​​flange 1004 and the lower side of the receiving groove 1001. When the inner furnace body 107 moves upward to the set highest position, the snap-fit ​​flange 1004 can snap onto the receiving groove 1001 to lock the upward movement of the inner furnace body 107.

[0105] As some examples of the present invention, a gap is reserved between the side wall of the receiving groove 1001 and the top surface of the inner furnace body 107. The height of this gap is the maximum stroke of the height adjustment of the inner furnace body 107. When the inner furnace body 107 moves downward to the set lowest position, the side wall of the receiving groove 1001 contacts the top surface of the inner furnace body 107. In this way, the receiving groove 1001 can provide receiving space and limit the elastic member 1002 while providing redundant support for the elastic member 1002, so as to avoid the elastic member 1002 being over-compressed.

[0106] As some examples of the present invention, in order to further strengthen the sealing connection between the inner furnace body 107 and the reaction furnace body 1, a sealing ring or other device may be provided between the outer side wall of the flange 1003 and the receiving groove 1001. It should be noted that the sealing device should be made of soft material, specifically so as not to affect the height adjustment of the inner furnace body 107.

[0107] Example 11 like Figures 14-15 As shown, a production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method differs from Example 10 above mainly in that: The elastic element 1002 in the adaptive spring-loaded height adjustment mechanism 10 is as follows: Figure 15 The W-shaped elastic structure shown has a bolt 1006 threadedly connected to the inner furnace body 107, which passes through the gap in the middle of the elastic element 1002 and is inserted into a blind hole preset in the receiving groove 1001. The main function of the bolt 1006 is to limit the inner furnace body 107, the elastic element 1002 and the receiving groove 1001 in the vertical direction.

[0108] Similarly, the inner furnace body 107 is installed on the reaction furnace body 1 mainly by the pressure it exerts on the elastic element 1002, and the degree of elastic deformation of the elastic element 1002 will be directly determined by the magnitude of the pressure of the inner furnace body 107.

[0109] As some examples of the present invention, a limiting block 1005 is provided in the receiving groove 1001. The lower end of the limiting block 1005 is inserted into the receiving groove 1001, the upper end is U-shaped, and a groove adapted to the shape of one side of the elastic member 1002 is formed on the bottom surface of the limiting block 1005. In this way, the elastic member 1002 can be further limited by the limiting block 1005, and the elastic member 1002 can be allowed to deform appropriately.

[0110] Similarly, a gap is reserved between the limiting block 1005 and the top surface of the inner furnace body 107. This gap can serve the same purpose as the gap reserved between the side wall of the receiving groove 1001 and the top surface of the inner furnace body 107 in the above embodiment 10, which will not be described in detail here.

[0111] As some examples of the present invention, a plurality of the adaptive spring-loaded height adjustment mechanisms 10 are provided at circumferential intervals in the reactor body 1 and the inner furnace body 107.

[0112] It should be noted that, since the elastic element 1002 cannot play a sealing role at this time, a reliable sealing structure must be set at the connection between the reaction furnace body 1 and the inner furnace body 107.

[0113] As some examples of the present invention, a sealing ring with a cylindrical cross-section or a sealing material that is attached and fixed to the connecting surface can be provided between the flange 1003 and the receiving groove 1001, which can achieve a rolling seal between the two while allowing the inner furnace body 107 to make a small range of height adjustments.

[0114] As some examples of the present invention, during production, the gas pressure inside the reactor body 1 can be adjusted so that it operates under a slightly negative pressure, thereby reducing the requirements for the sealing level of the reactor body.

[0115] Example 12 Preparation of anhydrous aluminum trichloride: The preparation process is divided into three stages: furnace start-up, normal production, and furnace shutdown.

[0116] Production preparation: Collect scrap aluminum materials such as pure aluminum processing scraps, waste aluminum foil, aluminum alloy scraps, and machined scraps. Remove organic impurities from the surface by alkaline washing and ultrasonic cleaning. Then dry and crush to a particle size of 0.1~200mm for later use. Furnace opening: Install the perforated plate, furnace cover, gas inlet and outlet, charging hopper, insulation blanket, preheating system, and aluminum material; then add the calculated amount of molten medium liquid through the medium inlet, and add aluminum material preheated to 260°C.

[0117] Normal production: Connect the chlorine gas pipe, introduce chlorine gas, and turn on the collector. Once the furnace temperature reaches the reaction temperature of 310℃, remove the insulation blanket and adjust the cooling airflow until the reaction gas outlet temperature reaches the rated value. Stabilize the chlorine gas flow rate, and normal production can begin. Representative products obtained include... Figure 16 and 17 As shown.

[0118] Shutdown: Shut down the furnace when there is a system malfunction or excessive impurities (such as LiCl, Al2O3, etc.) requiring cleaning. First, turn off the chlorine gas, add insulation blankets, and continue the reaction by venting hot air until no aluminum chloride gas is produced; then, ventilate with nitrogen to cool the system to room temperature. Open the furnace lid and remove the impurities.

[0119] Performance testing: The anhydrous aluminum trichloride prepared in Example 12 was tested, and the results are shown in Table 1 below: Table 1. Quality Inspection Results of Anhydrous Aluminum Trichloride Products Analysis shows that the production apparatus and process for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method described in this invention have the following characteristics: (1) Directly use waste aluminum as raw material, such as aluminum foil, aluminum shavings, aluminum shavings and other waste materials. On the one hand, the price of waste aluminum is much lower than that of pure aluminum ingots. On the other hand, some waste aluminum alloys are rich in valuable metals, such as tin, silver, copper, lithium, nickel and so on. This process can easily separate and recycle them, so the economic benefits are high.

[0120] (2) The reactor of this process is completely sealed and the reaction temperature is low. The reaction heat can be utilized and controlled by the added temperature control device, and the temperature and operating environment of the workshop are greatly improved.

[0121] (3) The product quality is better. Since the process is an indirect reaction, chlorine reacts with the medium first, and the residual chlorine will continue to react with the aluminum material. Therefore, the product and tail gas are basically free of chlorine. Moreover, the reaction is carried out at medium and low temperature, and the volatility of impurity chloride is very small, so the impurities in the product are also very low. Therefore, the product prepared by this process has high purity and is white. After testing, the purity of the product prepared by this invention is: AlCl3≧99.2%; while the purity of the product obtained by other existing methods is: AlCl3≧98.5%.

[0122] (4) The space of the reactor is divided into an upper aluminum containment chamber and a lower medium containment chamber by a perforated plate. By utilizing the characteristics of the medium material and solid aluminum material, the solid aluminum material and the molten medium material Me gradually come into contact and react sequentially in a small range, thereby achieving precise control of the violent reaction process. This can well serve the production process of anhydrous aluminum trichloride based on the low-temperature indirect chlorination method. (5) By optimizing and improving the temperature control system, the temperature gradient from the wall to the center of the furnace is significantly reduced, achieving uniform temperature control across the entire radial and axial regions. The improved temperature field uniformity can alleviate the surge in side reactions and the decrease in product selectivity caused by local high temperatures, thereby improving product quality while better controlling the reaction process.

[0123] The embodiments of this application have been described above with reference to the accompanying drawings. Unless otherwise specified, the embodiments and features in the embodiments of this application can be combined with each other. This application is not limited to the specific embodiments described above. The specific embodiments described above are merely illustrative and not restrictive. Those skilled in the art can make many other forms under the guidance of this application without departing from the spirit and scope of the claims, and all of these forms are within the protection scope of this application.

Claims

1. A production apparatus for preparing anhydrous aluminum trichloride based on a low-temperature indirect chlorination method, characterized in that, include: The reactor body (1) has its internal space divided into an upper aluminum receiving cavity (101) and a lower medium receiving cavity (102) by a perforated plate (103). An external temperature control device (4) is used to regulate the temperature of the reactor body (1); In use, solid aluminum material is placed in aluminum receiving cavity (101), and molten medium material is placed in medium receiving cavity (102). The filling amount of medium material is greater than the volume of medium receiving cavity (102), so that part of the molten medium material can overflow the perforated plate (103) and contact the solid aluminum material to form a micro-reaction zone (104) on the upper side of the perforated plate (103). The height ratio of the micro-reaction zone (104) to the medium receiving cavity (102) is 0.1~0.8:

1. In addition, a chlorine delivery device (5) is provided for delivering chlorine gas into the medium receiving cavity (102).

2. The production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method according to claim 1, characterized in that, The height of the microreaction zone (104) is ≥0.5cm.

3. The production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method according to claim 1, characterized in that, The reactor body (1) is equipped with: A gaseous aluminum trichloride discharge port (105) is located at the top of the reactor body (1) and is connected to a collector. The gaseous aluminum trichloride generated in the reactor body (1) can enter the collector through the gaseous aluminum trichloride discharge port (105) and be collected to obtain anhydrous aluminum trichloride product. Waste discharge port (106) is located at the bottom of the reactor body (1) and communicates with the medium receiving cavity (102) for discharging waste from the medium receiving cavity (102).

4. The production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method according to claim 1, characterized in that, The chlorine conveying device (5) includes a chlorine source and a chlorine conveying pipeline, with the outlet end of the chlorine conveying pipeline inserted downwards into the medium receiving cavity (102).

5. The production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method according to claim 1, characterized in that, The external temperature control device (4) includes: A semi-circular coil (401) or cooling jacket (403) is arranged around the outer wall of the reactor body (1). The heat exchanger (402) is connected to both ends of the semi-circular coil (401) or cooling jacket (403) via pipes, and forms a circulating cooling loop.

6. The production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method according to claim 1, characterized in that, The external temperature control device (4) includes: Cooling jacket (403) is a closed chamber heat exchange structure that wraps around the outside of the reactor body (1); The heat exchanger (402) is connected to the inlet and outlet of the cooling jacket (403) via pipes, forming a circulating cooling loop; And an external auxiliary cooling jacket (404), which is an open jacket heat exchange structure arranged around the cooling jacket (403).

7. The production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method according to claim 1, characterized in that, The external temperature control device (4) includes: Cooling jacket (403) is a closed chamber heat exchange structure that wraps around the outside of the reactor body (1); An external auxiliary cooling jacket (404) is a jacketed heat exchange structure surrounding the cooling jacket (403); And, heat exchanger (402); The heat exchange medium in the cooling jacket (403) and the external auxiliary cooling jacket (404) is the same; The lower parts of the cooling jacket (403) and the external auxiliary cooling jacket (404) are connected. The outlet of the cooling jacket (403) is connected to the high-temperature medium inlet of the heat exchanger (402) through a pipe. The high-temperature medium outlet of the heat exchanger (402) is connected to the upper part of the external auxiliary cooling jacket (404). After the heat exchange medium in the cooling jacket (403) is discharged from its outlet, it first flows through the heat exchanger (402) for cooling and temperature reduction. Then it enters the external auxiliary cooling jacket (404) from the upper part and flows from top to bottom to the lower part of the external auxiliary cooling jacket (404). After entering the lower part of the cooling jacket (403), it is discharged again from the upper part of the cooling jacket (403). This cycle is repeated to continuously cool the reactor body (1).

8. The production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method according to claim 1, characterized in that, The external temperature control device (4) includes: Cooling jacket (403) is a closed chamber heat exchange structure that wraps around the outside of the reactor body (1); An external auxiliary cooling jacket (404) is a jacketed heat exchange structure surrounding the cooling jacket (403); And, heat exchanger (402); The lower part of the inner cooling jacket (403) and the outer auxiliary cooling jacket (404) is filled with a first heat exchange medium, and the upper part of the outer auxiliary cooling jacket (404) is filled with a second heat exchange medium. The density of the second heat exchange medium is less than that of the first heat exchange medium, and the second heat exchange medium is immiscible with the first heat exchange medium. The lower parts of the cooling jacket (403) and the external auxiliary cooling jacket (404) are connected. The outlet of the cooling jacket (403) is connected to the high-temperature medium inlet of the heat exchanger (402) through a pipe. A return pipe is provided at the high-temperature medium outlet of the heat exchanger (402). The end of the return pipe extends into the external auxiliary cooling jacket (404), so that after the first heat exchange medium in the cooling jacket (403) is discharged from its outlet, it first flows through the heat exchanger (402) for cooling and cooling down. Then, it mixes with the first heat exchange medium in the external auxiliary cooling jacket (404) again through the return pipe, and then enters the lower part of the cooling jacket (403) and is discharged again from the upper part of the cooling jacket (403). This cycle is repeated to continuously cool the reactor body (1).

9. The production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method according to claim 1, 5, 6, 7, or 8, characterized in that, Also includes: The internal temperature control device (7) is a cooling and heat dissipation device set in the middle of the reactor body (1). The internal temperature control device (7) includes a cooling cavity and a phase change material filled in the cooling cavity. The cooling cavity is partially located inside the reactor body (1) and partially exposed outside the reactor body (1).

10. The production apparatus for preparing anhydrous aluminum trichloride based on the low-temperature indirect chlorination method according to claim 9, characterized in that, An inner furnace body (107) is provided inside the reactor body (1). The inner furnace body (107) is a cylindrical structure that can be slidably installed inside the reactor body (1). An internal temperature control device (7) is provided in the inner furnace body (1). The internal temperature control device (7) is a circular columnar structure. A hole is drilled in the bottom plate of the inner furnace body (107) to form an annular perforated plate (103). The inner furnace body (107) and the internal temperature control device (7) are integrated. The height of the inner furnace body (107) relative to the reaction furnace body (1) is adjustable.

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