Aluminum trichloride preparation system and method for preparing aluminum trichloride

By using gravity feeding devices and premixing devices in the production of titanium dioxide in chloride method, the problems of uneven injection of aluminum powder and excessive chlorine corrosion are solved, and the uniform distribution of aluminum particles and high-quality production of aluminum trichloride are achieved.

CN115501818BActive Publication Date: 2025-06-27HENAN BILLIONS NEW MATERIAL CO LTD
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Patent Information

Application Number
CN202211278902.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-10-19
Publication Date
2025-06-27
Estimated Expiration
2042-10-19

AI Technical Summary

Technical Problem

During the existing chlorinated titanium dioxide production process, aluminum powder sprays unevenly and the reaction is incomplete, resulting in equipment blockage, damage and excessive chlorine corrosion of the system.

Method used

The gravity feeding device is used to add aluminum particles through gravity, and combined with the premix device to accurately match chlorine and titanium tetrachloride to form an aluminum trichloride preparation system.

Benefits of technology

The uniform distribution of aluminum particles is achieved, the equipment is blocked and damaged, the equipment is reduced, and the product quality and system stability of aluminum chloride are improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

This application relates to the technical field of titanium dioxide production by the chlorination process, and particularly to a preparation system and a preparation method of aluminum trichloride. The aluminum trichloride preparation system includes a gravity feeding device, a reaction device, and a premixing device. Along the height direction of the reaction device, the gravity feeding device is arranged above the reaction device and is used to add excessive aluminum particles to the reaction device by gravity. The gravity feeding device includes a silo, a control valve, and a weighing sensor, and the aluminum particles placed in the silo are controlled by the control valve and the weighing sensor to add excessive aluminum particles to the reaction device according to a preset quantity and by gravity. The premixing device includes a premixing container and a premixing flowmeter arranged in the premixing container, and is used to premix appropriate amounts of chlorine gas and aluminum tetrachloride gas according to a preset ratio. The reaction device is used to mix and react the aluminum particles put by the gravity feeding device and the premixed gas transported by the premixing device to produce aluminum trichloride.
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Description

Technical Field

[0001] The present application relates to the technical field of titanium dioxide production by the chlorination process, and in particular to a system and method for preparing aluminum trichloride. Background Art

[0002] In the production process of titanium dioxide by the chlorination process, the core process is the gas-phase oxidation of refined TiCl4. In a very short time (<0.1 s), TiCl4 reacts with oxygen to form TiO2. However, most of the TiO2 formed is anatase type. In order to produce high-quality rutile-type titanium dioxide, a crystal form conversion agent must be added. Through practice, AlCl3 is the most excellent crystal form conversion agent.

[0003] Currently, it is generally adopted to spray aluminum powder into the reactor to directly react with an appropriate amount of chlorine gas to form AlCl3, and at the same time, it is mixed evenly with TiCl4 gas and then enters the oxidation reactor for reaction. However, the following problems generally exist: (1) In order to ensure the spraying effect of aluminum powder, the spray gun mostly adopts a sandwich structure and is prone to blockage, affecting production; (2) After the aluminum powder is sprayed in, the distribution effect is poor, the reaction is incomplete, there is deposition and sintering of aluminum powder, and it needs to be cleaned regularly. At the same time, the unreacted aluminum powder is carried into the system and reacts along the way, damaging the equipment; (3) In order to ensure the full reaction of aluminum powder and avoid carrying it into the system, excessive chlorine gas is often used, and the excessive chlorine gas aggravates the corrosion of the system.

[0004] Therefore, there is an urgent need to develop a system for preparing AlCl3 that is stable, reliable, does not require regular equipment cleaning, and has little corrosion to the equipment. Summary of the Invention

[0005] The purpose of the present application is to provide a system and method for preparing aluminum trichloride, which solves to a certain extent the technical problem in the prior art that there is an urgent need to develop a system for preparing AlCl3 that is stable, reliable, does not require regular equipment cleaning, and has little corrosion to the equipment.

[0006] The present application provides a system for preparing aluminum trichloride, including: a gravity feeding device, a reaction device, and a premixing device; wherein, along the height direction of the reaction device, the gravity feeding device is arranged above the reaction device and is used to add excessive aluminum particles to the reaction device by gravity.

[0007] The gravity feeding device includes a silo, a control valve, and a weighing sensor, and the aluminum particles placed in the silo are controlled by the control valve and the weighing sensor to add excessive aluminum particles to the reaction device according to a preset quantity and by gravity.

[0008] The premixing device includes a premixing container and a premixing flowmeter arranged on the premixing container, and is used to premix an appropriate amount of chlorine gas and aluminum tetrachloride gas according to a preset ratio.

[0009] The reaction device is used to mix and react the aluminum particles fed by the gravity feeding device and the premixed gas conveyed by the premixing device to produce aluminum trichloride.

[0010] In the above technical solution, further, the silo includes a storage silo, a vibrating feeder, and a feeding bin, and the storage silo, the vibrating feeder, and the feeding bin are sequentially connected and communicated along the material discharging direction; the weighing sensor is arranged at the discharging port of the feeding bin.

[0011] In any of the above technical solutions, further, the control valve includes a feeding bin exhaust valve, a feeding bin inlet valve, a feeding bin pressurizing valve, a charging pipeline pressurizing valve, a feeding bin discharging valve, a bottom air sealing valve, and a purging valve; wherein, the discharging port of the storage silo is connected to the feeding bin through the vibrating feeder, and the feeding bin inlet valve is arranged on the pipeline connecting the vibrating feeder and the feeding bin;

[0012] The feeding bin exhaust valve is arranged on the pipeline connecting the air port of the storage silo and the first ventilation port of the feeding bin; the discharging port at the bottom of the feeding bin is connected with a discharging pipeline, and the feeding bin discharging valve and the bottom air sealing valve are sequentially arranged on the discharging pipeline, and the feeding bin discharging valve is arranged close to the feeding bin;

[0013] The second ventilation port of the feeding bin is communicated with a first flow pipeline, the end of the first flow pipeline is connected with a second flow pipeline and a third flow pipeline, and the first flow pipeline, the second flow pipeline, and the third flow pipeline are communicated with each other;

[0014] The second flow pipeline is communicated with the pipeline between the feeding bin discharging valve and the bottom air sealing valve, and the charging pipeline pressurizing valve is arranged on the second flow pipeline; the third flow pipeline is communicated with an external gas source; the purging valve is arranged on the pipeline connecting the outlet end of the bottom air sealing valve and the gas source.

[0015] In any of the above technical solutions, further, the reaction device includes a furnace body and a distribution plate; wherein, an accommodation chamber is formed inside the furnace body, and the distribution plate is arranged in the accommodation chamber to divide the accommodation chamber into a gas collecting chamber and a reaction chamber which are arranged from bottom to top along its height direction;

[0016] Air inlet holes are formed on the distribution plate; a feeding port is formed at the top of the furnace body along its height direction, and the feeding port is communicated with the discharging pipeline of the feeding bin, and a sealing cut-off valve is arranged between the two;

[0017] An air inlet is formed on one side of the bottom of the furnace body, and the air inlet communicates with the gas collecting chamber; an air outlet is formed on one side of the top of the furnace body, and the air outlet communicates with the reaction chamber.

[0018] In any of the above technical solutions, further, the distribution plate includes a bottom flat plate and a side inclined plate, and the side inclined plate is arranged around the circumference of the bottom flat plate and is in a gradually expanding shape from bottom to top along the height direction of the furnace body; the side inclined plate is connected to the inner wall of the furnace body; the side inclined plate is formed with the air inlet holes, and the air inlet holes are arranged perpendicular to the height direction of the furnace body.

[0019] In any of the above technical solutions, further, the furnace body is formed with a discharge port communicating with the bottom of the reaction chamber, and the discharge port is provided with a valve or a cover that can be opened or closed;

[0020] The furnace body is formed with a transparent observation window;

[0021] The furnace body is formed with an inert filler feeding port that can be opened or closed;

[0022] The top of the furnace body along its height direction is formed with a spare feeding port that can be opened or closed.

[0023] The present application also provides a method for preparing aluminum trichloride, including the aluminum trichloride preparation system described in any of the above technical solutions. Therefore, it has all the beneficial technical effects of the aluminum trichloride preparation system and will not be elaborated here.

[0024] In the above technical solution, further, the method for preparing aluminum trichloride includes the following steps:

[0025] Batching: The aluminum pellets placed in the silo are controlled by the control valve and the weighing sensor to add an excessive amount of aluminum pellets to the reaction device by gravity according to a preset quantity;

[0026] Reaction: The aluminum pellets fall into the reaction chamber through the feeding port of the reaction device, the aluminum pellets melt at a preset temperature and move towards the bottom of the reaction chamber, and are mixed with the inert filler at the bottom of the reaction chamber;

[0027] An appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio. The mixed gas flow first enters the gas collecting chamber, and then passes through the distribution plate and enters the reaction chamber to react with the molten aluminum.

[0028] In any of the above technical solutions, further, the step that an appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio, the mixed gas flow first enters the gas collecting chamber, and then passes through the distribution plate and enters the reaction chamber to react with the molten aluminum includes the following steps:

[0029] An appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio. The mixed gas flow first enters the gas collection chamber, and then enters the reaction chamber horizontally through the distribution plate. After the mixed gas flow enters the reaction chamber, it moves upward, and the flow rate of the mixed gas flow gradually decreases radially from the center towards the furnace wall;

[0030] The gas flow stirs up the aluminum particles, and the aluminum particles follow the gas flow upward or are suspended in the gas flow. Chlorine gas reacts with aluminum to form aluminum trichloride. When the gas flow rises to the upper part of the reaction chamber, the flow rate slows down, and the inert filler and the reacted aluminum drop to the middle and lower parts of the reaction chamber due to the reduced flow rate and continue to react;

[0031] The heat released by the reaction of aluminum and chlorine gas heats titanium tetrachloride, and the generated gaseous aluminum trichloride is uniformly mixed in the titanium tetrachloride gas flow and discharged from the gas outlet of the reaction device.

[0032] In any of the above technical solutions, further, the batching includes the following steps: In the initial state, the storage bin is filled with materials and the feeding bin is empty; after the batching starts, the inlet valve of the feeding bin and the exhaust valve of the feeding bin are both in the open state; the discharge valve of the feeding bin, the pressurizing valve of the feeding bin, the pressure charging valve of the discharge pipeline, the bottom air sealing valve, and the purge valve are all in the closed state;

[0033] The vibrating feeder is started to start loading the feeding bin;

[0034] The inlet valve of the feeding bin and the exhaust valve of the feeding bin are closed, the pressurizing valve of the feeding bin is opened to pressurize the feeding bin, and when the pressure is equal to the pressure of the reaction device, the pressurization is stopped;

[0035] During unloading, the discharge valve of the feeding bin and the bottom air sealing valve are sequentially opened, the weighing sensor is monitored, and when the weighing no longer decreases, the discharge valve of the feeding bin is closed, the pressure charging valve of the discharge pipeline is opened until the bottom air sealing valve is closed in place, and after the pressure of the second flow pipeline is increased to be equal to the pressure of the reaction device, the pressurization is stopped;

[0036] The exhaust valve of the feeding bin is opened to discharge the gas in the feeding bin. After the pressure drops to atmospheric pressure, the inlet valve of the feeding bin is opened to wait for the next batching;

[0037] Among them, the purge valve is used as a spare for dredging and purging the gas source; during the operation of the reaction device, the second flow pipeline is always pressurized, and the pressure of the second flow pipeline is ensured to be higher than the pressure of the reaction device so that the corrosive gas in the process flow cannot enter the second flow pipeline.

[0038] In any of the above technical solutions, further, in the charging step, according to the set target weighing value, the method of rapid feeding with 90% range, slow feeding with 8% range, and jog feeding with 2% range is adopted. After the metering is completed, the weighing value is recorded.

[0039] Compared with the prior art, the beneficial effects of the present application are as follows:

[0040] The aluminum trichloride preparation system provided by the present application is equipped with a gravity feeding device. Through the gravity feeding device, accurate gravity feeding can be achieved, and thus various problems existing in the prior art in the method of spraying aluminum powder for feeding by a spray gun, such as blocking the spray gun and the need for regular cleaning, etc., will not occur.

[0041] In addition, aluminum grains are used instead of aluminum powder, and the aluminum grains are put into the reaction device by means of gravity feeding, so that the aluminum grains are more evenly distributed. There will be no problems in the prior art such as uneven distribution of aluminum powder, incomplete reaction, aluminum powder may be carried into the subsequent system and react in the subsequent system, damaging the equipment (a large amount of heat is released during the reaction), and the spray gun is easily damaged and blocked at high temperature and is expensive.

[0042] In addition, aluminum is in excess, and chlorine gas and titanium tetrachloride gas are accurately proportioned through a premixing device, that is, the method of appropriate amount of chlorine gas is adopted to ensure complete reaction of chlorine gas and reduce corrosion of the equipment; at the same time, the premixing of chlorine gas and titanium tetrachloride gas ensures that the generated aluminum trichloride is evenly mixed in the titanium tetrachloride gas stream, ensuring the stability of the quality of the subsequent product.

[0043] This method adopts the method of sealed vertical feeding and the upward boiling and melting aluminum method, so that the aluminum grains fall into the reaction chamber by gravity with the assistance of a small amount of nitrogen for sealing. The nitrogen flow rate is small, with a maximum of only 20 Nm³ / h. Compared with other feeding methods that require gas volumes of hundreds of cubic meters, the content of inert gas in the subsequent gas stream is greatly reduced, facilitating the subsequent utilization of chlorine gas in titanium dioxide chloride production. At the same time, it has the characteristics of accurate feeding and not easy to block;

[0044] In addition, the molten aluminum relies only on self-heating, and the reaction chamber has a structure of only a straight cylinder with a partition (distribution plate) inside. The production and control are simple. At the same time, the method of excessive aluminum grains, appropriate amount of chlorine gas, and pre-mixing of chlorine gas and titanium tetrachloride is adopted. The chlorine gas reacts completely, causing little corrosion to the equipment, and the service life of the equipment is long; at the same time, the prior mixing of chlorine gas and titanium tetrachloride ensures the uniform mixing of the generated aluminum trichloride and titanium tetrachloride, thereby ensuring the stability of the quality of the subsequent product. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] To more clearly illustrate the specific embodiments of the present application or the technical solutions in the prior art, the following will briefly introduce the drawings required for the description of the specific embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0046] Figure 1 Structural schematic diagram of the aluminum trichloride preparation system provided by an embodiment of the present application;

[0047] Figure 2 Structural schematic diagram of the gravity feeding device provided by an embodiment of the present application;

[0048] Figure 3 Structural schematic diagram of the reaction device provided by an embodiment of the present application;

[0049] Figure 4 Internal gas circulation structural schematic diagram of the reaction device provided by an embodiment of the present application.

[0050] Reference numerals:

[0051] 1 - Gravity feeding device, 101 - Feeding bin exhaust valve, 102 - Feeding bin inlet valve, 103 - Feeding bin pressurizing valve, 104 - Discharge pipeline pressurizing valve, 105 - Feeding bin discharge valve, 106 - Bottom air sealing valve, 107 - Purge valve, 108 - Storage bin, 109 - Vibrating feeder, 110 - Feeding bin, 111 - Gas source;

[0052] 2 - Reaction device, 21 - Furnace body, 211 - Gas collection chamber, 212 - Reaction chamber, 213 - Feeding port, 214 - Spare feeding port, 215 - Inlet port, 216 - Outlet port, 217 - Discharge port, 218 - Transparent observation window, 219 - Inert filler feeding port, 22 - Distribution plate, 221 - Bottom flat plate, 222 - Side inclined plate, 23 - Inert filler. Specific embodiments

[0053] The following will clearly and completely describe the technical solutions of the present application in conjunction with the drawings. Obviously, the described embodiments are some embodiments of the present application, rather than all embodiments.

[0054] The components of the embodiments of the present application usually described and shown in the drawings here can be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present application provided in the drawings is not intended to limit the scope of the present application claimed, but merely represents the selected embodiments of the present application.

[0055] Based on the embodiments in this application, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the scope of protection of this application.

[0056] In the description of this application, it should be noted that the orientation or positional relationship indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings. It is only for the convenience of describing this application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this application. In addition, the terms "first", "second", "third" are only used for descriptive purposes and cannot be construed as indicating or implying relative importance.

[0057] In the description of this application, it should be noted that unless otherwise clearly specified and limited, the terms "installed", "connected", "connected to" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific situations.

[0058] The following refers to Figures 1 to 4 Describe an aluminum trichloride preparation system and an aluminum trichloride preparation method according to some embodiments of this application.

[0059] Embodiment 1

[0060] Refer to Figure 1 As shown, the embodiment of this application provides an aluminum trichloride preparation system, including: a gravity feeding device 1, a reaction device 2, and a premixing device (note: the premixing device is not shown in the figure); wherein, along the height direction of the reaction device 2, the gravity feeding device 1 is arranged above the reaction device 2 and is used to add an excessive amount of aluminum pellets to the reaction device 2 by gravity.

[0061] The gravity feeding device 1 includes a silo, a control valve, and a weighing sensor, and the aluminum pellets placed in the silo are controlled by the control valve and the weighing sensor to add an excessive amount of aluminum pellets to the reaction device 2 according to a preset quantity and by gravity.

[0062] The premixing device includes a premixing container and a premixing flowmeter arranged on the premixing container, and is used to premix an appropriate amount of chlorine gas and aluminum tetrachloride gas according to a preset ratio.

[0063] The reaction device 2 is used to mix and react the aluminum pellets put in by the gravity feeding device 1 and the premixed gas conveyed by the premixing device to produce aluminum trichloride.

[0064] Based on the structures described above, it can be known that the aluminum trichloride preparation system provided in this application is equipped with a gravity feeding device 1. Through the gravity feeding device 1, accurate feeding by gravity can be achieved, and thus various problems existing in the method of spraying aluminum powder for feeding by a spray gun in the prior art can be avoided, such as blocking the spray gun and the problem of needing to be cleaned regularly, etc.

[0065] In addition, aluminum pellets are used instead of aluminum powder, and the aluminum pellets are put into the reaction device 2 by means of gravity feeding, so that the aluminum pellets are more evenly distributed, and the problems in the prior art such as uneven distribution of aluminum powder, incomplete reaction, aluminum powder may be carried into the subsequent system and react in the subsequent system, damaging the equipment (a large amount of heat is released during the reaction), and the spray gun is easily damaged and blocked at high temperature and is expensive due to the need to spray aluminum powder into the spray gun can be avoided.

[0066] In addition, an excessive amount of aluminum is used, and chlorine gas and titanium tetrachloride gas are accurately proportioned through a premixing device, that is, a method of appropriate amount of chlorine gas is adopted to ensure complete reaction of chlorine gas and reduce corrosion of the equipment; at the same time, chlorine gas and titanium tetrachloride gas are premixed to ensure that the generated aluminum trichloride is evenly mixed in the titanium tetrachloride gas stream and ensure the stability of the quality of the subsequent product.

[0067] In this embodiment, preferably, as Figure 2 shown, the silo includes a storage silo 108, a vibrating feeder 109, and a feeding silo 110, and the storage silo 108, the vibrating feeder 109, and the feeding silo 110 are connected in sequence along the feeding direction; a weighing sensor is arranged at the discharge port of the feeding silo 110.

[0068] Based on the structures described above, it can be known that the storage silo 108 is used to pre-place the material, that is, aluminum pellets, the vibrating feeder 109 is used to provide vibration to facilitate feeding, and the feeding silo 110 is used to feed the material fed by vibration to the reaction device 2.

[0069] Further, preferably, the vibrating feeder 109 is an electric vibrating feeder.

[0070] In this embodiment, preferably, as Figure 2 shown, the control valve includes a feeding silo exhaust valve 101, a feeding silo inlet valve 102, a feeding silo pressurizing valve 103, a charging pipeline pressurizing valve 104, a feeding silo discharge valve 105, a bottom air sealing valve 106, and a purging valve 107; among them, the discharge port of the storage silo 108 is connected to the feeding silo 110 through the vibrating feeder 109, and a feeding silo inlet valve 102 is arranged on the pipeline connecting the vibrating feeder 109 and the feeding silo 110;

[0071] A charging bin exhaust valve 101 is provided on the pipeline where the air port of the storage bin 108 is connected to the first ventilation port of the feeding bin 110; the discharge port at the bottom of the feeding bin 110 is connected to a discharge pipeline, and a feeding bin discharge valve 105 and a bottom air sealing valve 106 are sequentially arranged on the discharge pipeline, and the feeding bin discharge valve 105 is arranged close to the feeding bin 110;

[0072] The second ventilation port of the feeding bin 110 is communicated with a first circulation pipeline, the end of the first circulation pipeline is connected with a second circulation pipeline and a third circulation pipeline, and the first circulation pipeline, the second circulation pipeline and the third circulation pipeline are communicated with each other;

[0073] The second circulation pipeline is communicated with the pipeline between the feeding bin discharge valve 105 and the bottom air sealing valve 106, and a discharge pipeline pressurizing valve 104 is arranged on the second circulation pipeline; the third circulation pipeline is communicated with an external gas source 111 (and preferably, the gas source 111 is a nitrogen gas source 111); a purging valve 107 is arranged on the pipeline where the outlet end of the bottom air sealing valve 106 is connected to the gas source 111.

[0074] According to the structure described above, the batching process is as follows:

[0075] In the initial state, the storage bin 108 has materials and the feeding bin 110 is empty; after batching starts, both the feeding bin inlet valve 102 and the feeding bin exhaust valve 101 are in the open state; the feeding bin discharge valve 105, the feeding bin pressurizing valve 103, the discharge pipeline pressurizing valve 104, the bottom air sealing valve 106 and the purging valve 107 are all in the closed state;

[0076] The vibrating feeder 109 is started to start loading the feeding bin 110, and the feeding is carried out according to the following rules. According to the set target weighing value, the 90% range is fed quickly, the 8% range is fed slowly, and the 2% range is fed by jogging. After the metering is completed, the weighing value is recorded;

[0077] The feeding bin inlet valve 102 and the feeding bin exhaust valve 101 are closed, the feeding bin pressurizing valve 103 is opened to pressurize the feeding bin 110, and when the pressure is equal to the pressure of the reaction device 2, the pressurization is stopped;

[0078] When discharging, the feeding bin discharge valve 105 and the bottom air sealing valve 106 are sequentially opened, the weighing sensor is monitored, and when the weighing no longer decreases, the feeding bin discharge valve 105 is closed, the discharge pipeline pressurizing valve 104 is opened until the bottom air sealing valve 106 is closed in place, and after the pressure of the second circulation pipeline is increased to be equal to the pressure of the reaction device 2, the pressurization is stopped;

[0079] The feeding bin exhaust valve 101 is opened to discharge the gas in the feeding bin 110. After the pressure drops to atmospheric pressure, the feeding bin inlet valve 102 is opened to wait for the next batching.

[0080] That is to say, the system adopts a static metering method. When the system starts batching, the operator inputs the corresponding batching amount according to the system load. The storage bin 108 is at normal pressure, and the vibrating feeder starts to work. Through the fast-slow combination, the material is added to the feeding bin 110 to the set value. Subsequently, the inlet valve 102 of the feeding bin is closed, and the pressurizing valve 103 of the feeding bin is opened to pressurize the feeding bin 110. After the pressure is the same as that in the reaction device, the discharge valve 105 of the feeding bin and the bottom air sealing valve 106 are opened to complete the discharging. Subsequently, the exhaust valve 101 of the feeding bin is opened. After the pressure of the feeding bin 110 drops to normal pressure, the inlet valve 102 of the feeding bin is opened to prepare for the next batching. Preferably, the operation process of the whole system is fully automatically controlled by the PLC.

[0081] It can be seen that the aluminum particle feeding adopts normal pressure metering, and at the same time, large doses and rapid feeding are carried out. The small dose at the end adopts a slow feeding method, and the metering is accurate. Using aluminum particle feeding, it is safe and easy to control (aluminum powder is explosive), the feeding pipe is not blocked, and the feeding is stable and accurate, that is, high-precision batching is achieved.

[0082] Note: Among them, the purging valve 107 is used as a spare for dredging and purging the gas source 111; during the operation of the reaction device 2, the pressure of the second flow pipeline is always ensured to be higher than the pressure of the reaction device 2, so that the corrosive gas in the process flow cannot enter the second flow pipeline.

[0083] In this embodiment, preferably, as Figure 3 shown, the reaction device 2 includes a furnace body 21 and a distribution plate 22; among them, an accommodation chamber is formed inside the furnace body 21, and the distribution plate 22 is arranged in the accommodation chamber to divide the accommodation chamber into a gas collection chamber 211 and a reaction chamber 212 which are arranged from bottom to top along its height direction;

[0084] Air inlet holes are formed on the distribution plate 22; a feeding port 213 is formed at the top of the furnace body 21 along its height direction, and the feeding port 213 is communicated with the discharging pipeline of the feeding bin 110, and a sealing cut-off valve is arranged between the two. When the feeding to the reaction device 2 is completed, the sealing cut-off valve can be closed to ensure the sealing performance;

[0085] An air inlet 215 is formed on one side of the bottom of the furnace body 21, and the air inlet 215 is communicated with the gas collection chamber 211; an air outlet 216 is formed on one side of the top of the furnace body 21, and the air outlet 216 is communicated with the reaction chamber 212.

[0086] According to the structure described above, the working principle of the reaction device 2 is as follows:

[0087] Aluminum pellets fall into the reaction chamber 212 through the feeding port 213 of the reaction device 2. The aluminum pellets melt at a preset temperature and move towards the bottom of the reaction chamber 212 (the above-mentioned preset reaction temperature is about 450 °C), and are mixed with the inert filler 23 at the bottom of the reaction chamber 212;

[0088] An appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio (the temperature of titanium tetrachloride is 350 - 400 °C). The mixed gas flow first enters the gas collection chamber 211, and then enters the reaction chamber 212 horizontally through the distribution plate 22. After the mixed gas flow enters the reaction chamber 212, it moves upward, and the flow rate of the mixed gas flow gradually decreases radially from the center towards the furnace wall;

[0089] The gas flow flushes up the aluminum pellets, and the aluminum pellets follow the gas flow upward or are suspended in the gas flow. Chlorine reacts with aluminum to form aluminum trichloride. When the gas flow rises to the upper part of the reaction chamber 212, the flow rate slows down, and the inert filler 23 and the reacted aluminum drop to the middle and lower parts of the reaction chamber 212 due to the reduced flow rate and continue to react (see Figure 4 shown);

[0090] The exothermic reaction between aluminum and chlorine heats titanium tetrachloride (heated to 450 - 480 °C, and the subsequent exothermic reaction melts aluminum, saving energy). The generated gaseous aluminum trichloride is uniformly mixed in the titanium tetrachloride gas flow and is discharged from the gas outlet 216 of the reaction device 2.

[0091] It can be seen that the reaction uses the molten aluminum fluidization method to produce aluminum trichloride. Specifically, after chlorine gas and hot titanium tetrachloride gas are mixed, they enter from the bottom of the furnace body 21 and contact and react with the molten aluminum suspended in the reaction chamber 212 to form aluminum trichloride. The generated aluminum trichloride is uniformly mixed in the titanium tetrachloride gas flow, discharged from the upper outlet, and enters the subsequent process.

[0092] In this embodiment, preferably, as Figure 3 shown, the distribution plate 22 includes a bottom flat plate 221 and a side inclined plate 222, and the side inclined plate 222 is arranged around the circumference of the bottom flat plate 221 and is in a gradually expanding shape from bottom to top along the height direction of the furnace body 21; the side inclined plate 222 is connected to the inner wall of the furnace body 21.

[0093] According to the structure described above, the side inclined plate 222 is less likely to be blocked compared to an ordinary flat sieve plate. Specifically, the air inlet holes are horizontal, and the material will not enter the air inlet holes and the gas collection chamber 211. At the same time, after the gas enters the reaction chamber 212 through the air inlet holes, due to inertia, it all converges towards the center. The flow rate of the central air flow is large, and the flow rate near the furnace wall is small. After the aluminum particles are blown up and react, at the upper part of the reaction chamber 212, due to the average flow rate, the unreacted material moves downward at the near-wall position and is blown up and reacts again when it reaches the bottom, forming a cycle, and the reaction is more complete. At the same time, the common slugging phenomenon (due to the small diameter, high height, and large air flow causing the overall material to be pushed upward, and when the air flow breaks at a certain height, the material returns and reciprocates) in the fluidized bed reactor is avoided.

[0094] At the same time, inert filler 23 gravel of dioxide is added to avoid the adhesion of molten aluminum, keep the aluminum in a small-particle molten state, and enhance the mass transfer and fluidization effect. In addition, the reaction heat can increase the temperature of the titanium tetrachloride gas stream by 80 - 100 °C.

[0095] In this embodiment, preferably, as Figure 3 shown, the furnace body 21 is formed with a discharge port 217 communicating with the bottom of the reaction chamber 212, and the discharge port 217 is provided with a valve or a cover that can be opened or closed.

[0096] According to the structure described above, it can be known that when the production is completed, the remaining aluminum particles can be discharged through the discharge port 217.

[0097] Furthermore, preferably, the discharge port 217 is formed by a section of pipe fitting. One end of the pipe fitting is inserted into the bottom wall of the reaction chamber 212, and the opposite end of the pipe fitting passes through the bottom wall of the furnace body 21 and extends to the outside. Preferably, the pipe fitting can be welded to the bottom wall of the reaction chamber 212 and the bottom wall of the furnace body 21 respectively.

[0098] In this embodiment, preferably, as Figure 3 shown, the furnace body 21 is formed with a transparent observation window 218.

[0099] According to the structure described above, through the transparent observation window 218, the reaction condition inside the reaction device 2 can be clearly seen. That is to say, through the transparent observation window 218, the reaction situation and the bed height inside the reaction device 2 can be seen, avoiding the situation where the aluminum particles or the inert filler 23 are insufficient.

[0100] Furthermore, preferably, the transparent observation window 218 is arranged at the middle position of the furnace body 21. Preferably, the furnace body 21 is formed with an observation port extending obliquely upward, and a sight glass is arranged at the top of the observation port.

[0101] In this embodiment, preferably, as Figure 3As shown, the furnace body 21 is formed with an inert filler feeding port 219 that can be opened or closed.

[0102] According to the structure described above, inert filler 23 is added into the reaction chamber 212 through the inert filler feeding port 219. The inert filler 23 divides the molten aluminum into small particles, preventing adhesion while expanding the contact area between aluminum and chlorine gas, and increasing the reaction rate.

[0103] Furthermore, preferably, the furnace body 21 is formed with a pipe portion extending obliquely upward, and a switching valve or a cover is provided at the pipe orifice.

[0104] Furthermore, preferably, the inert filler 23 is solid particles such as silicon dioxide or zirconium-aluminum composite balls that do not react with high-temperature chlorine gas and titanium tetrachloride.

[0105] In this embodiment, preferably, as Figure 3 shown, a spare feeding port 214 that can be opened or closed is formed at the top of the furnace body 21 along its height direction, and preferably, the opening or closing of the spare feeding port 214 can be controlled in advance by a switching valve or a cover.

[0106] According to the structure described above, when there is a problem with the feeding port 213 of the reaction device 2, the spare feeding port 214 can be opened for use.

[0107] In summary, the aluminum trichloride preparation system provided by this application has the following advantages:

[0108] (1) By using the method of excessive aluminum pellets and appropriate amount of chlorine gas, it ensures that the chlorine gas reacts completely, avoids corrosion of the system caused by excess chlorine gas, and thus helps to extend the service life of the equipment.

[0109] (2) The reaction condition of the reactor is clearly visible: through the sight glass in the middle, the reaction situation and the bed height in the reactor can be seen, avoiding the situation of insufficient aluminum pellets or inert filler 23.

[0110] (3) Corrosive gases do not backflow, and the feeding bin 110 has good sealing performance: during the reaction, nitrogen sealing is provided. At the same time, the pressure of the gravity feeding device 1 is higher than the pressure inside the reaction device 2, and the gas does not backflow during feeding, and the equipment has good continuous operation effect.

[0111] (4) The feeding is stable and not easy to block: The aluminum pellet feeding adopts atmospheric pressure metering. At the same time, for large doses, rapid feeding is used, and for small doses at the end, slow feeding is used. The metering is accurate. In addition, using aluminum pellet feeding, it is safe and easy to control (aluminum powder is explosive), does not block, and the feeding is stable and accurate.

[0112] (5) The gas collecting chamber 211 is not easy to block: Compared with ordinary flat sieve plates, the air inlet holes are horizontal, and the material will not enter the air inlet holes and the gas collecting chamber 211.

[0113] (6) The side inclined plate 222 is less likely to be blocked compared with an ordinary flat sieve plate. In addition, the air inlet holes are horizontal, so that the material will not enter the air inlet holes and the air collecting chamber 211. At the same time, after the gas enters the reaction chamber 212 through the air inlet holes, it concentrates towards the center due to inertia. The flow velocity of the central air flow is large, and the flow velocity near the furnace wall is small. After the aluminum particles are blown up and react, due to the average flow velocity in the upper part of the reaction chamber 212, the unreacted material moves downward at the near-wall position and is blown up again to react when it reaches the bottom, forming a cycle, and the reaction is more complete. At the same time, the common slugging phenomenon (due to the small diameter, high height, and large air flow causing the whole material to be pushed upward, and when the air flow breaks at a certain height, the material returns reciprocally) in the boiling reactor is avoided.

[0114] At the same time, inert filler 23 gravel of dioxide is added to avoid the adhesion of molten aluminum, keep the aluminum in a small-particle molten state, and enhance the mass transfer and fluidization effect. In addition, the reaction heat can increase the temperature of the titanium tetrachloride gas stream by 80 - 100 °C.

[0115] (7) High system productivity: When preparing aluminum trichloride using this system, heat is released, which can increase the temperature of the titanium tetrachloride gas stream by more than 80 °C. Then, the initial temperature of the titanium tetrachloride entering the furnace body 21 is greatly reduced, and thus the energy consumption for initially raising the temperature of the titanium tetrachloride is greatly reduced.

[0116] (8) Aluminum particles are used instead of aluminum powder, and the aluminum particles are put into the reaction device 2 by means of gravity feeding, so that the aluminum particles are more evenly distributed. The problems in the prior art, such as incomplete reaction due to uneven distribution of aluminum powder, possible entry of aluminum powder into the subsequent system and reaction in the subsequent system, damaging the equipment (a large amount of heat is released during the reaction), and the need to spray aluminum powder with a spray gun, which is prone to damage and blockage at high temperatures and is expensive, will not occur.

[0117] (9) Nitrogen can be used to reduce the impurity gas in the system. In addition, high-level gravity feeding is adopted for feeding, and only a small amount of nitrogen is used for sealing. The nitrogen consumption is 20 Nm□ / h. Compared with the nitrogen consumption of hundreds of cubic meters in some cases, the purity of chlorine is higher after the subsequent reaction, and the recycling reaction is better.

[0118] (10) Good product quality: By the way of adding chlorine in advance to the TiCl4 gas stream, the mixing is more uniform, the aluminum trichloride generated after the reaction is also more uniform, the product conversion rate is high, and the quality is stable.

[0119] As can be seen from the above, this system adopts a sealed vertical feeding device, that is, a gravity feeding device 1 and a reaction device 2, so that the aluminum particles fall into the reaction formula by gravity with the assistance of a small amount of nitrogen for sealing. The nitrogen flow rate is small, only 20 Nm□ / h at most. Compared with other feeding methods with gas volumes of hundreds of cubic meters, the content of inert gas in the subsequent gas stream is greatly reduced, which is convenient for the subsequent utilization of chlorine in titanium dioxide chloride production. At the same time, this feeding device has the characteristics of accurate feeding and not being easily blocked;

[0120] The reaction device 2 of the present application adopts the upward boiling molten aluminum method, and the molten aluminum relies only on self-heating. At the same time, the reaction chamber 212 has a structure of only adding a partition plate (distribution plate 22) in a straight cylinder, which is simple to manufacture and control. At the same time, an excessive amount of aluminum particles and an appropriate amount of chlorine gas are used, and the chlorine gas and titanium tetrachloride are premixed. The chlorine gas reacts completely, causing little corrosion to the equipment, and the equipment has a long service life. At the same time, the premixing of chlorine gas and titanium tetrachloride ensures the uniform mixing of the generated aluminum trichloride and titanium tetrachloride, and the quality of the subsequent products is stable.

[0121] Example Two

[0122] Example Two of the present application also provides a method for preparing aluminum trichloride, which uses the aluminum trichloride preparation system described in Example One above. Therefore, it has all the beneficial technical effects of this aluminum trichloride preparation system, and the same technical features and beneficial effects will not be repeated.

[0123] In this embodiment, preferably, as Figures 1 to 4 shown, the method for preparing aluminum trichloride includes the following steps:

[0124] Batching: The aluminum particles placed in the silo are controlled by a control valve and a weighing sensor to add an excessive amount of aluminum particles to the reaction device 2 by gravity according to a preset quantity;

[0125] Reaction: The aluminum particles fall into the reaction chamber 212 through the feeding port 213 of the reaction device 2. The aluminum particles melt at a preset temperature and move towards the bottom of the reaction chamber 212, and are mixed with the inert filler 23 at the bottom of the reaction chamber 212;

[0126] An appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio. The mixed gas flow first enters the gas collecting chamber 211, and then passes through the distribution plate 22 and enters the reaction chamber 212 to react with the molten aluminum.

[0127] According to the above description, this method adopts the method of sealed vertical feeding and the upward boiling molten aluminum method, so that the aluminum particles fall into the reaction chamber 212 by gravity with the assistance of a small amount of nitrogen gas for sealing. The nitrogen gas flow rate is small, only up to 20 Nm³ / h at most. Compared with other feeding methods that require gas volumes of hundreds of cubic meters, the content of inert gas in the subsequent gas flow is greatly reduced, which is convenient for the subsequent utilization of chlorine gas in titanium dioxide production. At the same time, it has the characteristics of accurate feeding and not easy to block;

[0128] In addition, the molten aluminum relies only on self-heating. Meanwhile, the reaction chamber 212 has a structure with only a partition plate (distribution plate 22) added inside a straight cylinder, which is simple to manufacture and control. At the same time, an excessive amount of aluminum particles and an appropriate amount of chlorine gas are used, and chlorine gas and titanium tetrachloride are premixed. The chlorine gas reacts completely, causing little corrosion to the equipment and resulting in a long service life of the equipment. Meanwhile, the premixing of chlorine gas and titanium tetrachloride ensures the uniform mixing of the generated aluminum trichloride and titanium tetrachloride, thereby ensuring the stable quality of the subsequent products.

[0129] In this embodiment, preferably, as Figure 3 and Figure 4 shown, an appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio. The mixed gas flow first enters the gas collection chamber 211, and then passes through the distribution plate 22 and enters the reaction chamber 212 to react with the molten aluminum, including the following steps:

[0130] An appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio. The mixed gas flow first enters the gas collection chamber 211, and then enters the reaction chamber 212 horizontally through the distribution plate 22. After the mixed gas flow enters the reaction chamber 212, it moves upward, and the flow rate of the mixed gas flow gradually decreases radially from the center towards the furnace wall.

[0131] The gas flow lifts the aluminum particles, and the aluminum particles follow the gas flow upward or suspend in the gas flow. Chlorine gas and aluminum react to form aluminum trichloride. When the gas flow rises to the upper part of the reaction chamber 212, the flow rate slows down, and the inert filler 23 and the reacted aluminum drop to the middle and lower parts of the reaction chamber 212 due to the reduced flow rate and continue to react.

[0132] The heat released by the reaction of aluminum and chlorine gas heats titanium tetrachloride, and the generated gaseous aluminum trichloride is uniformly mixed in the titanium tetrachloride gas flow and discharged from the gas outlet 216 of the reaction device 2.

[0133] According to the above description, the reaction uses the molten aluminum fluidization method to produce aluminum trichloride. Specifically, an appropriate amount of chlorine gas and hot titanium tetrachloride gas are mixed and enter from the bottom of the furnace body 21, contact and react with the molten aluminum suspended in the reaction chamber 212 to form aluminum trichloride. The generated aluminum trichloride is uniformly mixed in the titanium tetrachloride gas flow, discharged from the upper outlet, and enters the subsequent process.

[0134] In this embodiment, preferably, as Figure 2 shown, the batching includes the following steps: In the initial state, the storage bin 108 has materials and the feeding bin 110 is empty; after the batching starts, the feeding bin inlet valve 102 and the feeding bin exhaust valve 101 are both in the open state; the feeding bin discharge valve 105, the feeding bin pressurizing valve 103, the pressure charging valve 104 of the discharge pipeline, the bottom air sealing valve 106, and the purging valve 107 are all in the closed state;

[0135] The vibrating feeder 109 is started to start loading the feeding bin 110;

[0136] Close the inlet valve 102 of the feeding bin and the exhaust valve 101 of the feeding bin, open the pressurizing valve 103 of the feeding bin, pressurize the feeding bin 110, and stop pressurizing when the pressure is equal to the pressure of the reaction device 2;

[0137] During discharging, sequentially open the discharging valve 105 of the feeding bin and the air sealing valve 106 at the bottom, monitor the weighing sensor, and when the weighing no longer decreases, close the discharging valve 105 of the feeding bin, open the pressurizing valve 104 of the discharging pipeline until the air sealing valve 106 at the bottom is closed in place, and stop pressurizing after the pressure of the second flow pipeline is increased to be equal to the pressure of the reaction device 2;

[0138] Open the exhaust valve 101 of the feeding bin to discharge the gas in the feeding bin 110. After the pressure drops to atmospheric pressure, open the inlet valve 102 of the feeding bin and wait for the next batching;

[0139] Among them, the purge valve 107 is used as a spare for dredging the purge gas source 111; during the operation of the reaction device 2, the second flow pipeline is always pressurized, and the pressure of the second flow pipeline is ensured to be higher than the pressure of the reaction device 2 so that the corrosive gas in the process flow cannot enter the second flow pipeline.

[0140] According to the above description, the system adopts a static metering method. When the system starts batching, the operator inputs the corresponding batching amount according to the system load. The storage bin 108 is at atmospheric pressure, and the vibrating feeder starts to work. Through the fast-slow combination, the material is added to the feeding bin 110 to the set value. Subsequently, close the inlet valve 102 of the feeding bin, open the pressurizing valve 103 of the feeding bin to pressurize the feeding bin 110. After the pressure is the same as that in the generating device, open the discharging valve 105 of the feeding bin and the air sealing valve 106 at the bottom to complete discharging; subsequently, open the exhaust valve 101 of the feeding bin. After the pressure of the feeding bin 110 drops to atmospheric pressure, open the inlet valve 102 of the feeding bin to prepare for the next batching. And preferably, the whole system operation process is fully automatically controlled by the PLC.

[0141] It can be seen that the aluminum granule feeding adopts atmospheric pressure metering, and at the same time, large-dose and rapid feeding are carried out. The small dose at the end adopts the slow feeding method, and the metering is accurate. Using aluminum granule feeding, it is safe and easy to control (aluminum powder is explosive), the feeding pipe is not blocked, the feeding is stable and accurate, that is, high-precision batching is realized.

[0142] Furthermore, preferably, according to the set target weighing value, the feeding is carried out at 90% of the range quickly, 8% of the range slowly, and 2% of the range by jog feeding. After the metering is completed, record the weighing value.

[0143] According to the above description, it can be seen that large-dose and rapid feeding are realized in the above way, and the small dose at the end adopts the slow feeding method, and the metering is accurate.

[0144] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features; and these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A preparation system for aluminum trichloride, characterized in that, Including: A gravity feeding device, a reaction device, and a premixing device; wherein, along the height direction of the reaction device, the gravity feeding device is arranged above the reaction device and is used to add an excessive amount of aluminum pellets to the reaction device by gravity. The gravity feeding device includes a storage bin, a control valve, and a weighing sensor, and the aluminum pellets placed in the storage bin are controlled by the control valve and the weighing sensor to be added to the reaction device in a preset quantity and by gravity in an excessive amount. The premixing device includes a premixing container and a premixing flowmeter arranged on the premixing container, and is used to premix an appropriate amount of chlorine gas and aluminum tetrachloride gas according to a preset ratio. The reaction device is used to mix and react the aluminum pellets put by the gravity feeding device and the premixed gas conveyed by the premixing device to produce aluminum trichloride. The storage bin includes a storage silo, a vibrating feeder, and a feeding bin, and the storage silo, the vibrating feeder, and the feeding bin are sequentially connected and communicated along the material discharging direction; the weighing sensor is arranged at the discharge port of the feeding bin. The control valve includes a feeding bin exhaust valve, a feeding bin inlet valve, a feeding bin pressurizing valve, a charging line pressurizing valve, a feeding bin discharge valve, a bottom airtight valve, and a purging valve; wherein, the discharge port of the storage silo is connected to the feeding bin through the vibrating feeder, and the feeding bin inlet valve is arranged on the pipeline connecting the vibrating feeder and the feeding bin. The reaction device includes a furnace body and a distribution plate; wherein, an accommodation chamber is formed inside the furnace body, and the distribution plate is arranged in the accommodation chamber to divide the accommodation chamber into a gas collecting chamber and a reaction chamber which are arranged from bottom to top along its height direction. Air inlet holes are formed on the distribution plate. The distribution plate includes a bottom flat plate and a side inclined plate, and the side inclined plate is arranged around the circumferential direction of the bottom flat plate and is in a gradually expanding shape from bottom to top along the height direction of the furnace body; the side inclined plate is connected to the inner wall of the furnace body; the side inclined plate is formed with the air inlet holes, and the air inlet holes are arranged along the direction perpendicular to the height direction of the furnace body. The furnace body is formed with a transparent observation window.

2. The aluminum trichloride preparation system according to claim 1, wherein The feeding bin exhaust valve is arranged on the pipeline connecting the air port of the storage silo and the first ventilation port of the feeding bin; the discharge port at the bottom of the feeding bin is connected with a discharging pipeline, and the feeding bin discharge valve and the bottom airtight valve are sequentially arranged on the discharging pipeline, and the feeding bin discharge valve is arranged close to the feeding bin. The second ventilation port of the feeding bin is communicated with a first flow pipeline, and the end of the first flow pipeline is connected with a second flow pipeline and a third flow pipeline, and the first flow pipeline, the second flow pipeline, and the third flow pipeline are communicated with each other. The second flow pipeline is communicated with the pipeline between the feeding bin discharge valve and the bottom airtight valve, and the discharging pipeline pressurizing valve is arranged on the second flow pipeline; the third flow pipeline is communicated with an external gas source; the purging valve is arranged on the pipeline connecting the outlet end of the bottom airtight valve and the gas source.

3. The aluminum trichloride preparation system according to claim 2, characterized in that, A charging port is formed at the top of the furnace body along its height direction, and the charging port is communicated with the discharging pipeline of the charging bin, and a sealing cut-off valve is arranged between the two; An air inlet is formed on one side of the bottom of the furnace body, and the air inlet is communicated with the air collecting chamber; an air outlet is formed on one side of the top of the furnace body, and the air outlet is communicated with the reaction chamber.

4. The aluminum trichloride preparation system according to claim 3, wherein The furnace body is formed with a discharge port communicated with the bottom of the reaction chamber, and the discharge port is provided with a valve or a cover that can be opened or closed; The furnace body is formed with an inert filler charging port that can be opened or closed; A spare charging port that can be opened or closed is formed at the top of the furnace body along its height direction.

5. A method for preparing aluminum trichloride, characterized in that, Using the aluminum trichloride preparation system according to claim 1, the aluminum trichloride preparation method comprises the following steps: Batching: The aluminum particles placed in the material bin are controlled by the control valve and the weighing sensor to add an excessive amount of aluminum particles to the reaction device by gravity according to a preset quantity; Reaction: The aluminum particles fall into the reaction chamber through the charging port of the reaction device, the aluminum particles melt at a preset temperature and move towards the bottom of the reaction chamber, and are mixed with the inert filler at the bottom of the reaction chamber; An appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio. The mixed gas flow first enters the air collecting chamber, and then enters the reaction chamber through the distribution plate, and reacts with the molten aluminum.

6. The preparation method of aluminum trichloride according to claim 5, characterized in that, The step that the appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio, the mixed gas flow first enters the air collecting chamber, and then enters the reaction chamber through the distribution plate and reacts with the molten aluminum comprises the following steps: An appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio. The mixed gas flow first enters the air collecting chamber, and then enters the reaction chamber horizontally through the distribution plate. After the mixed gas flow enters the reaction chamber, it moves upward, and the flow rate of the mixed gas flow gradually decreases radially from the center towards the furnace wall; The gas flow flushes up the aluminum particles, and the aluminum particles follow the gas flow upward or suspend in the gas flow. Chlorine gas and aluminum react to form aluminum trichloride. When the gas flow rises to the upper part of the reaction chamber, the flow rate slows down, and the inert filler and the reacted aluminum drop to the middle and lower parts of the reaction chamber due to the reduced flow rate and continue to react; The reaction of aluminum and chlorine gas releases heat to heat titanium tetrachloride, and the generated gaseous aluminum trichloride is uniformly mixed in the titanium tetrachloride gas flow and discharged from the air outlet of the reaction device.

7. The preparation method of aluminum trichloride according to claim 5, characterized in that The batching comprises the following steps: In the initial state, the storage bin has materials and the charging bin is empty; after the batching starts, the charging bin inlet valve and the charging bin exhaust valve are both in the open state; the charging bin discharge valve, the charging bin pressurizing valve, the discharging pipeline pressure charging valve, the bottom air sealing valve and the purging valve are all in the closed state; The vibrating feeder is started to start loading the charging bin; The charging bin inlet valve and the charging bin exhaust valve are closed, the charging bin pressurizing valve is opened, the charging bin is pressurized, and when the pressure is equal to the pressure of the reaction device, the pressurization is stopped; During discharging, sequentially open the discharge valve of the feeding bin and the bottom air sealing valve, monitor the load cell, and when the weighing no longer decreases, close the discharge valve of the feeding bin, open the pressure charging valve of the discharge pipeline, and stop pressurizing until the bottom air sealing valve is closed in place and the pressure of the second flow pipeline is increased to equal the pressure of the reaction device; Open the exhaust valve of the feeding bin to discharge the gas in the feeding bin. After the pressure drops to atmospheric pressure, open the inlet valve of the feeding bin and wait for the next batching; Among them, the purging valve is used as a spare for dredging and purging the gas source; during the operation of the reaction device, the second flow pipeline is always pressurized, and the pressure of the second flow pipeline is ensured to be higher than the pressure of the reaction device so that the corrosive gas in the process flow cannot enter the second flow pipeline.

8. The method for preparing aluminum trichloride according to claim 7, characterized in that, In the loading step, according to the set target weighing value, adopt the method of rapid feeding at 90% of the range, slow feeding at 8% of the range, and jog feeding at 2% of the range. After the metering is completed, record the weighing value.

Citation Information

Patent Citations

  • Aluminum trichloride preparation system

    CN218422679U