CN115501818A - Aluminum trichloride preparation system and aluminum trichloride preparation method - Google Patents

Abstract

The application relates to the technical field of titanium dioxide production by a chlorination method, in particular to an aluminum trichloride preparation system and an aluminum trichloride preparation method, wherein the aluminum trichloride preparation system comprises a gravity feeding device, a reaction device and a premixing device, and the gravity feeding device is arranged above the reaction device along the height direction of the reaction device and is used for feeding excessive aluminum particles to the reaction device in a gravity mode; the gravity feeding device comprises a storage bin, a control valve and a weighing sensor, and the aluminum particles in the storage bin are controlled by the control valve and the weighing sensor to be fed into the reaction device in an excessive amount in a gravity mode; the premixing device comprises a premixing container and a premixing flowmeter arranged in the premixing container, and is used for premixing a proper amount of chlorine and aluminum tetrachloride gas according to a preset proportion; the reaction device is used for mixing and reacting the aluminum particles put in by the gravity feeding device and the premixed gas conveyed by the premixing device to prepare the aluminum trichloride.

Description

Aluminum trichloride preparation system and aluminum trichloride preparation method

Technical Field

The application relates to the technical field of titanium dioxide production by a chlorination method, in particular to an aluminum trichloride preparation system and an aluminum trichloride preparation method.

Background

In the production process of titanium dioxide by chlorination method, the core process is refined TiCl ₄ In a very short time (< 0.1 s), tiCl ₄ React with oxygen to produce TiO ₂ But TiO formed ₂ Most of anatase titanium dioxide is anatase type, in order to generate high-quality rutile titanium dioxide, a crystal transformation agent must be added, and AlCl is proved by practice ₃ Is the most excellent crystal transformation agent.

At present, the aluminum powder is generally sprayed into a reactor to directly react with a proper amount of chlorine gas to generate AlCl ₃ Simultaneously with TiCl ₄ The gas enters an oxidation reactor for reaction after being uniformly mixed. However, the following problems are common: (1) In order to ensure the spraying effect of the aluminum powder, the spray gun adopts an interlayer structure, so that the spray gun is easy to block and influence the production; (2) AluminiumThe powder is poor in distribution effect after being sprayed, incomplete in reaction, deposited and sintered by aluminum powder, and needs to be cleaned regularly, and meanwhile, unreacted aluminum powder is brought into a system to react along the way, so that equipment is damaged; (3) In order to ensure the sufficient reaction of the aluminum powder and avoid the aluminum powder from being brought into a system, excessive chlorine is often adopted, and the excessive chlorine aggravates the corrosion of the system.

Therefore, the research and development of stable and reliable AlCl preparation which does not need to clean equipment regularly and has little corrosion to the equipment is urgently needed ₃ The system of (1).

Disclosure of Invention

The application aims to provide an aluminum trichloride preparation system and an aluminum trichloride preparation method, and solves the problems that the prior art is urgently needed to develop a stable and reliable preparation AlCl which is small in equipment corrosion, does not need to clean equipment regularly and is stable and reliable to a certain extent ₃ The technical problem of the system of (2).

The application provides an aluminium trichloride preparation system includes: the device comprises a gravity feeding device, a reaction device and a premixing device; the gravity feeding device is arranged above the reaction device along the height direction of the reaction device and is used for feeding excessive aluminum particles to the reaction device in a gravity mode;

the gravity feeding device comprises a storage bin, a control valve and a weighing sensor, and the aluminum particles in the storage bin are controlled by the control valve and the weighing sensor to be fed into the reaction device in an excessive amount in a gravity mode;

the premixing device comprises a premixing container and a premixing flowmeter arranged in the premixing container, and is used for premixing a proper amount of chlorine gas and aluminum tetrachloride gas according to a preset ratio;

the reaction device is used for mixing and reacting the aluminum particles put in by the gravity feeding device and the premixed gas conveyed by the premixing device to prepare the aluminum trichloride.

In the above technical solution, further, the storage bin includes a storage bin, a vibration feeder and a feeding bin, and the storage bin, the vibration feeder and the feeding bin are sequentially communicated along a feeding direction; the weighing sensor is arranged at the discharge hole of the feeding bin.

In any of the above technical solutions, further, the control valve includes a charging bin exhaust valve, a charging bin inlet valve, a charging bin pressurization valve, a discharge pipeline pressurization valve, a charging bin discharge valve, a bottom air-sealing valve, and a purge valve; the discharge port of the storage bin is communicated with the feeding bin through the vibrating feeder, and the feeding bin inlet valve is arranged on a pipeline communicated between the vibrating feeder and the feeding bin;

the pipeline through which the air port of the storage bin is communicated with the first air port of the feeding bin is provided with the feeding bin exhaust valve; a discharge hole at the bottom of the feeding bin is connected with a discharge pipeline, a feeding bin discharge valve and a bottom air sealing valve are sequentially arranged on the discharge pipeline, and the feeding bin discharge valve is arranged close to the feeding bin;

a second vent of the feeding bin is communicated with a first circulation pipeline, the tail 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;

the second circulation pipeline is communicated with a pipeline between the charging bin discharge valve and the bottom air sealing valve, and a discharge pipeline pressure charging valve is arranged on the second circulation pipeline; the third circulation pipeline is communicated with an external air source; and the pipeline at which the outlet end of the bottom air sealing valve is communicated with the air source is provided with the purging valve.

In any of the above technical solutions, further, the reaction device includes a furnace body and a distribution plate; the distribution plate is arranged in the accommodating chamber so as to divide the accommodating chamber into a gas collecting chamber and a reaction chamber which are arranged from bottom to top along the height direction of the accommodating chamber;

an air inlet is formed on the distribution plate; a charging opening is formed at the top of the furnace body along the height direction of the furnace body, the charging opening is communicated with a discharge pipeline of the charging bin, and a sealing block valve is arranged between the charging opening and the discharge pipeline;

an air inlet is formed at one side of the bottom of the furnace body and communicated with the air collection chamber; and a gas outlet is formed at one side of the top of the furnace body and communicated with the reaction chamber.

In any of the above technical solutions, the distribution plate further includes a bottom flat plate and a side inclined plate, and the side inclined plate is disposed around the circumference of the bottom flat plate and gradually expands from bottom to top along the height direction of the furnace body; the side inclined plate is connected with the inner wall of the furnace body; the side inclined plate is provided with the air inlet, and the air inlet is arranged along the direction perpendicular to the height direction of the furnace body.

In any one of the above technical solutions, further, the furnace body is provided with a discharge port communicated with the bottom of the reaction chamber, and the discharge port is provided with a valve or a cover which can be opened or closed;

the furnace body is provided with a transparent observation window;

the furnace body is provided with an inert filler feeding port which can be opened or closed;

the top of the furnace body along the height direction is provided with a standby charging opening which can be opened or closed.

The application also provides a method for preparing aluminum trichloride, which comprises any one of the technical schemes, so that the method has all beneficial technical effects of the aluminum trichloride preparation system, and is not repeated herein.

In the above technical solution, further, the preparation method of aluminum trichloride comprises the following steps:

preparing materials: the aluminum particles in the storage bin are controlled by the control valve and the weighing sensor to be added into the reaction device in an excessive manner by gravity according to a preset quantity;

reaction: the aluminum particles fall into the reaction chamber through a charging opening of the reaction device, are melted 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;

and a proper amount of chlorine and hot titanium tetrachloride are mixed according to a ratio, and the mixed gas flow firstly enters the gas collection chamber and then enters the reaction chamber through the distribution plate to react with molten aluminum.

In any of the above technical solutions, further, the mixing of the appropriate amount of chlorine gas and hot titanium tetrachloride according to a ratio, the flow of the mixture first entering the gas collection chamber, then entering the reaction chamber through the distribution plate, and reacting with the molten aluminum includes the following steps:

mixing a proper amount of chlorine and hot titanium tetrachloride according to a ratio, wherein a mixed gas flow firstly enters the gas collection chamber and then enters the reaction chamber from the horizontal direction through the distribution plate, the mixed gas flow moves upwards after entering the reaction chamber, and the flow velocity of the mixed gas flow is gradually reduced from the center to the radial direction of the furnace wall;

the air flow rushes up the aluminum particles, the aluminum particles are upwards or suspended in the air flow along with the air flow, chlorine and aluminum react to generate aluminum trichloride, when the air flow rises to the upper part of the reaction chamber, the flow speed is reduced, the inert filler and the reacted aluminum descend to the middle lower part of the reaction chamber due to the reduction of the flow speed, and the reaction is continued;

the titanium tetrachloride is heated by the exothermic reaction of aluminum and chlorine, and the generated gaseous aluminum trichloride is uniformly mixed in the titanium tetrachloride airflow and is discharged from the air outlet of the reaction device.

In any of the above technical solutions, further, the ingredients include the following steps: in an initial state, the storage bin is filled with materials, and the feeding bin is empty; after the batching is started, the inlet valve of the feeding bin and the exhaust valve of the feeding bin are both in an open state; the charging bin discharge valve, the charging bin pressure valve, the discharge pipeline pressure charging valve, the bottom air sealing valve and the blowing valve are all in a closed state;

starting the vibration feeder to start feeding the feeding bin;

closing the inlet valve of the feeding bin and the exhaust valve of the feeding bin, opening the pressurizing valve of the feeding bin, pressurizing the feeding bin, and stopping pressurizing when the pressure is equal to the pressure of the reaction device;

during discharging, sequentially opening the charging bin discharge valve and the bottom air sealing valve, monitoring the weighing sensor, closing the charging bin discharge valve when the weighing is not reduced any more, opening the discharging pipeline pressure charging valve until the bottom air sealing valve is closed in place, and stopping pressurizing after the pressure of a second circulation pipeline is added to be equal to the pressure of the reaction device;

opening the exhaust valve of the feeding bin, exhausting the gas of the feeding bin, opening the inlet valve of the feeding bin after the pressure is reduced to normal pressure, and waiting for next material mixing;

wherein the purge valve is used as a dredging purge gas source for standby; in the working process of the reaction device, the second circulation pipeline is pressurized all the time, and the pressure of the second circulation pipeline is higher than that of the reaction device, so that corrosive gas in the process flow cannot enter the second circulation pipeline.

In any of the above technical solutions, further, in the step of charging, according to a set target weighing value, a mode of 90% range fast feeding, 8% range slow feeding, and 2% range inching feeding is adopted, and after metering is completed, a weighing value is recorded.

Compared with the prior art, the beneficial effect of this application is:

the application provides an aluminium trichloride preparation system sets gravity feeding device, can realize the accurate unloading of gravity type through gravity feeding device, and then can not take place among the prior art and adopt the spray gun to spray various problems that exist in the reinforced mode of aluminite powder, for example block up the spray gun, the problem that needs regular cleaning etc..

In addition, use the aluminium shot to replace the aluminium powder, put into reaction unit with the aluminium shot through the mode of gravity input moreover for the aluminium shot distributes more evenly, because of aluminium powder maldistribution among the prior art can not appear, the reaction is incomplete, and the aluminium powder can be brought into follow-up system, reacts in follow-up system, damages equipment (the reaction is a large amount of exothermic), and the aluminium powder needs the spray gun to spout into, and the spray gun is easy to be damaged easily under the high temperature and is blocked up, and problem that the price is expensive.

In addition, the method that aluminum is excessive and is matched with chlorine and titanium tetrachloride gas to be accurately proportioned through a premixing device, namely, the chlorine is proper is adopted, so that the chlorine is ensured to completely react, and the corrosion to equipment is reduced; meanwhile, the chlorine gas and the titanium tetrachloride gas are premixed, so that the generated aluminum trichloride is uniformly mixed in the titanium tetrachloride gas flow, and the stability of the quality of subsequent products is ensured.

The method adopts a sealing vertical feeding method and an upward boiling molten aluminum method, so that aluminum particles fall into a reaction chamber by gravity under the assistance of a small amount of nitrogen and the maximum nitrogen flow is only 20Nm 9633h, and/h, compared with the method adopting other feeding methods, the method always adopts hundreds of gas flows, greatly reduces the content of inert gas in subsequent gas flows, is convenient for the subsequent utilization of chlorine in the production of titanium white chloride, and has the characteristics of accurate feeding and difficult blockage;

in addition, the molten aluminum only depends on self-heating, meanwhile, the reaction chamber is only in a structure of adding a partition plate (distribution plate) in a straight cylinder, the manufacture and the control are simple, meanwhile, the method of adopting excessive aluminum particles and proper amount of chlorine and premixing the chlorine and titanium tetrachloride is adopted, the chlorine completely reacts, the corrosion to equipment is small, and the service life of the equipment is long; meanwhile, the chlorine and the titanium tetrachloride are mixed in advance, so that the generated aluminum trichloride and the titanium tetrachloride are uniformly mixed, and the stable quality of subsequent products is further ensured.

Drawings

In order to more clearly illustrate the detailed description of the present application or the technical solutions in the prior art, the drawings used in the detailed description or the prior art description will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts.

FIG. 1 is a schematic structural diagram of an aluminum trichloride production system provided in an embodiment of the present application;

FIG. 2 is a schematic structural diagram of a gravity feeding device provided in an embodiment of the present application;

FIG. 3 is a schematic structural diagram of a reaction apparatus provided in an embodiment of the present application;

fig. 4 is a schematic view of an internal gas circulation structure of a reaction apparatus provided in an embodiment of the present application.

Reference numerals:

1-gravity feeding device, 101-feeding bin exhaust valve, 102-feeding bin inlet valve, 103-feeding bin pressure valve, 104-discharging pipeline pressure valve, 105-feeding bin discharge valve, 106-bottom air sealing valve, 107-purging valve, 108-storage bin, 109-vibration feeder, 110-feeding bin, 111-air source;

2-reaction device, 21-furnace body, 211-gas collection chamber, 212-reaction chamber, 213-charging hole, 214-spare charging hole, 215-gas inlet, 216-gas outlet, 217-discharge hole, 218-transparent observation window, 219-inert filler charging hole, 22-distribution plate, 221-bottom flat plate, 222-side inclined plate and 23-inert filler.

Detailed Description

The technical solutions of the present application will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are only some embodiments of the present application, but not all embodiments.

The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present application, as presented in the figures, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application.

All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

In the description of the present application, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a particular orientation, be constructed in a particular orientation, and operate, and thus should not be construed as limiting the present application. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.

In the description of the present application, it should be noted that, unless otherwise explicitly stated or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, a fixed connection, a detachable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in this application will be understood to be a specific case for those of ordinary skill in the art.

An aluminum trichloride production system and an aluminum trichloride production method according to some embodiments of the present application will be described below with reference to fig. 1 to 4.

Example one

Referring to fig. 1, an embodiment of the present application provides an aluminum trichloride production system, including: a gravity feeding device 1, a reaction device 2 and a premixing device (note: 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 for feeding excessive aluminum particles to the reaction device 2 in a gravity mode;

the gravity feeding device 1 comprises a storage bin, a control valve and a weighing sensor, and the aluminum particles in the storage bin are controlled by the control valve and the weighing sensor to be fed into the reaction device 2 in an excessive amount in a gravity mode;

the premixing device comprises a premixing container and a premixing flowmeter arranged in the premixing container, and is used for premixing a proper amount of chlorine and aluminum tetrachloride gas according to a preset proportion;

the reaction device 2 is used for mixing and reacting the aluminum particles put in by the gravity feeding device 1 and the premixed gas conveyed by the premixing device to prepare the aluminum trichloride.

Based on the structure that has just been described, the aluminium trichloride preparation system that this application provided sets up gravity feeding device 1, can realize gravity type's accurate unloading through gravity feeding device 1, and then can not take place the various problems that exist in the mode that adopts the spray gun to spray aluminium powder reinforced among the prior art, for example block up the spray gun, the problem that needs regular cleaning etc..

In addition, use the aluminium shot to replace the aluminium powder, put into reaction unit 2 through the mode of gravity input moreover with the aluminium shot for the aluminium shot distributes more evenly, because of aluminium powder maldistribution among the prior art can not appear, the reaction is incomplete, and the aluminium powder can be brought into follow-up system, reacts in follow-up system, damages equipment (the reaction is released heat in a large number), and the aluminium powder needs the spray gun to spout into, and the easy stifled easy of spray gun is damaged under the high temperature, and problem that the price is expensive.

In addition, the method that aluminum is excessive and the chlorine and titanium tetrachloride are matched to be accurately proportioned through a premixing device, namely, the chlorine is in a proper amount is adopted, so that the chlorine is ensured to react completely, and the corrosion to equipment is reduced; meanwhile, the chlorine gas and the titanium tetrachloride gas are premixed, so that the generated aluminum trichloride is uniformly mixed in the titanium tetrachloride gas flow, and the stability of the quality of subsequent products is ensured.

In this embodiment, preferably, as shown in fig. 2, the storage bin includes a storage bin 108, a vibratory feeder 109 and a feeding bin 110, and the storage bin 108, the vibratory feeder 109 and the feeding bin 110 are sequentially communicated along the blanking direction; the weighing sensor is arranged at the discharge hole of the feeding bin 110.

According to the above-described structure, the storage bin 108 is used for pre-placing materials, i.e. aluminum particles, the vibration feeder 109 is used for providing vibration to facilitate feeding, and the feeding bin 110 is used for feeding the materials subjected to vibration feeding to the reaction device 2.

Further, preferably, the vibration feeder 109 is an electric vibration feeder.

In this embodiment, preferably, as shown in fig. 2, the control valves include a feed bin vent valve 101, a feed bin inlet valve 102, a feed bin pressurization valve 103, a discharge line pressurization valve 104, a feed bin discharge valve 105, a bottom seal valve 106, and a purge valve 107; wherein, the discharge port of the storage bin 108 is communicated with the feeding bin 110 through the vibration feeder 109, and the feeding bin inlet valve 102 is arranged on the pipeline communicated between the vibration feeder 109 and the feeding bin 110;

a charging bin exhaust valve 101 is arranged on a pipeline which is communicated with a first air vent of the charging bin 110 through an air port of the storage bin 108; a discharge port at the bottom of the feeding bin 110 is connected with a discharge pipeline, 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;

a first circulation pipeline is communicated with a second vent of the feeding bin 110, the tail 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;

the second circulation pipeline is communicated with a pipeline between the charging bin discharge valve 105 and the bottom air sealing valve 106, and a discharge pipeline pressure charging 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 purge valve 107 is arranged on a pipeline of which the outlet end of the bottom gas seal valve 106 is communicated with a gas source 111.

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

in the initial state, the storage bin 108 is filled with materials, and the feeding bin 110 is empty; after the batching is started, the inlet valve 102 of the feeding bin and the exhaust valve 101 of the feeding bin are both in an opening state; the charging bin discharging valve 105, the charging bin pressurizing valve 103, the discharging pipeline pressurizing valve 104, the bottom gas sealing valve 106 and the purging valve 107 are all in a closed state;

starting the vibration feeder 109, starting to feed the feeding bin 110, and feeding according to the following rule, wherein according to a set target weighing value, a mode of fast feeding in 90% range, slow feeding in 8% range and inching feeding in 2% range is adopted, and after metering is finished, a weighing value is recorded;

closing the inlet valve 102 and the exhaust valve 101 of the feeding bin, opening the pressurizing valve 103 of the feeding bin, pressurizing the feeding bin 110, and stopping pressurizing when the pressure is equal to the pressure of the reaction device 2;

during discharging, the charging bin discharging valve 105 and the bottom air sealing valve 106 are sequentially opened, the weighing sensor is monitored, when the weighing is not reduced any more, the charging bin discharging valve 105 is closed, the discharging pipeline charging 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 added to be equal to the pressure of the reaction device 2, the pressurization is stopped;

and opening an exhaust valve 101 of the feeding bin, exhausting the gas of the feeding bin 110, and opening an inlet valve 102 of the feeding bin after the pressure is reduced to the normal pressure to wait for next material preparation.

That is, the system adopts a static metering mode, when the system starts to perform material mixing, an operator inputs corresponding material mixing amount according to system load, the storage bin 108 is at normal pressure, the vibration feeder starts to work, materials are added into the feeding bin 110 to a set value through fast-slow combination, then the inlet valve 102 of the feeding bin is closed, the pressurizing valve 103 of the feeding bin is opened to pressurize the feeding bin 110, and after the pressures in the generating device are the same, the discharging valve 105 of the feeding bin and the bottom air sealing valve 106 are opened to finish material discharging; then, the charging bin exhaust valve 101 opens the charging bin inlet valve 102 after the pressure of the charging bin 110 is reduced to normal pressure, so as to prepare for next batching, and preferably, the whole system operation process is fully automatically controlled by PLC.

Therefore, the aluminum particles are metered at normal pressure, large-dose and quick blanking is carried out simultaneously, small-dose at the tail end is fed slowly, and metering is accurate. The aluminum particles are used for feeding, the method is safe and easy to control (aluminum powder is easy to explode), the blanking pipe is not blocked, the feeding is stable and accurate, and high-precision batching is realized.

Note that: wherein, the purge valve 107 is used as a dredging purge gas source 111 for standby; in the working process of the reaction device 2, the pressure of the second circulation pipeline is always ensured to be higher than the pressure of the reaction device 2, so that corrosive gas in the process flow cannot enter the second circulation pipeline.

In this embodiment, preferably, as shown in fig. 3, the reaction apparatus 2 includes a furnace body 21 and a distribution plate 22; wherein, an accommodating chamber is formed inside the furnace body 21, and the distribution plate 22 is arranged in the accommodating chamber to divide the accommodating chamber into a gas collecting chamber 211 and a reaction chamber 212 which are arranged from bottom to top along the height direction of the accommodating chamber;

an air inlet is formed on the distribution plate 22; a feed inlet 213 is formed at the top of the furnace body 21 along the height direction thereof, the feed inlet 213 is communicated with the discharge pipeline of the feed bin 110, and a sealing cut-off valve is arranged between the feed inlet 213 and the discharge pipeline, and when the feeding to the reaction device 2 is completed, the sealing cut-off valve can be closed to ensure the sealing property;

an air inlet 215 is formed at one side of the bottom of the furnace body 21, and the air inlet 215 is communicated with the air collecting chamber 211; an air outlet 216 is formed at one side of the top of the furnace body 21, and the air outlet 216 communicates with the reaction chamber 212.

From the above-described structure, the reaction apparatus 2 operates as follows:

the aluminum particles fall into the reaction chamber 212 through the feed opening 213 of the reaction apparatus 2, and the aluminum particles melt at a predetermined temperature and move toward the bottom of the reaction chamber 212 (the predetermined reaction temperature is about 450 ℃), and are mixed with the inert filler 23 at the bottom of the reaction chamber 212;

mixing a proper amount of chlorine and hot titanium tetrachloride according to a ratio (the temperature of the titanium tetrachloride is 350-400 ℃), wherein a mixed gas flow firstly enters a gas collection chamber 211 and then enters a reaction chamber 212 from the horizontal direction through a distribution plate 22, the mixed gas flow moves upwards after entering the reaction chamber 212, and the flow speed of the mixed gas flow is gradually reduced from the center to the radial direction of a furnace wall;

the air flow rushes up the aluminum particles, the aluminum particles are upwards or suspended in the air flow along with the air flow, the chlorine and the aluminum react to generate aluminum trichloride, when the air flow rises to the upper part of the reaction chamber 212, the flow rate is reduced, the inert filler 23 and the reacted aluminum descend to the middle lower part of the reaction chamber 212 due to the reduction of the flow rate, and the reaction continues (see fig. 4);

the exothermic reaction of aluminum and chlorine heats titanium tetrachloride (to 450-480 ℃, and aluminum is melted by the exothermic subsequent reaction, thereby saving energy), and 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.

It can be seen that the reaction employs a molten aluminum fluidization method to produce aluminum trichloride, specifically, chlorine gas and hot titanium tetrachloride gas enter from the bottom of the furnace body 21 after being mixed, and contact with molten aluminum suspended in the reaction chamber 212 to react to produce aluminum trichloride, which is uniformly mixed in the titanium tetrachloride gas flow, discharged through the upper outlet, and enters the subsequent process.

In this embodiment, preferably, as shown in fig. 3, the distribution plate 22 includes a bottom plate 221 and a side inclined plate 222, and the side inclined plate 222 is disposed around the circumference of the bottom plate 221 and is gradually enlarged 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.

According to the structure described above, the side inclined plate 222 is less prone to blockage than a common flat screen plate, specifically, the air inlet hole is horizontal, and materials cannot enter the air inlet hole and the air collection chamber 211. Meanwhile, after the gas enters the reaction chamber 212 through the gas inlet holes, the gas is concentrated towards the center due to inertia, the flow rate of central gas flow is high, the flow rate close to the furnace wall is low, after aluminum particles are blown out for reaction, unreacted materials move downwards at the position close to the wall due to average flow rate at the upper part of the reaction chamber 212, and the unreacted materials are blown out for reaction again when the unreacted materials descend to the bottom, so that circulation is formed, and the reaction is more complete. Meanwhile, the common phenomenon of slugging (the material is pushed to move upwards due to small diameter and high height and large airflow, the airflow is broken at a certain height, and the material returns to and fro) of the boiling reactor is avoided.

Meanwhile, 23 gravels of the inert filler of the titanium dioxide are added to avoid the adhesion of molten aluminum, so that the aluminum is kept in a small-particle molten state, the mass transfer fluidization effect is improved, and in addition, the reaction heat can improve the temperature of the titanium tetrachloride airflow by 80-100 ℃.

In this embodiment, preferably, as shown in FIG. 3, 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.

According to the above-described structure, when the production is completed, the remaining aluminum particles can be discharged through the discharge opening 217.

Further, it is preferable that the discharge port 217 is formed by a length of a pipe member, one end of which is inserted into the bottom wall of the reaction chamber 212 and the other end of which extends to the outside through the bottom wall of the furnace body 21, and it is preferable that the pipe member is welded to the bottom wall of the reaction chamber 212 and the bottom wall of the furnace body 21, respectively.

In this embodiment, preferably, as shown in fig. 3, the furnace body 21 is formed with a transparent viewing window 218.

According to the above-described structure, the transparent viewing window 218 allows the reaction conditions inside the reaction apparatus 2 to be clearly seen, that is, the reaction conditions and the bed height inside the reaction apparatus 2 can be seen through the transparent viewing window 218, thereby avoiding the occurrence of insufficient aluminum particles or inert filler 23.

Further, it is preferable that the transparent observation window 218 is provided at a middle position of the furnace body 21, and it is preferable that the furnace body 21 is formed with an observation port extending obliquely upward, and a sight glass is provided at a top of the observation port.

In this embodiment, preferably, as shown in fig. 3, the furnace body 21 is formed with an inert filler feed port 219 that can be opened or closed.

According to the above-described structure, the inert filler 23 is fed into the reaction chamber 212 through the inert filler feed port 219, and the inert filler 23 divides the molten aluminum into small particles, so that the contact area between the aluminum and the chlorine gas is enlarged while preventing the adhesion, and the reaction rate is increased.

Further, it is preferable that the furnace body 21 is formed with a pipe portion extending obliquely upward, and an opening and closing valve or a cap is provided at the nozzle.

Further, it is preferable that the inert filler 23 is a solid particle such as silica or a zirconium-aluminum composite ball which does not react with high-temperature chlorine gas or titanium tetrachloride.

In this embodiment, it is preferable that, as shown in fig. 3, the top of the furnace body 21 in the height direction thereof is formed with a spare charge port 214 that can be opened or closed, and it is preferable that the opening or closing of the spare charge port 214 can be previously performed by using an on-off valve or a lid.

According to the above-described structure, when a problem occurs in the feed port 213 of the reaction apparatus 2, the auxiliary feed port 214 can be opened for use.

In conclusion, the aluminum trichloride preparation system that this application provided has following advantage:

(1) The method of excessive aluminum particles and proper chlorine is adopted to ensure complete reaction of the chlorine and avoid corrosion of the system caused by the redundant chlorine, thereby being beneficial to prolonging the service life of the equipment.

(2) The reaction conditions of the reactor are clearly visible: the reaction condition and the bed height in the reactor can be seen through the sight glass at the middle part, and the condition that the aluminum particles or the inert filler 23 is insufficient is avoided.

(3) Corrosive gas does not cross, and 110 leakproofness of reinforced storehouse is good: during the reaction, be equipped with nitrogen gas and seal, gravity feeding device 1's pressure is higher than the inside pressure of reaction unit 2 simultaneously, and gas is not anti-cluster during the feeding, and equipment continuous operation is effectual.

(4) The feeding is stable, and the blockage is not easy: the aluminum particles are fed by normal pressure metering, meanwhile, the large dosage is fed quickly, the small dosage at the tail end is fed slowly, the metering is accurate, and in addition, the feeding by the aluminum particles is safe and easy to control (aluminum powder is explosive), is not blocked and is stable and accurate.

(5) The gas collecting chamber 211 is not easy to be blocked: compared with a common flat screen plate, the air inlet hole is horizontal, and materials cannot enter the air inlet hole and the air collecting chamber 211.

(6) Compared with a common flat screen plate, the side inclined plate 222 is not easy to block, in addition, the air inlet hole is horizontal, and materials cannot enter the air inlet hole and the air collection chamber 211. Meanwhile, after the gas enters the reaction chamber 212 through the gas inlet holes, the gas is concentrated towards the center due to inertia, the flow rate of central gas flow is high, the flow rate close to the furnace wall is low, after aluminum particles are blown out for reaction, unreacted materials move downwards at the position close to the wall due to average flow rate at the upper part of the reaction chamber 212, and the unreacted materials are blown out for reaction again when the unreacted materials descend to the bottom, so that circulation is formed, and the reaction is more complete. Meanwhile, the phenomenon of common slugging (the material is pushed to move upwards due to small diameter and high height and large airflow, the airflow is broken at a certain height, and the material returns to reciprocate) of the boiling reactor is avoided.

Meanwhile, 23 gravels of the inert filler of the dioxide are added to avoid the bonding of the molten aluminum, so that the aluminum is kept in a small particle molten state, the mass transfer fluidization effect is improved, and in addition, the reaction heat can improve the temperature of the titanium tetrachloride airflow by 80-100 ℃.

(7) The system has high productivity: when the system is used for preparing aluminum trichloride, heat is released, the temperature of titanium tetrachloride airflow can be increased by over 80 ℃, so that the temperature of titanium tetrachloride initially entering a furnace body 21 is greatly reduced, and the energy consumption for increasing the temperature of titanium tetrachloride at the initial stage is further greatly reduced.

(8) Use aluminium grain to replace the aluminite powder, put into reaction unit 2 through the mode of gravity input moreover with the aluminium grain for the aluminium grain distributes more evenly, because of aluminium powder maldistribution among the prior art can not appear, the reaction is incomplete, and the aluminium powder can be brought into follow-up system, reacts in follow-up system, damages equipment (the reaction is a large amount of exothermic), and the aluminium powder needs the spray gun to spout into, and the spray gun is easy to be damaged easily under the high temperature and is blocked up, and problem that the price is expensive.

(9) The nitrogen can be used for reducing the impurity gas of the system, in addition, the feeding adopts high-position gravity feeding, only a small amount of nitrogen is used for sealing, the nitrogen dosage is 20Nm 9633h, compared with the nitrogen with hundreds of square in a short period, the purity of the chlorine is higher after the subsequent reaction, and the recycling reaction is good.

(10) The product quality is good: the mode of adding the TiCl4 airflow into the chlorine in advance is adopted, so that the mixing is more uniform, the aluminum trichloride generated after the reaction is more uniform, the product conversion rate is high, and the quality is stable.

The system adopts the sealed vertical feeding device, namely the gravity feeding device 1 and the reaction device 2, so that the aluminum particles fall into a reaction type by gravity under the auxiliary sealing of a small amount of nitrogen, the nitrogen flow is less, the maximum is only 20Nm 9633h/h, compared with the gas flow which is hundreds of times when other feeding methods are adopted, the content of inert gas in subsequent gas flow is greatly reduced, the subsequent utilization of chlorine in the production of titanium white chloride is facilitated, and meanwhile, the feeding device has the characteristics of accurate feeding and difficult blockage;

the reaction device 2 adopts an upward boiling molten aluminum method, molten aluminum only depends on self-heating, meanwhile, the reaction chamber 212 is only in a structure that a partition plate (distribution plate 22) is added in a straight cylinder, the manufacture and the control are simple, meanwhile, a method that aluminum particles are excessive, chlorine is proper and the chlorine and titanium tetrachloride are premixed is adopted, the chlorine completely reacts, the corrosion to equipment is small, and the service life of the equipment is long; meanwhile, the chlorine and the titanium tetrachloride are mixed in advance, so that the generated aluminum trichloride and the titanium tetrachloride are uniformly mixed, and the quality of subsequent products is stable.

Example two

An embodiment two of this application still provides an aluminum trichloride preparation method, utilizes above-mentioned embodiment one the aluminum trichloride preparation system, therefore, has all beneficial technological effects of this aluminum trichloride preparation system, and same technical characteristics and beneficial effect are no longer repeated.

In this embodiment, preferably, as shown in fig. 1 to 4, the method for producing aluminum trichloride includes the steps of:

preparing materials: the aluminum particles in the storage bin are controlled by a control valve and a weighing sensor to be added into the reaction device 2 in a gravity mode according to a preset quantity;

reaction: the aluminum particles fall into the reaction chamber 212 through the feed opening 213 of the reaction device 2, and the aluminum particles melt at a preset temperature and move towards the bottom of the reaction chamber 212 to be mixed with the inert filler 23 at the bottom of the reaction chamber 212;

a proper amount of chlorine gas and hot titanium tetrachloride are mixed according to the proportion, and the mixed gas flow firstly enters the gas collection chamber 211 and then enters the reaction chamber 212 through the distribution plate 22 to react with the molten aluminum.

According to the description, the method adopts a sealing vertical feeding method and an upward boiling molten aluminum method, so that aluminum particles fall into the reaction chamber 212 under the assistance of a small amount of nitrogen under sealing by gravity, the nitrogen flow is small, the maximum nitrogen flow is only 20Nm 9633h/h, compared with the gas flow of hundreds of directions in other feeding methods, the content of inert gas in subsequent gas flow is greatly reduced, the subsequent utilization of chlorine in titanium white chloride production is facilitated, and meanwhile, the method has the characteristics of accurate feeding and difficult blockage;

in addition, the molten aluminum is only self-heated, meanwhile, the reaction chamber 212 is only in a structure of adding a partition plate (distribution plate 22) in a straight cylinder, the manufacture and the control are simple, meanwhile, the method of excessive aluminum particles, proper amount of chlorine and premixing of the chlorine and titanium tetrachloride is adopted, the chlorine completely reacts, the corrosion to equipment is small, and the service life of the equipment is long; meanwhile, the chlorine and the titanium tetrachloride are mixed in advance, so that the generated aluminum trichloride and the titanium tetrachloride are uniformly mixed, and the stable quality of subsequent products is further ensured.

In this embodiment, preferably, as shown in fig. 3 and 4, the mixing of the appropriate amount of chlorine gas with the hot titanium tetrachloride is carried out in a ratio such that the mixed gas first enters the plenum chamber 211 and then enters the reaction chamber 212 through the distribution plate 22 to react with the molten aluminum, which comprises the following steps:

mixing a proper amount of chlorine and hot titanium tetrachloride according to a ratio, wherein a mixed gas flow firstly enters a gas collection chamber 211 and then enters a reaction chamber 212 from the horizontal direction through a distribution plate 22, the mixed gas flow moves upwards after entering the reaction chamber 212, and the flow velocity of the mixed gas flow is gradually reduced from the center to the radial direction of a furnace wall;

the air flow rushes up the aluminum particles, the aluminum particles are upwards or suspended in the air flow along with the air flow, the chlorine and the aluminum react to generate aluminum trichloride, when the air flow rises to the upper part of the reaction chamber 212, the flow rate is reduced, the inert filler 23 and the reacted aluminum descend to the middle lower part of the reaction chamber 212 due to the reduction of the flow rate, and the reaction is continued;

the exothermic reaction between aluminum and chlorine heats titanium tetrachloride, and the resulting gaseous aluminum trichloride is uniformly mixed in the titanium tetrachloride gas stream and discharged from the outlet 216 of the reaction apparatus 2.

As can be seen from the above description, the reaction produces aluminum trichloride by a molten aluminum fluidization method, specifically, an appropriate amount of chlorine gas and hot titanium tetrachloride gas are mixed and enter from the bottom of the furnace body 21, and contact-react with molten aluminum suspended in the reaction chamber 212 to produce aluminum trichloride, which is uniformly mixed in the titanium tetrachloride gas flow, discharged through the upper outlet, and enters the subsequent process.

In this embodiment, preferably, as shown in fig. 2, the dosing comprises the steps of: in the initial state, the storage bin 108 is filled with materials, and the feeding bin 110 is empty; after the material preparation starts, the inlet valve 102 of the feeding bin and the exhaust valve 101 of the feeding bin are both in an open state; the charging bin discharging valve 105, the charging bin pressurizing valve 103, the discharging pipeline pressurizing valve 104, the bottom gas sealing valve 106 and the purging valve 107 are all in a closed state;

the vibratory feeder 109 is started to start charging the feed bin 110;

closing the inlet valve 102 and the exhaust valve 101 of the feeding bin, opening the pressurizing valve 103 of the feeding bin, pressurizing the feeding bin 110, and stopping pressurizing when the pressure is equal to the pressure of the reaction device 2;

during discharging, the charging bin discharging valve 105 and the bottom air sealing valve 106 are sequentially opened, the weighing sensor is monitored, when the weighing is not reduced any more, the charging bin discharging valve 105 is closed, the discharging pipeline pressurizing valve 104 is opened until the bottom air sealing valve 106 is closed in place, and after the pressure of the second circulating pipeline is added to be equal to the pressure of the reaction device 2, the pressurization is stopped;

opening a charging bin exhaust valve 101, exhausting gas in a charging bin 110, opening a charging bin inlet valve 102 after the pressure is reduced to normal pressure, and waiting for next batching;

wherein, the purge valve 107 is used as a dredging purge gas source 111 for standby; in the working process of the reaction device 2, the second flow pipeline is pressurized all the time, and the pressure of the second flow pipeline is ensured to be higher than that of the reaction device 2, so that corrosive gas in the process flow cannot enter the second flow pipeline.

According to the above description, the system adopts a static metering mode, when the system starts to perform material mixing, an operator inputs corresponding material mixing amount according to the system load, the storage bin 108 is at normal pressure, the vibration feeder starts to work, materials are added into the feeding bin 110 to a set value through fast-slow combination, then the inlet valve 102 of the feeding bin is closed, the pressurizing valve 103 of the feeding bin is opened to pressurize the feeding bin 110, and after the pressures in the generating device are the same, the discharging valve 105 of the feeding bin and the bottom air sealing valve 106 are opened to complete material discharging; then, the charging bin exhaust valve 101 opens the charging bin inlet valve 102 after the pressure of the charging bin 110 is reduced to normal pressure, so as to prepare for next batching, and preferably, the whole system operation process is fully automatically controlled by PLC.

Therefore, the aluminum particle feeding adopts normal pressure metering, simultaneously, the large-dose and quick feeding is carried out, the small-dose tail end adopts a slow feeding mode, and the metering is accurate. The feeding of aluminum particles is safe and easy to control (aluminum powder is easy to explode), the blanking pipe is not blocked, the feeding is stable and accurate, and the high-precision batching is realized.

Further, preferably, according to a set target weighing value, a mode of 90% range fast feeding, 8% range slow feeding and 2% range inching feeding is adopted, and after metering is completed, the weighing value is recorded.

According to the above description, the high-dose and quick blanking is realized, the slow blanking mode is adopted for the small dose at the tail end, and the metering is accurate.

Finally, it should be noted that: the above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present application.

Claims (10)

1. An aluminum trichloride production system characterized by comprising: the device comprises a gravity feeding device, a reaction device and a premixing device; the gravity feeding device is arranged above the reaction device along the height direction of the reaction device and is used for feeding excessive aluminum particles to the reaction device in a gravity mode;

the gravity feeding device comprises a storage hopper, a control valve and a weighing sensor, and the aluminum particles in the storage hopper are controlled by the control valve and the weighing sensor to feed excessive aluminum particles to the reaction device in a gravity mode according to a preset quantity;

the premixing device comprises a premixing container and a premixing flowmeter arranged in the premixing container, and is used for premixing a proper amount of chlorine and aluminum tetrachloride gas according to a preset proportion;

the reaction device is used for mixing and reacting the aluminum particles put in by the gravity feeding device and the premixed gas conveyed by the premixing device to prepare the aluminum trichloride.

2. The aluminum trichloride preparation system according to claim 1, wherein the storage bin comprises a storage bin, a vibrating feeder and a feeding bin, and the storage bin, the vibrating feeder and the feeding bin are communicated in sequence along a feeding direction; the weighing sensor is arranged at the discharge hole of the feeding bin.

3. The system for preparing aluminum trichloride according to claim 2, wherein the control valve comprises a charging bin exhaust valve, a charging bin inlet valve, a charging bin pressurizing valve, a discharging pipeline pressurizing valve, a charging bin discharging valve, a bottom air sealing valve and a purging valve; the discharge port of the storage bin is communicated with the feeding bin through the vibrating feeder, and the feeding bin inlet valve is arranged on a pipeline communicated between the vibrating feeder and the feeding bin;

the pipeline through which the air port of the storage bin is communicated with the first air port of the feeding bin is provided with the feeding bin exhaust valve; a discharge hole at the bottom of the feeding bin is connected with a discharge pipeline, a feeding bin discharge valve and a bottom air sealing valve are sequentially arranged on the discharge pipeline, and the feeding bin discharge valve is arranged close to the feeding bin;

a first circulation pipeline is communicated with a second vent of the feeding bin, the tail 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;

the second circulation pipeline is communicated with a pipeline between the charging bin discharge valve and the bottom air sealing valve, and a discharge pipeline pressure charging valve is arranged on the second circulation pipeline; the third circulation pipeline is communicated with an external air source; and the purging valve is arranged on a pipeline for communicating the outlet end of the bottom air sealing valve with the air source.

4. The aluminum trichloride preparation system according to claim 3, wherein the reaction apparatus comprises a furnace body and a distribution plate; the distribution plate is arranged in the accommodating chamber so as to divide the accommodating chamber into a gas collecting chamber and a reaction chamber which are arranged from bottom to top along the height direction of the accommodating chamber;

an air inlet is formed on the distribution plate; a charging opening is formed at the top of the furnace body along the height direction of the furnace body, the charging opening is communicated with a discharging pipeline of the charging bin, and a sealing block valve is arranged between the charging opening and the discharging pipeline;

an air inlet is formed at one side of the bottom of the furnace body and communicated with the air collection chamber; and a gas outlet is formed at one side of the top of the furnace body and communicated with the reaction chamber.

5. The aluminum trichloride preparation system according to claim 4, wherein the distribution plate includes a bottom flat plate and a side inclined plate, and the side inclined plate is disposed around the circumference of the bottom flat plate and is gradually enlarged from bottom to top along the height direction of the furnace body; the side inclined plate is connected with the inner wall of the furnace body; the side inclined plate is provided with the air inlet, and the air inlet is arranged along the direction perpendicular to the height direction of the furnace body.

6. The aluminum trichloride production system according to claim 4,

the furnace body is provided with a discharge port communicated with the bottom of the reaction chamber, and the discharge port is provided with a valve or a sealing cover which can be opened or closed;

the furnace body is provided with a transparent observation window;

the furnace body is provided with an inert filler feeding port which can be opened or closed;

the top of the furnace body along the height direction is provided with a standby charging opening which can be opened or closed.

7. A method for producing aluminum trichloride, characterized by using the system for producing aluminum trichloride according to claim 5, and comprising the steps of:

preparing materials: the aluminum particles in the storage bin are controlled by the control valve and the weighing sensor to be added into the reaction device in an excessive manner by gravity according to a preset quantity;

reaction: the aluminum particles fall into the reaction chamber through a charging opening of the reaction device, are melted 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;

and a proper amount of chlorine and hot titanium tetrachloride are mixed according to a ratio, and the mixed gas flow firstly enters the gas collection chamber and then enters the reaction chamber through the distribution plate to react with molten aluminum.

8. The method for preparing aluminum trichloride according to claim 7, wherein the appropriate amount of chlorine gas is mixed with hot titanium tetrachloride according to a ratio, and the mixed gas flow firstly enters the gas collection chamber and then enters the reaction chamber through the distribution plate to react with molten aluminum, and the method comprises the following steps:

mixing a proper amount of chlorine and hot titanium tetrachloride according to a ratio, wherein a mixed gas flow firstly enters the gas collection chamber and then enters the reaction chamber from the horizontal direction through the distribution plate, the mixed gas flow moves upwards after entering the reaction chamber, and the flow velocity of the mixed gas flow is gradually reduced from the center to the radial direction of the furnace wall;

the air flow rushes up the aluminum particles, the aluminum particles are upwards or suspended in the air flow along with the air flow, chlorine and aluminum react to generate aluminum trichloride, when the air flow rises to the upper part of the reaction chamber, the flow speed is reduced, the inert filler and the reacted aluminum descend to the middle lower part of the reaction chamber due to the reduction of the flow speed, and the reaction is continued;

the titanium tetrachloride is heated by the exothermic reaction of the aluminum and the chlorine, and the generated gaseous aluminum trichloride is uniformly mixed in the titanium tetrachloride airflow and is discharged from the air outlet of the reaction device.

9. The method of claim 7, wherein the compounding comprises the steps of: in an initial state, the storage bin is filled with materials, and the feeding bin is empty; after the material preparation is started, the inlet valve of the feeding bin and the exhaust valve of the feeding bin are both in an opening state; the charging bin discharge valve, the charging bin pressure valve, the discharge pipeline pressure valve, the bottom air sealing valve and the purging valve are all in a closed state;

starting the vibration feeder to start feeding the feeding bin;

closing the inlet valve of the feeding bin and the exhaust valve of the feeding bin, opening the pressurizing valve of the feeding bin, pressurizing the feeding bin, and stopping pressurizing when the pressure is equal to the pressure of the reaction device;

during discharging, sequentially opening the charging bin discharge valve and the bottom air sealing valve, monitoring the weighing sensor, closing the charging bin discharge valve when the weighing is not reduced any more, opening the discharging pipeline pressure charging valve until the bottom air sealing valve is closed in place, and stopping pressurizing after the pressure of a second circulation pipeline is added to be equal to the pressure of the reaction device;

opening the exhaust valve of the feeding bin, exhausting the gas of the feeding bin, opening the inlet valve of the feeding bin after the pressure is reduced to normal pressure, and waiting for next material mixing;

wherein the purge valve is used as a dredging purge gas source for standby; in the working process of the reaction device, the second circulation pipeline is pressurized all the time, and the pressure of the second circulation pipeline is higher than that of the reaction device, so that corrosive gas in the process flow cannot enter the second circulation pipeline.

10. The method for preparing aluminum trichloride as claimed in claim 9, wherein in the charging step, according to the set target weighing value, a 90% range fast feeding mode, an 8% range slow feeding mode and a 2% range inching feeding mode are adopted, and after the metering is completed, the weighing value is recorded.

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