Automatic crystallization device for anhydrous aluminum trichloride

Abstract

The invention belongs to the field of aluminum trichloride preparation, and particularly relates to an anhydrous aluminum trichloride automatic crystallization device which comprises a crystallization kettle and a quantification box, the output end of the quantification box is fixedly connected with a heat preservation pipe, an air inlet pipe is fixedly connected to the position, close to the top, of the outer side of the crystallization kettle, and the tail end of the air inlet pipe is communicated with the interior of the crystallization kettle in a tangential mode. A conveying valve is fixedly connected to the top of the quantitative box, an exhaust pipe is fixedly connected to the top of the crystallization kettle, a heat exchange cavity is formed in the crystallization kettle, a plurality of heat exchange valves communicated with the heat exchange cavity are fixedly connected to the outer side of the crystallization kettle, a sealing valve and a discharging valve are installed at the bottom of the crystallization kettle, the sealing valve is located above the discharging valve, and the discharging valve is located above the discharging valve. By means of the arrangement, the efficient crystallization process of aluminum trichloride is achieved, the interior of the whole crystallization kettle is completely isolated from the outside, the crystallization process can be automatically selected according to requirements, and high-quality anhydrous aluminum trichloride is effectively prepared.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of aluminum trichloride preparation, in particular to an automatic crystallization device for anhydrous aluminum trichloride. BACKGROUND

[0002] Aluminum trichloride is also called an inorganic salt compound. At room temperature, aluminum chloride is colorless or white hexagonal crystal, and industrial products are light yellow, which is mainly used as a core catalyst for petroleum chemical industry and organic synthesis. The preparation method generally adopts the metal aluminum method, and high-temperature aluminum trichloride gas can be prepared. After cooling and crystallization, it can be collected and stored.

[0003] The traditional crystallization device often uses a simple structure of a desublimation kettle. After the aluminum trichloride gas is introduced, the internal temperature is reduced, and the aluminum trichloride is slowly crystallized. After the crystallization is completed, the crystallization is recovered from the kettle bottom. Usually, there are many crystallizations remaining on the kettle wall. Due to the lack of air flow guidance, the crystallization degree is different at different positions, which not only affects the quality, but also needs to use artificial knocking or scraping to completely recover the crystallization. Not only the efficiency is affected, but also the kettle opening, feeding, and scraping will pollute the crystallization and affect the quality of the finished product.

[0004] Therefore, the application provides an automatic crystallization device for anhydrous aluminum trichloride. SUMMARY

[0005] In order to make up for the deficiencies of the prior art and solve at least one technical problem in the background art.

[0006] The technical scheme adopted by the application to solve the technical problem is: the automatic crystallization device for anhydrous aluminum trichloride, comprising a crystallization kettle and a quantitative tank, the output end of the quantitative tank is fixedly connected with a heat preservation pipe, the outer side of the top of the crystallization kettle is fixedly connected with an air inlet pipe, the tail end of the air inlet pipe is in tangential communication with the inside of the crystallization kettle, the top of the quantitative tank is fixedly connected with a conveying valve, the top of the crystallization kettle is fixedly connected with an exhaust pipe, the inside of the crystallization kettle is provided with a heat exchange cavity, the outer side of the crystallization kettle is fixedly connected with a plurality of heat exchange valves in communication with the heat exchange cavity, the bottom of the crystallization kettle is provided with a sealing valve and a discharge valve, the sealing valve is located above the discharge valve, and a storage cavity is formed between the two, and a drive motor is arranged below the crystallization kettle for controlling the shaking of the crystallization kettle. This operation can realize uninterrupted and uninterrupted crystallization process, and the continuous shedding of crystallization maintains the smoothness of the inner wall of the crystallization kettle, so that the gas flow can directly contact the inner wall, instead of being cooled by the already crystallized product to recrystallize the gas, which can better control the temperature and make the crystallization process more smoothly. It should be noted that before the equipment is operated, the protective gas needs to be filled into the quantitative tank, and the crystallization kettle is filled along the heat preservation pipe, so as to eliminate the influence factors such as air in the equipment and ensure the quality of crystallization. Through this setting, not only the efficient crystallization process of aluminum chloride is realized, but also the whole crystallization kettle is completely isolated from the outside world, and the crystallization process can be selected according to the needs, so as to effectively prepare high-quality anhydrous aluminum chloride.

[0007] Preferably, the outer side of the crystallization kettle is provided with a support frame, the support frame comprises a plurality of fixing frames fixed on the outer side of the crystallization kettle, and a bottom support frame arranged at the bottom of the crystallization kettle, a hole adapted to the position of the discharge valve is formed in the middle of the bottom support frame, and the fixing frame and the bottom support frame are fixed by a plurality of vertical columns. The driving end of the driving motor is connected with the bottom support frame. During operation, the crystallization kettle is fixed by the fixing frame, and the fixing frame and the bottom support frame are fixed by the vertical column. In this way, the vibration generated by the driving motor on the bottom support frame can be transmitted to the crystallization kettle, so that the crystallization kettle can be shaken, so that the crystallization on the kettle wall can fall off under the shaking. When the crystallization needs to be recovered, the discharge valve is opened, and the crystallization can fall from the bottom hole of the bottom support frame.

[0008] Preferably, the driving end of the driving motor faces upward and is fixed with an eccentric disc, a support column deviating from a circular shape is arranged at the top of the eccentric disc, a circular hole is formed in the bottom of the bottom support frame, and a rotating shaft is installed in the circular hole. The support column is fixed with the rotating shaft, and lifting discs are arranged at the bottom of the bottom support frame on both sides. During operation, when the driving motor starts, it will drive the eccentric disc to rotate, thereby driving the support column at the top of the eccentric disc to move in a circular motion. Since the support column is inserted in the bottom support frame, the bottom support frame will be moved. With the arrangement of the rotating shaft, the rotation of the support column will not affect the bottom support frame, but only drive the bottom support frame to translate within the range of circular motion, thereby driving the whole crystallization kettle to horizontally shake within a certain range. By controlling the output power of the driving motor, the shaking intensity can be adjusted to cope with different states of crystallization shedding. The lifting disc is arranged to support the whole support frame and keep the support frame stable in the horizontal position. A plurality of ball bearings can be installed at the top of the support frame to reduce the resistance caused by friction.

[0009] Preferably, the crystallization kettle is arranged in a concave shape at the bottom position, the sealing valve is fixed in the concave area, the heat exchange cavity is divided into two areas which do not interfere with each other and are connected by different heat exchange valves, and the two areas are located on the upper and lower sides of the sealing valve. During operation, the structure of the crystallization kettle allows the falling crystals to accumulate on the top of the sealing valve. When the sealing valve is opened, the crystals can be smoothly transferred to the lower side under the action of gravity. During the transfer process, the device can also be shaken to assist the transfer process. When the crystals are stored at the bottom, the internal temperature can be lowered to maintain the state of the crystals. By dividing the heat exchange cavity into two areas, the internal temperature can be adjusted at will to maintain the storage state of the crystals. Temperature monitoring devices are arranged in each area for real-time observation.

[0010] Preferably, a plurality of knocking blocks for knocking the inner wall of the crystallization kettle are arranged in the crystallization kettle. The plurality of knocking blocks are divided into multiple groups, and the plurality of knocking blocks in each group are arranged in a ring shape at equal intervals. The multiple groups of knocking blocks are arranged at equal intervals in the vertical plane. The knocking block comprises a center body, an expansion sleeve wrapped outside the center body, and a sealing tube sleeved outside the expansion sleeve. A filling valve is fixed to the tail end of the expansion sleeve and located outside the crystallization kettle. During operation, in order to ensure the smooth detachment of the crystals, a plurality of knocking blocks are arranged in the crystallization kettle. The knocking blocks are made of elastic deformable material. When the crystallization kettle is shaken, the part of the knocking block inside the crystallization kettle will sway. During the swaying process, the knocking block will continuously knock the inner wall of the crystallization kettle. The knocking part is focused on the removal of the crystals, and at the same time, the inner wall of the crystallization kettle is vibrated at high frequency to assist the detachment of the whole crystal. Through this arrangement, the detachment and recovery of the crystals are more effectively realized, and the residual crystals are reduced. At the same time, the structure of the knocking block allows air to be filled from the outside filling valve to the inside, so that the expansion sleeve expands. Not only does it seal the gap between itself and the sealing tube to prevent air leakage, but also ensures the sealing of the device due to thermal expansion and contraction during operation. At the same time, when the work is stopped, the air pressure is removed, the whole expansion sleeve and center body are pulled out, and the replacement or maintenance is carried out. The center body is arranged to give the end of the knocking block a certain mass, so that the knocking has a certain force. At the same time, the expansion sleeve is soft in texture and will not cause damage to the crystallization kettle when it hits.

[0011] Preferably, the outer side of the expansion sleeve is sleeved with a sealing pipe, the sealing pipe penetrates the inner wall of the crystallization kettle and communicates with the heat exchange cavity, the surface of the expansion sleeve is covered with a metal gasket, and the tail end of the expansion sleeve is provided with a lock disc; in operation, the sealing pipe is fixedly connected with the crystallization kettle, directly isolating the heat exchange cavity to prevent leakage of the coolant; meanwhile, the sealing pipe is more closely attached to the outer surface of the expansion sleeve, so that the expansion sleeve is not damaged due to overexpansion; after the expansion sleeve is placed in position, the lock disc is used to fix the filling valve, thereby fixing the overall knock block; the metal gasket can increase the impact strength, but the hardness of the gasket needs to be less than that of the crystallization kettle to reduce the impact damage; meanwhile, the expansion sleeve is directly in contact with the sealing pipe, and the metal gasket can quickly transfer heat, so that the aluminum chloride in the gas flow can crystallize when contacting the metal gasket; due to the provision of multiple knock blocks, the knock blocks not only have the function of assisting the crystallization and falling off, but also increase the crystallization area to assist the overall crystallization process.

[0012] Preferably, the lower part of the inner part of the crystallization kettle is further provided with a snap ring, the snap ring is located above the sealing valve, the snap ring is slidably connected with the inner wall of the crystallization kettle, the heat exchange cavity is divided into three regions that do not interfere with each other, and different heat exchange valves are used for communication, and the three regions are arranged in order from top to bottom; in operation, when the mixed gas flow moves to the bottom, it needs to be discharged upward; in order to ensure that the aluminum chloride in the discharged gas flow has been crystallized, the snap ring is arranged at the bottom of the crystallization kettle, directly attached to the heat exchange cavity of the middle layer, and the temperature of the heat exchange cavity is lower than that of the upper layer, so that the aluminum chloride can quickly crystallize; meanwhile, the snap ring swings around the circumference of the crystallization kettle and rotates, so that the crystallization attached to the surface quickly falls off, and then accumulates on the sealing valve under the action of gravity, thereby ensuring that the aluminum chloride in the bottom gas flow quickly crystallizes and reducing the residue of the finished product in the discharged air; meanwhile, the rotating snap ring can assist the transfer process of the finished product, so that the crystallization does not adhere to the inner wall of the crystallization kettle during the falling process.

[0013] Preferably, the bottom of the exhaust pipe is located in the middle of the crystallization kettle, and the bottom height is lower than the height of the air inlet pipe; a hose is fixedly connected between the air inlet pipe and the heat preservation pipe; in operation, the mixed gas that moves to the bottom moves upward from the center through the exhaust pipe due to the air outlet channel only at the top; in order to ensure that the gas that just enters is not discharged from the exhaust pipe, it is necessary to not only control the air inlet speed, but also to lower the exhaust pipe to reduce the early discharge of the mixed gas.

[0014] Preferably, the middle part of the exhaust pipe is provided with a spiral disc, the spiral disc comprises a vertical rod and spiral blades, the upper and lower ends of the exhaust pipe are fixedly connected with restraint frames, the vertical rod is rotationally connected in the middle part of the restraint frame, and when working, after the gas finally enters the exhaust pipe, the gas needs to rise spirally through the spiral disc, when contacting the spiral disc, the remaining aluminum chloride gas can be crystallized on the surface of the spiral disc, further reducing the gas content of aluminum chloride in the exhaust gas, when the whole device swings, the crystallization can be shaken off and recovered under the action of gravity.

[0015] Preferably, the outside of the exhaust pipe is fixedly connected with a flow valve, the inside of the restraint frame is provided with a cavity, the flow valve is in communication with the cavity, and when working, the upper and lower restraint frames are cooled through the flow valve and the cavity, serving as the last line of defense, the exhaust gas is finally cooled and crystallized, reducing the loss of finished products and the leakage of aluminum chloride.

[0016] The beneficial effects of the present application are as follows: 1. The automatic crystallization device of anhydrous aluminum chloride disclosed by the present application, through the setting of the crystallization kettle, the quantitative tank and the driving motor, not only realizes the efficient crystallization process of aluminum chloride, but also effectively makes the crystallization in the device quickly separate in the recovery stage, which not only effectively accelerates the recovery efficiency, but also ensures that the device inside recovers quickly, does not affect the subsequent production process, the whole crystallization kettle is completely isolated from the outside, the crystallization process can also be selected according to the demand, under the intermittent process, the inside and outside are completely isolated, the production efficiency is controllable, and the finished product quality is higher; under the uninterrupted production process, the production efficiency is extremely high, the device runs in order, and high-quality finished products are output at high frequency; so that the device can meet different production demands.

[0017] 2. The anhydrous aluminum chloride automatic crystallization device, in order to ensure the smooth separation of crystallization, a plurality of knocking blocks are installed in the inside of the crystallization kettle, the knocking block is made of elastic deformable material, when the crystallization kettle shakes, the part of the knocking block in the inside of the crystallization kettle swings, the inside wall of the crystallization kettle is continuously knocked in the swinging process, the crystallization of the knocking part is removed, and meanwhile, the inside wall of the crystallization kettle is vibrated at high frequency, the whole crystallization is assisted to fall off, the crystallization is more effectively separated and recovered, and the residual crystallization is reduced; meanwhile, the structure of the knocking block is arranged, air is filled from the outside filling valve to the inside, the expansion sleeve is expanded, the gap between the sealing tube and the sealing tube is sealed, air leakage is prevented, and meanwhile, the sealing property of the equipment is ensured due to thermal expansion and cold contraction in the working process; meanwhile, when the working is stopped, the air pressure is removed, the expansion sleeve and the center body are pulled out, and replacement or maintenance is carried out; the center body is arranged, so that the end of the knocking block has a certain quality, the knocking has a certain force, and meanwhile, the expansion sleeve is soft, and the crystallization kettle is not damaged when the expansion sleeve is hit. BRIEF DESCRIPTION OF DRAWINGS

[0018] The application will be further described below in combination with the drawings.

[0019] Figure 1 is a perspective view of the application; Figure 2 is a perspective view of the crystallization kettle of the application; Figure 3 is a perspective view of the lifting disc and the driving motor of the application; Figure 4 is a perspective view of the crystallization kettle and the sealing valve of the application; Figure 5 is a sectional view of the crystallization kettle of the application; Figure 6 is a sectional view of the exhaust pipe of the application; Figure 7 is a structural schematic view of the knocking block and the clasp ring of the application; In the drawings: 1, crystallization kettle; 2, quantitative box; 3, heat preservation pipe; 4, conveying valve; 5, hose; 6, air inlet pipe; 7, exhaust pipe; 8, support frame; 9, lifting disc; 10, driving motor; 11, heat exchange valve; 12, fixed frame; 13, bottom support frame; 14, eccentric disc; 15, knocking block; 16, sealing valve; 17, discharge valve; 18, heat exchange cavity; 19, clasp ring; 20, flow valve; 21, restraint frame; 22, spiral disc; 23, sealing tube; 24, expansion sleeve; 25, center body; 26, filling valve; 27, lock disc. DETAILED DESCRIPTION

[0020] In order to make the technical means, creative features, purposes and effects of the present application easy to understand, the present application is further described below in conjunction with specific embodiments.

[0021] As shown in Figures 1 to 7 The automatic crystallization device for anhydrous aluminum chloride comprises a crystallization kettle 1 and a quantitative tank 2, the output end of the quantitative tank 2 is fixedly connected with a heat preservation pipe 3, the outer side of the top of the crystallization kettle 1 is fixedly connected with an air inlet pipe 6, the tail end of the air inlet pipe 6 is in tangential communication with the inside of the crystallization kettle 1, the top of the quantitative tank 2 is fixedly connected with a conveying valve 4, the top of the crystallization kettle 1 is fixedly connected with an exhaust pipe 7, the inside of the crystallization kettle 1 is provided with a heat exchange cavity 18, the outer side of the crystallization kettle 1 is fixedly connected with a plurality of heat exchange valves 11 in communication with the heat exchange cavity 18, the bottom of the crystallization kettle 1 is provided with a sealing valve 16 and a discharge valve 17, the sealing valve 16 is located above the discharge valve 17, and a storage cavity is formed between the two, and a driving motor 10 is arranged below the crystallization kettle 1 for controlling the shaking of the crystallization kettle 1. The high-purity gaseous anhydrous aluminum chloride prepared by the metal aluminum method needs to be crystallized for the final purification and convenient storage and transportation. The gaseous aluminum chloride is introduced into the bottom of the quantitative tank 2, and the temperature of the gaseous aluminum chloride is about 700 degrees Celsius at this time. The high-temperature gas moves upward and gathers at the top of the quantitative tank 2. The delivery valve 4 is connected with the protective gas, and the protective gas can be high-purity nitrogen. Through the delivery of nitrogen, part of the aluminum chloride is mixed and passes through the heat preservation pipe 3 and the air inlet pipe 6 into the crystallization kettle 1. The heat preservation pipe 3 is externally connected with the heating device, which can detect the temperature of the mixed gas. When the temperature is low, heating is performed to reduce the problem of early crystallization of aluminum chloride to block the pipeline. By adjusting the delivery power of the delivery valve 4, the mixed gas enters the crystallization kettle 1 at high speed. Under the action of centrifugal force, the entering gas flow rotates along the inner wall of the crystallization kettle 1. By injecting the cooling medium into the heat exchange valve 11, the inside of the crystallization kettle 1 is kept at a predetermined temperature. In industrial production, the crystallization temperature of aluminum chloride is between 120 degrees Celsius and 150 degrees Celsius. At this temperature, the crystal shape is regular, the particle size is large, and the crystal shape is easy to fall off and collect. In order to maintain the temperature, the protective water vapor is used as the cooling medium to maintain the wall of the crystallization kettle 1 within the crystallization temperature range. In this way, when the mixed gas contacts the wall of the crystallization kettle 1, the aluminum chloride in the mixed gas will quickly crystallize. The high-speed rotating mixed gas spirally moves downward along the inner wall of the crystallization kettle 1, so that the aluminum chloride is uniformly crystallized on the inner wall of the crystallization kettle 1. When the gas flow flows to the bottom, it will be concentrated in the center. Since there is no air outlet at the bottom, the final mixed gas flow will move upward from the bottom and finally be discharged from the exhaust pipe 7. At this time, the aluminum chloride in the mixed gas flow has completed crystallization, and only the protective gas is left, which can be normally discharged or recycled. When the equipment has been running for a period of time, the air inlet pipe 6 and the exhaust pipe 7 at the top are closed, and the overall crystallization kettle 1 is controlled to shake by using the driving motor 10, so that the aluminum chloride crystallized on the inner wall of the crystallization kettle 1 falls off to the bottom. Then the sealing valve 16 is opened to let the crystallization fall into the storage cavity above the discharge valve 17. The sealing valve 16 is closed to temporarily save the crystallization. When it is needed to be recycled, the discharge valve 17 can be opened for centralized collection. This method can also reduce the influence of the external environment on the inside of the crystallization kettle 1. The crystallization kettle 1 can also be continuously shaken during the crystallization process. When the accumulated aluminum chloride crystallization reaches a certain degree, it directly falls off in the process and gradually accumulates at the bottom, so that the crystallization process can be continuously carried out. Then, in the final recycling stage, the shaking amplitude is increased to ensure that all the crystallization falls off and is uniformly collected. This operation can realize the uninterrupted and continuous crystallization process, and the continuous falling off of the crystallization maintains the smoothness of the inner wall of the crystallization kettle 1, so that the gas flow can directly contact the inner wall instead of being cooled by the already crystallized product. This can better control the temperature and make the crystallization process more smoothly.Before operation, a protective gas is first filled into the metering tank 2 and simultaneously filled into the crystallization vessel 1 through the insulation pipe 3. This eliminates influencing factors such as air inside the equipment, ensuring the quality of crystallization. This setup not only achieves a highly efficient crystallization process for aluminum trichloride but also allows for rapid detachment of crystals during the recovery phase. This significantly accelerates recovery efficiency and ensures the equipment quickly returns to its original state, without affecting subsequent production processes. Furthermore, the entire crystallization vessel 1 is completely isolated from the outside environment. The crystallization process can be selected according to requirements. In intermittent production, complete internal and external isolation ensures controllable production efficiency and high-quality finished products. In continuous production, extremely high efficiency is achieved, with the equipment operating smoothly and producing high-quality, high-frequency finished products. This allows the equipment to meet diverse production needs.

[0022] A support frame 8 is provided on the outside of the crystallization vessel 1. The support frame 8 includes multiple fixed frames 12 fixed on the outside of the crystallization vessel 1 and a bottom support frame 13 provided at the bottom of the crystallization vessel 1. The bottom support frame 13 has a hole in the middle that matches the position of the discharge valve 17. The fixed frames 12 and the bottom support frame 13 are fixed together by multiple columns. The drive end of the drive motor 10 is connected to the bottom support frame 13. During operation, the crystallization vessel 1 is fixed by the fixing frame 12, and then the fixing frame 12 is fixed to the bottom support frame 13 by the column. In this way, the vibration generated by the drive motor 10 to the bottom support frame 13 can be transmitted to the crystallization vessel 1, allowing the crystallization vessel 1 to shake, so that the crystals on the vessel wall fall off under the shaking. When it is necessary to recover the crystals, the discharge valve 17 is opened to allow the crystals to fall from the bottom hole of the bottom support frame 13.

[0023] The drive end of the drive motor 10 faces upward and is fixedly connected to an eccentric disk 14. The top of the eccentric disk 14 is provided with a support column that deviates from the circle. The bottom of the bottom support frame 13 is provided with a circular hole and a rotating shaft is installed in the circular hole. The support column is fixedly connected to the rotating shaft. The bottom of the bottom support frame 13 is provided with lifting disks 9 on both sides. During operation, when the drive motor 10 starts, it drives the eccentric disk 14 to rotate, which in turn drives the support column on top of the eccentric disk 14 to move in a circular motion. Since the support column is inserted into the bottom support frame 13, it will also drive the bottom support frame 13 to move. With the setting of the rotating shaft, the rotation of the support column will not affect the bottom support frame 13, but will only drive the bottom support frame 13 to move horizontally within the range of the circular motion, thereby causing the entire crystallization kettle 1 to shake horizontally within a certain range. By controlling the output power of the drive motor 10, the shaking intensity can be adjusted to deal with different crystal shedding situations. The support plate 9 is set to support the overall support frame 8 and keep the support frame 8 stable in a horizontal position for shaking. Multiple ball bearings can be installed on the top of the support frame 8 to reduce the resistance caused by friction.

[0024] The crystallization kettle 1 is arranged in a concave shape at the bottom position, the sealing valve 16 is fixed in the concave area, the heat exchange cavity 18 is divided into two areas which do not interfere with each other and are connected by different heat exchange valves 11, and the two areas are located on the upper and lower sides of the sealing valve 16 respectively. In operation, the structure of the crystallization kettle 1 allows the falling crystals to accumulate on the top of the sealing valve 16, and when the sealing valve 16 is opened, the crystals can be smoothly transferred to the lower side under the action of gravity. During the transfer process, the device can also be shaken to assist the transfer process. When the crystals are stored at the bottom, the internal temperature can be lowered to prevent high-temperature gasification and maintain the state of the crystals. By dividing the heat exchange cavity 18 into two areas, the internal temperature can be adjusted at will to maintain the storage state of the crystals. Temperature monitoring devices are provided in each area for real-time observation.

[0025] A plurality of knocking blocks 15 for knocking the inner wall of the crystallization kettle 1 are installed in the crystallization kettle 1. The plurality of knocking blocks 15 are divided into multiple groups, the knocking blocks 15 in each group are arranged in a ring shape at equal intervals, and the multiple groups of knocking blocks 15 are arranged at equal intervals in the vertical plane. The knocking block 15 comprises a center body 25, the outer side of the center body 25 is wrapped with an expansion sleeve 24, the outer side of the expansion sleeve 24 is sleeved with a sealing tube 23, the tail end of the expansion sleeve 24 is fixedly connected with a filling valve 26, and the filling valve 26 is located outside the crystallization kettle 1. In operation, in order to ensure the smooth detachment of the crystals, a plurality of knocking blocks 15 are installed in the crystallization kettle 1. The knocking blocks 15 are made of elastic and deformable material. When the crystallization kettle 1 is shaken, the part of the knocking block 15 inside the crystallization kettle 1 will sway. During the swaying process, the knocking block 15 will continuously knock the inner wall of the crystallization kettle 1. The knocking part is particularly important for removing the crystals. At the same time, the inner wall of the crystallization kettle 1 is subjected to high-frequency vibration, which assists the overall crystal detachment process. Through this arrangement, the crystal detachment and recovery work is more effectively realized, and the crystal residue is reduced. At the same time, the structure of the knocking block 15 is arranged to fill air from the outside filling valve 26 inward during the working process, so that the expansion sleeve 24 expands. Not only does it seal the gap between itself and the sealing tube 23 to prevent air leakage, but also ensures the sealing of the device during the working process due to the high temperature inside the device and thermal expansion and contraction. At the same time, when the work is stopped, the air pressure is removed, the entire expansion sleeve 24 and the center body 25 are pulled out outward, and replacement or maintenance can be performed. The center body 25 is provided to give the end of the knocking block 15 a certain mass, so that the knocking has a certain force. At the same time, the expansion sleeve 24 is soft in texture and will not cause damage to the crystallization kettle 1 when it is hit.

[0026] The expansion sleeve 24 is sleeved with a sealing tube 23 on the outside. The sealing tube 23 penetrates the inner wall of the crystallization kettle 1 and communicates with the heat exchange cavity 18. The surface of the expansion sleeve 24 is covered with a metal gasket, and the tail end of the expansion sleeve 24 is provided with a lock disc 27. When working, the sealing pipe 23 is fixedly connected with the crystallization kettle 1, directly isolates the heat exchange cavity 18, prevents leakage of the coolant, and the sealing pipe 23 is more closely attached to the outer surface of the expansion sleeve 24, so that the expansion sleeve 24 will not be damaged due to excessive expansion. After the expansion sleeve 24 is placed in place, the filling valve 26 is fixed by using the locking disc 27, so as to fix the whole knocking block 15. The metal gasket can increase the impact strength, but the hardness of the gasket needs to be less than the hardness of the crystallization kettle 1, so as to reduce the impact damage. At the same time, the expansion sleeve 24 is directly in contact with the sealing pipe 23, and the metal gasket can quickly transfer heat, so that the aluminum chloride in the gas flow can crystallize when contacting the metal gasket. Due to the arrangement of multiple knocking blocks 15, the knocking blocks 15 not only have the function of assisting crystallization and falling off, but also increase the crystallization area and assist the whole crystallization process.

[0027] The lower part of the inside of the crystallization kettle 1 is also provided with a snap ring 19, which is located above the sealing valve 16 and is in sliding connection with the inner wall of the crystallization kettle 1. The heat exchange cavity 18 is divided into three non-interfering areas, and different heat exchange valves 11 are used for communication. The three areas are arranged in order from top to bottom. When working, the mixed gas flow needs to be discharged upward after moving to the bottom. In order to ensure that the aluminum chloride in the discharged gas flow has been crystallized, the snap ring 19 is arranged at the bottom of the crystallization kettle 1 and directly attached to the middle layer of the heat exchange cavity 18. The temperature of this heat exchange cavity 18 is lower than that of the upper layer, which can quickly crystallize the aluminum chloride. At the same time, the snap ring 19 will rotate under the swing of the circumference of the crystallization kettle 1, so that the crystallization attached to the surface can quickly fall off. After falling off, it will accumulate on the sealing valve 16 under the action of gravity. This not only ensures that the aluminum chloride in the bottom gas flow quickly crystallizes and reduces the residue of finished products in the discharged air, but also assists the transfer process of the finished products. The crystallization is not attached to the inner wall of the crystallization kettle 1 during the falling process.

[0028] The bottom of the exhaust pipe 7 is located in the middle of the crystallization kettle 1, and the bottom height is lower than the height of the air inlet pipe 6. The soft pipe 5 is fixedly connected between the air inlet pipe 6 and the heat preservation pipe 3. When working, the mixed gas moving to the bottom will move upward from the center through the exhaust pipe 7 because there is only an air outlet channel at the top. In order to ensure that the gas flow just entering will not be discharged from the exhaust pipe 7, it is necessary to not only control the air inlet speed, but also to lower the exhaust pipe 7 to reduce the early discharge of the mixed gas.

[0029] The middle part of the exhaust pipe 7 is provided with a spiral disc 22, which includes a vertical rod and spiral blades. The upper and lower ends of the exhaust pipe 7 are fixedly connected with a restraint frame 21, and the vertical rod is rotatably connected in the middle of the restraint frame 21. When the gas finally enters the exhaust pipe 7, it needs to rise spirally through the spiral disc 22. When it contacts the spiral disc 22, the remaining aluminum chloride gas will crystallize on the surface of the spiral disc 22, further reducing the gas content of aluminum chloride in the exhaust gas. When the entire device is swinging, the crystallization will also be shaken off and recycled under the action of gravity.

[0030] The outer side of the exhaust pipe 7 is fixedly connected with a flow valve 20, and the inside of the restraint frame 21 is provided with a cavity, and the flow valve 20 is in communication with the cavity. When working, the upper and lower restraint frames 21 are cooled through the flow valve 20 and the cavity, which is the last line of defense for the last cooling and crystallization of the exhaust gas, reducing the loss of finished products and reducing the leakage of aluminum chloride.

[0031] In operation, the high-purity gaseous anhydrous aluminum chloride prepared by the aluminum metal method needs to be crystallized for final purification and convenient storage and transportation. The gaseous aluminum chloride is introduced into the bottom of the quantitative tank 2, and the temperature of the gaseous aluminum chloride is about 700 degrees Celsius at this time. The high-temperature gas moves upward and gathers at the top of the quantitative tank 2. The delivery valve 4 is connected with the protective gas, and the protective gas can be high-purity nitrogen. Through the delivery of nitrogen, part of the aluminum chloride is mixed and passes through the heat preservation pipe 3 and the air inlet pipe 6 into the crystallization kettle 1. The heat preservation pipe 3 is externally connected with the heating device, which can detect the temperature of the mixed gas. When the temperature is low, heating is performed to reduce the problem of early crystallization of aluminum chloride to block the pipeline. By adjusting the delivery power of the delivery valve 4, the mixed gas enters the crystallization kettle 1 at high speed. Under the action of centrifugal force, the entering gas flow rotates along the inner wall of the crystallization kettle 1. By injecting the cooling medium into the heat exchange valve 11, the inside of the crystallization kettle 1 is kept at a predetermined temperature. In industrial production, the crystallization temperature of aluminum chloride is between 120 degrees Celsius and 150 degrees Celsius. At this temperature, the flaky or needle-shaped crystals with regular morphology and large particle size can be quickly formed, which are easy to fall off and collect. In order to maintain the temperature, the protective water vapor can be used as the cooling medium to keep the wall of the crystallization kettle 1 within the crystallization temperature range. In this way, when the mixed gas contacts the wall of the crystallization kettle 1, the aluminum chloride in the mixed gas will quickly crystallize. The high-speed rotating mixed gas spirally moves downward along the inner wall of the crystallization kettle 1, so that the aluminum chloride is uniformly crystallized on the inner wall of the crystallization kettle 1. When the gas flow flows to the bottom, it will be concentrated in the center. Since there is no air outlet at the bottom, the final mixed gas flow will move upward from the bottom and finally be discharged from the exhaust pipe 7. At this time, the aluminum chloride in the mixed gas flow has completed crystallization, and only the protective gas is left, which can be normally discharged or recycled. When the equipment has been running for a period of time, the air inlet pipe 6 and the exhaust pipe 7 at the top are closed, and the overall crystallization kettle 1 is shaken by using the driving motor 10 to make the aluminum chloride crystallized on the inner wall of the crystallization kettle 1 fall off to the bottom. Then the sealing valve 16 is opened to let the crystallization fall into the storage cavity above the discharge valve 17. The sealing valve 16 is closed to temporarily save the crystallization. When it is needed to be recycled, the discharge valve 17 can be opened for centralized collection. This method can also reduce the influence of the external environment on the inside of the crystallization kettle 1. The crystallization kettle 1 can also be continuously shaken during the crystallization process. When the accumulated aluminum chloride crystallization reaches a certain degree, it directly falls off in the process and gradually accumulates at the bottom, so that the crystallization process can be continuously carried out. Then, in the final recycling stage, the shaking amplitude is increased to ensure that all the crystallization falls off and is uniformly collected. This operation can realize the uninterrupted and continuous crystallization process, and the continuous falling off of the crystallization keeps the inner wall of the crystallization kettle 1 smooth, so that the gas flow can directly contact the inner wall instead of being cooled by the already crystallized product to re-crystallize the gas. This can better control the temperature and make the crystallization process more smoothly.Before the device operates, the quantitative tank 2 needs to be filled with protective gas, and the crystallizer 1 is filled along the heat preservation pipe 3, so as to exclude the influence factors such as air in the device, and ensure the quality of crystallization; through the setting, not only the efficient crystallization process of aluminum chloride is realized, but also the crystallization in the device can be quickly separated in the recovery stage, which not only effectively speeds up the recovery efficiency, but also ensures that the device quickly recovers, does not affect the subsequent production process, and the whole crystallizer 1 is completely isolated from the outside world, and the crystallization process can also be selected according to the demand, in the intermittent process, the inside and outside are completely isolated, the production efficiency is controllable, and the finished product quality is higher; in the uninterrupted production process, the production efficiency is very high, the device runs in order, and the finished product is output with high quality and high frequency; so that the device can meet different production demands.

[0032] The crystallizer 1 is fixed through the fixing frame 12, and the fixing frame 12 and the bottom support frame 13 are fixed through the column; in this way, the vibration of the driving motor 10 to the bottom support frame 13 can be transmitted to the crystallizer 1, so that the crystallizer 1 can shake, so that the crystals on the wall of the crystallizer 1 fall off under the shaking; when the crystals need to be recovered, the discharge valve 17 is opened, so that the crystals can fall from the bottom hole of the bottom support frame 13.

[0033] When the driving motor 10 starts, the eccentric disc 14 rotates, thereby driving the support column at the top of the eccentric disc 14 to move in a circle. Since the support column is inserted in the bottom support frame 13, the bottom support frame 13 is driven to move, and the rotation of the support column does not affect the bottom support frame 13, but only drives the bottom support frame 13 to move in a circle, thereby driving the whole crystallizer 1 to shake horizontally within a certain range. By controlling the output power of the driving motor 10, the shaking intensity can be adjusted to cope with different states of crystal falling. The lifting disc 9 is arranged to support the whole support frame 8 and keep the support frame 8 stable in the horizontal position. A plurality of ball bearings can be installed at the top of the support frame 8 to reduce the resistance caused by friction.

[0034] The structure of the crystallizer 1 allows the falling crystals to accumulate on the top of the sealing valve 16. When the sealing valve 16 is opened, the crystals can be transferred to the lower part under the action of gravity. During the transfer process, the device can also be shaken to assist the transfer process. When the crystals are stored at the bottom, the internal temperature can be lowered to maintain the state of the crystals. The heat exchange cavity 18 is divided into two regions, and the internal temperature can be adjusted at will to maintain the storage state of the crystals. Temperature monitoring devices are arranged in each region to observe in real time.

[0035] In order to ensure the smooth separation of crystallization, a plurality of knock blocks 15 are installed inside the crystallization kettle 1, the knock blocks 15 are made of elastically deformable material, when the crystallization kettle 1 is shaken, the part of the knock block 15 inside the crystallization kettle 1 will swing, and will continuously knock the inner wall of the crystallization kettle 1 during the swinging process, which can not only remove the crystallization at the knocking part, but also make the inner wall of the crystallization kettle 1 vibrate at high frequency, which can assist the overall crystallization to fall off, and the setting can more effectively realize the falling off and recovery of the crystallization, and reduce the residual crystallization; At the same time, the structure of the knock block 15 is set, and the air is filled from the outside filling valve 26 to the inside, so that the expansion sleeve 24 expands, not only seals the gap between itself and the sealing pipe 23 to prevent air leakage, but also ensures the sealing of the equipment due to thermal expansion and contraction during work; At the same time, when the work is stopped, the air pressure is removed, the whole expansion sleeve 24 and the center body 25 are pulled out, and the replacement or maintenance is carried out; The setting of the center body 25 is to make the end of the knock block 15 have a certain quality, so that the knocking has a certain intensity, and the expansion sleeve 24 is soft, which will not cause damage to the crystallization kettle 1 when impacting.

[0036] The sealing pipe 23 is fixedly connected with the crystallization kettle 1, which directly separates the heat exchange cavity 18 from the isolation, prevents the leakage of the coolant, and the sealing pipe 23 is more matched with the outer surface of the expansion sleeve 24, so that the expansion sleeve 24 will not be damaged due to excessive expansion. When the expansion sleeve 24 is placed in place, the filling valve 26 is fixed by using the lock disc 27, so as to fix the whole knock block 15. The metal gasket can increase the impact strength, but the hardness of the gasket should be less than the hardness of the crystallization kettle 1 to reduce the impact damage. At the same time, the expansion sleeve 24 directly contacts with the sealing pipe 23, and the metal gasket can quickly transfer heat, so that the aluminum chloride in the airflow can crystallize when contacting with the metal gasket. Due to the setting of a plurality of knock blocks 15, the knock blocks 15 not only have the function of assisting the crystallization to fall off, but also can increase the crystallization area to assist the overall crystallization process.

[0037] When the mixed gas flow moves to the bottom, it needs to be discharged upward. In order to ensure that the aluminum chloride in the discharged gas flow has been crystallized, a snap ring 19 is arranged at the bottom of the crystallization kettle 1, and the snap ring 19 is directly matched with the heat exchange cavity 18 of the middle layer. The temperature of the heat exchange cavity 18 is lower than that of the upper layer, which can quickly crystallize the aluminum chloride. At the same time, the snap ring 19 will rotate under the circumferential swing of the crystallization kettle 1, so that the crystallization attached to the surface can quickly fall off, and after falling off, it will accumulate on the sealing valve 16 under the action of gravity, which not only ensures that the aluminum chloride in the bottom gas flow quickly crystallizes, and reduces the residual product in the discharged air; At the same time, the rotating snap ring 19 can assist the final product transfer process, so that the crystallization is not attached to the inner wall of the crystallization kettle 1 during falling.

[0038] The mixed gas moving to the bottom will move upward from the center and finally pass through the exhaust pipe 7 because only the top has an exhaust passage. In order to ensure that the newly entered gas flow will not be discharged from the exhaust pipe 7, not only the air inlet speed needs to be controlled, but also the exhaust pipe 7 needs to be lowered to reduce the premature discharge of the mixed gas. When the gas finally enters the exhaust pipe 7, it needs to rise spirally through the spiral disc 22. When contacting the spiral disc 22, the remaining aluminum chloride gas will crystallize on the surface thereof, further reducing the gas content of aluminum chloride in the exhaust gas. When the entire device is swinging, the crystallization will also be shaken off and recycled under the action of gravity.

[0039] The upper and lower two restraint frames 21 are cooled through the flow-through valve 20 and the cavity, which is the last line of defense for the last cooling and crystallization of the discharged gas, reducing the loss of finished products and reducing the leakage of aluminum chloride.

[0040] The above shows and describes the basic principles, main features and advantages of the present application. Those skilled in the art should understand that the present application is not limited to the above examples, and the above examples and descriptions in the specification are only to illustrate the principles of the present application. Without departing from the spirit and scope of the present application, various changes and improvements can be made to the present application, and these changes and improvements all fall within the scope of the present application. The scope of protection of the present application is defined by the appended claims and their equivalents.

Claims

1. An automatic crystallization device for anhydrous aluminum trichloride, characterized in that: The system includes a crystallization vessel and a metering tank. An insulation pipe is fixedly connected to the output end of the metering tank. An air inlet pipe is fixedly connected to the top of the outer side of the crystallization vessel, and the end of the air inlet pipe is tangentially connected to the interior of the crystallization vessel. A conveying valve is fixedly connected to the top of the metering tank, and an exhaust pipe is fixedly connected to the top of the crystallization vessel. A heat exchange chamber is opened inside the crystallization vessel. Multiple heat exchange valves connected to the heat exchange chamber are fixedly connected to the outer side of the crystallization vessel. A sealing valve and a discharge valve are installed at the bottom of the crystallization vessel. The sealing valve is located above the discharge valve, and a storage chamber is formed between the two. A drive motor for controlling the shaking of the crystallization vessel is installed below the crystallization vessel.

2. The anhydrous aluminum trichloride automatic crystallization device according to claim 1, characterized in that: A support frame is provided on the outside of the crystallization vessel. The support frame includes multiple fixed frames fixed on the outside of the crystallization vessel and a bottom support frame provided at the bottom of the crystallization vessel. The bottom support frame has a hole in the middle that matches the position of the discharge valve. The fixed frames and the bottom support frame are fixed together by multiple columns. The drive end of the drive motor is connected to the bottom support frame.

3. The anhydrous aluminum trichloride automatic crystallization device according to claim 2, characterized in that: The drive end of the drive motor faces upward and is fixedly connected to an eccentric disk. The top of the eccentric disk is provided with a support column that deviates from the circle. The bottom of the bottom support frame has a circular hole, and a rotating shaft is installed in the circular hole. The support column is fixedly connected to the rotating shaft. The bottom of the bottom support frame is provided with lifting disks on both sides.

4. The anhydrous aluminum trichloride automatic crystallization device according to claim 3, characterized in that: The crystallization vessel is recessed at the bottom, and the sealing valve is fixed in this recessed area. The heat exchange chamber is divided into two non-interfering areas, which are connected by different heat exchange valves. The two areas are located on the upper and lower sides of the sealing valve, respectively.

5. The anhydrous aluminum trichloride automatic crystallization device according to claim 4, characterized in that: The crystallization vessel is equipped with multiple striking blocks for striking the inner wall of the crystallization vessel. The multiple striking blocks are divided into multiple groups, and the multiple striking blocks in each group are arranged in a ring at equal intervals. The multiple groups of striking blocks are arranged at equal intervals on a vertical plane. Each striking block includes a central body, and an expansion sleeve is wrapped around the outside of the central body. A sealing tube is sleeved on the outside of the expansion sleeve, and a filling valve is fixed to the tail end of the expansion sleeve and located on the outside of the crystallization vessel.

6. The anhydrous aluminum trichloride automatic crystallization device according to claim 5, characterized in that: The expansion sleeve is fitted with a sealing tube on its outer side. The sealing tube penetrates the inner wall of the crystallization vessel and communicates with the heat exchange chamber. The surface of the expansion sleeve is covered with a metal gasket, and a locking plate is provided at the tail end of the expansion sleeve.

7. The anhydrous aluminum trichloride automatic crystallization device according to claim 6, characterized in that: A retaining ring is also provided at the lower part of the interior of the crystallization vessel. The retaining ring is located above the sealing valve and is slidably engaged with the inner wall of the crystallization vessel. The heat exchange chamber is divided into three non-interfering areas, which are connected by different heat exchange valves. The three areas are arranged sequentially from top to bottom.

8. The anhydrous aluminum trichloride automatic crystallization apparatus according to claim 7, characterized in that: The bottom of the exhaust pipe is located in the middle of the crystallization vessel, and the bottom height is lower than the height of the air inlet pipe. A flexible hose is fixed between the air inlet pipe and the insulation pipe.

9. The anhydrous aluminum trichloride automatic crystallization device according to claim 8, characterized in that: A spiral disc is provided in the middle of the exhaust pipe. The spiral disc includes a vertical rod and spiral blades. Both the upper and lower ends of the exhaust pipe are fixed with restraint frames. The vertical rod is rotatably locked in the middle of the restraint frame.

10. The anhydrous aluminum trichloride automatic crystallization device according to claim 9, characterized in that: A flow valve is fixed to the outside of the exhaust pipe, and a cavity is opened inside the restraint frame, with the flow valve communicating with the cavity.

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