Anti-disproportionation reactor and anti-disproportionation catalyst filling and activating method
By designing feed tanks and multi-venting pipelines in the anti-dispersation reactor, uniform addition of catalysts and uniform dispersion of heat are achieved, the problem of difficult to control the catalyst activation temperature is solved, the reaction efficiency is improved and the operating cost is reduced.
Patent Information
- Application Number
- CN202411990702.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-31
- Publication Date
- 2025-04-18
AI Technical Summary
In the anti-disproportionation reactor, the catalyst activation temperature is difficult to control, which easily leads to local inactivation, thereby reducing reaction efficiency and increasing operating costs.
An anti-dispersification reactor is designed, using a feeding tank and a multi-venting pipeline. Catalysts are gradually added through the feeding tank, and a specific gas flow distribution is formed using nitrogen in the venting pipeline to promote uniform mixing of silicon tetrachloride and the catalyst and uniform dispersion of heat.
By accurately controlling the catalyst addition rate and nitrogen flow, local temperature overheating and carbonization inactivation are effectively avoided, the activity and reaction efficiency of the catalyst are improved, and the operating cost is reduced.
Smart Images
Figure CN119838511A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of anti-disproportionation reactors, and in particular relates to an anti-disproportionation reactor and an anti-disproportionation catalyst filling and activation method. Background Art
[0002] In the field of chemical production, especially in the production process related to trichlorosilane, impurity separation and recovery are important links. Among them, the cold hydrogenation distillation tower is responsible for separating impurities in trichlorosilane, and the light components extracted from the distillation contain a mixture of dichlorosilane and trichlorosilane; in order to effectively recover dichlorosilane, it is usually necessary to add a deproportionation reactor.
[0003] During the operation cycle of the anti-disproportionation reactor, the activity of the catalyst will gradually decrease with the use time, so it is very important to replace the catalyst regularly and activate it before use. The traditional activation method is to place the catalyst in the reactor first, then dry it with nitrogen, and add silicon tetrachloride after drying to control the reaction temperature to achieve the purpose of activation. However, in this process, when silicon tetrachloride is added, the internal temperature of the reactor is required not to exceed 80°C, otherwise the catalyst will be deactivated, and it is extremely difficult to accurately control this temperature in actual operation.
[0004] More importantly, the trace amount of water contained in the catalyst will release heat violently when it comes into contact with silicon tetrachloride. Due to the poor heat transfer performance of the fixed bed reactor, uneven temperature distribution is prone to occur when the reaction releases a large amount of heat. In addition, the large amount of heat generated is difficult to disperse quickly, which leads to excessively high local temperatures of the catalyst, and then causes local carbonization and deactivation. This local carbonization and deactivation not only reduces the overall activity of the catalyst, but also greatly reduces the conversion efficiency of the anti-disproportionation reaction, ultimately leading to an increase in the operating cost of the device. In addition, the catalyst is fixed in the fixed bed reactor. Once problems such as local high-temperature carbonization and deactivation occur during the activation process, the catalyst cannot be replaced in time during operation, further affecting the overall performance and reaction efficiency of the reactor. Summary of the invention
[0005] The invention provides a deproportionation reactor and a deproportionation catalyst filling and activation method to solve the problems of difficult control of catalyst activation temperature and easy local deactivation.
[0006] In order to solve the above technical problems, the technical solution adopted by the present invention is: On the one hand, the present application provides a deproportionation reactor, comprising a reactor, wherein a feeding tank for adding silicon tetrachloride and a catalyst into the reactor is provided on the top of the reactor; A plurality of ventilation pipes are arranged inside the reactor along the height direction of the reactor; a first feed port for supplying silicon tetrachloride into the reactor is opened through the bottom of the feeding tank, and a plurality of second feed ports for supplying the catalyst into the reactor are opened on the side wall of the feeding tank, and opening and closing valves are arranged at the plurality of the second feed ports, and different opening and closing valves are set with different starting temperature thresholds.
[0007] Furthermore, the ventilation pipe is annularly sleeved around the reactor and is used to introduce nitrogen into the reactor; A plurality of exhaust holes communicating with the interior of the reactor are arranged at intervals on the inner wall of the ventilation pipe.
[0008] Furthermore, several of the exhaust holes are each provided with an exhaust valve with an adjustable angle, the jet direction of the exhaust valve is arranged at an angle with the inner wall of the reactor, and each of the exhaust valves is biased clockwise or counterclockwise.
[0009] Furthermore, a central column is provided in the reactor, and a plurality of temperature sensors are arranged at intervals along the height direction on the central column, and the temperature sensor is electrically connected to the start valve of the second feed port.
[0010] Furthermore, the feeding tank includes a feeding hopper and a feeding pipe extending into the reactor, the second feed port is circumferentially arranged on the circumferential side of the feeding pipe, and the second feed ports are arranged in multiple layers at intervals, and the opening and closing valves of each layer of the second feed ports have different starting temperature thresholds.
[0011] Furthermore, the top of the central column is a pointed structure, and the central axis of the central column and the central axis of the feeding pipe are colinear.
[0012] Furthermore, the feed pipe is rotatably connected to the feeding hopper, and the feeding tank includes a driving source for driving the feed pipe to rotate.
[0013] Furthermore, a first vent is provided at the bottom of the feeding tank, and a second vent is provided at the bottom of the reactor.
[0014] Furthermore, an electric opening and closing valve for controlling the opening and closing of the first feed port is provided at the bottom of the feed pipe.
[0015] On the other hand, the present application also provides a method for loading and activating a deproportionation catalyst, using the deproportionation reactor, comprising the following steps: S1: Install a feed tank at the spare port on the top of the anti-disproportionation reactor; S2: Dry the inside of the reactor until the dew point is below -55°C, close the second feed inlet, open the first feed inlet, and add 70% liquid level of silicon tetrachloride into the reactor through the feed tank; S3: introducing nitrogen into the reactor through the ventilation pipe and the second ventilation port to increase the disturbance of silicon tetrachloride; S4: After the silicon tetrachloride in the feeding tank is exhausted, nitrogen is continuously introduced into the feeding tank through the first vent to achieve purging of the feeding tank and maintain a nitrogen environment in the feeding tank; S5: Close the first feed inlet, control the opening number of the second feed inlet according to the temperature in the reactor, and use the feed tank to slowly and gradually add the catalyst into the reactor to control the internal temperature below 70°C.
[0016] The present invention can achieve the following beneficial effects: 1. The present invention is provided with a feeding tank, through which the catalyst is added into the reactor. A plurality of second feed ports are provided, and the number of openings of the second feed ports can be adjusted in real time according to the temperature in the reactor, so that the rate of addition of the catalyst can be controlled more accurately, thereby alleviating the problem of excessively violent reaction and difficult temperature control due to too fast a catalyst addition rate, thereby reducing the risk of catalyst deactivation due to excessively high local temperature.
[0017] 2. Multiple ventilation pipes are arranged in the reactor along the height direction, and nitrogen can be introduced into the reactor through the ventilation pipes. Exhaust holes are opened on the ventilation pipes, and exhaust valves with adjustable angles and biased in a certain direction are arranged in the exhaust holes, so that the nitrogen forms a specific airflow distribution in the reactor, which is conducive to the uniform dispersion of heat.
[0018] 3. In the process of adding the catalyst, nitrogen is continuously introduced through the ventilation pipe and the second ventilation port at the bottom of the reactor, so that the silicon tetrachloride and the catalyst in the reactor are in a nitrogen disturbance environment. The flow of nitrogen can promote the uniform mixing of silicon tetrachloride and the catalyst, so that the two are fully in contact, thereby improving the uniformity and efficiency of the reaction; at the same time, the nitrogen disturbance also helps to evenly transfer heat in the reactor, further avoiding the occurrence of local overheating and ensuring the activity of the catalyst and the reaction effect. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The present invention will be further described below in conjunction with the accompanying drawings and embodiments: Figure 1 The vertical cutaway front view of a deproportionation reactor of the present invention.
[0020] In the accompanying drawings, the components represented by the reference numerals are listed as follows: 1. Reactor; 11. Center column; 12. Second vent; 2. Feed tank; 21. Feed hopper; 22. Feed pipe; 221. First feed port; 222. Second feed port; 23. First vent; 3. Ventilation duct; 31. Exhaust hole; 32. Exhaust valve; 4. Electric opening and closing valve. DETAILED DESCRIPTION
[0021] In order to facilitate understanding of the present application, the present application will be described more fully below with reference to the relevant drawings. Embodiments of the present application are provided in the drawings. However, the present application can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present application more thorough and comprehensive.
[0022] like Figure 1 As shown, a deproportionation reactor includes a reactor 1, a feeding tank 2 is installed on the top of the reactor 1, and silicon tetrachloride and a catalyst are added into the reactor 1 through the feeding tank 2 to achieve a deproportionation reaction. Specifically, the feeding tank 2 includes a feeding hopper 21 and a feeding pipe 22 extending into the reactor 1, the feeding pipe 22 and the feeding hopper 21 are rotatably connected, and the feeding tank 2 also includes a driving source for driving the feeding pipe 22 to rotate, and the driving source can be a driving motor, which is not shown in the figure.
[0023] One end of the feed pipe 22 extending into the reactor 1 is penetrated and formed with a first feed port 221 for supplying silicon tetrachloride into the reactor 1. A plurality of second feed ports 222 are provided in the circumferential direction of the side wall of the feed pipe 22. The second feed ports 222 are arranged in multiple layers at intervals. Each second feed port 222 is provided with an opening and closing valve, and different opening and closing valves are set with different starting temperature thresholds. In one embodiment, a starting temperature threshold is set for the opening and closing valves of each layer of the second feed port 222. When the reaction temperature in the reactor 1 is high, the number of opening layers of the second feed port 222 can be reduced; when the reaction rate in the reactor 1 is slow, the number of opening layers of the second feed port 222 can be increased. In other embodiments, the starting temperature threshold of the second feed port 222 can also be set in other ways.
[0024] The reactor 1 is provided with a central column 11, which is fixed at the bottom center of the reactor 1, and a plurality of temperature sensors are arranged at intervals along the height direction of the central column 11. The temperature sensor can measure the reaction temperature inside the reactor 1 in real time, and the temperature inside the reactor 1 is measured by the temperature sensor to control the opening and closing of the second feed port 222. Specifically, the temperature sensor feeds back the measured temperature to the control center in real time, and the optimal reaction temperature of the anti-disproportionation reaction is set in the control center. If the temperature inside the reactor 1 is lower than the optimal reaction temperature, the number of the second feed port 222 opened is increased; if the temperature inside the reactor 1 is higher than the optimal reaction temperature, the number of the second feed port 222 opened is reduced, thereby accurately controlling the rate of catalyst addition and realizing temperature control inside the reactor 1.
[0025] The feed pipe 22 and the hopper 21 are rotatably connected. When the catalyst is added into the reactor 1, the feed pipe 22 is driven to rotate, so that the catalyst can be evenly thrown out around the circumference of the feed pipe 22 through the second feed port 222 under the action of centrifugal force, so that the catalyst can be more evenly spread into the reactor 1, achieving uniform mixing and contact with silicon tetrachloride, and reducing the situation where the heat release in the local area of the reactor 1 is too much due to the concentrated addition of the catalyst, and the reaction in some areas is insufficient.
[0026] The top of the central column 11 is a pointed structure, and the central axis of the central column 11 and the central axis of the feed pipe 22 are colinear. When silicon tetrachloride is introduced into the reactor 1 through the feed pipe 22, the silicon tetrachloride falls onto the central column 11 or is evenly scattered into the reactor 1 from the side of the central column 11. The central column 11 plays a guiding role, so that the silicon tetrachloride is more evenly scattered into the reactor 1. It should be noted that the feed pipe 22 is provided with an electric opening and closing valve 4 near the first feed port 221, and the opening and closing of the first feed port 221 is controlled by the electric opening and closing valve 4; firstly, the first feed port 221 is opened, and silicon tetrachloride is added into the reactor 1 through the feed tank 2, and then the first feed port 221 is closed by the electric opening and closing valve 4, and the second feed port 222 is opened, and the catalyst is added through the second feed port 222.
[0027] The central column 11 of the present application is arranged at the center of the reactor 1, so that the reaction temperature can be measured more accurately by the temperature sensor. In other embodiments, stirring blades can be arranged around the central column 11, and the stirring of the stirring blades can make the chemical reaction in the reactor 1 more complete.
[0028] The reactor 1 is also sleeved and fixed with multiple ventilation pipes 3 along its height direction, and nitrogen is introduced into the reactor 1 through the ventilation pipes 3; nitrogen is introduced into the reactor 1 through the ventilation pipes 3. On the one hand, drying and purging in the reactor 1 can be achieved; on the other hand, the nitrogen introduced can make silicon tetrachloride and the catalyst evenly mixed and fully contacted for reaction; on the third hand, the introduction of nitrogen can disperse the heat concentration area when the reaction heat is concentrated, reduce the local temperature during the reaction process, and cause the catalyst to be carbonized and deactivated. It should be noted that the nitrogen mentioned in this application can be replaced by other inert gases, and nitrogen is only one embodiment of the gas introduced, and does not play a role in limiting the type of gas introduced.
[0029] Specifically, a plurality of exhaust holes 31 connected to the interior of the reactor 1 are spaced apart on the inner wall of the ventilation pipe 3, and an exhaust valve 32 with an adjustable angle is provided in each exhaust hole 31. The jet direction of the exhaust valve 32 is set at an angle with the inner wall of the reactor 1, and each exhaust valve 32 is biased clockwise or counterclockwise; in one embodiment, the exhaust valve 32 is 45° to the inner wall of the reactor 1, and is biased clockwise, so that the nitrogen forms a uniform turbulent state in the reactor 1, thereby promoting the uniform distribution and heat exchange of silicon tetrachloride in the reactor 1.
[0030] Furthermore, the bottom of the reactor 1 is also provided with a second vent 12 for introducing nitrogen into the reactor 1, and the second vent 12 is used to achieve disturbance mixing of silicon tetrachloride in the area below the ventilation pipe 3 of the reactor 1, as well as drying and purging of the inner wall of the reactor 1. The bottom of the feed tank 2 is provided with a first vent 23 for introducing nitrogen. Since the feed tank 2 needs to introduce both silicon tetrachloride and catalyst into the reactor 1, in order to reduce the adhesion of silicon tetrachloride to the inner wall of the feed tank 2, the introduction of nitrogen through the first vent 23 can achieve purging inside the feed tank 2, so that silicon tetrachloride and the catalyst can be more stably put into the reactor 1 through the feed tank 2.
[0031] The present application also provides a method for loading and activating a deproportionation catalyst, using the deproportionation reactor, comprising the following steps: S1: Add a feed tank 2 to the spare port on the top of the anti-disproportionation reactor 1; S2: Dry the interior of the reactor 1 until the dew point is lower than -55°C, close the second feed port 222, open the first feed port 221, and add 70% liquid level of silicon tetrachloride into the reactor 1 through the feed tank 2; S3: introducing nitrogen into the reactor 1 through the ventilation pipe 3 and the second ventilation port 12 to increase the disturbance of silicon tetrachloride; S4: After the silicon tetrachloride in the feeding tank 2 is exhausted, nitrogen is continuously introduced into the feeding tank 2 through the first vent 23 to achieve purging of the feeding tank 2 and maintain a nitrogen environment in the feeding tank 2; S5: Close the first feed port 221 and open the second feed port 222, and discharge the catalyst into the reactor 1 through the second feed port 222; during the reaction, control the opening number of the second feed port 222 according to the temperature in the reactor 1, and use the feeding tank 2 to slowly and gradually add the catalyst into the reactor 1 to control the internal temperature below 70°C.
[0032] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims
1. A deproportionation reactor, characterized in that: The method comprises a reactor (1), wherein a feeding tank (2) for adding silicon tetrachloride and a catalyst into the reactor (1) is arranged on the top of the reactor (1); A plurality of ventilation pipes (3) are arranged in the reactor (1) along the height direction of the reactor (1); a first feed port (221) for supplying silicon tetrachloride to the reactor (1) is provided through the bottom of the feed tank (2); a plurality of second feed ports (222) for supplying the catalyst to the reactor (1) are provided on the side wall of the feed tank (2); opening and closing valves are arranged at the plurality of second feed ports (222); and different opening and closing valves are set with different start-up temperature thresholds.
2. A deproportionation reactor according to claim 1, characterized in that: The ventilation pipe (3) is annularly sleeved on the circumference of the reactor (1) and is used to introduce nitrogen into the reactor (1); A plurality of exhaust holes (31) communicating with the interior of the reactor (1) are provided at intervals on the inner wall of the ventilation pipe (3).
3. A deproportionation reactor according to claim 2, characterized in that: A plurality of the exhaust holes (31) are each provided with an exhaust valve (32) capable of adjusting an angle, the jetting direction of the exhaust valve (32) being arranged at an angle with the inner wall of the reactor (1), and each exhaust valve (32) is inclined in a clockwise or counterclockwise direction.
4. A deproportionation reactor according to claim 1, characterized in that: The reactor (1) is provided with a central column (11), and a plurality of temperature sensors are arranged at intervals along the height direction on the central column (11), and the temperature sensors are electrically connected to the start valve of the second feed port (222).
5. A deproportionation reactor according to claim 4, characterized in that: The feeding tank (2) comprises a feeding hopper (21) and a feeding pipe (22) extending into the reactor (1); the second feeding ports (222) are circumferentially arranged on the circumferential side of the feeding pipe (22); and the second feeding ports (222) are arranged in multiple layers at intervals; the opening and closing valves of the second feeding ports (222) in each layer have different actuation temperature thresholds.
6. A deproportionation reactor according to claim 5, characterized in that: The top of the central column (11) is a pointed structure, and the central axis of the central column (11) and the central axis of the feed pipe (22) are collinear.
7. A deproportionation reactor according to claim 6, characterized in that: The feed pipe (22) is rotatably connected to the feed hopper (21), and the feed tank (2) comprises a driving source for driving the feed pipe (22) to rotate.
8. The anti-disproportionation reactor according to claim 1, characterized in that: The bottom of the feeding tank (2) is provided with a first vent (23), and the bottom of the reactor (1) is provided with a second vent (12).
9. A deproportionation reactor according to claim 6, characterized in that: An electric on-off valve (4) for controlling the opening and closing of the first feed port (221) is provided at the bottom of the feed pipe (22).
10. A method for loading and activating a deproportionation catalyst, using a deproportionation reactor as claimed in any one of claims 1 to 9, characterized in that: The following steps are involved: S1: installing a feed tank (2) at the spare port on the top of the anti-disproportionation reactor (1); S2: Dry the interior of the reactor (1) to a dew point lower than -55°C, close the second feed inlet (222), open the first feed inlet (221), and add 70% liquid level of silicon tetrachloride into the interior of the reactor (1) through the feed tank (2); S3: introducing nitrogen into the reactor (1) through the ventilation pipe (3) and the second ventilation port (12) to increase the disturbance of silicon tetrachloride; S4: After the silicon tetrachloride in the feeding tank (2) is completely discharged, nitrogen is continuously introduced into the feeding tank (2) through the first vent (23) to achieve flushing of the feeding tank (2) and maintain a nitrogen environment in the feeding tank (2); S5: closing the first feed port (221), controlling the number of second feed ports (222) opened according to the temperature in the reactor (1), and using the feed tank (2) to slowly and gradually add the catalyst into the reactor (1), controlling the internal temperature to be below 70°C.