Arsenic trichloride preparation reaction device

Abstract

The utility model provides an arsenic trichloride preparation reaction device, which belongs to the technical field of reaction furnaces, and comprises a chlorination column, a packed column and a tail gas absorption tower, one side of the chlorination column is provided with a chlorine gas inlet hole, a bottom pipeline is arranged between the packed column and the chlorination column, and the tail gas absorption tower is arranged in the bottom pipeline. One side of the bottom pipeline is provided with a discharge pipe, the discharge pipe is communicated with the bottom pipeline, the side part of the packed column is provided with an exhaust pipe, and the exhaust pipe is connected with the tail gas absorption tower. A temperature and pressure safety interlocking system is jointly formed, alarm values and cut-off values are set for the temperature and the pressure, when the temperature of a chlorination column and the temperature of a filler column reach the alarm values, automatic alarm is conducted, chlorine supply is automatically cut off and automatically converted into nitrogen supply when the temperature and the pressure of a tank body reach the cut-off values, and safe operation of chlorination can be guaranteed; by adding the filler column, chlorine which is not completely reacted in the chlorination column enters the filler column through a pipeline to continue chlorination reaction.

Description

Technical Field

[0001] The utility model relates to the technical field of reaction furnaces, in particular to an arsenic trichloride preparation reaction device. Background Art

[0002] Arsenic trichloride is a highly corrosive and toxic inorganic compound that is widely used in chemical synthesis, semiconductor manufacturing, and drug development. Its preparation technology is used in both industry and laboratories. It mainly uses solid arsenic as a raw material to react with chlorine to produce liquid arsenic trichloride. According to the characteristics of arsenic trichloride and chlorine themselves, the reaction process and products need to be strictly controlled to eliminate safety hazards and the possibility of environmental pollution. In addition, arsenic trichloride is highly toxic and corrosive, and the preparation of arsenic trichloride needs to be carried out in an environment with good ventilation and safety protection measures. With the development of the chemical industry, the technology for preparing arsenic trichloride has been continuously improved to improve efficiency and safety.

[0003] In the current prior art, when preparing arsenic trichloride, it is impossible to monitor the temperature of the chlorination reaction process in real time, and the reaction process will also produce corrosive gases, and the chlorine reaction is incomplete and the tail gas generated by the volatilization of arsenic trichloride is not completely absorbed, which greatly reduces the safety and operability of the environment. In the prior art, it is also impossible to monitor the sudden increase in temperature during the combustion phenomenon in the reaction process in real time, which has a large safety hazard and the possibility of explosion. When the temperature rises and there is a safety hazard, the chlorine cannot be cut off in time, which also causes the chlorination reaction to be unable to run safely. Utility Model Content

[0004] In order to make up for the above shortcomings, the utility model provides an arsenic trichloride preparation reaction device which overcomes the above technical problems or at least partially solves the above problems.

[0005] The utility model is achieved in this way:

[0006] The utility model provides an arsenic trichloride preparation reaction device, comprising a chlorination column, a packing column and a tail gas absorption tower, wherein a chlorine gas inlet hole is arranged on one side of the chlorination column, a bottom pipeline is arranged between the packing column and the chlorination column, a discharge pipe is arranged on one side of the bottom pipeline, the discharge pipe and the bottom pipeline are connected, an exhaust pipe is arranged on the side of the packing column, the exhaust pipe is connected to the tail gas absorption tower, a connecting pipe is arranged on one side of the chlorination column, and one end of the connecting pipe is connected to the side of the packing column.

[0007] In one embodiment of the utility model, the bottoms of the chlorination column, the packing column and the tail gas absorption tower are all provided with supporting legs around them.

[0008] In one embodiment of the utility model, an observation hole is provided at the front of the chlorination column, a first hand hole is provided at the other side of the chlorination column, and a second hand hole is provided at the side of the packing column.

[0009] In one embodiment of the utility model, a chlorine gas inlet hole on the side of the chlorination column is provided with a special-shaped tube, a gas dissipation structure is provided inside the chlorination column, a flow meter is provided on the single-row tube of the special-shaped tube, and a first solenoid valve and a second solenoid valve are provided on the double-row tube of the special-shaped tube.

[0010] In one embodiment of the utility model, a gas dispersion structure is provided in the packing column, a first pressure sensor and a first machine pressure gauge are provided on the top of one side of the packing column, a first temperature sensor located on the second hand hole is provided on one side of the packing column, the packing column is provided with an exhaust pipe, and an exhaust absorption tower is provided on one side of the exhaust pipe.

[0011] In one embodiment of the utility model, a second pressure sensor and a second machine pressure gauge are provided on the top of one side of the chlorination column, and a second temperature sensor is provided on the first hand hole.

[0012] In one embodiment of the utility model, a first logic controller is provided on the side of the packing column, and the first logic controller is electrically connected to the first pressure sensor and the first machine pressure gauge respectively. A second logic controller is provided on the side of the chlorination column, and the second logic controller is electrically connected to the second pressure sensor, the second temperature sensor, the first solenoid valve and the second solenoid valve respectively.

[0013] The utility model provides an arsenic trichloride preparation reaction device, and its beneficial effects include:

[0014] 1. A temperature and pressure safety interlocking system is formed by setting a flow meter, a first temperature sensor, a first pressure sensor, a first machine pressure gauge, a second pressure sensor, a second machine pressure gauge, a second temperature sensor, a first solenoid valve, a second solenoid valve, a first logic controller and a second logic controller, etc., and setting alarm values ​​and cut-off values ​​for temperature and pressure. When the temperature of the chlorination column and the packing column reaches the alarm value, an automatic alarm is given, and when the temperature and pressure of the tank reach the cut-off value, the chlorine supply is automatically cut off and automatically switched to nitrogen supply, so as to ensure that the chlorination can operate safely.

[0015] 2. By setting up a chlorination column gas dispersion structure, a packing column and a tail gas absorption tower, the reaction efficiency of chlorine is improved, and the excess chlorine in the reaction process enters the packing column for secondary reaction, so that the chlorine is fully utilized, the generation of waste gas is reduced, and the environmental conditions are improved.

[0016] 3. By setting up an exhaust gas absorption tower, the toxic gases generated by the volatilization of residual chlorine and arsenic trichloride are collected and treated in a centralized manner, which improves the indoor environment and avoids the pollution of the environment caused by the exhaust gas generated. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solution of the implementation mode of the utility model, the drawings required for use in the implementation mode will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the utility model and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without paying creative work.

[0018] Figure 1 It is a structural schematic diagram provided by an embodiment of the utility model;

[0019] Figure 2 A schematic diagram of the control relationship provided for an implementation mode of the utility model.

[0020] In the figure: 1, chlorination column; 102, chlorine gas inlet hole; 103, observation hole; 104, first hand hole; 2, packing column; 202, second hand hole; 3, special-shaped pipe; 301, bottom pipe; 302, discharge pipe; 303, exhaust pipe; 304, connecting pipe; 4, flow meter; 401, first temperature sensor; 402, first pressure sensor; 403, first machine pressure gauge; 404, second pressure sensor; 405, second machine pressure gauge; 406, second temperature sensor; 407, first solenoid valve; 408, second solenoid valve; 5, first logic controller; 6, second logic controller; 7, tail gas absorption tower; 8, gas dispersion structure. DETAILED DESCRIPTION

[0021] In order to make the purpose, technical solution and advantages of the implementation of the utility model clearer, the technical solution in the implementation of the utility model will be clearly and completely described below in conjunction with the drawings in the implementation of the utility model. Obviously, the described implementation is a part of the implementation of the utility model, not all of the implementations. Based on the implementation of the utility model, all other implementations obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model. Example

[0022] Reference Figure 1-Figure 2The technical scheme provides an arsenic trichloride preparation reaction device, comprising a chlorination column 1, a packing column 2 and a tail gas absorption tower 7, wherein a chlorine gas inlet hole 102 is provided on one side of the chlorination column 1, a bottom pipe 301 is provided between the packing column 2 and the chlorination column 1, a discharge pipe 302 is provided on one side of the bottom pipe 301, and the discharge pipe 302 and the bottom pipe 301 are connected, an exhaust pipe 303 is provided on the side of the packing column 2, and a tail gas absorption tower 7 is provided on one side of the exhaust pipe, a connecting pipe 304 is provided on one side of the chlorination column 1, one end of the connecting pipe 304 is connected to the side of the packing column 2, and an observation hole 103 is provided at the front of the chlorination column 1.

[0023] Solid arsenic material is put into the chlorination column 1 through the upper cover, and chlorine gas with a set flow rate is introduced through the chlorine gas inlet hole 102 to perform a chlorination reaction to generate liquid arsenic trichloride, which is discharged from the bottom pipe 301, and the liquid level is observed through the observation hole 103;

[0024] At the same time, excess chlorine is introduced into the packing column 2 through the connecting pipe 304 to react with the remaining chlorine, thereby improving the utilization rate of chlorine and reducing the amount of tail gas generated. Finally, the tail gas is discharged to the tail gas absorption tower through the exhaust pipe 303 for tail gas absorption treatment.

[0025] In one embodiment of the utility model, the chlorination column 1, the packing column 2 and the tail gas absorption tower 7 are all provided with feet around the bottom to increase the contact area with the ground and improve the stability of the device.

[0026] In one embodiment of the present invention, a first hand hole 104 is provided on the other side of the chlorination column 1 , and a second hand hole 202 is provided on the side of the packing column 2 .

[0027] In one embodiment of the utility model, a chlorine gas inlet hole 102 on the side of the chlorination column 1 is provided with a special-shaped tube 3, a flow meter 4 is provided on a single row of the special-shaped tube 3, a gas dispersing structure 8 is provided in the chlorination column, and a first solenoid valve 407 and a second solenoid valve 408 are provided on a double row of the special-shaped tube 3.

[0028] In one embodiment of the utility model, a gas dispersion structure 8 is provided inside the packing column 2, a first pressure sensor 402 and a first machine pressure gauge 403 are provided on the top of one side of the packing column 2, a first temperature sensor 401 located on the second hand hole 202 is provided on one side of the packing column 2, and a tail gas absorption tower 7 is provided on one side of the packing column 2.

[0029] In one embodiment of the utility model, a second pressure sensor 404 and a second machine pressure gauge 405 are provided on the top of one side of the chlorination column 1 , and a second temperature sensor 406 is provided on the first hand hole 104 .

[0030] In one embodiment of the utility model, a first logic controller 5 is provided on the side of the packing column 2, and the first logic controller 5 is electrically connected to the first pressure sensor 402 and the first machine pressure gauge 403 respectively; a second logic controller 6 is provided on the side of the chlorination column 1, and the second logic controller 6 is electrically connected to the second pressure sensor 404, the second temperature sensor 406, the first solenoid valve 407 and the second solenoid valve 408 respectively; in the preparation process of arsenic trichloride, the preparation device can monitor the temperature and pressure of the reaction process, automatically interlock, have good safety performance, large contact area, high reaction efficiency, can timely detect abnormal changes in temperature and pressure, and prevent the occurrence of dangerous situations. When the temperature is too high and may cause the reactant to decompose or explode, the monitoring system can issue an alarm in time, which is convenient for taking emergency cooling measures, which is helpful to optimize the reaction conditions. By analyzing the temperature and pressure data, the most suitable reaction parameters can be found, the selectivity and yield of the reaction can be improved, and it is determined at what temperature and pressure arsenic trichloride can be generated to the greatest extent, while reducing side reactions.

[0031] A second temperature sensor 406 and a first temperature sensor 401 are respectively arranged on the first hand hole 104 and the second hand hole 202, a first pressure sensor 404 and a second pressure sensor 402 are respectively arranged on the chlorination column 1 and the packing column 2, and a first machine pressure gauge 403 and a second machine pressure gauge 405 are arranged, and a flow meter 4 is arranged on the single row pipe, and the temperature sensor, the pressure sensor, the flow meter, the solenoid valve and the machine pressure gauge together constitute a temperature and pressure safety interlocking system, and alarm values ​​and cut-off values ​​are set for the temperature and pressure. When the temperature of the chlorination column 1 and the packing column 2 reaches the alarm value, an automatic alarm is given, and when the temperature and pressure of the chlorination column 1 reach the cut-off value, the chlorine supply is automatically cut off and automatically converted to nitrogen supply, so as to ensure that the chlorination can operate safely.

[0032] The tail gas absorption tower 7 is located on one side of the tail gas pipe 303, and the gas dispersion structure 8 is respectively located inside the chlorination column 1 and the packing column 2. After the chlorine enters the chlorination column through 102, it passes through the chlorination column evenly through the gas dispersion pipe 8, so that the chlorine reaction is fully carried out. The incompletely reacted chlorine enters the gas dispersion structure 8 of the packing column 2 through the tail gas pipe 304, and the secondary chlorination reaction of the remaining chlorine is carried out, so that the chlorine reaction is complete, thereby reducing the generation of waste gas from the source.

[0033] A tail gas absorption tower 7 is provided on one side of the tail gas pipe 303. The residual chlorine in the packing column 2 and the volatilized arsenic trichloride gas in the chlorination column 1 and the packing column 2 enter the tail gas absorption tower 7 through the tail gas pipe 303. The tail gas absorption tower 7 collects and processes the residual chlorine and the volatilized arsenic trichloride gas, thereby improving the environmental conditions.

[0034] Specifically, the working process or working principle of the arsenic trichloride preparation reaction device is as follows: solid arsenic material is put into the metal chlorination column 1, and chlorine gas with a set flow rate is introduced through the chlorine gas inlet hole 102 to perform a chlorination reaction to generate liquid arsenic trichloride, and the arsenic trichloride is discharged from the bottom pipeline 301, and then the liquid level is observed through the observation hole 103, and the excess chlorine gas is introduced into the packing column 2 through the connecting pipe 304 to perform a residual chlorine reaction, thereby improving the utilization rate of chlorine gas and reducing the amount of tail gas generated, and finally the tail gas is discharged through the discharge pipe 302 to the external tail gas absorption tower 7 for tail gas absorption treatment, thereby improving the environmental conditions, and the flow meter 4. The first temperature sensor 401, the first pressure sensor 402, the first machine pressure gauge 403, the second pressure sensor 404, the second machine pressure gauge 405, the second temperature sensor 406, the first solenoid valve 407, the second solenoid valve 408, the first logic controller 5 and the second logic controller 6 together constitute a temperature and pressure safety interlocking system, and alarm values ​​and cut-off values ​​are set for temperature and pressure. When the temperature of the packing column 2 reaches the alarm value, an automatic alarm is given, and when the temperature and pressure of the tank reach the cut-off value, the chlorine supply is automatically cut off and automatically switched to nitrogen supply, so as to ensure that the chlorination can operate safely.

Claims

1. An arsenic trichloride preparation reaction device, comprising a chlorination column (1), a packing column (2) and a tail gas absorption tower (7), characterized in that: A chlorine gas inlet hole (102) is provided on one side of the chlorination column (1); a bottom pipe (301) is provided between the packing column (2) and the chlorination column (1); a discharge pipe (302) is provided on one side of the bottom pipe (301); the discharge pipe (302) and the bottom pipe (301) are connected; an exhaust pipe (303) is provided on the side of the packing column (2); the exhaust pipe (303) is connected to a tail gas absorption tower (7); a connecting pipe (304) is provided on one side of the chlorination column (1); one end of the connecting pipe (304) is connected to the side of the packing column (2); and a gas dispersion structure (8) is provided in the chlorination column and the packing column.

2. The arsenic trichloride preparation reaction device according to claim 1, characterized in that: The bottoms of the chlorination column (1), the packing column (2) and the tail gas absorption tower (7) are all provided with supporting legs around them.

3. A arsenic trichloride preparation reaction device according to claim 1, characterized in that: The front of the chlorination column (1) is provided with an observation hole (103), the other side of the chlorination column (1) is provided with a first hand hole (104), the side of the packing column (2) is provided with a second hand hole (202), and the interior of the chlorination column (1) is provided with a gas dispersion structure (8).

4. A reaction device for preparing arsenic trichloride according to claim 3, characterized in that: A shaped tube (3) is provided on the chlorine gas inlet hole (102) on the side of the chlorination column (1), a flow meter (4) is provided on the single-row tube of the shaped tube (3), and a first solenoid valve (407) and a second solenoid valve (408) are provided on the double-row tube of the shaped tube (3).

5. A reaction device for preparing arsenic trichloride according to claim 4, characterized in that: A first pressure sensor (402) and a first machine pressure gauge (403) are provided at the top of one side of the packing column (2), a first temperature sensor (401) located on the second hand hole (202) is provided at one side of the packing column (2), and a gas dispersion structure (8) is provided inside the packing column (2).

6. The arsenic trichloride preparation reaction device according to claim 5, characterized in that: A second pressure sensor (404) and a second machine pressure gauge (405) are provided on the top of one side of the chlorination column (1), and a second temperature sensor (406) is provided on the first hand hole (104).

7. The arsenic trichloride preparation reaction device according to claim 1, characterized in that: A first logic controller (5) is provided on the side of the packing column (2), and the first logic controller (5) is electrically connected to a first pressure sensor (402) and a first machine pressure gauge (403) respectively. A second logic controller (6) is provided on the side of the chlorination column (1), and the second logic controller (6) is electrically connected to a second pressure sensor (404), a second temperature sensor (406), a first solenoid valve (407), and a second solenoid valve (408) respectively.

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