CN217961975U - Nitrogen trifluoride electrolysis trough positive pole tail gas recovery processing device - Google Patents
Nitrogen trifluoride electrolysis trough positive pole tail gas recovery processing device Download PDFInfo
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- CN217961975U CN217961975U CN202222382606.9U CN202222382606U CN217961975U CN 217961975 U CN217961975 U CN 217961975U CN 202222382606 U CN202222382606 U CN 202222382606U CN 217961975 U CN217961975 U CN 217961975U
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Abstract
The utility model provides a nitrogen trifluoride electrolysis trough anode tail gas recovery processing device, including electrolysis trough, falling liquid film absorber, caustic wash tower, except that water tower, knockout tower and crude jar, the electrolysis trough is connected with cooling water outlet pipe and washing water conveyer pipe through first duct connection falling liquid film absorber on the falling liquid film absorber, and the falling liquid film absorber is connected with the hydrofluoric acid drain pipe, and the falling liquid film absorber passes through second duct connection caustic wash tower, and the lower extreme of caustic wash tower connects the circulating equipment. The utility model discloses a falling liquid film absorber retrieves hydrogen fluoride in the electrolysis trough anode tail gas to make 50% hydrofluoric acid, make full use of the material, retrieve the nitrogen trifluoride in the electrolysis trough anode tail gas through the knockout tower, improved the product yield, realized sustainable development, very big reduction manufacturing cost, strengthened recycle's practicality.
Description
Technical Field
The utility model belongs to the technical field of fine chemistry industry, concretely relates to nitrogen trifluoride electrolysis trough anode tail gas recovery processing device.
Background
NF 3 Gases are widely used in the electronics industry as etchants and cleaning agents. NF 3 The gas production methods are classified into direct chemical methods and electrolytic methods. The direct chemical method adopts a chemical reaction form to prepare NF 3 But the process is not easy to control, and the chemical reaction process is complex; electrolysis process using electrolytic fusion of NH 4 The NF can be prepared by only one step from the F-xHF mixture 3 And the used equipment has low production cost and high product yield, so the electrolytic method is widely applied in the industry。
Electrolytic production of NF 3 In the process, the electrolytic cell can continuously generate anode tail gas, the main components of which are nitrogen, nitrogen trifluoride and hydrogen fluoride, wherein patent CN114028900A introduces a method for treating the anode tail gas of the electrolytic cell, nitrogen trifluoride is firstly cracked, then hydrogen fluoride is removed by adopting alkali washing, the nitrogen trifluoride and the hydrogen fluoride are not recovered, so that resource waste is caused, and aiming at the defects, a treatment device for recovering the anode tail gas of the nitrogen trifluoride electrolytic cell needs to be designed to improve the resource utilization rate.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that the not enough to above-mentioned prior art provides a nitrogen trifluoride electrolysis trough anode tail gas recovery processing device, and the device structural design scientific and reasonable, easy operation can carry out recycle to remaining material, improves the product yield, has reduced the wasting of resources, has reduced manufacturing cost.
In order to solve the technical problem, the utility model discloses a technical scheme is: the utility model provides a nitrogen trifluoride electrolysis trough anode tail gas recovery processing device, its characterized in that, includes electrolysis trough, falling film absorber, caustic wash tower, removes water tower, knockout tower and crude jar, the electrolysis trough is through first conveyer pipe connection falling film absorber, the falling film absorber passes through second conveyer pipe connection caustic wash tower, the caustic wash tower removes the water tower through fourth conveyer pipe connection, it passes through seventh conveyer pipe connection knockout tower to remove the water tower, the knockout tower removes the water tower through fifth conveyer pipe connection, the knockout tower passes through sixth conveyer pipe connection crude jar.
Preferably, the alkaline tower is connected with a third conveying pipe, the third conveying pipe is provided with a circulating pump, one end of the third conveying pipe is connected to the bottom of the alkaline tower, the other end of the third conveying pipe penetrates through the upper part of the side part of the alkaline tower and extends into the alkaline tower to be connected with a spraying pipe, the spraying pipe is provided with a plurality of nozzles at equal intervals, and the spraying pipe is fixedly installed on the inner wall of the alkaline tower.
Preferably, the separation tower is connected with a liquid nitrogen inlet pipe and a nitrogen evacuation pipe, the water removal tower is connected with a nitrogen evacuation pipe, and the falling film absorber is connected with a hydrofluoric acid outlet pipe, a cooling water outlet pipe and a washing water conveying pipe.
Preferably, a cooling water upper water pipe is connected to the falling film absorber.
Preferably, the working temperature of the electrolytic cell is 70-100 ℃, the working pressure is-0.005 Mpa, the tube pass working temperature of the falling film absorber is 10-40 ℃, the tube pass working pressure is-0.005 Mpa, the shell pass working temperature of the falling film absorber is 7-18 ℃, and the shell pass working pressure is 0.2-0.3 Mpa; the working temperature of the alkaline washing tower is 10-40 ℃, and the working pressure is-0.02 to-0.01 Mpa; the working temperature of the water removal tower is-110 to-90 ℃, and the working pressure is-0.02 to-0.01 Mpa; the working temperature of the separation tower in the collection stage is-150 to-120 ℃, and the working pressure is-0.02 to-0.01 Mpa; the working temperature of the separation tower in the exhaust stage is-120 to 20 ℃, and the working pressure is 0.1 to 0.2Mpa.
Compared with the prior art, the utility model has the following advantage:
1. the utility model discloses structural design scientific and reasonable, through absorption of falling liquid film absorber, the water that sprays in the alkaline washing tower, the water removal tower that washes with alkaline, separation in the knockout tower finally obtain nitrogen trifluoride and the hydrofluoric acid that has the reutilization value, effectively reduce the wasting of resources, improve economic benefits, reduce cost drops into.
2. The utility model discloses the input cost is low, easy operation, and recovery efficiency is high, retrieves effectually, safe and reliable.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Description of reference numerals:
1-an electrolytic cell; 2-falling film absorber; 3-alkaline washing tower;
4-water removal tower; 5-a separation column; 6, a crude product tank;
7-cooling the upper water pipe; 8-hydrofluoric acid drain pipe; 9-cooling water outlet pipe;
10-washing water delivery pipe; 11-nitrogen vent pipe; 12-liquid nitrogen inlet pipe;
13-nitrogen evacuation tube; 14-a first delivery pipe; 15-a second delivery pipe;
16-a third delivery pipe; 17-a circulating pump; 18-a fourth delivery pipe;
19-a fifth delivery pipe; 20-sixth delivery pipe; 21-seventh delivery pipe
Detailed Description
As shown in fig. 1, the utility model discloses an including electrolysis trough 1, falling liquid film absorber 2, alkaline tower 3, water removal tower 4, knockout tower 5 and crude jar 6, electrolysis trough 1 connects the left side wall upper portion of falling liquid film absorber 2 through first conveyer pipe 14, the left side wall lower part of alkaline tower 3 is connected through second conveyer pipe 15 to the bottom of falling liquid film absorber 2, the left side wall lower part of removing water tower 4 is connected through fourth conveyer pipe 18 in the top of alkaline tower 3, the knockout tower 5 is connected through seventh conveyer pipe 21 in the right side wall upper portion of removing water tower 4, the top of removing water tower 4 is connected through fifth conveyer pipe 19 in the right side wall lower part of knockout tower 5, the crude jar 6 is connected through sixth conveyer pipe 20 in the top of knockout tower 5.
In this embodiment, a third delivery pipe 16 is connected to the alkaline washing tower 3, a circulation pump 17 is installed on the third delivery pipe 16, one end of the third delivery pipe 16 is connected to the bottom of the alkaline washing tower 3, the other end of the third delivery pipe passes through the upper portion of the right side wall of the alkaline washing tower 3 and extends into the alkaline washing tower 3 to be connected with a spray pipe, a plurality of spray nozzles are equidistantly arranged on the spray pipe, and the spray pipe is fixedly installed on the inner wall of the alkaline washing tower 3.
In this embodiment, the top of separation tower 5 is connected with liquid nitrogen feed liquor pipe 12 and nitrogen gas evacuation pipe 13, nitrogen gas blow-down pipe 11 is connected at the top that removes water tower 4, the bottom of falling film absorber 2 is connected with hydrofluoric acid drain pipe 8, and cooling water outlet pipe 9 is connected on the right side wall upper portion of falling film absorber 2, and washing water conveyer pipe 10 is connected at the top of falling film absorber 2.
In this embodiment, a cooling water supply pipe 7 is connected to a lower portion of a left side wall of the falling film absorber 2.
In this example, the target of electrolysis in the electrolytic cell 1 was NH 4 F-xHF, the working temperature of the electrolytic bath 1 is 70-100 ℃, the working pressure is-0.005 Mpa, the tube pass working temperature of the falling film absorber 2 is 10-40 ℃, the tube pass working pressure is-0.005 Mpa, the shell pass working temperature of the falling film absorber 2 is 7-18 ℃, and the shell pass working pressure is 0.2-0.3 Mpa; the working temperature of the alkaline washing tower 3 is 10-40 ℃, and the working pressure is-0.02 to-0.01 Mpa; the working temperature of the water removal tower 4 is-110 to-90 ℃, and the working pressure is-0.02 to-0.01 Mpa; the working temperature of the separation tower 5 in the collection stage is-150 to-120 ℃, and the working pressure is-0.02 to-0.01 Mpa; the working temperature of the separation tower 5 in the exhaust stage is-120 to 20 ℃, and the working pressure is 0.1 to 0.2Mpa.
The falling film absorber in this example is model YK. i-60-12/12-50.
In this embodiment, the separation tower 5 is connected to an external vacuum pumping system through a nitrogen pumping port 13; a heat exchange tube is arranged in the separation tower 5 and is connected with a liquid nitrogen inlet tube 12, liquid nitrogen is introduced into the heat exchange tube in the collection stage, nitrogen trifluoride gas is liquefied, nitrogen is pumped by a vacuum pumping system, and nitrogen trifluoride and nitrogen are separated; after the collection is finished, the bottom of the separation tower 5 is heated by an external heating furnace, and the nitrogen trifluoride is vaporized and enters a crude product tank for storage.
When the device is used, anode tail gas of an electrolytic tank containing nitrogen, hydrogen fluoride and nitrogen trifluoride enters the top of a falling film absorber 2 through a first conveying pipe 14, washing water is introduced into the top of the falling film absorber 2, the anode tail gas and the washing water are mixed in a pipe pass, hydrogen fluoride impurities are absorbed by the water, the anode tail gas containing nitrogen, nitrogen trifluoride and a very small amount of hydrogen fluoride flows out of a gas outlet at the bottom of the falling film absorber 2 and enters an alkaline tower 3, hydrofluoric acid flows out of a hydrofluoric acid liquid outlet pipe 8 at the bottom of the falling film absorber 2 and is stored in an acid tank, heat emitted when the hydrogen fluoride is absorbed by cooling water in a shell pass of the falling film absorber 2, the anode tail gas enters the lower part of the alkaline tower 3 and flows out of the top of the alkaline tower 3, a potassium hydroxide solution with the mass fraction of 18% is sprayed on the upper part of the alkaline tower 3, and the solution is discharged from the bottom of the tower and is circularly sprayed through a circulating pump 17 for use; the anode tail gas discharged from the alkaline washing tower 3 enters from the lower part of the water removal tower 4 and flows out from the top of the tower, cold nitrogen in the water removal tower 4 is discharged from the separation tower 5, moisture in the anode tail gas is removed through cooling, and nitrogen at the outlet of the water removal tower 4 is discharged to the air; the water removal tower 4 sends the anode tail gas into a separation tower 5, a heat exchange tube is arranged in the separation tower 5, liquid nitrogen is introduced into the heat exchange tube in the collection stage, nitrogen trifluoride gas is liquefied, nitrogen is pumped by a vacuum pumping system, and the nitrogen trifluoride and the nitrogen are separated; after collection is complete, the separation column 5 is heated and the nitrogen trifluoride is vaporized into a crude product tank 6 for storage.
Application example 1
The flow of the anode tail gas of the electrolytic cell is 50m 3 H, nitrogen content 80%, hydrogen fluoride 10%, nitrogen trifluoride 10%.
The working temperature of the electrolytic bath 1 is 70 ℃, and the working pressure is-0.005 MPa; the working temperature of the tube pass of the falling film absorber 2 is 10 ℃, the working pressure is-0.005 MPa, the working temperature of the shell pass is 7 ℃, and the working pressure is 0.3MPa; the working temperature of the alkaline washing tower 3 is 10 ℃, and the working pressure is-0.02 MPa; the working temperature of the water removal tower 4 is minus 110 ℃, and the working pressure is minus 0.02MPa; the working temperature of the separation tower 5 in the collection stage is-150 ℃, the working pressure is-0.02 MPa, the working temperature in the exhaust stage is (-150-20) DEG C, and the working pressure is (0.1-0.2) MPa.
Example 2
The flow and the components of the anode tail gas of the electrolytic cell are the same as those of the application example 1;
the working temperature of the electrolytic cell 1 is 80 ℃, and the working pressure is 0MPa; the working temperature of the tube pass of the falling film absorber 2 is 23 ℃, the working pressure is 0MPa, the working temperature of the shell pass is 12 ℃, and the working pressure is 0.3MPa; the working temperature of the alkaline washing tower 3 is 25 ℃, and the working pressure is-0.015 MPa; the working temperature of the water removal tower 4 is-100 ℃, and the working pressure is-0.015 MPa; the working temperature of the separation tower 5 in the collection stage is-130 ℃, the working pressure is-0.015 MPa, the working temperature in the exhaust stage is (-130-20) DEG C, and the working pressure is (0.1-0.2) MPa.
Example 3
The flow and the components of the anode tail gas of the electrolytic cell are the same as those of the application example 1;
the working temperature of the electrolytic bath 1 is 100 ℃, and the working pressure is 0.005MPa; the working temperature of the tube pass of the falling film absorber 2 is 40 ℃, the working pressure is 0.005MPa, the working temperature of the shell pass is 18 ℃, and the working pressure is 0.3MPa; the working temperature of the alkaline washing tower 3 is 40 ℃, and the working pressure is-0.01 MPa; the working temperature of the water removal tower 4 is minus 90 ℃, and the working pressure is minus 0.01MPa; the working temperature of the separation tower 5 in the collection stage is-120 ℃, the working pressure is-0.01 MPa, the working temperature in the exhaust stage is-120-20 ℃, and the working pressure is (0.1-0.2) MPa.
The hydrofluoric acid yields and nitrogen trifluoride recovery for the three application examples are shown in table 1:
TABLE 1
According to the application examples, 50% hydrofluoric acid (56-64) t can be produced annually, nitrogen trifluoride (112-115) t can be recovered annually, materials can be recovered sufficiently, and excessive resource waste is avoided.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modifications, changes and equivalent changes made to the above embodiments according to the technical spirit of the present invention all fall within the protection scope of the technical solution of the present invention.
Claims (4)
1. The utility model provides a nitrogen trifluoride electrolysis trough anode tail gas recovery processing apparatus, its characterized in that, includes electrolysis trough (1), falling film absorber (2), caustic wash tower (3), removes water tower (4), knockout tower (5) and crude jar (6), electrolysis trough (1) is through first conveyer pipe (14) connection falling film absorber (2), falling film absorber (2) are through second conveyer pipe (15) connection caustic wash tower (3), caustic wash tower (3) are through fourth conveyer pipe (18) connection removal water tower (4), remove water tower (4) and connect knockout tower (5) through seventh conveyer pipe (21), knockout tower (5) are through fifth conveyer pipe (19) connection removal water tower (4), knockout tower (5) are through sixth conveyer pipe (20) connection crude jar (6).
2. The nitrogen trifluoride electrolyzer anode tail gas recovery processing device according to claim 1, characterized in that a third delivery pipe (16) is connected to the caustic tower (3), a circulating pump (17) is installed on the third delivery pipe (16), one end of the third delivery pipe (16) is connected to the bottom of the caustic tower (3), the other end of the third delivery pipe passes through the upper part of the side part of the caustic tower (3) and extends into the caustic tower (3) to be connected with a spray pipe, a plurality of spray heads are arranged on the spray pipe at equal intervals, and the spray pipe is fixedly installed on the inner wall of the caustic tower (3).
3. The recovery and treatment device for anode tail gas of nitrogen trifluoride electrolyzer according to claim 1, characterized in that the separation tower (5) is connected with a liquid nitrogen inlet pipe (12) and a nitrogen gas exhaust pipe (13), the water removal tower (4) is connected with a nitrogen gas vent pipe (11), and the falling film absorber (2) is connected with a hydrofluoric acid outlet pipe (8), a cooling water outlet pipe (9) and a washing water delivery pipe (10).
4. The nitrogen trifluoride electrolyzer anode tail gas recovery processing device according to claim 1, characterized in that a cooling water upper water pipe (7) is connected to the falling film absorber (2).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222382606.9U CN217961975U (en) | 2022-09-08 | 2022-09-08 | Nitrogen trifluoride electrolysis trough positive pole tail gas recovery processing device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202222382606.9U CN217961975U (en) | 2022-09-08 | 2022-09-08 | Nitrogen trifluoride electrolysis trough positive pole tail gas recovery processing device |
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| CN217961975U true CN217961975U (en) | 2022-12-06 |
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| CN202222382606.9U Active CN217961975U (en) | 2022-09-08 | 2022-09-08 | Nitrogen trifluoride electrolysis trough positive pole tail gas recovery processing device |
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- 2022-09-08 CN CN202222382606.9U patent/CN217961975U/en active Active
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