CN216223702U - Device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride - Google Patents
Device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride Download PDFInfo
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- CN216223702U CN216223702U CN202122784630.0U CN202122784630U CN216223702U CN 216223702 U CN216223702 U CN 216223702U CN 202122784630 U CN202122784630 U CN 202122784630U CN 216223702 U CN216223702 U CN 216223702U
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Abstract
The utility model provides a device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride, which comprises a first buffer tank, a primary water-washing absorption tower, a secondary water-washing absorption tower and a second buffer tank, wherein the first buffer tank is communicated with the primary water-washing absorption tower, the first buffer tank is communicated with a primary circulating liquid tank, and the primary water-washing absorption tower is communicated with a gas inlet of the secondary water-washing absorption tower; the first-stage washing absorption tower is communicated with a second graphite heat exchanger, the second-stage washing absorption tower is communicated with a first graphite heat exchanger, and the second-stage washing absorption tower is communicated with a second circulating liquid tank; the second buffer tank is connected with a water ring compressor, the second buffer tank is connected with a secondary circulating liquid tank, and the water ring compressor is externally connected with a neutralization tower; after most of the hydrogen fluoride impurities are removed, the amount of calcium hydroxide used in the neutralization tower is greatly reduced, and the treatment cost is reduced.
Description
Technical Field
The utility model belongs to the technical field of trifluoromethanesulfonyl fluoride purification devices, and particularly relates to a device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride.
Background
The preparation of the trifluoromethanesulfonyl fluoride comprises a photolysis method, a chemical direct fluorination method and an electrolytic method, and the electrolytic method is most widely applied. The electrolytic method adopts methanesulfonyl fluoride or methanesulfonyl chloride and excessive hydrogen fluoride as raw materials, and the produced crude trifluoromethanesulfonyl fluoride gas contains a large amount of hydrogen fluoride impurities and needs to be purified and removed.
Patent CN111116424A reports a method for preparing trifluoromethanesulfonic acid by continuous hydrolysis. The method comprises the steps of introducing trifluoromethanesulfonyl fluoride with hydrogen fluoride into a falling film absorber, and neutralizing and absorbing the hydrogen fluoride by using an alkali metal hydroxide solution. The above method has the following problems:
1. hydrofluoric acid is directly neutralized by alkaline solution and is not reasonably utilized;
2. the use of the alkali metal hydroxide is too high, and the treatment cost is increased.
SUMMERY OF THE UTILITY MODEL
The present invention provides a device for removing hydrogen fluoride from trifluoromethanesulfonyl fluoride, which solves the above-mentioned problems in the prior art.
In order to solve the technical problems, the utility model adopts the technical scheme that: a device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride comprises a first buffer tank, a primary water washing absorption tower, a secondary water washing absorption tower and a second buffer tank, wherein the first buffer tank and the second buffer tank are respectively provided with an air inlet, an air outlet and an acid discharge port;
the gas outlet of the first buffer tank is communicated with a primary washing absorption tower, the acid discharge port of the first buffer tank is communicated with a primary circulating liquid tank, and the gas outlet of the primary washing absorption tower is communicated with the gas inlet of a secondary washing absorption tower;
a circulating liquid inlet of the primary washing absorption tower is communicated with a second graphite heat exchanger, and an acid discharge port of the primary washing absorption tower is also communicated with a primary circulating liquid tank;
the gas outlet of the secondary washing absorption tower is connected with the gas inlet of the second buffer tank, the circulating liquid inlet of the secondary washing absorption tower is communicated with the first graphite heat exchanger, and the acid discharge port of the secondary washing absorption tower is communicated with the secondary circulating liquid tank;
a gas outlet of the second buffer tank is connected with a water ring compressor, an acid discharge port of the second buffer tank is connected with a secondary circulating liquid tank, and the water ring compressor is externally connected with a neutralization tower;
and an acid discharge port of the primary circulating liquid tank is respectively connected with the second graphite heat exchanger and the finished product acid tank, and an acid discharge port of the secondary circulating liquid tank is respectively connected with the first graphite heat exchanger and the primary circulating liquid tank.
Furthermore, a water filling port is formed in a connecting pipeline between the acid discharging port of the second buffer tank and the secondary circulating liquid tank, and a water filling port is also formed in a communicating pipeline between the acid discharging port of the secondary circulating liquid tank and the primary circulating liquid tank.
Furthermore, a first magnetic pump is connected to an acid discharge port of the primary circulating liquid tank, and a second magnetic pump is connected to an acid discharge port of the secondary circulating liquid tank.
Furthermore, the first graphite heat exchanger and the second graphite heat exchanger are respectively externally connected with an independent circulating water interface.
Furthermore, the first buffer tank, the first-stage washing absorption tower, the second buffer tank, the finished product acid tank, the first-stage circulating liquid tank and the second-stage circulating liquid tank are all made of Monel or steel lining PTFE materials.
Further, the first graphite heat exchanger and the second graphite heat exchanger are both round block hole type graphite heat exchangers or floating head tube type graphite heat exchangers, and the heat exchange area of the first graphite heat exchanger and the second graphite heat exchanger is 10-15 m2In the meantime.
Compared with the prior art, the utility model has the following advantages:
most of hydrogen fluoride impurities in the crude trifluoromethanesulfonyl fluoride product gas are removed through water washing, 50% hydrofluoric acid is prepared for sale, and full utilization of materials is achieved; after most of the hydrogen fluoride impurities are removed, the amount of calcium hydroxide used in the neutralization tower is greatly reduced, and the treatment cost is reduced.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
Description of reference numerals:
1-a first buffer tank; 2-first-stage washing absorption tower; 3-a second-stage washing absorption tower; 4-a second buffer tank; 6-a first graphite heat exchanger; 10-a second graphite heat exchanger; 13-finished product acid tank; 14-a first magnetic drive pump; 15-first-stage circulating liquid tank; 16-a second magnetic drive pump; 17-a secondary circulating liquid tank; 18-water ring compressor; 19-neutralization column.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1, as shown in fig. 1, the present invention provides a technical solution: a device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride comprises a first buffer tank 1, a primary water washing absorption tower 2, a secondary water washing absorption tower 3 and a second buffer tank 4, wherein the first buffer tank 1 and the second buffer tank 4 are respectively provided with an air inlet, an air outlet and an acid discharge port;
the gas outlet of the first buffer tank 1 is communicated with a first-stage washing absorption tower 2, the acid discharge port of the first buffer tank 1 is communicated with a first-stage circulating liquid tank 15, and the gas outlet of the first-stage washing absorption tower 2 is communicated with the gas inlet of a second-stage washing absorption tower 3;
a circulating liquid inlet of the primary washing absorption tower 2 is communicated with a second graphite heat exchanger 10, and an acid discharge port of the primary washing absorption tower 2 is also communicated with a primary circulating liquid tank 15;
the gas outlet of the secondary washing absorption tower 3 is connected with the gas inlet of the second buffer tank 4, the circulating liquid inlet of the secondary washing absorption tower 3 is communicated with the first graphite heat exchanger 6, and the acid discharge port of the secondary washing absorption tower 3 is communicated with the secondary circulating liquid tank 17;
a gas outlet of the second buffer tank 4 is connected with a water ring compressor 18, an acid discharge port of the second buffer tank 4 is connected with a secondary circulating liquid tank 17, and the water ring compressor 18 is externally connected with a neutralization tower 19;
and an acid discharge port of the primary circulating liquid tank 15 is respectively connected with the second graphite heat exchanger 10 and the finished product acid tank 13, and an acid discharge port of the secondary circulating liquid tank 17 is respectively connected with the first graphite heat exchanger 6 and the primary circulating liquid tank 15.
And a water filling port is formed in a connecting pipeline between the acid discharging port of the second buffer tank 4 and the secondary circulating liquid tank 17, and a water filling port is also formed in a communicating pipeline between the acid discharging port of the secondary circulating liquid tank 17 and the primary circulating liquid tank 15.
The acid discharge port of the primary circulating liquid tank 15 is connected with a first magnetic pump 14, and the acid discharge port of the secondary circulating liquid tank 17 is connected with a second magnetic pump 16.
When the device is used, the trifluoromethanesulfonyl fluoride gas with hydrogen fluoride impurities enters the first buffer tank 1 through a valve and a pipeline, the working temperature of the first buffer tank 1 is 30-50 ℃, the working pressure is 0-0.1 MPa, water vapor in the first-stage washing absorption tower 2 can be prevented from entering an electrolytic bath, and liquid hydrogen fluoride exists at the bottom of the first buffer tank 1 and flows into the first-stage circulating liquid tank 15 through the valve and the pipeline in the operation process;
the first buffer tank 1 gives vent to anger and enters the inferior part of the first class washing absorption tower 2, flow out from the top of the first class washing absorption tower 2, the top of the first class washing absorption tower 2 has absorption liquid of spraying, absorption liquid and trifluromethylsulfonyl fluoride crude gas are in reverse contact on the surface of packing, most hydrogen fluoride impurity is absorbed, absorption liquid enters the first class circulating fluid reservoir 15 from the tower bottom of the first class washing absorption tower 2, the effluent liquid of the first class circulating fluid reservoir 15 enters the tower top to continue spraying and absorbing after passing the second graphite heat exchanger 10 and lowering the temperature on one hand;
on the other hand, when the hydrofluoric acid concentration is detected to be 50%, it flows into the product acid tank 13 through a pipe to be stored.
The external water enters the first-stage circulating liquid tank 15 through a valve and a pipeline.
The working temperature of the primary washing absorption tower 2 is 10-30 ℃, and the working pressure is-0.005-0.095 MPa;
the outlet gas of the first-stage water washing absorption tower 2 enters the lower part of the second-stage water washing absorption tower 3 and flows out from the top of the second-stage water washing absorption tower 3.
The top of the second-stage washing absorption tower 3 sprays absorption liquid, the absorption liquid enters a second-stage circulating liquid tank 17 from the bottom of the second-stage washing absorption tower 3, the liquid discharged from the second-stage circulating liquid tank 17 enters the top of the tower after being cooled by the first graphite heat exchanger 6 to continue spraying and absorbing on one hand, and flows into a first-stage circulating liquid tank 15 through a pipeline on the other hand.
The external water enters a secondary circulating liquid tank through a valve and a pipeline.
The working temperature of the secondary washing absorption tower 3 is 10-30 ℃, and the working pressure is-0.01-0.09 MPa;
the gas discharged from the secondary washing absorption tower 3 enters a second buffer tank 4, and a small amount of acid liquor deposited at the bottom of the second buffer tank 4 flows into a secondary circulating liquid tank 17;
the gas discharged from the second buffer tank 4 enters a neutralization tower through a water ring compressor 18, the neutralization tower is in a filler absorption tower form, the gas enters from the bottom of the neutralization tower, a calcium hydroxide solution is sprayed from the top of the neutralization tower and contacts with the calcium hydroxide solution in the gas rising process, and the hydrogen fluoride is neutralized by the calcium hydroxide on the surface of the filler to complete the gas neutralization and remove residual hydrogen fluoride impurities.
The hydrogen fluoride dissolves exothermically, leads to first order washing absorption tower 2, 3 temperature risees of second grade washing absorption tower, reduces the absorption effect, consequently sets up first graphite heat exchanger 6 and second graphite heat exchanger 10 and reduces washing absorption tower temperature.
The first graphite heat exchanger 6 and the second graphite heat exchanger 10 are both round block hole type graphite heat exchangers or floating head tube type graphite heat exchangers, and the heat exchange area is 10-15 m2Between, first graphite heat exchanger 6 and second graphite heat exchanger 10 are external to have independent circulating water interface respectively, and first graphite heat exchanger 6 and second graphite heat exchanger 10 hot-fluid are hydrofluoric acid, and the cold fluid is the circulating water, and the circulating water temperature is 7 ~ 12 ℃.
The first buffer tank 1, the first-stage washing absorption tower 2, the second-stage washing absorption tower 3, the second buffer tank 4, the finished product acid tank 13, the first-stage circulating liquid tank 15 and the second-stage circulating liquid tank 17 are all made of Monel or steel lining PTFE materials.
In experimental example 1, the working temperature of the first buffer tank 1 was 30 ℃ and the working pressure was 0 MPa; the working temperature of the primary washing absorption tower 2 is 10 ℃, and the working pressure is-0.005 MPa; the working temperature of the secondary washing absorption tower 3 is 10 ℃, and the working pressure is-0.01 MPa; the working temperature and pressure of the second buffer tank 4 are the same as those of the second-stage washing absorption tower; the working temperature of the neutralization tower is 10 ℃, and the working pressure is 0.1 MPa.
In the experimental example 2, the working temperature of the first buffer tank 1 is 40 ℃, and the working pressure is 0.05 MPa; the working temperature of the first-stage washing absorption tower 2 is 20 ℃, and the working pressure is 0.045 MPa; the working temperature of the secondary washing absorption tower 3 is 20 ℃, and the working pressure is 0.04 MPa; the working temperature and pressure of the second buffer tank 4 are the same as those of the second-stage water washing absorption tower 3. The working temperature of the neutralization tower is 20 ℃, and the working pressure is 0.15 MPa.
In experimental example 3, the working temperature of the first buffer tank 1 was 50 ℃ and the working pressure was 0.1 MPa; the working temperature of the primary washing absorption tower 2 is 30 ℃, and the working pressure is 0.095 MPa; the working temperature of the secondary washing absorption tower 3 is 30 ℃, and the working pressure is 0.099 MPa; the working temperature and pressure of the second buffer tank 4 are the same as those of the second-stage water washing absorption tower 3. The working temperature of the neutralization tower is 30 ℃, and the working pressure is 0.2 MPa.
The hydrofluoric acid yields and calcium hydroxide amounts in the three experimental examples are specified in the following table:
| yield of hydrofluoric acid, t/year | Dosage of calcium hydroxide, t/year | |
| Experimental example 1 | 75 | 20 |
| Experimental example 2 | 75 | 20 |
| Experimental example 3 | 75 | 20 |
Compared with the prior art, the experimental examples can save 140 tons of calcium hydroxide per year, and reduce the treatment cost; and 75 tons of hydrofluoric acid are produced annually, so that the full utilization of materials is realized.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the utility model, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride is characterized in that: the device comprises a first buffer tank (1), a primary washing absorption tower (2), a secondary washing absorption tower (3) and a second buffer tank (4), wherein the first buffer tank (1) and the second buffer tank (4) are respectively provided with an air inlet, an air outlet and an acid discharge port;
an air outlet of the first buffer tank (1) is communicated with the first-stage water washing absorption tower (2), an acid discharge port of the first buffer tank (1) is communicated with a first-stage circulating liquid tank (15), and an air outlet of the first-stage water washing absorption tower (2) is communicated with an air inlet of the second-stage water washing absorption tower (3);
a circulating liquid inlet of the primary washing absorption tower (2) is communicated with a second graphite heat exchanger (10), and an acid discharge port of the primary washing absorption tower (2) is also communicated with a primary circulating liquid tank (15);
the gas outlet of the secondary washing absorption tower (3) is connected with the gas inlet of the second buffer tank (4), the circulating liquid inlet of the secondary washing absorption tower (3) is communicated with a first graphite heat exchanger (6), and the acid discharge port of the secondary washing absorption tower (3) is communicated with a secondary circulating liquid tank (17);
a gas outlet of the second buffer tank (4) is connected with a water ring compressor (18), an acid discharge port of the second buffer tank (4) is connected with a secondary circulating liquid tank (17), and the water ring compressor (18) is externally connected with a neutralization tower (19);
and an acid discharge port of the primary circulating liquid tank (15) is respectively connected with the second graphite heat exchanger (10) and the finished product acid tank (13), and an acid discharge port of the secondary circulating liquid tank (17) is respectively connected with the first graphite heat exchanger (6) and the primary circulating liquid tank (15).
2. The device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein a water filling port is formed in a connecting pipeline between the acid discharge port of the second buffer tank (4) and the secondary circulation liquid tank (17), and a water filling port is also formed in a connecting pipeline between the acid discharge port of the secondary circulation liquid tank (17) and the primary circulation liquid tank (15).
3. The device for removing the hydrogen fluoride in the trifluoromethanesulfonyl fluoride according to claim 1, wherein a first magnetic pump (14) is connected to an acid discharge port of the primary circulation liquid tank (15), and a second magnetic pump (16) is connected to an acid discharge port of the secondary circulation liquid tank (17).
4. The device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein the first graphite heat exchanger (6) and the second graphite heat exchanger (10) are externally connected with independent circulating water connectors respectively.
5. The device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein the first buffer tank (1), the first washing absorption tower (2), the second washing absorption tower (3), the second buffer tank (4), the finished acid tank (13), the first circulating liquid tank (15) and the second circulating liquid tank (17) are all made of Monel or steel-lined PTFE materials.
6. The device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride according to claim 1, wherein the first graphite heat exchanger (6) and the second graphite heat exchanger (10) are both round block hole type graphite heat exchangers or floating head tube type graphite heat exchangers, and the heat exchange area of the first graphite heat exchanger is 10 to E15m2In the meantime.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122784630.0U CN216223702U (en) | 2021-11-15 | 2021-11-15 | Device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122784630.0U CN216223702U (en) | 2021-11-15 | 2021-11-15 | Device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride |
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| CN216223702U true CN216223702U (en) | 2022-04-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202122784630.0U Active CN216223702U (en) | 2021-11-15 | 2021-11-15 | Device for removing hydrogen fluoride in trifluoromethanesulfonyl fluoride |
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