CN216653450U - Hydrogen fluoride condensation reflux device - Google Patents
Hydrogen fluoride condensation reflux device Download PDFInfo
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- CN216653450U CN216653450U CN202220088343.8U CN202220088343U CN216653450U CN 216653450 U CN216653450 U CN 216653450U CN 202220088343 U CN202220088343 U CN 202220088343U CN 216653450 U CN216653450 U CN 216653450U
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Abstract
The utility model relates to the technical field of electrolytic fluorine production, and provides a hydrogen fluoride condensation reflux device. The device provided by the utility model comprises a tower body 3, wherein the tower body 3 is provided with an air inlet 1, an air outlet 2, a refrigerant inlet 5, a refrigerant outlet 6 and a temperature measuring port; the side surface of the tower body 3 is wrapped with a heat-insulating interlayer 8; a cooling coil 4 is arranged inside the tower body 3, and a refrigerant flow regulating valve 10 is arranged on a refrigerant pipeline; the temperature measuring device 7 measures the temperature inside the tower body 3 through the temperature measuring port, measured data is accessed to the temperature control central system 9, and the temperature control central system 9 controls the opening degree of the refrigerant flow regulating valve 10 according to the received data. The hydrogen fluoride condensation reflux device provided by the utility model has the advantages of simple structure and high condensation efficiency, can effectively realize the condensation reflux of hydrogen fluoride, reduce the loss of hydrogen fluoride, reduce the pressure of purification and post-treatment processes, improve the use efficiency of hydrogen fluoride, greatly reduce the production cost and have good economic benefit.
Description
Technical Field
The utility model relates to the technical field of electrolytic fluorine production, in particular to a hydrogen fluoride condensation reflux device.
Background
Fluorine is a non-metallic element with the strongest electronegativity and the most active chemical property, and can react with almost all elements. High purity fluorine gas (F)2) Is a gas with very active property, has strong oxidizing property and can react with most inorganic or organic matters at room temperatureOr below room temperature, release large amounts of heat, often resulting in combustion and explosion. High-purity fluorine gas is an important raw material in the field of fine chemical engineering, and is widely applied to the fields of electronics, laser technology, scientific research, medical plastics and the like; because of its strong oxidizing property, it can be used for glass etching, surface passivation treatment of metal material and pipeline, and can be used for making rocket propellant in national defence; sulfur hexafluoride and carbon tetrafluoride generated by the reaction of fluorine gas with sulfur and carbon are good electric insulation and arc extinguishing materials; f2Can be used as cleaning agent for CVD reaction chamber and NF3In contrast, F2Has stronger reactivity and does not cause greenhouse effect, and has great application potential in the field of semiconductors; chlorine trifluoride synthesized by fluorine gas and chlorine gas can be used as a strong longitudinal fire agent, a rocket propellant and a catalyst for manufacturing aviation gasoline; fluorine gas reacts with metal tungsten or germanium and the like to generate metal fluoride which can be used as vapor deposition gas or doping gas in the field of semiconductor manufacturing; the high-purity fluorine gas can be mixed with inert gases such as nitrogen, ammonia, neon, argon and the like in any concentration ratio to prepare mixed gas.
In general, potassium hydrogen fluoride is used as an electrolyte in industry, and anhydrous hydrofluoric acid is electrolyzed and purified to obtain fluorine gas. In the electrolysis process, the crude fluorine gas generated at the anode and the hydrogen gas generated at the cathode both contain a large amount of hydrogen fluoride, and the content is about 10-20% (volume ratio). In the prior art, the crude fluorine gas is generally removed from the hydrogen fluoride in the purification process through processes of low-temperature condensation, low-temperature rectification, adsorption and the like; the hydrogen gas is removed by the steps of water washing, alkali washing, etc. The crude fluorine gas and hydrogen gas carrying a large amount of hydrogen fluoride not only easily cause pipeline blockage, but also greatly increase the pressure of the post-treatment process, and simultaneously, the volatilization of a large amount of hydrogen fluoride also reduces the use efficiency of the hydrogen fluoride in the electrolysis process, and improves the production cost.
SUMMERY OF THE UTILITY MODEL
In view of the above, the present invention provides a hydrogen fluoride condensation and reflux apparatus. The device provided by the utility model can condense and reflux the hydrogen fluoride, improve the utilization rate of the hydrogen fluoride in the electrolysis process and reduce the production cost.
In order to achieve the purpose of the utility model, the utility model provides the following technical scheme:
a hydrogen fluoride condensate reflux apparatus comprising:
the device comprises a tower body 3, wherein the bottom of the tower body 3 is provided with an air inlet 1, the top of the tower body is provided with an air outlet 2, and the side surface of the tower body is provided with a refrigerant inlet 5, a refrigerant outlet 6 and a temperature measuring port; the outside of the tower body 3 is wrapped with a heat-insulating interlayer 8;
the cooling device comprises a cooling coil 4 arranged inside a tower body 3, wherein two ends of the cooling coil 4 are respectively communicated with a refrigerant inlet 5 and a refrigerant outlet 6;
the cooling medium pipeline is communicated with the cooling medium inlet 5 of the tower body 3, and a cooling medium flow regulating valve 10 is arranged on the cooling medium pipeline;
a temperature measuring device 7; the temperature measuring device 7 measures the temperature inside the tower body 3 through the temperature measuring port;
a temperature control central system 9; the temperature measuring device 7 accesses the measured data into the temperature control central system 9, and the temperature control central system 9 controls the opening degree of the refrigerant flow regulating valve 10 according to the received data.
Preferably, the tower body 3 is made of stainless steel, low carbon steel or monel.
Preferably, the material of the cooling coil 4 is stainless steel, low carbon steel or copper.
Preferably, the cooling coil 4 is a spiral pipe.
Preferably, the heat insulation material used by the heat insulation interlayer 8 is polyurethane foam or heat insulation rock wool.
Preferably, the thickness of the heat-insulating interlayer 8 is 50-120 mm.
Preferably, the cooling medium inlet 5 is arranged at the lower end of the tower 3, and the cooling medium outlet 6 is arranged at the upper end of the tower 3.
Preferably, the temperature measuring device 7 is a platinum resistance thermometer.
The utility model provides a hydrogen fluoride condensation reflux device which comprises a tower body 3, wherein the bottom of the tower body 3 is provided with an air inlet 1, the top of the tower body is provided with an air outlet 2, and the side surface of the tower body is provided with a refrigerant inlet 5, a refrigerant outlet 6 and a temperature measuring port; the side surface of the tower body 3 is wrapped with a heat-insulating interlayer 8; a cooling coil 4 is arranged inside the tower body 3, a refrigerant inlet 5 is communicated with a refrigerant pipeline, and a refrigerant flow regulating valve 10 is arranged on the refrigerant pipeline; the temperature measuring device 7 measures the temperature inside the tower body 3 through the temperature measuring port, measured data is connected into the temperature control central system 9, and the temperature control central system 9 controls the opening degree of the refrigerant flow regulating valve 10 according to the received data, so that the temperature inside the tower body 3 is controlled. The hydrogen fluoride condensation reflux device provided by the utility model has the advantages of simple structure, safety, reliability and high condensation efficiency, can effectively realize the condensation reflux of hydrogen fluoride, reduce the loss of raw material hydrogen fluoride, reduce the pressure of purification and post-treatment processes, improve the use efficiency of hydrogen fluoride, greatly reduce the production cost and have good economic benefit.
In addition, the temperature measuring device 7 is arranged in the condensation reflux device, and the temperature measuring device 7 is linked with the temperature control central system 9, so that the accurate control of the internal temperature of the tower body 3 can be realized, and the condensation efficiency of HF (hydrogen fluoride) is improved; in addition, the heat insulation material is wrapped outside the tower body 3, so that the loss of cold energy can be avoided, the cooling efficiency is improved, and the energy consumption is reduced.
Drawings
Fig. 1 is a schematic structural diagram of a hydrogen fluoride condensation reflux apparatus provided by the present invention, wherein: 1-air inlet, 2-air outlet, 3-tower, 4-cooling coil, 5-coolant inlet, 6-coolant outlet, 7-temperature measuring device, 8-heat preservation interlayer, 9-temperature control central system and 10-coolant flow regulating valve.
Detailed Description
The utility model provides a hydrogen fluoride condensation reflux device, which comprises:
the device comprises a tower body 3, wherein the bottom of the tower body 3 is provided with an air inlet 1, the top of the tower body is provided with an air outlet 2, and the side surface of the tower body is provided with a refrigerant inlet 5, a refrigerant outlet 6 and a temperature measuring port; the outside of the tower body 3 is wrapped with a heat-insulating interlayer 8;
the cooling device comprises a cooling coil 4 arranged inside a tower body 3, wherein two ends of the cooling coil 4 are respectively communicated with a refrigerant inlet 5 and a refrigerant outlet 6;
the cooling medium pipeline is communicated with the cooling medium inlet 5 of the tower body 3, and a cooling medium flow regulating valve 10 is arranged on the cooling medium pipeline;
a temperature measuring device 7; the temperature measuring device 7 measures the temperature inside the tower body 3 through the temperature measuring port;
a temperature control central system 9; the temperature measuring device 7 accesses the measured data to the temperature control central system 9, and the temperature control central system 9 controls the opening degree of the refrigerant flow regulating valve 10 according to the received data.
The structure schematic diagram of the hydrogen fluoride condensation reflux device provided by the utility model is shown in fig. 1, and the detailed description is provided below with reference to fig. 1.
The hydrogen fluoride condensation reflux device provided by the utility model comprises a tower body 3. In the utility model, the bottom of the tower body 3 is provided with an air inlet 1, the top of the tower body is provided with an air outlet 2, the specifications of the interface flanges at the air inlet 1 and the air outlet 2 are selected according to actual requirements, and in the specific embodiment of the utility model, the specifications of the interface flanges at the air inlet 1 and the air outlet 2 are preferably DN 80; the side surface of the tower body 3 is provided with a refrigerant inlet 5, a refrigerant outlet 6 and a temperature measuring port, specifically, the refrigerant inlet 5 is arranged at the lower end of the side surface of the tower body 3, the refrigerant outlet 6 is arranged at the upper end of the side surface of the tower body 3, and the temperature measuring port is arranged in the middle of the side surface of the tower body 3; the flange specifications of the refrigerant inlet 5 and the refrigerant outlet 6 are preferably DN 25; the tower body 3 is preferably of a straight cylinder type, and in one embodiment of the utility model, the inner diameter of the tower body 3 is preferably DN180 mm-DN 220 mm.
In the utility model, the outside of the tower body 3 is wrapped with a heat-insulating interlayer 8, and the heat-insulating material used by the heat-insulating interlayer 8 is preferably polyurethane foam or heat-insulating rock wool; the thickness of the heat-insulating interlayer 8 is preferably 50-120 mm, and the heat-insulating material has a better heat-insulating effect, can avoid the dissipation of cold in the tower body 3, and improves the condensation and backflow effects of HF. In a specific embodiment of the present invention, the thermal insulation layer 8 preferably completely covers the outer surface of the tower body 3, and fig. 1 is a schematic view, and the thermal insulation layer 8 is not completely shown.
In the present invention, the material of the tower body 3 is preferably stainless steel, low carbon steel or monel.
The hydrogen fluoride condensation reflux device provided by the utility model comprises a cooling coil 4 arranged in a tower body 3, wherein two ends of the cooling coil 4 are respectively communicated with a refrigerant inlet 5 and a refrigerant outlet 6. In the present invention, the material of the cooling coil 4 is preferably stainless steel, low carbon steel or copper; the outer diameter of the cooling coil 4 is preferably phi 15-40 mm, and more preferably phi 20-30 mm; the cooling coil 4 is preferably a spiral pipe, and the length of the cooling coil is preferably determined according to the amount of cooled gas and the heat exchange area; the utility model adopts the cooling coil pipe with the shape, can fully cool HF, and improves the reflux efficiency.
The hydrogen fluoride condensation reflux device provided by the utility model comprises a refrigerant pipeline communicated with a refrigerant inlet 5 of the tower body 3, and a refrigerant flow regulating valve 10 is arranged on the refrigerant pipeline. In the present invention, the refrigerant flow regulating valve 10 is used for regulating the flow of the refrigerant, and the temperature inside the tower body 3 is regulated and controlled by controlling the flow of the refrigerant.
The hydrogen fluoride condensation reflux device provided by the utility model comprises a temperature measuring device 7. In the present invention, the temperature measuring device 7 measures the temperature inside the tower body 3 through a temperature measuring port of the tower body 3, and the temperature measuring device 7 is preferably a platinum resistance thermometer.
The hydrogen fluoride condensation reflux device provided by the utility model comprises a temperature control center system 9. In the utility model, the temperature measuring device 7 accesses the measured data into the temperature control central system 9, and the temperature control central system 9 controls the opening degree of the refrigerant flow regulating valve 10 according to the received data, thereby realizing the regulation and control of the temperature in the tower body 3. The present invention has no special requirement for the temperature control center system 9, and a temperature control center system known to those skilled in the art can be adopted.
The method for performing hydrogen fluoride condensation reflux by using the device provided by the utility model preferably comprises the following steps:
the hydrogen fluoride condensation reflux device is arranged on a pipeline at an anode chamber outlet and/or a cathode chamber outlet of the electrolytic cell, a refrigerant is continuously introduced into the cooling coil 4 from a refrigerant inlet 5, the temperature inside the tower body 3 is measured through the temperature measuring device 7, the measured data is accessed into the temperature control central system 9, the temperature control central system 9 controls the opening degree of the refrigerant flow regulating valve 10 according to the received data, and the temperature inside the tower body 3 is controlled below 10 ℃;
crude gas generated at the anode and/or cathode outlet of the electrolytic cell enters the hydrogen fluoride condensation reflux device from the gas inlet 1, hydrogen fluoride in the crude gas is condensed and refluxed into the electrolytic cell, and the rest gas is discharged from the gas outlet 2.
In the present invention, the electrolysis is preferably performed by electrolyzing fluorine, nitrogen trifluoride, carbon tetrafluoride, sulfur hexafluoride, or tungsten hexafluoride, but is not limited to the above-described electrolysis process, and in the specific embodiment of the present invention, the apparatus and method of the present invention may be used as long as it relates to an electrolysis process in which HF needs to be refluxed; in the electrolysis process, gas containing hydrogen fluoride is generated at both the cathode and the anode of the electrolytic cell, for example, in the process of preparing fluorine by electrolysis, crude fluorine gas generated at the anode and hydrogen gas generated at the cathode both contain 10-20% of hydrogen fluoride by volume fraction.
The hydrogen fluoride condensation and reflux device is arranged on an anode chamber outlet and/or a cathode chamber outlet pipeline of the electrolytic cell, in the specific embodiment of the utility model, the hydrogen fluoride condensation and reflux device is preferably arranged on the anode chamber outlet pipeline or the cathode chamber outlet pipeline of the electrolytic cell according to actual needs, or one condensation and reflux device is respectively arranged on the anode chamber outlet and the cathode chamber outlet pipeline, and when two condensation and reflux devices are arranged, the operation methods of the two devices are consistent.
The utility model continuously introduces the refrigerant into the cooling coil 4 from the refrigerant inlet 5, measures the temperature inside the tower body 3 through the temperature measuring device 7, and accesses the measured data into the temperature control central system 9, the temperature control central system 9 controls the opening degree of the refrigerant flow regulating valve 10 according to the received data, and controls the temperature inside the tower body 3 below 10 ℃. In the utility model, the refrigerant is preferably liquid nitrogen, glycol aqueous solution or frozen oil; the temperature inside the tower body 3 is preferably-80 to 10 ℃, more preferably-40 to-10 ℃, and further preferably-30 to-20 ℃. The temperature measuring device 7 and the refrigerant flow regulating valve 10 are interlocked, so that the temperature in the tower body 3 can be conveniently regulated and controlled, and the condensation efficiency of the hydrogen fluoride can be improved.
In the utility model, crude gas generated at the anode and/or cathode outlet of the electrolytic cell enters the hydrogen fluoride condensation reflux device from the gas inlet 1, hydrogen fluoride in the crude gas is condensed and refluxed into the electrolytic cell, and the rest gas is discharged from the gas outlet 2. In the specific embodiment of the utility model, when the electrolysis is to produce fluorine by electrolysis, the outlet 2 of the condensation reflux device arranged at the anode discharges fluorine gas with higher purity, and the outlet 2 of the condensation reflux device arranged at the cathode discharges hydrogen gas with higher purity.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
The structure of the hydrogen fluoride condensation reflux device is shown in figure 1, wherein the specifications of the interface flanges of an air inlet 1 and an air outlet 2 of the device are DN 80; the refrigerant air inlet 5 and the refrigerant air outlet 6 are provided with flanges with the specification of DN25 mm; the tower body 3 is made of stainless steel and has the diameter of DN200 mm; the cooling coil 4 is made of copper material, and the outer diameter is phi 25 mm; liquid nitrogen is used as a low-temperature refrigerant, temperature measurement is carried out through a platinum resistance thermometer 7, measurement data are accessed into a temperature control central system 9, and the temperature of the tower body 3 is controlled to be-30 to-20 ℃ through an automatic control valve 10.
The hydrogen fluoride condensation reflux device is arranged at the outlet of the anode of an electrolytic cell for preparing fluorine by electrolysis, the electrolysis device is normally started, and the flow of crude fluorine gas generated by the anode is 6.8m3And h, arranging sampling analysis ports on pipelines of an air inlet and an air outlet of the condensation reflux device, and detecting the purity change condition of the fluorine gas on line.
The volume fraction of fluorine gas at the gas inlet of the condensing and refluxing device is detected to be 85.25%, and the volume fraction of HF is detected to be 14.75%. After condensation reflux treatment, the volume fraction of fluorine gas at the gas outlet of the condensation reflux device is increased to 98.75 percent, the volume fraction of HF is reduced to 1.25 percent, and the removal rate of hydrogen fluoride reaches 91.53 percent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A hydrogen fluoride condensation reflux device is characterized by comprising:
the device comprises a tower body (3), wherein the bottom of the tower body (3) is provided with an air inlet (1), the top of the tower body is provided with an air outlet (2), and the side surface of the tower body is provided with a refrigerant inlet (5), a refrigerant outlet (6) and a temperature measuring port; the outside of the tower body (3) is wrapped with a heat-insulating interlayer (8);
the cooling coil (4) is arranged in the tower body (3), and two ends of the cooling coil (4) are respectively communicated with the refrigerant inlet (5) and the refrigerant outlet (6);
the cooling medium pipeline is communicated with a cooling medium inlet (5) of the tower body (3), and a cooling medium flow regulating valve (10) is arranged on the cooling medium pipeline;
a temperature measuring device (7); the temperature measuring device (7) measures the temperature inside the tower body (3) through the temperature measuring port;
a temperature control central system (9); the temperature measuring device (7) accesses the measured data into the temperature control central system (9), and the temperature control central system (9) controls the opening degree of the refrigerant flow regulating valve (10) according to the received data.
2. The apparatus of claim 1, wherein the tower body (3) is made of stainless steel, mild steel or monel.
3. The hydrogen fluoride condensate reflux device according to claim 1, wherein the cooling coil (4) is made of stainless steel, mild steel or copper.
4. The hydrogen fluoride condensate reflux apparatus according to claim 1 or 3, wherein the cooling coil (4) is a spiral type pipe.
5. The hydrogen fluoride condensation and reflux device as claimed in claim 1, wherein the heat-insulating material used for the heat-insulating interlayer (8) is polyurethane foam or heat-insulating rock wool.
6. The hydrogen fluoride condensation and reflux device as claimed in claim 1 or 5, wherein the thickness of the heat insulation interlayer (8) is 50-120 mm.
7. The hydrogen fluoride condensate reflux device according to claim 1, wherein the coolant inlet (5) is arranged at the lower end of the tower body (3), and the coolant outlet (6) is arranged at the upper end of the tower body (3).
8. The hydrogen fluoride condensate return apparatus of claim 1, wherein the temperature measuring means (7) is a platinum resistance thermometer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220088343.8U CN216653450U (en) | 2022-01-13 | 2022-01-13 | Hydrogen fluoride condensation reflux device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220088343.8U CN216653450U (en) | 2022-01-13 | 2022-01-13 | Hydrogen fluoride condensation reflux device |
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| CN216653450U true CN216653450U (en) | 2022-06-03 |
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| CN202220088343.8U Active CN216653450U (en) | 2022-01-13 | 2022-01-13 | Hydrogen fluoride condensation reflux device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115990346A (en) * | 2023-03-22 | 2023-04-21 | 东营联合石化有限责任公司 | Solvent regeneration tower |
| CN117414601A (en) * | 2023-12-19 | 2024-01-19 | 福建德尔科技股份有限公司 | Primary purification equipment for preparing electronic grade chlorine trifluoride |
-
2022
- 2022-01-13 CN CN202220088343.8U patent/CN216653450U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115990346A (en) * | 2023-03-22 | 2023-04-21 | 东营联合石化有限责任公司 | Solvent regeneration tower |
| CN115990346B (en) * | 2023-03-22 | 2023-08-01 | 东营联合石化有限责任公司 | Solvent regeneration tower |
| CN117414601A (en) * | 2023-12-19 | 2024-01-19 | 福建德尔科技股份有限公司 | Primary purification equipment for preparing electronic grade chlorine trifluoride |
| CN117414601B (en) * | 2023-12-19 | 2024-03-12 | 福建德尔科技股份有限公司 | Primary purification equipment for preparing electronic grade chlorine trifluoride |
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