CN110656344B - A device and method for removing water from anhydrous hydrogen fluoride - Google Patents
A device and method for removing water from anhydrous hydrogen fluoride Download PDFInfo
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- CN110656344B CN110656344B CN201911072765.5A CN201911072765A CN110656344B CN 110656344 B CN110656344 B CN 110656344B CN 201911072765 A CN201911072765 A CN 201911072765A CN 110656344 B CN110656344 B CN 110656344B
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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Abstract
本发明公开了一种无水氟化氢除水的装置，包括电解槽槽体、电解槽上盖、阳极板、阴极板和隔板，电解槽槽体内设有电解腔，阳极板、阴极板和隔板均位于电解腔内，阳极板固定于电解槽槽体内并分隔电解腔的下部空间，阴极板固定于电解槽上盖并向电解腔的底部延伸，隔板固定于电解槽上盖并位于阳极板和阴极板之间，隔板将电解腔的上部空间分隔成阳极气室和阴极气室。通过对电极片、电解槽的创新设计，实现无水氟化氢连续除水处理，提高去除效率。本发明还公开了基于上述无水氟化氢除水的装置的无水氟化氢除水的方法，采用电解方法去除无水氟化氢中的微量水分，可以实现连续处理，并且不需使用氟气等氧化试剂或吸附剂，处理过程简洁、高效。
The present invention discloses a device for removing water from anhydrous hydrogen fluoride, comprising an electrolytic cell body, an electrolytic cell upper cover, an anode plate, a cathode plate and a partition. An electrolytic chamber is arranged in the electrolytic cell body, and the anode plate, the cathode plate and the partition are all located in the electrolytic chamber. The anode plate is fixed in the electrolytic cell body and separates the lower space of the electrolytic chamber. The cathode plate is fixed to the electrolytic cell upper cover and extends to the bottom of the electrolytic chamber. The partition is fixed to the electrolytic cell upper cover and is located between the anode plate and the cathode plate. The partition separates the upper space of the electrolytic chamber into an anode gas chamber and a cathode gas chamber. Through the innovative design of the electrode sheet and the electrolytic cell, continuous water removal treatment of anhydrous hydrogen fluoride is achieved, and the removal efficiency is improved. The present invention also discloses a method for removing water from anhydrous hydrogen fluoride based on the above-mentioned device for removing water from anhydrous hydrogen fluoride. The electrolytic method is used to remove trace water in anhydrous hydrogen fluoride, and continuous treatment can be achieved. No oxidizing agent or adsorbent such as fluorine gas is required, and the treatment process is simple and efficient.
Description
Technical Field
The invention relates to the field of inorganic fine chemical industry, in particular to a device and a method for removing water from anhydrous hydrogen fluoride.
Background
Anhydrous hydrogen fluoride is a chemical product with wide application, the content of hydrogen fluoride is more than 99.8%, the appearance is colorless fuming liquid, and the anhydrous hydrogen fluoride is easy to gasify under reduced pressure or high temperature. Anhydrous hydrogen fluoride is widely used in industries such as atomic energy, chemical industry, petroleum, etc., and is a strong oxidant, or is a basic raw material for preparing elemental fluorine, various fluorine refrigerants and inorganic fluorides, and various organic fluorides can be prepared into various aqueous hydrofluoric acid for various purposes, and is used for preparing graphite, catalysts for manufacturing organic compounds, etc. Is a raw material for producing refrigerant Freon, fluorine-containing resin, organic fluoride and fluorine. Can be used as a catalyst for organic diaphragm formation such as alkylation, polymerization, condensation, isomerization and the like in chemical production. It is also used for corroding stratum and extracting rare-earth elements and radioactive elements when mining some ore beds. The uranium hexafluoride is a raw material for manufacturing uranium hexafluoride in the atomic energy industry and in the nuclear weapon production, and is also a raw material for manufacturing rocket fuels and additives. In addition, anhydrous hydrogen fluoride is also used as a solvent for synthesizing lithium hexafluorophosphate serving as an electrolyte of a lithium battery.
When anhydrous hydrogen fluoride is used for organic synthesis, fluorine production and lithium hexafluorophosphate production, trace moisture in the anhydrous hydrogen fluoride is easy to cause product quality degradation and can bring about serious potential safety hazards. Therefore, it is often necessary to remove water from the anhydrous hydrogen fluoride feedstock prior to the reaction. The anhydrous hydrogen fluoride is usually prepared by rectifying hydrofluoric acid, and according to the requirements of GB7746-2011 industrial anhydrous hydrogen fluoride, the water content of the qualified industrial anhydrous hydrogen fluoride II products is less than or equal to 600ppm, and the water content of I products is less than or equal to 50ppm. On the one hand, the rectification cost required for meeting the water requirement of class I is high, and meanwhile, anhydrous hydrogen fluoride can absorb water in the environment in the process of filling, storage and transportation to cause the water content to be increased. In the case of carrying out the synthesis reaction, it is often necessary to reduce the moisture content in anhydrous hydrogen fluoride to 20ppm or less, and therefore, the anhydrous hydrogen fluoride needs to be treated to reduce the moisture content before the reaction.
The current method for removing the water from the hydrogen fluoride mainly comprises an adsorption method, a fluorine gas oxidation method and an electrochemical oxidation method.
U.S. patent No. 5597545 discloses a method for adsorbing moisture in hydrogen fluoride through a carbon molecular sieve comprising contacting hydrogen fluoride with a carbon molecular sieve to adsorb water in the hydrogen fluoride and also to adsorb a portion of the hydrogen fluoride, then heating the molecular sieve to desorb the adsorbed water and hydrogen fluoride, then continuing to heat to complete brief analysis hydrogen fluoride, and recovering the carbon molecular sieve. The method has low water removal efficiency and high treatment cost.
Fluorine gas oxidizes moisture in hydrogen fluoride to produce hydrogen fluoride and oxygen difluoride, which has a boiling point of-154 ℃ and a boiling point of 19.5 ℃, so that oxygen difluoride is easily separated from liquid anhydrous hydrogen fluoride:
2F2+H2O→2HF+OF2
However, the preparation cost of fluorine gas electrolysis is high, the oxidizing property of fluorine gas is very strong, the water removal reaction is severe, the requirements on equipment materials are high, and the danger is high.
Disclosure of Invention
According to one aspect of the invention, there is provided a device for removing water from anhydrous hydrogen fluoride, comprising an electrolytic tank body, an electrolytic tank upper cover, an anode plate, a cathode plate and a partition plate, wherein an electrolytic cavity is arranged in the electrolytic tank body, one end of the electrolytic tank body is provided with a liquid inlet, the other end of the electrolytic tank body is provided with a liquid outlet, the upper end of the electrolytic tank body is opened, the electrolytic tank upper cover is fixed on the electrolytic tank body and seals the upper end of the electrolytic tank body, the anode plate, the cathode plate and the partition plate are all positioned in the electrolytic cavity, the anode plate is fixed on the electrolytic tank body and separates the lower space of the electrolytic cavity, the cathode plate is fixed on the electrolytic tank upper cover and extends towards the bottom of the electrolytic cavity, and the partition plate is fixed on the electrolytic tank upper cover and positioned between the anode plate and the cathode plate and separates the upper space of the electrolytic cavity into an anode air chamber and a cathode air chamber.
In some embodiments, the electrolytic cell upper cover is provided with an anode gas chamber gas outlet and a cathode gas chamber gas outlet, the anode gas chamber gas outlet is communicated with the anode gas chamber, and the cathode gas chamber gas outlet is communicated with the cathode gas chamber.
In some embodiments, the anode plate, the cathode plate and the separator are all arranged in a plurality of blocks, and the anode plate and the cathode plate are sequentially and alternately arranged to form an S-shaped liquid flow channel between a liquid inlet and a liquid outlet of the electrolytic tank body.
In some embodiments, the anode plate, the cathode plate and the separator are vertically spaced and uniformly arranged in parallel, the anode plate and the cathode plate are made of stainless steel or nickel, and the separator is made of polytetrafluoroethylene.
In some embodiments, a liquid level line is arranged in the electrolytic tank body, the upper end of the anode plate is lower than the liquid level line, and the lower end of the baffle plate is lower than the liquid level line.
In some embodiments, the distance between the lower end of the cathode plate and the bottom surface of the electrolysis cavity is 10 mm-150 mm, and the distance between the cathode and the anode is 15 mm-300 mm.
In some embodiments, the anhydrous hydrogen fluoride water removal device further comprises a direct current power supply, the anode plate is connected with the positive electrode of the direct current power supply, the cathode plate is connected with the negative electrode of the direct current power supply, and the voltage of the direct current power supply is 3V-7V.
In some embodiments, the device for removing water from anhydrous hydrogen fluoride further comprises a liquid inlet valve and a liquid outlet valve, wherein the liquid inlet valve is connected with the liquid inlet, and the liquid outlet valve is connected with the liquid outlet.
According to another aspect of the present invention, there is provided a method for removing water from anhydrous hydrogen fluoride comprising the steps of:
1) Opening a liquid inlet valve, and conveying anhydrous hydrogen fluoride into an electrolytic cavity through a liquid inlet;
2) Electrifying the anode plate and the cathode plate to generate ionization reaction on the anode plate and the cathode plate and decompose moisture in the hydrogen fluoride, generating oxydifluoride gas on the anode plate and generating hydrogen gas on the cathode plate;
3) After the liquid level of the hydrogen fluoride reaches a liquid level line, a liquid outlet valve is opened, so that the dehydrated anhydrous hydrogen fluoride is led into a reaction device or is collected in a product storage tank, and the hydrogen fluoride continuously passes through an electrolytic tank body to continuously treat the water content in the hydrogen fluoride.
In some embodiments, the method further comprises the steps of:
4) Collecting gas generated on the anode plate by using an anode air chamber, and collecting gas generated on the cathode plate by using a cathode air chamber;
5) The gas collected in the anode gas chamber and the cathode gas chamber is condensed and reflowed into hydrogen fluoride respectively, and the non-condensable gas is purified and discharged after reaching standards. The noncondensable gas in the anode gas chamber is OF 2, alkali liquor is used for absorption, sodium fluoride and oxygen are generated by reaction, and part OF uncondensed hydrogen fluoride also reacts with alkali to generate sodium fluoride:
OF2+2NaOH→2NaF+H2O+O2↑
HF+NaOH→NaF+H2O
The non-condensable gas in the cathode air chamber is H 2, and is also washed and purified by alkali liquor, and part of uncondensed hydrogen fluoride reacts with alkali to generate sodium fluoride.
The invention has the beneficial effects that the device and the method for removing the water of the anhydrous hydrogen fluoride are reasonably designed by utilizing the electrolysis principle, and the continuous water removal treatment of the anhydrous hydrogen fluoride is realized by the innovative design of the electrode plates and the electrolytic tank, so that the removal efficiency is improved. The device is made of corrosion-resistant materials, and can effectively avoid hydrofluoric acid corrosion. The electrolysis method is adopted to remove trace moisture in anhydrous hydrogen fluoride, continuous treatment can be realized, and oxidizing reagents such as fluorine gas and the like or adsorbents are not needed, so that the treatment process is simple and efficient.
Drawings
FIG. 1 is a schematic diagram of an apparatus for removing water from anhydrous hydrogen fluoride according to an embodiment of the present invention;
FIG. 2 is a top view of A-A of the apparatus for removing water from anhydrous hydrogen fluoride shown in FIG. 1;
FIG. 3 is a schematic view of the cathode plate of the apparatus for removing water from anhydrous hydrogen fluoride shown in FIG. 1;
fig. 4 is a view showing the use state of the apparatus for removing water from anhydrous hydrogen fluoride shown in fig. 1.
Detailed Description
Example 1
Fig. 1-4 schematically illustrate an apparatus for anhydrous hydrogen fluoride removal according to one embodiment of the present invention.
Referring to fig. 1-4, a device for removing water from anhydrous hydrogen fluoride comprises an electrolytic tank body 1, an electrolytic tank upper cover 2, an anode plate 3, a cathode plate 4, a baffle plate 5, a liquid inlet valve 6, a liquid outlet valve 7 and a direct current power supply 8.
The electrolytic tank body 1 is square, and an electrolytic cavity 13 is arranged in the electrolytic tank body 1. One end of the electrolytic tank body 1 is provided with a liquid inlet 11, and the other end of the electrolytic tank body 1 is provided with a liquid outlet 12. The upper end of the electrolytic tank body 1 is opened, the edge of the electrolytic tank upper cover 2 is fixed on the edge of the electrolytic tank body 1 by bolts and seals the upper end of the electrolytic tank body 1, so that the electrolytic cavity 13 is a closed space. The anode plate 3, the cathode plate 4 and the partition plate 5 are all positioned in the electrolytic cavity, the anode plate 3 is fixed in the electrolytic tank body 1 and separates the lower space of the electrolytic cavity 13, and the cathode plate 4 is fixed on the electrolytic tank upper cover 2 and extends towards the bottom of the electrolytic cavity 13. A separator 5 is fixed to the upper cover 2 of the electrolytic tank and located between the anode plate 3 and the cathode plate 4, and the separator 5 divides the upper space of the electrolytic chamber 13 into an anode gas chamber 14 and a cathode gas chamber 15.
The upper cover 2 of the electrolytic tank is provided with an anode air chamber air outlet 21 and a cathode air chamber air outlet 22, the anode air chamber air outlet 21 is communicated with the anode air chamber 14, and the cathode air chamber air outlet 22 is communicated with the cathode air chamber 15. The anode gas chamber gas outlet 21 and the cathode gas chamber gas outlet 22 are respectively communicated with a reflux device 91 and a purifying device 92.
The anode plates 3, the cathode plates 4 and the partition plates 5 are vertically arranged at intervals and are uniformly arranged in parallel, the anode plates 3, the cathode plates 4 and the partition plates 5 are arranged into a plurality of blocks, and the anode plates 3 and the cathode plates 4 are sequentially and alternately arranged to form an S-shaped liquid flow channel between the liquid inlet 11 and the liquid outlet 12 of the electrolytic tank body 1.
A liquid level line 16 is arranged in the electrolytic tank body 1, the upper end of the anode plate 3 is lower than the liquid level line 16, and the lower end of the baffle plate 5 is lower than the liquid level line 16. When the liquid in the electrolytic tank body 1 reaches the liquid level line 16, the smooth circulation of the liquid in the electrolytic tank body 1 in an S-shaped line can be ensured.
The anode plate 3 and the cathode plate 4 can be made of stainless steel or nickel, and the separator 5 can be made of polytetrafluoroethylene. The distance between the lower end of the cathode plate 4 and the bottom surface of the electrolysis cavity 13 is 10 mm-150 mm, and the distance between the cathode and the anode is 15 mm-300 mm.
The anode plate 3 is connected with the positive electrode of the direct current power supply 8, the cathode plate 4 is connected with the negative electrode of the direct current power supply 8, and the voltage of the direct current power supply 8 is 3V-7V.
The liquid inlet valve 6 is connected with a liquid inlet 11, and the liquid outlet valve 7 is connected with a liquid outlet 12. The liquid level and the liquid circulation speed of the liquid in the electrolytic tank body 1 can be controlled through the liquid inlet valve 6 and the liquid outlet valve 7.
The upper part of the cathode plate 4 is provided with a notch 41 penetrating through the cathode plate 4, so that two sides of the cathode plate 4 form a communicated space, and thus, two sides of the cathode plate 4 only need to share one air outlet.
The outside of the electrolytic tank body 1 is also provided with the heat preservation layer 17, the heat preservation layer 17 can ensure the temperature stability of the electrolytic tank body 1, and ensure that anhydrous hydrogen fluoride is always in a liquid state in the electrolytic tank, and the electrolytic process is smoothly carried out. The electrolytic tank body 1 and the electrolytic tank upper cover 2 are provided with sealing rings to ensure the tightness between the electrolytic tank body 1 and the electrolytic tank upper cover 2.
By the structural design of the electrolytic tank body, the separator 5 and the anhydrous HF liquid level divide the gas phase space at the upper part in the tank into an anode gas chamber 14 and a cathode gas chamber 15. Because the density of the gas generated on the surfaces of the anode plate 3 and the cathode plate 4 is smaller, the gas respectively enters the anode air chamber 14 and the cathode air chamber 15 after floating upwards, and respectively enters the condensation reflux device through the anode air chamber air outlet 21 and the cathode air chamber air outlet 22. By separately arranging the anode air chamber 14 and the cathode air chamber 15, potential safety hazards caused by contact between hydrogen generated by the cathode plate 4 and oxidizing gas generated by the anode plate 3 are avoided. The lower end of the cathode has a certain gap with the bottom surface of the electrolytic tank, and the anode is directly fixed on the bottom surface of the electrolytic tank, and the anhydrous HF is in an up-down S-shaped baffle in the electrolytic tank through the arrangement of the anode and the cathode, so that the anhydrous HF is fully contacted with the surface of the electrode for electrolytic water removal, and the water removal efficiency is improved.
Example 2
A method for an apparatus for anhydrous hydrogen fluoride removal of example 1 comprising the steps of:
1) Opening a liquid inlet valve 6, and conveying the anhydrous hydrogen fluoride in the storage container into an electrolytic cavity 13 through a liquid inlet 11;
2) The direct current power supply 8 is turned on to electrify the anode plate 3 and the cathode plate 4 so as to generate ionization reaction on the anode plate 3 and the cathode plate 4 to decompose moisture in hydrogen fluoride, generate oxydifluoride gas on the anode plate 3 and generate hydrogen gas on the cathode plate 4;
The electrolysis of anhydrous hydrogen fluoride also removes trace moisture therefrom. The principle is that due to the existence of water, part of hydrogen fluoride is ionized into hydrogen ions and fluorine ions, after the power is on, hydrogen ions are generated at a cathode to obtain electrons to precipitate hydrogen, and water molecules at an anode are oxidized to generate oxygen difluoride:
Cathode 4H ++4e→2H2 ≡
Anode H 2O+4F--4e-→OF2 ++2HF
3) After the liquid level of the hydrogen fluoride reaches the liquid level line 16, the liquid outlet valve 7 is opened, so that the dehydrated anhydrous hydrogen fluoride is led into a reaction device or collected in a product storage tank, and the hydrogen fluoride can continuously pass through the electrolytic tank body 1. Can realize continuous treatment of water in hydrogen fluoride and provide technical and equipment support for continuous industrial production.
4) The oxygen difluoride gas generated on the anode plate 3 is collected through an anode gas chamber 14 arranged on the upper part of the anode plate 3, the hydrogen gas generated on the cathode plate 4 is collected through a cathode gas chamber 15 arranged on the upper part of the cathode plate 4, and the gases generated on the anode plate 3 and the cathode plate 4 are respectively collected, so that potential safety hazards caused by contact of the hydrogen generated by the cathode and the oxidizing gas generated by the anode are avoided.
5) The gas collected in the anode gas chamber 14 and the cathode gas chamber 15 is separated and recovered by a reflux device 91, and the non-condensable gas is purified by a purifying device 92 and discharged after reaching standards. The gas collected by the anode plenum 14 includes hydrogen and gaseous HF, and the gas collected by the anode plenum 14 includes OF 2 and gaseous HF. The waste gas is purified by sodium hydroxide solution or sodium carbonate solution respectively, and can be directly discharged after absorbing OF 2 and HF.
After the treatment by the equipment and the method, anhydrous HF with the water content of about 150ppm can be reduced to 10ppm after the electrolytic water removal.
What has been described above is merely some embodiments of the present invention. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit of the invention.
Claims (6)
1. The utility model provides a device that anhydrous hydrogen fluoride removed, its characterized in that, including electrolysis cell body (1), electrolysis cell upper cover (2), anode plate (3), negative plate (4), baffle (5), feed liquor valve (6) and play liquid valve (7), be equipped with electrolysis chamber (13) in electrolysis cell body (1), the one end of electrolysis cell body (1) is equipped with inlet (11), the other end of electrolysis cell body (1) is equipped with outlet (12), the upper end of electrolysis cell body (1) is opened, and electrolysis cell upper cover (2) are fixed in electrolysis cell body (1) and seal electrolysis cell body (1) upper end, anode plate (3), negative plate (4) and baffle (5) all are located electrolysis chamber, anode plate (3) are fixed in electrolysis cell body (1) and separate the lower space of electrolysis chamber (13), negative plate (4) are fixed in electrolysis cell upper cover (2) and extend to the bottom of electrolysis chamber (13), baffle (5) are fixed in electrolysis cell body (2) and are located anode plate (4) and are located air chamber (14) and air chamber (14) are separated into with anode plate (4) and air chamber (13) between each other The cathode plate (4) and the partition plate (5) are arranged to be a plurality of pieces, the anode plate (3) and the cathode plate (4) are sequentially and alternately arranged to enable an S-shaped liquid flow channel to be formed between a liquid inlet (11) and a liquid outlet (12) of the electrolytic tank body (1), an upper cover (2) of the electrolytic tank is provided with an anode air chamber air outlet (21) and a cathode air chamber air outlet (22), the anode air chamber air outlet (21) is communicated with an anode air chamber (14), the cathode air chamber air outlet (22) is communicated with a cathode air chamber (15), the liquid inlet valve (6) is connected with the liquid inlet (11), and the liquid outlet valve (7) is connected with the liquid outlet (12).
2. The anhydrous hydrogen fluoride water removing device according to claim 1, wherein the anode plate (3), the cathode plate (4) and the separator (5) are vertically arranged at intervals and are uniformly arranged in parallel, the anode plate (3) and the cathode plate (4) are made of stainless steel or nickel, and the separator (5) is made of polytetrafluoroethylene.
3. The anhydrous hydrogen fluoride water removing device according to claim 1 or 2, wherein a liquid level line (16) is arranged in the electrolytic tank body (1), the upper end of the anode plate (3) is lower than the liquid level line (16), and the lower end of the partition plate (5) is lower than the liquid level line (16).
4. A device for removing water from anhydrous hydrogen fluoride according to claim 3, wherein the distance between the lower end of the cathode plate (4) and the bottom surface of the electrolytic cavity (13) is 10 mm-150 mm, and the distance between the cathode and the anode is 15 mm-300 mm.
5. The anhydrous hydrogen fluoride water removal device according to claim 1, further comprising a direct current power supply (8), wherein the anode plate (3) is connected with the positive electrode of the direct current power supply (8), the cathode plate (4) is connected with the negative electrode of the direct current power supply, and the voltage of the direct current power supply is 3-7 v.
6. A method of anhydrous hydrogen fluoride removal for an anhydrous hydrogen fluoride removal unit as claimed in claim 3, comprising the steps of:
1) Opening a liquid inlet valve (6) and conveying anhydrous hydrogen fluoride into an electrolytic cavity (13) through a liquid inlet (11);
2) Electrifying the anode plate (3) and the cathode plate (4) to generate ionization reaction on the anode plate (3) and the cathode plate (4) and decompose moisture in hydrogen fluoride, generating oxygen difluoride gas on the anode plate (3) and generating hydrogen gas on the cathode plate (4);
3) After the liquid level of the hydrogen fluoride reaches a liquid level line (16), a liquid outlet valve (7) is opened, so that the dehydrated anhydrous hydrogen fluoride is led into a reaction device or is collected in a product storage tank, and the hydrogen fluoride continuously passes through an electrolytic tank body (1) to continuously treat the moisture in the hydrogen fluoride;
4) Collecting gas generated on the anode plate (3) by an anode gas chamber (14), and collecting gas generated on the cathode plate (4) by a cathode gas chamber (15);
5) The gases collected in the anode air chamber (14) and the cathode air chamber (15) are respectively condensed and reflowed to hydrogen fluoride, and the non-condensable gases are respectively purified and discharged after reaching standards.
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