CN110656344A - Device and method for removing water by using anhydrous hydrogen fluoride - Google Patents
Device and method for removing water by using anhydrous hydrogen fluoride Download PDFInfo
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- CN110656344A CN110656344A CN201911072765.5A CN201911072765A CN110656344A CN 110656344 A CN110656344 A CN 110656344A CN 201911072765 A CN201911072765 A CN 201911072765A CN 110656344 A CN110656344 A CN 110656344A
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910000040 hydrogen fluoride Inorganic materials 0.000 title claims abstract description 84
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000007789 gas Substances 0.000 claims abstract description 78
- 210000005056 cell body Anatomy 0.000 claims abstract description 33
- 210000004027 cell Anatomy 0.000 claims abstract description 20
- 238000005192 partition Methods 0.000 claims abstract description 12
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 67
- 229910000127 oxygen difluoride Inorganic materials 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 abstract description 12
- 239000011737 fluorine Substances 0.000 abstract description 12
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003463 adsorbent Substances 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 208000005156 Dehydration Diseases 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 239000002808 molecular sieve Substances 0.000 description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 4
- 239000011775 sodium fluoride Substances 0.000 description 4
- 235000013024 sodium fluoride Nutrition 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001506 inorganic fluoride Inorganic materials 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- SANRKQGLYCLAFE-UHFFFAOYSA-H uranium hexafluoride Chemical compound F[U](F)(F)(F)(F)F SANRKQGLYCLAFE-UHFFFAOYSA-H 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/245—Fluorine; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses a device for removing water from anhydrous hydrogen fluoride, which comprises an electrolytic cell body, an electrolytic cell upper cover, an anode plate, a cathode plate and a partition plate, wherein an electrolytic cavity is arranged in the electrolytic cell body, the anode plate, the cathode plate and the partition plate are all positioned in the electrolytic cavity, the anode plate is fixed in the electrolytic cell body and separates the lower space of the electrolytic cavity, the cathode plate is fixed in the electrolytic cell upper cover and extends towards the bottom of the electrolytic cavity, the partition plate is fixed in the electrolytic cell upper cover and positioned between the anode plate and the cathode plate, and the partition plate divides the upper space of the electrolytic cavity into an anode gas chamber and a cathode gas chamber. Through the innovative design of the electrode slice and the electrolytic cell, the anhydrous hydrogen fluoride continuous dehydration treatment is realized, and the removal efficiency is improved. The invention also discloses a method for removing water from anhydrous hydrogen fluoride based on the device for removing water from anhydrous hydrogen fluoride, which can realize continuous treatment by removing trace water in the anhydrous hydrogen fluoride by an electrolysis method, does not need an oxidizing agent or an adsorbent such as fluorine gas and the like, and has simple and efficient treatment process.
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 by using anhydrous hydrogen fluoride.
Background
The anhydrous hydrogen fluoride is a chemical product with wide application, the content of the hydrogen fluoride is more than 99.8 percent, the appearance is colorless fuming liquid, and the hydrogen fluoride is easy to gasify under reduced pressure or high temperature. The anhydrous hydrogen fluoride is widely used in atomic energy, chemical industry, petroleum and other industries, is a strong oxidant, is a basic raw material for preparing elemental fluorine, various fluorine refrigerants, inorganic fluorides and various organic fluorides, can be prepared into various kinds of water-containing hydrofluoric acid, and is used as a catalyst for preparing graphite and organic compounds. Is a raw material for producing a refrigerant Freon, fluorine-containing resin, organic fluoride and fluorine. Can be used as a catalyst for organic diaphragm synthesis of alkylation, polymerization, condensation, isomerization and the like in chemical production. It is also used for corroding stratum during mining of some ore deposit and extracting rare earth elements and radioactive elements. In the nuclear industry and nuclear weapons production are the feedstocks for uranium hexafluoride production, and also for rocket fuels and additives. In addition, the anhydrous hydrogen fluoride is also used as a solvent for synthesizing lithium hexafluorophosphate serving as the lithium battery electrolyte.
When anhydrous hydrogen fluoride is used for organic synthesis, fluorine preparation and lithium hexafluorophosphate preparation, the quality of products is easily reduced due to trace moisture in the anhydrous hydrogen fluoride, and serious potential safety hazards are brought. Therefore, it has been necessary to remove water from the anhydrous hydrogen fluoride starting material before 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 moisture content of qualified products of II types of industrial anhydrous hydrogen fluoride is less than or equal to 600ppm, and the moisture content of I types of industrial anhydrous hydrogen fluoride is less than or equal to 50 ppm. On one hand, the distillation cost required for meeting the moisture requirement of the type I is higher, and meanwhile, the anhydrous hydrogen fluoride can absorb moisture in the environment in the processes of filling, storage and transportation to cause the moisture content to rise. In the synthesis reaction, the moisture content in the anhydrous hydrogen fluoride is often required to be reduced to 20ppm or less, and therefore, the anhydrous hydrogen fluoride is not required to be treated to reduce the moisture content before the reaction.
At present, methods for removing water from hydrogen fluoride mainly comprise an adsorption method, a fluorine gas oxidation method and an electrochemical oxidation method.
US patent US5597545 discloses a method for adsorbing moisture from hydrogen fluoride by means of a carbon molecular sieve, which method comprises: contacting hydrogen fluoride with a carbon molecular sieve to adsorb water in the hydrogen fluoride and simultaneously adsorb a part of the hydrogen fluoride; then heating the molecular sieve to resolve the adsorbed water and hydrogen fluoride; then heating is continued, hydrogen fluoride is completely and briefly analyzed, and the carbon molecular sieve is recovered. The method has low water removal efficiency and high treatment cost.
Fluorine gas can oxidize moisture in hydrogen fluoride to generate hydrogen fluoride and oxygen difluoride, the boiling point of the oxygen difluoride is-154 ℃, and the boiling point of the hydrogen fluoride is 19.5 ℃, so that the oxygen difluoride can be easily separated from liquid anhydrous hydrogen fluoride:
2F2+H2O→2HF+OF2
however, the electrolytic preparation cost of fluorine gas is high, the fluorine gas has very strong oxidizability, the water removal reaction is severe, the requirement on equipment material is high, and the danger is large.
Disclosure of Invention
According to one aspect of the invention, a device for removing water from anhydrous hydrogen fluoride is provided, which comprises an electrolytic cell body, an electrolytic cell upper cover, an anode plate, a cathode plate and a separator, an electrolytic cavity is arranged in the electrolytic bath body, a liquid inlet is arranged at one end of the electrolytic bath body, a liquid outlet is arranged at the other end of the electrolytic bath body, the upper end of the electrolytic cell body is open, the electrolytic cell upper cover is fixed on the electrolytic cell body and seals the upper end of the electrolytic cell body, the anode plate, the cathode plate and the clapboard are all positioned in the electrolytic cavity, the anode plate is fixed in the electrolytic cell body and separates the lower space of the electrolytic cavity, the negative plate is fixed on the upper cover of the electrolytic cell and extends towards the bottom of the electrolytic cavity, the separator is fixed on the upper cover of the electrolytic cell and is positioned between the positive plate and the negative plate, and the separator divides the upper space of the electrolytic cavity into an anode gas chamber and a cathode gas 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 plates, the cathode plates and the partition plates are all provided in a plurality of pieces, and the anode plates and the cathode plates are alternately arranged in sequence to form an S-shaped liquid flow channel between a liquid inlet and a liquid outlet of the electrolytic bath body.
In some embodiments, the anode plate, the cathode plate and the separator are vertically arranged at intervals and are parallel and uniformly arranged, 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 cell body, the upper end of the anode plate is lower than the liquid level line, and the lower end of the partition 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 apparatus for removing water from anhydrous hydrogen fluoride further comprises a dc power supply, the anode plate is connected to the positive electrode of the dc power supply, the cathode plate is connected to the negative electrode of the dc power supply, and the voltage of the dc power supply is 3V to 7V.
In some embodiments, the apparatus for removing water from anhydrous hydrogen fluoride further comprises a liquid inlet valve connected to the liquid inlet and a liquid outlet valve connected to 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 the 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 oxygen difluoride 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, the dehydrated anhydrous hydrogen fluoride is led into the reaction device or collected in a product storage tank, and the hydrogen fluoride continuously passes through the electrolytic bath body to continuously treat the moisture in the hydrogen fluoride.
In some embodiments, the method further comprises the steps of:
4) collecting the gas generated on the anode plate by using an anode gas chamber, and collecting the gas generated on the cathode plate by using a cathode gas chamber;
5) the gases collected in the anode gas chamber and the cathode gas chamber are respectively condensed and refluxed with hydrogen fluoride, and the non-condensable gases are respectively purified and discharged after reaching the standard. The noncondensable gas OF the anode gas chamber is OF2And absorbing by using alkali liquor, reacting to generate sodium fluoride and oxygen, and reacting part of uncondensed hydrogen fluoride with alkali to generate sodium fluoride:
OF2+2NaOH→2NaF+H2O+O2↑
HF+NaOH→NaF+H2O
the noncondensable gas in the cathode gas chamber is H2And the hydrogen fluoride 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 invention reasonably designs the device and the method for removing water from anhydrous hydrogen fluoride by utilizing the electrolysis principle, realizes the continuous water removal treatment of the anhydrous hydrogen fluoride by the innovative design of the electrode plate and the electrolytic cell, and improves the removal efficiency. 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 the anhydrous hydrogen fluoride, so that continuous treatment can be realized, oxidation reagents or adsorbents such as fluorine gas and the like are not needed, and the treatment process is simple and efficient.
Drawings
FIG. 1 is a schematic structural 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 A-A of the apparatus for removing water from anhydrous hydrogen fluoride shown in FIG. 1;
FIG. 3 is a schematic diagram of the cathode plate of the apparatus for removing water from anhydrous hydrogen fluoride shown in FIG. 1;
FIG. 4 is a diagram illustrating the operation 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 removing water from anhydrous hydrogen fluoride according to an embodiment of the present invention.
Referring to fig. 1-4, a device for removing water from anhydrous hydrogen fluoride comprises an electrolytic cell body 1, an electrolytic cell upper cover 2, an anode plate 3, a cathode plate 4, a partition plate 5, a liquid inlet valve 6, a liquid outlet valve 7 and a direct current power supply 8.
The electrolytic cell body 1 is square, and an electrolytic cavity 13 is arranged in the electrolytic cell body 1. One end of the electrolytic cell body 1 is provided with a liquid inlet 11, and the other end of the electrolytic cell body 1 is provided with a liquid outlet 12. The upper end of the electrolytic cell body 1 is opened, the edge of the electrolytic cell upper cover 2 is fixed to the edge of the electrolytic cell body 1 by bolts and seals the upper end of the electrolytic cell body 1, so that the electrolytic chamber 13 becomes a closed space. The anode plate 3, the cathode plate 4 and the separator 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 electrolytic cell upper cover 2 and located between the anode plate 3 and the cathode plate 4, the separator 5 partitioning the upper space of the electrolysis chamber 13 into an anode gas chamber 14 and a cathode gas chamber 15.
The upper cover 2 of the electrolytic cell 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 outlet 21 and the cathode gas chamber outlet 22 are respectively communicated with the reflux device 91 and the purification device 92.
The anode plate 3, the cathode plate 4 and the baffle plate 5 are vertically arranged at intervals and are parallel and evenly arranged, the anode plate 3, the cathode plate 4 and the baffle plate 5 are all arranged into a plurality of blocks, and the anode plate 3 and the cathode plate 4 are sequentially and alternately arranged to form an S-shaped liquid flow channel from a liquid inlet 11 to a liquid outlet 12 of the electrolytic bath body 1.
A liquid level line 16 is arranged in the electrolytic cell 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. When the liquid in the electrolytic cell body 1 reaches the liquid level line 16, the liquid in the electrolytic cell body 1 can be ensured to flow smoothly through the S-shaped line.
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 electrolytic 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 pole of the direct current power supply 8, the cathode plate 4 is connected with the negative pole 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 the liquid inlet 11, and the liquid outlet valve 7 is connected with the liquid outlet 12. The liquid level and the liquid flowing speed of the liquid in the electrolytic bath body 1 can be controlled through the liquid inlet valve 6 and the liquid outlet valve 7.
The upper portion of the cathode plate 4 is provided with a notch 41 penetrating the cathode plate 4, so that both sides of the cathode plate 4 form a communicated space, thereby allowing both sides of the cathode plate 4 to share only one air outlet.
The outer side of the electrolytic cell body 1 is also provided with a heat preservation layer 17, the heat preservation layer 17 can ensure the temperature stability of the electrolytic cell body 1, and ensure that anhydrous hydrogen fluoride is always in a liquid state in the electrolytic cell, so that 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 sealing performance between the electrolytic tank body 1 and the electrolytic tank upper cover 2.
By the structural design of the electrolytic cell body, the gas phase space at the upper part in the cell is divided into an anode gas chamber 14 and a cathode gas chamber 15 by the partition plate 5 and the anhydrous HF liquid level. Because the gas generated on the surfaces of the anode plate 3 and the cathode plate 4 has low density, the gas respectively enters the anode gas chamber 14 and the cathode gas chamber 15 after floating up, and then respectively enters the condensation reflux device through the anode gas chamber air outlet 21 and the cathode gas chamber air outlet 22. By arranging the anode gas chamber 14 and the cathode gas chamber 15, potential safety hazards caused by the contact of 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, the anode is directly fixed on the bottom surface of the electrolytic tank, and the anhydrous HF is baffled in the electrolytic tank in an up-and-down S-shaped manner through the arrangement of the anode and the cathode, so that the anhydrous HF and the surface of the electrode are fully contacted for electrolytic dewatering, and the moisture removal efficiency is improved.
Example 2
A method applied to the apparatus for removing water from anhydrous hydrogen fluoride of example 1, comprising the steps of:
1) opening the liquid inlet valve 6, and conveying the anhydrous hydrogen fluoride in the storage container into the electrolysis cavity 13 through the liquid inlet 11;
2) turning on the direct current power supply 8, electrifying the anode plate 3 and the cathode plate 4 to generate ionization reaction on the anode plate 3 and the cathode plate 4 to decompose moisture in the hydrogen fluoride, generating oxygen difluoride gas on the anode plate 3 and generating hydrogen gas on the cathode plate 4;
the electrolysis of anhydrous hydrogen fluoride also removes trace amounts of water. The principle is as follows: because of the existence of water, part of hydrogen fluoride is ionized into hydrogen ions and fluorine ions, after the power is switched on, the reaction that the hydrogen ions are obtained by electrons at the cathode to separate out hydrogen gas occurs, and the reaction that water molecules are oxidized to generate oxygen difluoride occurs at the anode:
cathode: 4H++4e-→2H2↑
Anode: h2O+4F--4e-→OF2↑+2HF
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 introduced into the reaction device or collected in a product storage tank, and the hydrogen fluoride can continuously pass through the electrolytic cell body 1. Can realize continuous treatment of water in the hydrogen fluoride and provide technical and equipment support for continuous industrial production.
4) Collecting the oxygen difluoride gas generated on the anode plate 3 by means of an anode gas chamber 14 provided at the upper portion of the anode plate 3, and collecting the hydrogen gas generated on the cathode plate 4 by means of a cathode gas chamber 15 provided at the upper portion of the cathode plate 4; the gases generated on the anode plate 3 and the cathode plate 4 are respectively collected, so that potential safety hazards caused by the contact of the hydrogen generated by the cathode and the oxidizing gas generated by the anode are avoided.
5) The gases collected in the anode gas chamber 14 and the cathode gas chamber 15 are respectively separated and recycled by the reflux device 91, and the non-condensable gases are respectively purified by the purification device 92 and discharged after reaching the standard. The gas collected by the anode gas chamber 14 comprises hydrogen and gaseous HF, and the gas collected by the anode gas chamber 14 comprises OF2And gaseous HF. Purifying with sodium hydroxide solution or sodium carbonate solution to absorb OF2And may be discharged directly after HF.
After the treatment by the equipment and the method, the water content of the anhydrous HF with the water content of about 150ppm can be reduced to 10ppm after the water is removed by electrolysis.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept herein, and it is intended to cover all such modifications and variations as fall within the scope of the invention.
Claims (10)
1. The device for removing water from anhydrous hydrogen fluoride is characterized by comprising an electrolytic cell body (1), an electrolytic cell upper cover (2), an anode plate (3), a cathode plate (4) and a partition plate (5), wherein an electrolytic cavity (13) is arranged in the electrolytic cell body (1), one end of the electrolytic cell body (1) is provided with a liquid inlet (11), the other end of the electrolytic cell body (1) is provided with a liquid outlet (12), the upper end of the electrolytic cell body (1) is open, the electrolytic cell upper cover (2) is fixed on the electrolytic cell body (1) and seals the upper end of the electrolytic cell body (1), 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 cell body (1) and separates the lower space of the electrolytic cavity (13), the cathode plate (4) is fixed on the electrolytic cell upper cover (2) and extends to the bottom of the electrolytic cavity (13), the separator (5) is fixed on the upper cover (2) of the electrolytic tank and positioned between the anode plate (3) and the cathode plate (4), and the separator (5) divides the upper space of the electrolytic cavity (13) into an anode air chamber (14) and a cathode air chamber (15).
2. The anhydrous hydrogen fluoride water removal device according to claim 1, wherein the upper cover (2) of the electrolytic cell is provided with an anode gas chamber outlet (21) and a cathode gas chamber outlet (22), the anode gas chamber outlet (21) is communicated with the anode gas chamber (14), and the cathode gas chamber outlet (22) is communicated with the cathode gas chamber (15).
3. The device for removing water by anhydrous hydrogen fluoride according to claim 2, characterized in that the anode plates (3), the cathode plates (4) and the partition plates (5) are all provided in a plurality of pieces, and the anode plates (3) and the cathode plates (4) are alternately arranged in sequence to form an S-shaped liquid flow channel from the liquid inlet (11) to the liquid outlet (12) of the electrolytic bath body (1).
4. The anhydrous hydrogen fluoride water removal device according to claim 3, 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.
5. The device for removing water from anhydrous hydrogen fluoride according to any one of claims 1 to 4, wherein a liquid level line (16) is arranged in the electrolytic cell 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).
6. The anhydrous hydrogen fluoride water removal device according to claim 5, wherein the distance between the lower end of the cathode plate (4) and the bottom surface of the electrolysis chamber (13) is 10 mm-150 mm, and the distance between the cathode and the anode is 15 mm-300 mm.
7. The device for removing water by anhydrous hydrogen fluoride according to claim 1, further comprising a direct current power supply (8), wherein the anode plate (3) is connected with the positive pole of the direct current power supply (8), the cathode plate (4) is connected with the negative pole of the direct current power supply, and the voltage of the direct current power supply is 3-7V.
8. The apparatus for removing water from anhydrous hydrogen fluoride according to claim 1, further comprising a liquid inlet valve (6) and a liquid outlet valve (7), wherein the liquid inlet valve (6) is connected to the liquid inlet (11), and the liquid outlet valve (7) is connected to the liquid outlet (12).
9. A method for removing water from anhydrous hydrogen fluoride is characterized by comprising the following steps:
1) opening a liquid inlet valve (6), and conveying anhydrous hydrogen fluoride into an electrolysis 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 the 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, the dehydrated anhydrous hydrogen fluoride is introduced into a reaction device or collected in a product storage tank, and the hydrogen fluoride continuously passes through the electrolytic bath body (1) to continuously treat the water in the hydrogen fluoride.
10. The apparatus for removing water from anhydrous hydrogen fluoride according to claim 1, further comprising the steps of:
4) collecting the gas generated on the anode plate (3) by an anode gas chamber (14) and collecting the gas generated on the cathode plate (4) by a cathode gas chamber (15);
5) the gases collected in the anode gas chamber (14) and the cathode gas chamber (15) are respectively condensed and refluxed with hydrogen fluoride, and the non-condensable gases are respectively purified and discharged after reaching standards.
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Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4444631A (en) * | 1981-05-11 | 1984-04-24 | Occidental Chemical Corporation | Electrochemical purification of chlor-alkali cell liquor |
| CN1100152A (en) * | 1993-02-10 | 1995-03-15 | 拜尔公司 | Process for purifying hydrogen fluoride |
| US5411726A (en) * | 1993-02-10 | 1995-05-02 | Bayer Ag | Process for purifying hydrogen fluoride |
| CN1441857A (en) * | 2000-04-07 | 2003-09-10 | 东洋炭素株式会社 | Apparatus for generating fluorine gas |
| WO2006104416A1 (en) * | 2005-03-31 | 2006-10-05 | Zakrytoe Aktsionernoe Obschestvo 'astor-Electronics' | Nitrogen trifluoride production method |
| KR20070057489A (en) * | 2005-12-02 | 2007-06-07 | 주식회사 효성 | The electrolyzer for manufacturing nitrogen tri-fluoride to minimize the amount of a vaporized hydrogen flouride and the manufacturing method using the same |
| CN101213325A (en) * | 2006-01-20 | 2008-07-02 | 东洋炭素株式会社 | Electrolytic apparatus for producing fluorine or nitrogen trifluoride |
| CN101748424A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for preparing trifluoromethyl sulfuryl fluoride CF3SO2F by electrochemical fluorination of methanesulfonyl fluoride CH3SO2F |
| CN202778277U (en) * | 2012-09-10 | 2013-03-13 | 昆明理工大学 | Water-removing device for water-containing methanol |
| CN203639569U (en) * | 2013-12-10 | 2014-06-11 | 福建省邵武市永晶化工有限公司 | Dewatering device for electrolyte in sulfur hexafluoride production |
| KR20150144496A (en) * | 2014-06-17 | 2015-12-28 | (주)대룡이앤씨 | Facility for electrowinning of copper with high purity from wastewater and method therefor |
| CN205893401U (en) * | 2016-07-07 | 2017-01-18 | 洛阳高昌机电科技有限公司 | High -efficient fluorine gas preparation facilities |
| CN108059142A (en) * | 2017-12-13 | 2018-05-22 | 江苏新泰材料科技有限公司 | Minor amount of water minimizing technology in lithium hexafluoro phosphate production technology |
| CN109468658A (en) * | 2018-12-11 | 2019-03-15 | 浙江巨圣氟化学有限公司 | A kind of preparation method of carbonyl fluoride |
| CN211689249U (en) * | 2019-11-05 | 2020-10-16 | 贵州理工学院 | Device for dewatering anhydrous hydrogen fluoride |
-
2019
- 2019-11-05 CN CN201911072765.5A patent/CN110656344A/en active Pending
Patent Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4444631A (en) * | 1981-05-11 | 1984-04-24 | Occidental Chemical Corporation | Electrochemical purification of chlor-alkali cell liquor |
| CN1100152A (en) * | 1993-02-10 | 1995-03-15 | 拜尔公司 | Process for purifying hydrogen fluoride |
| US5411726A (en) * | 1993-02-10 | 1995-05-02 | Bayer Ag | Process for purifying hydrogen fluoride |
| CN1441857A (en) * | 2000-04-07 | 2003-09-10 | 东洋炭素株式会社 | Apparatus for generating fluorine gas |
| WO2006104416A1 (en) * | 2005-03-31 | 2006-10-05 | Zakrytoe Aktsionernoe Obschestvo 'astor-Electronics' | Nitrogen trifluoride production method |
| KR20070057489A (en) * | 2005-12-02 | 2007-06-07 | 주식회사 효성 | The electrolyzer for manufacturing nitrogen tri-fluoride to minimize the amount of a vaporized hydrogen flouride and the manufacturing method using the same |
| CN101213325A (en) * | 2006-01-20 | 2008-07-02 | 东洋炭素株式会社 | Electrolytic apparatus for producing fluorine or nitrogen trifluoride |
| CN101748424A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for preparing trifluoromethyl sulfuryl fluoride CF3SO2F by electrochemical fluorination of methanesulfonyl fluoride CH3SO2F |
| CN202778277U (en) * | 2012-09-10 | 2013-03-13 | 昆明理工大学 | Water-removing device for water-containing methanol |
| CN203639569U (en) * | 2013-12-10 | 2014-06-11 | 福建省邵武市永晶化工有限公司 | Dewatering device for electrolyte in sulfur hexafluoride production |
| KR20150144496A (en) * | 2014-06-17 | 2015-12-28 | (주)대룡이앤씨 | Facility for electrowinning of copper with high purity from wastewater and method therefor |
| CN205893401U (en) * | 2016-07-07 | 2017-01-18 | 洛阳高昌机电科技有限公司 | High -efficient fluorine gas preparation facilities |
| CN108059142A (en) * | 2017-12-13 | 2018-05-22 | 江苏新泰材料科技有限公司 | Minor amount of water minimizing technology in lithium hexafluoro phosphate production technology |
| CN109468658A (en) * | 2018-12-11 | 2019-03-15 | 浙江巨圣氟化学有限公司 | A kind of preparation method of carbonyl fluoride |
| CN211689249U (en) * | 2019-11-05 | 2020-10-16 | 贵州理工学院 | Device for dewatering anhydrous hydrogen fluoride |
Non-Patent Citations (1)
| Title |
|---|
| 郭爱红等: "电解法去除氟化氢中微量水", 《南开大学学报（自然科学版）》, vol. 38, no. 5, 31 October 2005 (2005-10-31), pages 62 - 64 * |
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