CN111847385B - Electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis - Google Patents
Electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis Download PDFInfo
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- CN111847385B CN111847385B CN202010899342.7A CN202010899342A CN111847385B CN 111847385 B CN111847385 B CN 111847385B CN 202010899342 A CN202010899342 A CN 202010899342A CN 111847385 B CN111847385 B CN 111847385B
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- ring
- hydrogen fluoride
- electrolytic
- electrolytic tank
- anhydrous hydrogen
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910000040 hydrogen fluoride Inorganic materials 0.000 title claims abstract description 41
- -1 hexafluorophosphate Chemical compound 0.000 title claims abstract description 26
- 230000018044 dehydration Effects 0.000 title claims abstract description 15
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 15
- 230000015572 biosynthetic process Effects 0.000 title claims description 10
- 238000003786 synthesis reaction Methods 0.000 title claims description 10
- 238000007789 sealing Methods 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 230000005540 biological transmission Effects 0.000 claims description 9
- 239000003792 electrolyte Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 4
- 239000004917 carbon fiber Substances 0.000 claims description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 25
- 238000005868 electrolysis reaction Methods 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 10
- 208000035208 Ring chromosome 20 syndrome Diseases 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910001507 metal halide Inorganic materials 0.000 description 2
- 150000005309 metal halides Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000752 ionisation method Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- OBCUTHMOOONNBS-UHFFFAOYSA-N phosphorus pentafluoride Chemical compound FP(F)(F)(F)F OBCUTHMOOONNBS-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/195—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses an electrolytic dehydration device of anhydrous hydrogen fluoride for synthesizing hexafluorophosphate, which comprises a cavity guiding structure which is arranged in an electrolytic tank and surrounds the outer circumference of positive and negative electrode rods, and a sucking structure which is movably opened and closed at the bottom of the electrolytic tank, wherein an outlet of the sucking structure is connected with an outer cavity sealing structure, the cavity guiding structure comprises an outer ring and an inner ring, and the positive and negative electrode rods are vertically inserted at the joint of the outer ring and the inner ring.
Description
Technical Field
The invention relates to anhydrous hydrogen fluoride purification equipment, in particular to an electrolytic dehydration device of anhydrous hydrogen fluoride for synthesizing hexafluorophosphate.
Background
In the prior art, lithium hexafluorophosphate is generally synthesized by utilizing the reaction of phosphorus pentafluoride and lithium fluoride in a non-aqueous solvent of hydrogen fluoride liquid, so that the purity of the electrolyte is improved, the hydrogen fluoride is dehydrated, is a colorless and pungent poisonous gas in a normal state, has very strong hygroscopicity, generates white smoke when being contacted with air, is easy to dissolve in water, can be infinitely dissolved with water to form hydrofluoric acid, has hygroscopicity and is fuming after being absorbed in the air.
Based on the above description, the present inventors have found that the conventional electrolytic dehydration device for anhydrous hydrogen fluoride for hexafluorophosphate synthesis mainly has the following disadvantages, such as:
The prior art only carries out simple reaction water absorption on hydrogen fluoride, has poor water removal performance, is easy to react with substances in electrolyte to reduce the purity of the electrolyte, and has the advantages that part of the hydrogen fluoride is electrolyzed in an electrolysis mode, metal halide is adopted as a conductive agent in an electrolysis solution, the metal halide is gradually consumed in the electrolysis, the electron conduction effect in the electrolysis solution is influenced along with the progress of the electrolysis reaction, so that water molecules in the later period of the electrolysis process are more difficult to ionize, and the electrolysis process usually needs to last for a long time to be capable of carrying out the water molecules in the solution
Disclosure of Invention
In order to solve the technical problems, the invention provides an electrolytic dehydration device of anhydrous hydrogen fluoride for synthesizing hexafluorophosphate, which aims to solve the existing problems.
In order to achieve the above object, the present invention is realized by the following technical scheme: an apparatus for electrolytic dehydration of anhydrous hydrogen fluoride for hexafluorophosphate synthesis, comprising:
A power supply, an electrolytic tank of the positive and negative electrode bars and air receiving cavities locked at two ends of the electrolytic tank;
The guide cavity structure is arranged in the electrolytic tank and surrounds the outer circumferential surfaces of the anode rod and the cathode rod, and the guide cavity structure is also provided with a suction structure which is movably opened and closed at the bottom of the electrolytic tank, and an outlet of the suction structure is connected with the outer cavity sealing structure;
the guide cavity structure comprises an outer ring and an inner ring, and the positive electrode rod and the negative electrode rod are vertically inserted into the joint of the outer ring and the inner ring.
According to one embodiment, the outer ring comprises a ring, the inner wall of the ring is composed of a plurality of layers of transmission nets, a sleeve is inlaid at the position where the ring vertically intersects with the anode rod and the cathode rod, and the ring are connected together through a column and are located on the same vertical plane.
According to one embodiment, the transmission network is formed by combining and connecting a plurality of regular hexagonal fixed frames, and a through channel is formed between the fixed frames.
According to one embodiment, the suction structure comprises a rotary pipe, wherein the center of the rotary pipe is a solid support column, the outside of the rotary pipe is a hollow spring structure, and the top end of the rotary pipe is connected with the bottom of the electrolytic tank through a valve.
According to one embodiment, the bottom of each circle of the inner wall of the rotary pipe is locked with a launder, the liquid flowing in the launder is concentrated sulfuric acid, and the outlet of the rotary pipe is fastened with a pump.
According to one embodiment, the gas-receiving chamber has a height of 5cm from the electrolyte in the electrolytic cell.
According to one embodiment, the outer ring, the inner ring and all structures inside the outer ring and the inner ring are made of any one of carbon nanotubes, carbon fibers and graphene.
According to one embodiment, the outer and inner rings have a height that is higher than the height of the portion of the anode and cathode bars immersed in the solution.
The invention relates to an electrolytic dehydration device of anhydrous hydrogen fluoride for synthesizing hexafluorophosphate, which has the advantages of reasonable design, strong functionality and the following advantages:
according to the invention, the cavity guide structure is arranged in the hydrogen fluoride liquid flowing near and between the positive electrode rod and the negative electrode rod of the electrolytic tank, so that the circulation of electrons in the liquid can be quickened, the electrolytic effect between the positive electrode and the negative electrode is improved, the water molecules in the hydrogen fluoride can be ionized more completely, the water content in the hydrogen fluoride liquid is reduced to the minimum, and the water in the hydrogen fluoride liquid is better removed.
According to the invention, through the suction structure arranged after the electrolysis process, the solution with lower water content after the ionization process can be introduced into the channel with the concentrated sulfuric acid, and the solution can be contacted with the concentrated sulfuric acid in the flowing and conveying process each time, so that the water content in the solution with the water content of less than 30ppm can be reduced again by the concentrated sulfuric acid, the purity of the hydrogen fluoride solution is improved again, and the influence of water in the hydrogen fluoride solution on the hexafluorophosphate reaction is reduced.
Drawings
In order to more clearly illustrate the technical solution of the embodiments of the present invention, the following detailed description of the drawings in the description of the embodiments will be presented, so that other features, objects and advantages of the present invention will become more apparent:
FIG. 1 is a schematic diagram showing the structure of an apparatus for electrolytic dehydration of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to the present invention.
Fig. 2 is a schematic top view of the guide cavity structure of the present invention.
Fig. 3 is a schematic view of a three-dimensional half-section structure of an outer ring of the present invention.
Fig. 4 is a schematic structural view of the transmission network of the present invention after the section thereof is unfolded.
Fig. 5 is a schematic view of the structure of the transmission net of the present invention when installed inside the loop.
Fig. 6 is a detailed schematic diagram of the suction structure of the present invention.
Reference numerals illustrate: an electrolytic tank-0, a gas collecting cavity-1, a guide cavity structure-2,
Suction structure-3, outer ring-20, inner ring-21, ring-200,
The device comprises a transmission network-201, a through channel-010, a fixed frame-011 and a rotary pipe-31.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The same or similar reference numerals in the drawings of the present embodiment correspond to the same or similar components; in the description of the present invention, it should be understood that, if there is an azimuth or positional relationship indicated by terms such as "upper", "lower", "left", "right", etc., based on the azimuth or positional relationship shown in the drawings, it is only for convenience of describing the present invention and simplifying the description, but it is not indicated or implied that the apparatus or element referred to must have a specific azimuth, be constructed and operated in a specific azimuth, and thus terms describing the positional relationship in the drawings are merely illustrative and should not be construed as limitations of the present patent, and specific meanings of the terms described above may be understood by those skilled in the art according to specific circumstances.
Examples are as follows:
As shown in the accompanying drawings from 1 to 6, the invention provides an electrolytic dehydration device of anhydrous hydrogen fluoride for synthesizing hexafluorophosphate, which comprises a power supply, an electrolytic tank 0 of positive and negative electrode rods and a gas receiving cavity 1 locked at two ends of the electrolytic tank 0, wherein the electrolytic tank 0 is internally provided with a moisture monitoring structure, the moisture content in a hydrogen fluoride solution can be checked in real time, the power supply is kept between 4.5 and 7V during electrolysis, and the time is controlled between 15 and 18 hours;
The cavity guiding structure 2 is arranged in the electrolytic tank 0 and surrounds the outer circumferential surfaces of the anode rod and the cathode rod, not only can surround the periphery of the anode rod to enhance the charge and discharge effect of electrons around the anode rod, but also can be positioned in any position of a reaction area to improve the conductivity in the whole area, and also comprises a suction structure 3 which is movably opened and closed at the bottom of the electrolytic tank 0, wherein an outlet of the suction structure 3 is connected with an outer cavity sealing structure;
the cavity guiding structure 2 comprises an outer ring 20 and an inner ring 21, the positive and negative electrode rods are vertically inserted into the joint of the outer ring 20 and the inner ring 21, the outer ring 20 is wrapped on the outer side of the electrode rod, the inner ring 21 is tightly attached to the inner side of the electrode rod, and the electric conduction and reaction effects of the electrode rod can be mainly stimulated and enhanced.
As shown in fig. 3, the outer ring 20 includes a ring 200, the inner wall of the ring 200 is formed by a plurality of layers of transmission nets 201, a sleeve 202 is inlaid at a position where the ring 200 and the anode and cathode bars vertically intersect, the ring 200 and the ring 200 are connected together by a column 203 and are positioned on the same vertical plane, the sleeve 202 is continuously connected with the column 203 from top to bottom, so that the electrode bars can be completely wrapped, the mobility of electrons of the electrode bars in the charging and discharging process is better enhanced, and the electrode bars are relatively uniform from top to bottom and spread over the electrolyte in the whole electrolytic tank 0.
As shown in fig. 4, the transmission network 201 is formed by combining and connecting a plurality of regular hexagonal solid frames 011, through channels 010 are formed between the solid frames 011 and 011, and the like-honeycomb flow structure can prevent the hydrogen ions and hydronium ions from flowing to the cathode and the anode due to the restriction of the frames, the solid frames 011 formed by carbon elements can improve the conductivity and the integral ionization degree, and other consumable conductive agents can be selectively added into the through channels 010, so that the conductivity of the solution in one stage is enhanced, and the electrolysis speed can be greatly improved in the initial stage.
As shown in fig. 5, the suction structure 3 includes a rotary tube 31, the center of the rotary tube 31 is a solid support column, the outside is a hollow spring structure, the top end is connected with the bottom of the electrolytic tank 0 via a valve, the bottom of each circle of the inner wall of the rotary tube 31 is locked with a launder 30, the liquid flowing in the launder 30 is concentrated sulfuric acid, the outlet of the rotary tube 31 is fastened with a pump 32, and the suction effect can be performed again after electrolytic dehydration, and the concentrated sulfuric acid which does not react with hydrogen fluoride is adopted, so that the water content in hydrogen cyanide is reduced while other impurities are not generated.
As shown in figure 1, the height of the gas receiving cavity 1 from electrolyte in the electrolytic tank 0 is 5cm, so that gas generated during electrolysis can be quickly taken away and recycled, pollution is prevented from being timely recycled, and reversible reaction is prevented from being caused by accumulation in the equipment.
As shown in fig. 2, the materials used in the outer ring 20, the inner ring 21 and all the structures inside may be any one of carbon nanotubes, carbon fibers and graphene, and the priority of the materials is carbon nanotube carbon fiber graphene, which are all formed by combining carbon structures, and do not react with hydrogen fluoride and can improve the mobility of electrons.
As shown in fig. 1, the heights of the outer ring 20 and the inner ring 21 are higher than the height of the parts of the positive and negative electrode rods immersed in the solution, and the higher than hydrogen fluoride solution can prevent the mobility of solution electrons approaching the top layer of the liquid surface from being influenced by the fact that the mobility cannot be accelerated due to the fact that the mobility cannot be contacted with the guide cavity structure 2.
Before hexafluorophosphate is needed to be prepared, the invention adopts an electrolytic method to dehydrate the hydrogen fluoride solution, the hydrogen fluoride solution is introduced into a closed electrolytic tank 0 to prevent more water molecules from being formed by reaction with water vapor in the air in the electrolytic process, a power supply OF the electrolytic tank 0 is activated after the introduction, so that the positive and negative electrode bars OF the electrolytic tank 0 start to generate current, the solution in the electrolytic tank is electrolyzed, when the electrolysis occurs, hydrogen ions can move to a cathode to cause hydrogen generation, namely 2H+ & fwdarw H2 #, the anode is that water reacts with hydrogen fluoride to generate hydronium ions, namely H2O+HF- & gtH2O++ F-, H2O+ generates OF2 #, under the fluorination OF the hydrogen fluoride, so that the water is continuously separated into gas by the electrolysis, and the hydrogen ions and the fluorine ions generated during the electrolysis are dissociated in the solution on the basis OF the reaction, the traction OF the outer ring 20 and the inner ring 21 is more obvious near the positive and negative electrode rods, both positive and negative particles and electrons in the hydrogen fluoride solution are accelerated, the speed and volume OF hydrogen ion synthesis hydrogen are improved, the speed and quantity OF water synthesized by hydrogen ions are increased, water in the hydrogen fluoride is gradually decomposed by electrolytic reaction to form gas which is discharged from the gas collecting cavity 1, the reaction is stopped after the water content OF the hydrogen fluoride is less than 30ppm, the gas is pumped into the rotary tube 31 after the hydrogen fluoride solution after the electrolysis is completed, the hydrogen fluoride solution is contacted with concentrated sulfuric acid in the launder 30 when flowing down for one circle, the trace water in the hydrogen fluoride solution is treated once again when contacting, the concentrated sulfuric acid is not taken away, the water content in the hydrogen fluoride solution is far less than 30ppm, the purity OF the hydrogen fluoride is improved, reducing the interference to the preparation of hexafluorophosphate.
The embodiments of the invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Claims (4)
1. An apparatus for electrolytic dehydration of anhydrous hydrogen fluoride for hexafluorophosphate synthesis, comprising:
An electrolytic tank (0) of a power supply and positive and negative electrode rods and an air receiving cavity (1) locked at two ends of the electrolytic tank, which is characterized in that:
The guide cavity structure (2) is arranged in the electrolytic tank (0) and surrounds the outer circumferential surfaces of the anode rod and the cathode rod, and the guide cavity structure is also provided with a suction structure (3) which is movably opened and closed at the bottom of the electrolytic tank (0), and an outlet of the suction structure (3) is connected with the outer cavity sealing structure;
the guide cavity structure (2) comprises an outer ring (20) and an inner ring (21), and the anode rod and the cathode rod are vertically inserted into the joint of the outer ring (20) and the inner ring (21);
The outer ring (20) comprises a ring (200), the inner wall of the ring (200) is composed of a plurality of layers of transmission nets (201), a sleeve (202) is inlaid at the position where the ring (200) is perpendicularly intersected with the anode rod and the cathode rod, and the ring (200) are connected together through stand columns (203) and are positioned on the same vertical plane;
the transmission network (201) is formed by combining and connecting a plurality of regular hexagonal fixed frames (011), and a through channel (010) is formed between the fixed frames (011);
the outer ring (20), the inner ring (21) and all the structures inside are made of any one of carbon nano tubes, carbon fibers and graphene.
2. An apparatus for electrolytic dehydration of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 1, wherein: the suction structure (3) comprises a rotary pipe (31), the center of the rotary pipe (31) is a solid support column, the outside is a hollow spring structure, and the top end of the rotary pipe is connected with the bottom of the electrolytic tank (0) through a valve.
3. An apparatus for electrolytic dehydration of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 1, wherein: the height of the gas receiving cavity (1) from electrolyte in the electrolytic tank (0) is 5cm.
4. An apparatus for electrolytic dehydration of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 1, wherein: the heights of the outer ring (20) and the inner ring (21) are higher than the height of the positive and negative electrode rods immersed in the solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010899342.7A CN111847385B (en) | 2020-08-31 | 2020-08-31 | Electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010899342.7A CN111847385B (en) | 2020-08-31 | 2020-08-31 | Electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis |
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| Publication Number | Publication Date |
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| CN111847385A CN111847385A (en) | 2020-10-30 |
| CN111847385B true CN111847385B (en) | 2024-05-10 |
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| US4950370A (en) * | 1988-07-19 | 1990-08-21 | Liquid Air Corporation | Electrolytic gas generator |
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| CN212292799U (en) * | 2020-08-31 | 2021-01-05 | 福建省龙德新能源股份有限公司 | Electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis |
-
2020
- 2020-08-31 CN CN202010899342.7A patent/CN111847385B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB861978A (en) * | 1958-07-30 | 1961-03-01 | Ici Ltd | Improvements in or relating to a process for the electrolytic production of fluorineand apparatus therefor |
| US4950370A (en) * | 1988-07-19 | 1990-08-21 | Liquid Air Corporation | Electrolytic gas generator |
| CN1231348A (en) * | 1998-04-07 | 1999-10-13 | 黄衍政 | Hydrogen-oxygen mixed gas electrolysis, process and apparatus thereof |
| CN2895439Y (en) * | 2006-03-22 | 2007-05-02 | 李�荣 | Medium-temperature fluorine-making electrolytic tank |
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