CN212292799U - 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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- CN212292799U CN212292799U CN202021866745.3U CN202021866745U CN212292799U CN 212292799 U CN212292799 U CN 212292799U CN 202021866745 U CN202021866745 U CN 202021866745U CN 212292799 U CN212292799 U CN 212292799U
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Abstract
The utility model discloses an anhydrous hydrogen fluoride's electrolytic dehydration device is used in hexafluorophosphate synthesis, including arranging in the electrolysis trough and surrounding the parcel at the positive negative pole stick outer periphery lead the chamber structure, the absorption structure that opens and shuts in the electrolysis trough bottom in addition activity, the export and the exocoel seal structure of absorption structure are connected, it includes outer ring circle and inner ring circle to lead the chamber structure, positive negative pole stick vertical cut inlays the junction at outer ring circle and inner ring circle, the utility model discloses a set up in the hydrogen fluoride liquid of circulation near and between the two positive negative pole stick of electrolysis trough and lead the chamber structure, can accelerate the circulation of electron in the solution, improve the electrolytic effect between the positive negative pole, make the hydrone in the hydrogen fluoride can be by more complete of ionization, fall to minimum with the water content in the hydrogen fluoride solution, better get rid of the water in the hydrogen fluoride solution.
Description
Technical Field
The utility model relates to an anhydrous hydrogen fluoride purification equipment especially relates to an anhydrous hydrogen fluoride's electrolytic dehydration device for hexafluorophosphate synthesis.
Background
Hexafluorophosphate, especially lithium hexafluorophosphate, has become one of the important electrolytes for manufacturing secondary lithium ion batteries because of its unique physicochemical and electrochemical properties, and the synthesis of lithium hexafluorophosphate in the prior art generally adopts the reaction of phosphorus pentafluoride and lithium fluoride in the hydrogen fluoride liquid of a non-aqueous solvent to synthesize lithium hexafluorophosphate, and in order to improve the purity of the electrolyte, the hydrogen fluoride is dehydrated, and is a colorless, pungent and toxic gas in a normal state, and has very strong hygroscopicity, and white smoke is generated when contacting air, and is easily soluble in water, can be dissolved into water infinitely to form hydrofluoric acid, and hydrogen fluoride has hygroscopicity and is "fuming" after absorbing moisture in air.
Based on the above description, the present inventors found that the existing anhydrous hydrogen fluoride electrolytic dehydration device for hexafluorophosphate synthesis mainly has the following disadvantages, for example:
the prior art only carries out simple reaction to hydrogen fluoride and absorbs water, it is relatively poor to remove water performance, easily react with the material in the electrolyte and reduce the purity of electrolyte, some adopt the electrolytic mode to electrolyze hydrogen fluoride, adopt metal halide as the conducting agent in electrolytic solution, can be consumed gradually in the electrolysis, can receive the influence along with the electron conduction effect in the electrolytic solution of carrying out of electrolytic reaction, make the hydrone in the later stage of electrolytic process more difficult to be ionized, and electrolytic process often needs to last very long can with the hydrone in the solution
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problem, the utility model provides an electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis, which aims to solve the existing problem.
In order to achieve the above purpose, the present invention is realized by the following technical solution: an electrolytic dehydration apparatus for anhydrous hydrogen fluoride for hexafluorophosphate synthesis, comprising:
the electrolytic bath comprises a power supply, an anode bar, a cathode bar and gas collecting cavities locked at two ends of the electrolytic bath;
the guide cavity structure is arranged in the electrolytic bath and surrounds and wraps the outer circumferential surfaces of the positive and negative electrode bars, the suction structure is movably opened and closed at the bottom of the electrolytic bath, and an outlet of the suction structure is connected with the outer cavity sealing structure;
the cavity guide structure comprises an outer ring and an inner ring, and the positive and negative electrode bars are vertically inserted at the joint of the outer ring and the inner ring.
According to one implementation mode, the outer ring comprises a ring, the inner wall of the ring is formed by a plurality of layers of transmission nets, sleeves are embedded in the positions, perpendicular to the positive and negative rods, of the ring, and the ring and the anode rod are connected together through the stand columns and are located on the same perpendicular plane.
According to one implementation mode, the transmission network is formed by combining and connecting a plurality of regular hexagonal fixed frames, and a through passage is formed between the fixed frames.
According to one possible embodiment, the suction structure comprises a rotary tube, the centre of which is a solid support column and the outside of which is a hollow spring structure, the top end of which is connected with the bottom of the electrolytic cell via a valve.
According to an implementation mode, a flow groove is locked at the bottom of each circle of the inner wall of the rotary pipe, the liquid flowing in the flow groove is concentrated sulfuric acid, and a pump is buckled at the outlet of the rotary pipe.
According to one possible embodiment, the height of the gas collection chamber from the electrolyte liquid in the electrolytic cell is 5 cm.
According to an implementation mode, the material adopted by all the structures of the outer ring, the inner ring and the inner part can be any one of carbon nanotubes, carbon fibers and graphene.
According to an embodiment, the height of the outer ring and the inner ring is higher than the height of the anode and cathode rods immersed in the solution.
The utility model relates to an anhydrous hydrogen fluoride's electrolytic dehydration device is used in hexafluorophosphate synthesis, reasonable in design, functional strong has following beneficial effect:
the utility model discloses a set up near the positive negative pole stick of electrolysis trough and between the two in the hydrogen fluoride liquid of circulation and lead the chamber structure, can accelerate the circulation of electron in the solution, improve the electrolysis effect between the positive negative pole, make the hydrone in the hydrogen fluoride can be by more complete of ionization, fall to the water content in the hydrogen fluoride solution minimum, better get rid of the water in the hydrogen fluoride solution.
The utility model discloses a suction structure of establishhing behind the electrolysis process can let in the passageway that possesses the concentrated sulfuric acid with the lower solution of water content behind the ionization process, all can contact with the concentrated sulfuric acid at the in-process of the transmission that flows at every turn, makes the concentrated sulfuric acid reduce the water content in the solution that the water content originally was less than 30ppm once more, improves the purity of hydrogen fluoride solution once more, reduces the influence of water in the hydrogen fluoride solution to hexafluorophosphate reaction.
Drawings
Other features, objects, and advantages of the present invention will become more apparent from the following detailed description of the embodiments of the invention when taken in conjunction with the accompanying drawings, in which:
fig. 1 is a schematic structural diagram of the anhydrous hydrogen fluoride electrolytic dehydration device for hexafluorophosphate synthesis of the present invention.
Fig. 2 is a schematic structural view of the cavity structure of the present invention.
Fig. 3 is a schematic structural view of a three-dimensional half-section of the outer ring of the present invention.
Fig. 4 is a schematic structural diagram of the cross section of the transmission network according to the present invention after expansion.
Fig. 5 is a schematic view of the structure of the transmission network of the present invention when installed inside a ring.
Fig. 6 is a schematic structural diagram of the suction structure of the present invention.
Description of reference numerals: an electrolytic bath-0, a gas receiving cavity-1, a guide cavity structure-2,
A suction structure-3, an outer ring-20, an inner ring-21, a ring-200,
A transmission network-201, a through passage-010, a fixed frame-011 and a rotary pipe-31.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit 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 are the terms "upper", "lower", "left", "right", etc. indicating the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, it is only for convenience of description and simplification of the description, but it is not intended to indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore the terms describing the positional relationship in the drawings are only for illustrative purposes and are not to be construed as limitations of the present patent, and those skilled in the art can understand the specific meanings of the terms according to specific situations.
The examples are as follows:
as shown in attached figures 1 to 6, the utility model provides an electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis, which comprises an electrolytic tank 0 with a power supply and a positive and negative pole bar and a gas receiving cavity 1 locked at the two ends of the electrolytic tank, wherein the electrolytic tank 0 is provided with a moisture monitoring structure, the moisture content in the hydrogen fluoride solution can be checked in real time, the power supply is kept between 4.5V and 7V during electrolysis, and the time is controlled at 15 h to 18 h;
the cavity guide structure 2 is arranged in the electrolytic bath 0 and surrounds and wraps the outer circumferential surfaces of the positive and negative electrode rods, not only can surround the periphery of the electrode rods to enhance the electronic charging and discharging effect of the periphery of the electrode rods, but also can be positioned in any position of a reaction area to improve the conductivity in the whole area, and the cavity guide structure also comprises a suction structure 3 movably opened and closed at the bottom of the electrolytic bath 0, wherein the 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 rods are vertically inserted and embedded at the joint of the outer ring 20 and the inner ring 21, the outer ring 20 wraps the outer side of the pole rods, and the inner ring 21 is tightly attached to the inner side of the pole rods, so that the electric conduction and reaction effects at the pole rods 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, sleeves 202 are embedded at the positions where the ring 200 is vertically intersected with the positive and negative electrode rods, the ring 200 and the ring 200 are connected together through columns 203 and are located on the same vertical plane, the sleeves 202 and the columns 203 are continuously connected from top to bottom, the electrode rods can be completely wrapped, the mobility of electrons of the electrode rods in the charging and discharging process is better enhanced, the electrode rods are uniform from top to bottom, and the electrolyte is distributed throughout the whole electrolytic cell 0.
As shown in fig. 4, the transmission network 201 is formed by combining and connecting a plurality of regular hexagonal solid frames 011, a through channel 010 is disposed between the solid frames 011 and 011, and a honeycomb-like flow structure is provided, so that the speed of hydrogen ions and hydronium ions flowing to the cathode and the anode is not hindered due to the limitation of the frame, the solid frame 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 channel 010 to enhance the conductivity of the solution in one stage, thereby greatly improving the electrolysis speed in the initial stage.
As shown in fig. 5, suction structure 3 is including rotary pipe 31, rotary pipe 31 center is solid support column, and the outside is hollow spring structure, and the top links together via the bottom of valve and electrolysis trough 0, the bottom of every round of rotary pipe 31 inner wall all locks has chute 30, and the liquid that flows in chute 30 is concentrated sulfuric acid, and rotary pipe 31's exit lock has been had pump machine 32, can carry out absorption effect once more after the electrolytic dehydration, adopts the concentrated sulfuric acid that does not react with hydrogen fluoride, reduces the water content in the hydrogen cyanide when not producing other impurity, and concentrated sulfuric acid wraps up the one deck tympanic membrane outward, but the two is mutually soluble again when can guaranteeing to contact with hydrogen fluoride.
As shown in the attached drawing 1, the gas collecting cavity 1 is 5cm away from electrolyte liquid in the electrolytic cell 0, so that gas generated during electrolysis can be rapidly taken away and recycled, on one hand, pollution is prevented from being timely recycled, and on the other hand, reversible reaction caused by accumulation in equipment is prevented.
As shown in fig. 2, the material used for 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 material is selected from carbon nanotubes, carbon fibers and graphene, which are all formed by combining carbon structures, do not react with hydrogen fluoride and can improve the mobility of electrons.
As shown in fig. 1, the height of the outer ring 20 and the inner ring 21 is higher than the height of the anode and cathode rods immersed in the solution, and higher than the hydrogen fluoride solution can prevent the flow rate of solution electrons near the top layer of the liquid surface from being affected and unable to be accelerated due to the fact that the solution electrons cannot contact with the guide cavity structure 2.
Before hexafluorophosphate needs to be prepared, the hydrogen fluoride solution needs to be dehydrated firstly, the utility model discloses an electrolysis method is dehydrated, the hydrogen fluoride solution is led into a closed electrolytic cell 0, more water molecules are prevented from being formed by reaction with water vapor in the air in the electrolytic process, the power supply OF the electrolytic cell 0 is activated after the hydrogen fluoride solution is led into, the positive and negative electrode bars OF the electrolytic cell 0 begin to generate current, the solution in the electrolytic cell is electrolyzed, when the electrolysis occurs, hydrogen ions can move to the cathode to cause the generation OF hydrogen, namely 2H + → H2 ×, the anode is the hydronium ions generated by the reaction OF water and hydrogen fluoride, namely H2O + HF → H3O + + F-, H3O + generates OF2 × (F) under the fluorination OF hydrogen fluoride, so that water is continuously electrolyzed and separated into gas to overflow, on the basis OF the reaction, the hydrogen ions and the fluorine ions generated during the electrolysis are dissociated in the solution and can be pulled by the outer ring 20 and the inner ring 21, more obvious near the anode and cathode bars, the anode and cathode particles and electrons in the hydrogen fluoride solution are accelerated, the speed and the volume of hydrogen synthesized by hydrogen ions are improved, the speed and the quantity of water decomposed into hydronium ions are increased, the water in the hydrogen fluoride is gradually decomposed by the electrolytic reaction to form gas which is discharged from the gas receiving cavity 1, the reaction is stopped after the water content of the hydrogen fluoride is less than 30ppm, the gas is pumped out by the hydrogen fluoride solution after the electrolysis is finished, and then the gas is introduced into the rotary pipe 31, when the pipeline in the rotary pipe 31 flows downwards, the pipeline contacts with concentrated sulfuric acid in the launder 30 every time the pipeline flows downwards for one circle, the trace moisture in the hydrogen fluoride solution is treated once again, and concentrated sulfuric acid is not taken away when the hydrogen fluoride is contacted, so that the water content in the hydrogen fluoride solution is far less than 30ppm, the purity of the hydrogen fluoride is improved, and the interference on the preparation of the hexafluorophosphate is reduced.
The embodiments of the present 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 embodiment was 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 (8)
1. An electrolytic dehydration apparatus for anhydrous hydrogen fluoride for hexafluorophosphate synthesis, comprising:
an electrolysis trough (0) of power and positive and negative pole stick and lock receipts gas chamber (1) at its both ends, its characterized in that:
the guide cavity structure (2) is arranged in the electrolytic bath (0) and surrounds and wraps the outer circumferential surfaces of the positive and negative electrode bars, the suction structure (3) is movably opened and closed at the bottom of the electrolytic bath (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 positive and negative electrode bars are vertically inserted and embedded at the joint of the outer ring (20) and the inner ring (21).
2. The electrolytic dehydration apparatus of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 1, characterized in that: 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), sleeves (202) are embedded in the positions, which are perpendicular to the positive and negative rods, of the ring (200), and the ring (200) are connected together through a stand column (203) and are positioned on the same vertical plane.
3. The electrolytic dehydration apparatus of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 2, wherein: the transmission network (201) is formed by combining and connecting a plurality of regular hexagonal fixed frames (011), and a through passage (010) is arranged between the fixed frames (011).
4. The electrolytic dehydration apparatus of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 1, characterized in that: the suction structure (3) comprises a rotary pipe (31), the center of the rotary pipe (31) is a solid supporting column, the outer part of the rotary pipe is of 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.
5. The electrolytic dehydration apparatus of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 4, wherein: the bottom of each circle of the inner wall of the rotary pipe (31) is locked with a flow groove (30), liquid flowing in the flow groove (30) is concentrated sulfuric acid, and the outlet of the rotary pipe (31) is buckled with a pump (32).
6. The electrolytic dehydration apparatus of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 1, characterized in that: the height between the gas collecting cavity (1) and electrolyte liquid in the electrolytic bath (0) is 5 cm.
7. The electrolytic dehydration apparatus of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 2, wherein: the materials adopted by the outer ring (20), the inner ring (21) and all the internal structures can be any one of carbon nanotubes, carbon fibers and graphene.
8. The electrolytic dehydration apparatus of anhydrous hydrogen fluoride for hexafluorophosphate synthesis according to claim 7, wherein: the height of the outer ring (20) and the inner ring (21) is higher than that of the part of the positive and negative electrode rods immersed in the solution.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111847385A (en) * | 2020-08-31 | 2020-10-30 | 福建省龙德新能源股份有限公司 | Electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111847385A (en) * | 2020-08-31 | 2020-10-30 | 福建省龙德新能源股份有限公司 | Electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis |
| CN111847385B (en) * | 2020-08-31 | 2024-05-10 | 福建省龙德新能源有限公司 | Electrolytic dehydration device of anhydrous hydrogen fluoride for hexafluorophosphate synthesis |
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Address after: No. 30, Gongye Road, Pingpu village, Jiaoyang Town, Shanghang County, Longyan City, Fujian Province, 364000 Patentee after: Fujian Longde new energy Co.,Ltd. Address before: 364000 Jiaoyang Industrial Development Zone, Shanghang County, Longyan City, Fujian Province Patentee before: Fujian Longde new energy Co.,Ltd. |
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