CN112323093B - Electrochemical fluorination monopolar parallel filter-pressing type electrolytic cell - Google Patents
Electrochemical fluorination monopolar parallel filter-pressing type electrolytic cell Download PDFInfo
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- CN112323093B CN112323093B CN202011068196.XA CN202011068196A CN112323093B CN 112323093 B CN112323093 B CN 112323093B CN 202011068196 A CN202011068196 A CN 202011068196A CN 112323093 B CN112323093 B CN 112323093B
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Abstract
The invention discloses an electrochemical fluorination single-pole parallel filter-pressing type electrolytic cell, which comprises a cell body, wherein a left-end polar plate and a right-end polar plate are arranged in the cell body, a plurality of pull rods are arranged between the left-end polar plate and the right-end polar plate, and two ends of each pull rod are locked and fixed on the left-end polar plate and the right-end polar plate through disc springs and fastening nuts; a plurality of anode plates and a plurality of cathode plates are arranged between the left end polar plate and the right end polar plate, wherein the anode plates and the cathode plates are alternately arranged; the left end polar plate, the right end polar plate and the negative plate are electrically connected to the negative total conducting bar; the anode plate is electrically connected to the positive electrode total conductive bar. The invention distributes the left end polar plate, the plurality of anode plates, the plurality of cathode plates and the right end polar plate side by side and forms a filter-pressing type serial and parallel structure by serially connecting and fixing the pull rods and the fastening nuts, has the characteristics of equal voltage, compact structure, high current efficiency, strong corrosion resistance and the like, and is suitable for industrial production.
Description
Technical Field
The invention relates to an electrochemical fluorination electrolytic cell, in particular to an electrochemical fluorination unipolar parallel filter-pressing type electrolytic cell.
Background
Fluorochemical compounds and derivatives thereof (also sometimes referred to as organofluoro compounds or fluorochemical compounds) are substances that contain a moiety that is fluoroaliphatic or fluorocarbon in nature, e.g., the moiety is non-polar, hydrophobic, oleophobic, and chemically inert, and, in addition, may contain a moiety that is functional in nature, e.g., the moiety is polar and chemically active. Such materials include commercially available products that are well known to the public, such as those that impart oil-, water-, soil-and soil-repellent properties to textiles, for example, scoth-gard carpet protectants.
One method for producing a variety of fluorine-containing compounds (e.g., perfluorinated and partially fluorinated organofluoro compounds) is electrochemical fluorination, which was first commercialized by 3M corporation, simmons, U.S. chemists. The simons electrolyzer is characterized in that an electrode stack is placed in a cylindrical or square tank and comprises a tank cover, an insulating sealing gasket, a tank body, a tank bottom plate, an anode assembly, a cathode assembly, a serpentine cooler, a reflux cooler, a feeding pipe, a discharging pipe, a power supply lead plate and the like, wherein the cathode assembly and the anode assembly are vertically suspended in the electrolyzer in an insulating and crossed mode at intervals. The mixture of hydrogen fluoride and electrolyte is subjected to electrochemical fluorination reaction at the cathode and the anode of the electrode stack, hydrogen is produced at the cathode, and the required product is produced by oxidation of the anode electrolyte. Simons cells are unipolar cells, each electrode assembly being connected in parallel to a low voltage dc power supply by a terminal, the electrodes being of the same polarity on both sides, i.e. both being cathodic or anodic.
An electrode stack of the Simmons electrolytic cell is hung on a cover of the electrolytic cell, and is insulated by polytetrafluoroethylene, so that a short circuit phenomenon caused by pad burning is easy to occur, and the electric connection between the cell stack and an external connecting line is soaked in hydrogen fluoride electrolyte or gas-phase atmosphere to cause corrosion of the electric connection between the cell stack and the end cover; the heat is generated in the electrolytic process of the Simmons electrolytic cell, the heat exchange assembly and the electrode stack are mixed in the electrolytic cell, and the heat exchange wall is corroded to penetrate the cavity, so that the risk of mutual connection of electrolyte and a refrigerant exists; the upper part of the electrolytic cell is provided with a cathode gas phase space and an anode gas phase space, so that the explosion phenomenon is easy to occur.
Disclosure of Invention
The object of the present invention is to provide an electrochemical fluorination monopolar parallel filter-press type electrolytic cell which solves the problems mentioned in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: an electrochemical fluorination unipolar parallel filter-pressing type electrolytic cell comprises a cell body, wherein a left end polar plate and a right end polar plate which are relatively parallel are arranged in the cell body, an electrolysis region between the left end polar plate and the right end polar plate is provided with a plurality of pull rods which are relatively parallel, and two ends of each pull rod are locked and fixed on the left end polar plate and the right end polar plate through disc springs and fastening nuts; a plurality of anode plates and a plurality of cathode plates are arranged between the left end polar plate and the right end polar plate, the anode plates and the cathode plates are alternately arranged, and the left end polar plate, the plurality of anode plates, the plurality of cathode plates and the right end polar plate are distributed side by side and are connected in series in a filter-pressing manner through pull rods and fastening nuts; the left end pole plate and the right end pole plate are welded with binding posts, the anode binding post is arranged on the anode plate, and the cathode binding post is arranged on the cathode plate; the binding posts of the left end polar plate and the right end polar plate and the negative binding post on the negative plate are connected to the negative total conducting bar through negative copper soft connection, and the positive binding post on the positive plate is connected to the positive total conducting bar through positive copper soft connection; the left end polar plate, the right end polar plate and each cathode plate are electrically connected to a negative electrode main conducting bar, and each anode plate is electrically connected to a positive electrode main conducting bar; an electrolytic liquid inlet is arranged at the middle position of the lower side of the left end polar plate, and an electrolytic gas-liquid outlet is arranged at the upper side of the right end polar plate and close to the middle position.
Furthermore, the electrolysis gas-liquid outlet is divided into an anode gas-liquid outlet and a cathode gas-liquid outlet, the electrolysis liquid inlet is communicated with the lower liquid inlet of each small electrolysis chamber, and the anode gas-liquid outlet and the cathode gas-liquid outlet are respectively communicated with the upper vapor-liquid outlet of each small electrolysis chamber.
Furthermore, insulating sealing gaskets are arranged among the left end pole plate, the plurality of anode plates, the plurality of cathode plates and the right end pole plate, and the insulating sealing gaskets are annular.
Furthermore, the insulating sealing gasket is made of carbon fiber and polytetrafluoroethylene composite or polytetrafluoroethylene material.
Furthermore, a diaphragm used for isolating the cathode and the anode is arranged in an electrolysis area among the left end polar plate, the anode plate, the cathode plate and the right end polar plate, and the diaphragm is made of polytetrafluoroethylene materials and allows ions in electrolyte to permeate but not allow gas phases of the cathode and the anode to permeate.
Furthermore, a polytetrafluoroethylene mesh plate for isolating the cathode and the anode is arranged in an electrolysis region among the left end polar plate, the anode plate, the cathode plate and the right end polar plate; the polytetrafluoroethylene mesh plate mutually compresses the cathode plate, the auxiliary pole catalytic plate and the anode plate.
Furthermore, the anode plate and the cathode plate are both single polar plates, the surfaces of the left side and the right side are both provided with concave-convex structures, the concave-convex structures on the two sides are respectively provided with a secondary catalytic plate, and a plurality of electrolyte channels are formed between the anode plate and the secondary catalytic plate and between the cathode plate and the secondary catalytic plate; the anode plate (6), the auxiliary catalytic plate, the diaphragm, the auxiliary catalytic plate and the cathode plate are in close contact with each other to form an electrolysis small chamber.
Further, the auxiliary pole catalytic plate is a nickel wire mesh or a nickel stretching mesh; the electrode distance of the electrolysis chamber is 1-10 mm, and the current density is 20-1000 mA/cm 2 。
Furthermore, the left end polar plate, the anode plate, the cathode plate and the right end polar plate are all square or circular, and the pull rods are uniformly distributed and fixed along the periphery of the left end polar plate and the right end polar plate.
Furthermore, the number of the pull rods is 4-20, and the pull rods are uniformly distributed and fixed along the periphery of the left end pole plate and the right end pole plate, compared with the prior art, the invention has the beneficial effects that:
(1) The cathode and anode power supply structures are arranged outside the electrolytic cell, so that corrosion caused by electric connection between the galvanic pile and the end cover due to the fact that the power supply structure is soaked in hydrogen fluoride electrolyte or in gas-phase atmosphere in the Simmons electrolytic cell is avoided, the advantages of unipolarity and equal voltage of the Simmons electrolytic cell are kept, the potential control of the cathode plate and the anode plate of the electrode pile is smaller than the corrosion prone potential, the corrosion risk of the polar plate is reduced, and meanwhile, the anode reaction is accurately controlled to produce high-quality products.
(2) The filter-pressing tandem assembly mode of external clamping is adopted, so that the device has the advantages of compact structure, reliable work, convenient maintenance and the like; meanwhile, the invention has good sealing property and corrosion resistance, and is suitable for industrial production.
(3) The heat exchange assembly is separated from the electrode stack, no heat exchange component is arranged in the electrolytic cell, resistance heat generated by the electrolytic cell is exchanged through an external heat exchanger, electrolyte in the electrolytic cell is not in direct contact with a refrigerant, no intermixing danger exists, and the electrolytic process is guaranteed to be reliably carried out.
(4) The cathode plate and the anode plate are provided with the auxiliary catalytic plate, so that the contact surfaces of the two sides of the cathode plate and the anode plate are increased, the zero distance between the electrode and the diaphragm is effectively ensured, and the electrolysis efficiency is improved.
Drawings
FIG. 1 is a schematic front view of the present invention;
FIG. 2 is a schematic partial cross-sectional view of FIG. 1;
FIG. 3 is a left side view schematically illustrating the structure of embodiments 1 to 2 of the present invention;
FIG. 4 is a left side view of the structure of embodiment 3 of the present invention;
wherein, 1, a left end polar plate; 2. an electrolytic liquid inlet; 3. a pole plate; 4. a diaphragm; 5. a secondary catalytic plate; 6. an anode plate; 7. a cathode plate; 8. a positive electrode total conductive bar; 9. soft connection of male copper; 10. a male terminal; 11. a female terminal; 12. carrying out female copper soft connection; 13. a negative total conductive bar; 14. a disc spring; 15. fastening a nut; 16. a pull rod; 17. an electrolytic gas-liquid outlet; 18. a binding post; 19. a right end polar plate; 20. an anode gas-liquid outlet; 21. a cathode gas-liquid outlet; 22. an insulating gasket.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An electrochemical fluorination unipolar parallel filter-pressing type electrolytic cell is shown in figure 1, and comprises a cell body, wherein a left end polar plate 1 and a right end polar plate 19 which are relatively parallel are arranged in the cell body, an electrolysis region between the left end polar plate 1 and the right end polar plate 19 is provided with a plurality of pull rods 16 which are relatively parallel, and two ends of each pull rod 16 are locked and fixed on the left end polar plate 1 and the right end polar plate 19 through belleville springs 14 and fastening nuts 15; a plurality of anode plates 6 and a plurality of cathode plates 7 are arranged between the left end polar plate 1 and the right end polar plate 19, the anode plates 6 and the cathode plates 7 are alternately arranged, and the left end polar plate 1, the anode plates 6, the cathode plates 7 and the right end polar plate 19 are distributed side by side and are fixed in a filter-press type serial connection mode through pull rods 16 and fastening nuts 15; the left end pole plate 1 and the right end pole plate 19 are both welded with binding posts 18, the anode binding post 10 is arranged on the anode plate 6, and the cathode binding post 11 is arranged on the cathode plate 7; the binding post 18 of the left end polar plate 1 and the right end polar plate 19 and the negative binding post 11 on each negative plate 7 are connected to a negative total conductive bar 13 through a negative copper soft joint 12, and the positive binding post 10 on each positive plate 6 is connected to a positive total conductive bar 8 through a positive copper soft joint 9; an electrolytic liquid inlet 2 is arranged at the middle position of the lower side of the left end polar plate 1, and an electrolytic gas-liquid outlet 17 is arranged at the upper side of the right end polar plate and close to the middle position.
Further, the electrolysis gas-liquid outlet is divided into an anode gas-liquid outlet 20 and a cathode gas-liquid outlet 21, the electrolysis liquid inlet 2 is communicated with the lower liquid inlet of each small electrolysis chamber, and the anode gas-liquid outlet 20 and the cathode gas-liquid outlet 21 are respectively communicated with the upper gas-liquid outlet of each small electrolysis chamber.
All be provided with insulating sealed 22 between left end polar plate 1, a plurality of anode plate 6, a plurality of cathode plate 7, the right-hand member polar plate 19 and in order to prevent the weeping, insulating sealed 22 is the annular, and the material is compound or the polytetrafluoroethylene material of carbon fiber polytetrafluoroethylene.
And a diaphragm used for isolating the cathode and the anode is arranged between the left end polar plate, the anode plate, the cathode plate and the right end polar plate, and the diaphragm is made of polytetrafluoroethylene, allows ions in the electrolyte to permeate but not allow the cathode gas phase and the anode gas phase to permeate so as to prevent the cathode gas phase and the anode gas phase from reacting.
The anode plate 6 and the cathode plate 7 are both single polar plates, the surfaces of the left side and the right side are both provided with concave-convex structures, the concave-convex structures on the two sides are respectively provided with the auxiliary catalytic plate 5, and a plurality of electrolyte channels are formed between the anode plate 6 and the auxiliary catalytic plate 5 and between the cathode plate 7 and the auxiliary catalytic plate 5; the anode plate 6, the auxiliary catalytic plate 5, the diaphragm 4, the auxiliary catalytic plate 5 and the cathode plate 7 are in close contact with each other to form an electrolysis small chamber. The electrode space of the electrolysis chamber is 1-10 mm, and the current density is 20-1000 mA/cm 2 。
The auxiliary pole catalytic plate 5 is a nickel wire mesh or a nickel stretching mesh, can increase the electrode area and reduce the electrolytic potential, and is a part where the main reactions of the cathode and the anode occur.
In this embodiment, the left end plate 1, the anode plate 6, the cathode plate 7 and the right end plate 19 are all circular as shown in fig. 3.
The number of the pull rods 16 is 4-20, and the pull rods are uniformly distributed and fixed along the periphery of the left end pole plate 1 and the right end pole plate 19.
Example 2
The structure of the present embodiment is substantially the same as that of embodiment 1, and the difference is that: when substances generated by the cathode and the anode are relatively inert, the cathode plate 7, the auxiliary pole catalytic plate 5 and the anode plate 6 are mutually pressed and short circuit is prevented by using a polytetrafluoroethylene mesh plate instead of the diaphragm 4. After the diaphragm 4 is removed, the electrolytic tank has no diaphragm resistance, thereby saving more electricity and energy, and simultaneously, the tank body has simpler and more compact structure and is convenient to maintain.
Example 3
The structure of the present embodiment is substantially the same as that of embodiment 1, and the difference is that: the left end polar plate 1, the anode plate 6, the cathode plate 7 and the right end polar plate 19 are all square as shown in figure 4. Because the nickel board that the supplier provided is mostly square, if process into circular can waste a large amount of expensive nickel boards, consequently, directly set up the electrolysis trough into squarely to reduce the waste to the nickel board.
The number of the pull rods 16 is 4-20, and the pull rods are uniformly distributed and fixed along the peripheries of the left end polar plate 1 and the right end polar plate 19.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. An electrochemical fluorination unipolar parallel filter-pressing type electrolytic cell comprises a cell body, wherein a left end polar plate (1) and a right end polar plate (19) which are relatively parallel are arranged in the cell body, an electrolysis region between the left end polar plate (1) and the right end polar plate (19) is provided with a plurality of relatively parallel pull rods (16), and two ends of each pull rod (16) are locked and fixed on the left end polar plate (1) and the right end polar plate (19) through disc springs (14) and fastening nuts (15); the method is characterized in that: a plurality of anode plates (6) and a plurality of cathode plates (7) are arranged between the left end polar plate (1) and the right end polar plate (19), the anode plates (6) and the cathode plates (7) are alternately arranged, and the left end polar plate (1), the plurality of anode plates (6), the plurality of cathode plates (7) and the right end polar plate (19) are distributed side by side and are connected in series in a filter-pressing manner through pull rods (16) and fastening nuts (15); the left end polar plate (1) and the right end polar plate (19) are both welded with binding posts (18), the anode plate (6) is provided with a male binding post (10), and the cathode plate (7) is provided with a female binding post (11); the binding post (18) of the left end polar plate (1) and the right end polar plate (19) and the negative binding post (11) on the negative plate (7) are connected to the negative total conducting bar (13) through the negative copper soft connection (12), and the positive binding post (10) on the positive plate (6) is connected to the positive total conducting bar (8) through the positive copper soft connection (9); an electrolytic liquid inlet (2) is formed in the middle of the lower side of the left end polar plate (1), and an electrolytic gas-liquid outlet (17) is formed in the position, close to the middle, of the upper side of the right end polar plate; an electrolysis region among the left end polar plate (1), the anode plate (6), the cathode plate (7) and the right end polar plate (19) is provided with a diaphragm (4) made of polytetrafluoroethylene and used for separating a cathode from an anode, and the diaphragm allows ions in electrolyte to permeate and prevents cathode gas and anode gas from permeating so as to prevent the reaction between cathode gas and anode gas; all be provided with insulating sealing pad (22) between left end polar plate (1), a plurality of anode plate (6), a plurality of cathode plate (7), right-hand member polar plate (19), insulating sealing pad (22) is the annular.
2. An electrochemical fluorinated monopolar parallel filter press cell according to claim 1, wherein: the electrolysis gas-liquid outlet is divided into an anode gas-liquid outlet (20) and a cathode gas-liquid outlet (21), the electrolysis liquid inlet (2) is communicated with the lower liquid inlet of each small electrolysis chamber, and the anode gas-liquid outlet (20) and the cathode gas-liquid outlet (21) are respectively communicated with the upper gas-liquid outlet of each small electrolysis chamber.
3. An electrochemical fluorinated monopolar parallel filter press cell according to claim 2, wherein: the insulating sealing gasket (22) is made of a carbon fiber polytetrafluoroethylene composite material or a polytetrafluoroethylene material.
4. An electrochemical fluorinated monopolar parallel filter press cell according to claim 3, wherein: the anode plate (6) and the cathode plate (7) are both single-polarity polar plates, the surfaces of the left side and the right side are both provided with concave-convex structures, the concave-convex structures on the two sides are respectively provided with the auxiliary catalytic plate (5), and a plurality of electrolyte channels are formed between the anode plate (6) and the auxiliary catalytic plate (5) and between the cathode plate (7) and the auxiliary catalytic plate (5); the anode plate (6), the auxiliary pole catalysis plate (5), the diaphragm (4), the auxiliary pole catalysis plate (5) and the cathode plate (7) are in close contact with each other to form an electrolysis small chamber.
5. An electrochemical fluorinated monopolar parallel filter press cell according to claim 4, wherein: the auxiliary pole catalytic plate (5) is a nickel wire mesh or a nickel stretchA net; the polar distance of the electrolytic cell is 1 to 10mm, and the current density is 20 to 1000m A/cm 2 。
6. An electrochemical fluorinated monopolar parallel filter-press cell according to claim 1, wherein: the left end polar plate (1), the anode plate (6), the cathode plate (7) and the right end polar plate (19) are circular or square.
7. An electrochemical fluorinated monopolar parallel filter press cell according to claim 1, wherein: the number of the pull rods (16) is 4-20, and the pull rods are uniformly distributed and fixed along the periphery of the left end polar plate (1) and the right end polar plate (19).
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| CN202011068196.XA CN112323093B (en) | 2020-10-08 | 2020-10-08 | Electrochemical fluorination monopolar parallel filter-pressing type electrolytic cell |
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| CN202011068196.XA CN112323093B (en) | 2020-10-08 | 2020-10-08 | Electrochemical fluorination monopolar parallel filter-pressing type electrolytic cell |
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| CN112323093B true CN112323093B (en) | 2022-11-25 |
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| CN115267299B (en) * | 2022-08-24 | 2023-05-30 | 海卓动力(北京)能源科技有限公司 | Online monitoring and overhauling device for filter-pressing type electrolytic tank |
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| CN100577882C (en) * | 2007-08-27 | 2010-01-06 | 叶元珠 | Fluoelectrolysis reactor and reaction method |
| CN202430295U (en) * | 2011-12-16 | 2012-09-12 | 上海高企新能源科技有限公司 | Filter-pressing type bipolar electrolytic bath |
| CN104532287B (en) * | 2015-01-07 | 2017-01-25 | 黎明化工研究设计院有限责任公司 | Electrochemistry fluorination electrolytic bath |
| CN106947980A (en) * | 2017-04-28 | 2017-07-14 | 深圳骏涵实业有限公司 | A kind of electrochemical fluorination electrolytic cell and its method |
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