Electrolytic preparation device for chloroauric acid

The electrolytic preparation device addresses anode passivation in chloroauric acid production by using a passivation cleaning mechanism with hydrochloric acid spraying and brush rollers, ensuring continuous electrolytic efficiency without manual intervention.

CN119220998APending Publication Date: 2024-12-31TAICANG HUSHI REAGENT
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Patent Information

Application Number
CN202411332774.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-24
Publication Date
2024-12-31

AI Technical Summary

Technical Problem

The surface passivation of the Au anode electrode in existing chloroauric acid preparation devices at a voltage of 1.30V necessitates manual washing or inhibition, affecting electrolytic preparation efficiency.

Method used

An electrolytic preparation device with a passivation cleaning mechanism that includes a U-shaped three-way pipe for hydrochloric acid spraying and brush rollers driven by a servo motor to clean the anode in situ, preventing passivation by oxidizing the trivalent crystalline oxide and supplementing the electrolyte.

Benefits of technology

The device effectively inhibits anode passivation and maintains electrolytic efficiency by in-situ cleaning, eliminating the need for manual intervention and enhancing electrolyte generation.

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Abstract

The invention discloses a device for preparing chloroauric acid through an electrolytic method, and particularly relates to the technical field of chloroauric acid preparation. The electrolytic preparation device for the chloroauric acid comprises a preparation pool, liquid discharge pipes are arranged on the two sides of the lower portion of the front end of the preparation pool, a central partition plate is arranged in the middle of the interior of the preparation pool, a flange plate frame is arranged in the central partition plate, and an anion exchange membrane is arranged in the flange plate frame; a reference electrode is arranged on one side of the anion exchange membrane, an anode plate is arranged on one side of the reference electrode, a cathode plate is arranged on the other side of the anion exchange membrane, connecting frames are arranged above the anode plate and the cathode plate, and a passivation cleaning mechanism is further arranged above the anode plate. And through the passivation cleaning mechanism, the problems that when the voltage in the groove of an existing preparation device rises to 1.30 V, the surface of an Au positive electrode is passivated, the positive electrode needs to be taken out to be washed or inhibited, and the electrolytic preparation efficiency is affected are solved.
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Description

Technical Field

[0001] The invention relates to the technical field of chloroauric acid preparation, in particular to a device for preparing chloroauric acid by electrolysis. Background Art

[0002] As a very important raw material in gold plating and nano-gold preparation processes, the demand for chloroauric acid in the fields of electronics, decoration and atomic energy is increasing year by year.

[0003] Electrolysis is a common method for preparing chloroauric acid. In this method, chlorine is prepared by ion membrane electrolysis at room temperature, and the auxiliary oxidation of H2O2 is used to increase the electrolysis rate of chloroauric acid. The electrolyte Cl– concentration, electrolyte pH, and H2O2 content are adjusted and optimized to obtain the optimal process conditions.

[0004] However, when the voltage in the cell of the existing preparation device rises to 1.30V, the surface of the Au anode electrode will be passivated. At this time, the anode electrode needs to be taken out and washed or inhibited, which affects the electrolytic preparation efficiency. For this reason, we provide an electrolytic preparation device for chloroauric acid. Summary of the invention

[0005] Technical problem: In view of the problem that when the voltage in the cell of the existing preparation device rises to 1.30V, the surface of the Au anode will be passivated. At this time, the anode needs to be taken out and washed or inhibited, which affects the efficiency of electrolytic preparation. The present invention proposes an electrolytic preparation device for chloroauric acid.

[0006] Technical solution: An electrolytic preparation device for chloroauric acid comprises a preparation pool, both sides of the lower front end of the preparation pool are provided with drainage pipes, a central partition is provided at the middle position inside the preparation pool, a flange plate frame is provided inside the central partition, an anion exchange membrane is provided inside the flange plate frame, a reference electrode is provided on one side of the anion exchange membrane, an anode plate is provided on one side of the reference electrode, a cathode plate is provided on the other side of the anion exchange membrane, a connecting frame is provided above the anode plate and the cathode plate, a support rod is installed on the upper end of the connecting frame, both ends of the support rod are connected to the preparation pool through a bracket, and a passivation cleaning mechanism is also provided above the anode plate;

[0007] Among them, the passivation cleaning mechanism includes a transmission seat at the top of the support rod above the anode plate, docking joints are arranged on both sides of the lower end of the transmission seat, a connecting head is installed at the lower end of the docking joint, a brush roller is installed at the lower end of the connecting head, an asynchronous motor is installed at the upper end of the transmission seat, a guide rail is arranged on one side of the transmission seat, the transmission seat is connected to the guide rail through an active slider, a servo motor is installed at one end of the guide rail, spray pipes are arranged on both sides of the support rod of the anode plate, a plurality of branch pipes are arranged at the lower end of the spray pipe, and the plurality of branch pipes are equidistant, and the front ends of the spray pipes on both sides are connected through a U-shaped three-way pipe.

[0008] Furthermore, a screw rod is installed inside the guide rail, and the screw rod is transmission-connected to the active slider, and the output end of the servo motor passes through and extends to the inside of the guide rail, and is transmission-connected to the screw rod.

[0009] Furthermore, a guide column is provided on the other side of the transmission seat, both ends of the guide column are fixedly connected to the preparation tank through a support, and the transmission seat is slidably connected to the guide column through a driven slider.

[0010] Furthermore, a first bearing is installed at the connection between the driven slider and the guide column.

[0011] Furthermore, a docking groove is provided inside the docking joint, limiting holes are provided on both sides of the docking joint, and the limiting holes are communicated with the docking joint, shrinkage grooves are provided inside both sides of the connecting head, a spring is installed inside the shrinkage groove, a clamping block is installed on the end of the spring, and the connecting head is clamped and connected with the limiting holes on the docking joint through the clamping block.

[0012] Furthermore, the upper end of the docking joint passes through and extends to the interior of the transmission seat, and is installed with a driven gear. The output end of the asynchronous motor passes through and extends to the interior of the transmission seat, and is installed with a driving gear. The output end of the asynchronous motor is meshed and connected with the driven gear through the driving gear, and a second bearing is installed at the connection between the docking joint and the transmission seat.

[0013] Furthermore, a plurality of nozzles are installed on the inner side of the branch pipe, and the plurality of nozzles are distributed at equal distances, and the nozzles are arranged to be tilted downward.

[0014] Furthermore, the anode plate is Au, the cathode plate is graphite, and the reference electrode is a saturated calomel electrode.

[0015] Furthermore, fasteners are installed at the connection points between the two ends of the support rod and the bracket.

[0016] Furthermore, the four corners of the flange plate frame are connected to the central partition flange by bolts.

[0017] Beneficial effects: Compared with the prior art, the present invention has the following notable features:

[0018] 1. In the electrolysis process of the present invention, when the surface of the Au anode plate is about to be passivated, a U-shaped three-way pipe can be connected to an external pumping device to pump hydrochloric acid into a spray pipe along the U-shaped three-way pipe, and a plurality of branch pipe nozzles below the spray pipe are used to spray the hydrochloric acid solution onto the Au anode plate. Since the main product of the passivation of the anode plate is a trivalent crystalline oxide, which is easily soluble in hydrochloric acid, it is oxidized and dissolved in the preparation pool under the spraying action of hydrochloric acid, generating hydrogen ions and combining with chloride ions in the electrolyte to form hydrogen chloride, which promotes the generation and supplements the electrolyte.

[0019] 2. When the Au anode plate is subjected to spray depassivation treatment, the present invention can drive the servo motor to operate, drive the screw to rotate, and transmit to the active slider to move the transmission seat along the guide rail. During the movement, the asynchronous motor above the transmission seat drives the active gear to rotate and mesh with the driven gears on both sides, so that the two groups of brush rollers rotate and move together to brush the two sides of the anode plate, thereby further inhibiting the passivation of the Au anode plate. The entire brushing process can be carried out directly in the preparation tank without disassembling and removing the Au anode plate, thereby solving the problem that when the voltage in the tank of the existing preparation device rises to 1.30V, the surface of the Au anode electrode will be passivated, and the anode electrode needs to be taken out to be brushed or inhibited, thereby affecting the electrolytic preparation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0021] Figure 2 This is a schematic diagram of the bamboo braided support structure of the present invention;

[0022] Figure 3 It is a schematic diagram of the transmission shaft and the extended outer rod structure of the present invention;

[0023] Figure 4 It is a partial structural enlarged schematic diagram of the electrolytic preparation device of chloroauric acid of the present invention;

[0024] Figure 5 It is a schematic diagram of the structure of the reset frame and the pressing plate of the present invention;

[0025] Figure 6 It is a schematic diagram of the structure of the butt joint of the present invention;

[0026] In the figure: 1. preparation tank; 2. drainage pipe; 3. center partition; 4. flange plate frame; 5. anion exchange membrane; 6. bolt; 7. reference electrode; 8. anode plate; 9. cathode plate; 10. connecting frame; 11. support rod; 12. bracket; 13. fastener; 14. transmission seat; 15. asynchronous motor; 16. guide rail; 17. servo motor; 18. guide column; 19. support; 20. driven slider; 21. first bearing; 22. spray pipe; 23. branch pipe; 24. nozzle; 25. U-shaped three-way pipe; 26. screw rod; 27. active slider; 28. brush roller; 29. ​​connector; 30. docking joint; 31. active gear; 32. driven gear; 33. second bearing; 34. block; 35. limit hole; 36. docking groove; 37. contraction groove; 38. spring. DETAILED DESCRIPTION

[0027] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0028] like Figure 1-5 As shown, the present invention provides an electrolytic preparation device of chloroauric acid, comprising a preparation pool 1, both sides of the lower front end of the preparation pool 1 are provided with drainage pipes 2, a central partition plate 3 is provided at the middle position inside the preparation pool 1, a flange plate frame 4 is provided inside the central partition plate 3, an anion exchange membrane 5 is provided inside the flange plate frame 4, a reference electrode 7 is provided on one side of the anion exchange membrane 5, an anode plate 8 is provided on one side of the reference electrode 7, a cathode plate 9 is provided on the other side of the anion exchange membrane 5, a connecting frame 10 is installed above the anode plate 8 and the cathode plate 9, a support rod 11 is installed on the upper end of the connecting frame 10, both ends of the support rod 11 are connected to the preparation pool 1 through a bracket 12, a transmission seat 14 is provided above the support rod 11 of the anode plate 8, and both sides of the lower end of the transmission seat 14 are provided. A docking joint 30 is provided, a connector 29 is installed at the lower end of the docking joint 30, a brush roller 28 is installed at the lower end of the connector 29, an asynchronous motor 15 is installed at the upper end of the transmission seat 14, a guide rail 16 is provided on one side of the transmission seat 14, the transmission seat 14 is transmission-connected to the guide rail 16 through an active slider 27, a servo motor 17 is installed at one end of the guide rail 16, spray pipes 22 are provided on both sides of the support rod 11 of the anode plate 8, a plurality of branch pipes 23 are provided at the lower end of the spray pipe 22, and the plurality of branch pipes 23 are equidistant, and the front ends of the spray pipes 22 on both sides are connected by a U-shaped three-way pipe 25; a plurality of nozzles 24 are installed on the inner side of the branch pipe 23, and the plurality of nozzles 24 are equidistantly distributed, and the nozzles 24 are arranged to be tilted downward, which can increase the coverage of the nozzles 24 and improve the cleaning efficiency.

[0029] Preferably, five branch pipes 23 are provided on both sides of the spray pipe 22, but the number is not limited to five and the number of branch pipes 23 can be adjusted according to usage requirements; six nozzles 24 are provided on the inner side of the branch pipe 23, but the number is not limited to six and the number of nozzles 24 can be adjusted according to usage requirements.

[0030] like Figure 3 As shown, a screw rod 26 is installed inside the guide rail 16, and the screw rod 26 is connected to the active slider 27. The output end of the servo motor 17 passes through and extends to the inside of the guide rail 16, and is connected to the screw rod 26. The output end of the servo motor 17 can drive the screw rod 26 to rotate, transmit the active slider 27, and drive the transmission seat 14 to move along the guide rail 16.

[0031] Preferably, a guide column 18 is provided on the other side of the transmission seat 14, and both ends of the guide column 18 are fixedly connected to the preparation pool 1 through the support 19. The transmission seat 14 is slidably connected to the guide column 18 through the driven slider 20. When the transmission seat 14 moves along the guide rail 16, the driven slider 20 on the other side can slide with the guide column 18, which plays an auxiliary guiding effect and avoids deviation during the transmission process.

[0032] A first bearing 21 is installed at the connection between the driven slider 20 and the guide column 18 . The first bearing 21 can improve the sliding accuracy between the driven slider 20 and the guide column 18 .

[0033] like Figure 4 and Figure 6 As shown, a docking groove 36 is provided inside the docking joint 30, and limiting holes 34 are provided on both sides of the docking joint 30, and the limiting holes 34 are communicated with the docking joint 30, and shrinkage grooves 37 are provided inside both sides of the connecting head 29, and a spring 38 is installed inside the shrinkage groove 37, and a clamping block 35 is installed at the end of the spring 38. The connecting head 29 is clamped and connected with the limiting hole 34 on the docking joint 30 through the clamping block 35. The docking joint 30 and the connecting head 29 adopt a spring-type clamping structure, which is convenient for disassembly and assembly. When the brush roller 28 needs to be separated, replaced or cleaned, it is only necessary to press the clamping blocks 35 on both sides to shrink them into the shrinkage grooves 37, and then pull down the connecting head 29 to separate the connecting head 29 from the docking joint 30.

[0034] like Figure 5 As shown, the upper end of the docking joint 30 passes through and extends to the interior of the transmission seat 14, and is installed with a driven gear 32. The output end of the asynchronous motor 15 passes through and extends to the interior of the transmission seat 14, and is installed with a driving gear 31. The output end of the asynchronous motor 15 is meshed and connected with the driven gear 32 through the driving gear 31, and a second bearing 33 is installed at the connection between the docking joint 30 and the transmission seat 14.

[0035] Preferably, the anode plate 8 is Au, the cathode plate 9 is graphite, and the reference electrode 7 is a saturated calomel electrode.

[0036] like Figure 1 As shown, fasteners 13 are installed at the connection between the two ends of the support rod 11 and the bracket 12, and the anode plate 8, the cathode plate 9 and the reference electrode 7 are all detachable structures for easy maintenance.

[0037] Preferably, the four corners of the flange frame 4 are flange-connected to the central partition plate 3 by bolts 6, and the anion exchange membrane 5 can be disassembled together with the flange frame 4 for easy replacement.

[0038] Working principle: the preparation pool 1 is made of organic glass, and the anion exchange membrane 5 is fixed between the cathode chamber and the anode chamber through the flange frame 4. Au is used as the anode plate 8, graphite is used as the cathode plate 9, and the saturated calomel electrode is used as the reference electrode 7. Chloroauric acid is prepared by electrolysis in a three-electrode double-chamber tank. 0.1 mol / L hydrochloric acid (80 mL) is poured into the anode chamber and the cathode chamber, and electrolysis is carried out at a constant potential of 1.25 V (vs. SCE). The pH of the electrolyte is adjusted by dripping sodium hydroxide solution, and the required mass of sodium chloride solid is calculated according to the concentration formula to adjust the Cl- concentration of the electrolyte. After the electrolysis is completed, the yellow liquid in the anode chamber is the chloroauric acid solution. The chloroauric acid solution in the anode chamber is taken out, evaporated at 100°C to a brown viscous state, and cooled and crystallized at room temperature to obtain orange-yellow needle-shaped crystals, that is, orange-yellow chloroauric acid solid is obtained. During the electrolysis process, when the surface of the Au anode plate 8 is about to be passivated, it can be removed by a U-shaped three-way The pipe 25 is externally connected to a pumping device, and hydrochloric acid is pumped into the spray pipe 22 along the U-shaped three-way pipe 25. The hydrochloric acid solution is sprayed onto the Au anode plate 8 through the nozzles 24 of the several branch pipes 23 below the spray pipe 22. Because the main product of the passivation of the anode plate 8 is a trivalent crystalline oxide, it is easily soluble in hydrochloric acid. Under the spraying action of the hydrochloric acid, it is oxidized and dissolved in the preparation pool 1, generating hydrogen ions and combining with the chloride ions in the electrolyte to form hydrogen chloride, which promotes the generation and supplements the electrolyte. During spraying, the servo motor 17 can be driven to operate, drive the screw 26 to rotate, and transmit with the active slider 27, so that the transmission seat 14 moves along the guide rail 16. During the movement, the asynchronous motor 15 above the transmission seat 14 is driven to drive the active gear 31 to rotate and mesh with the driven gears 32 on both sides, so that the two sets of brush rollers 28 rotate, and the two sides of the anode plate 8 are brushed in coordination with the movement, so as to further inhibit the passivation of the Au anode plate 8.

Claims

1. An electrolytic preparation device for chloroauric acid, comprising a preparation pool (1), wherein both sides below the front end of the preparation pool (1) are provided with drainage pipes (2), characterized in that: A central partition (3) is arranged at a middle position inside the preparation tank (1), a flange plate frame (4) is arranged inside the central partition (3), an anion exchange membrane (5) is arranged inside the flange plate frame (4), a reference electrode (7) is arranged on one side of the anion exchange membrane (5), an anode plate (8) is arranged on one side of the reference electrode (7), a cathode plate (9) is arranged on the other side of the anion exchange membrane (5), a connecting frame (10) is arranged above the anode plate (8) and the cathode plate (9), a support rod (11) is installed at the upper end of the connecting frame (10), both ends of the support rod (11) are connected to the preparation tank (1) through a bracket (12), and a passivation cleaning mechanism is also arranged above the anode plate (8); The passivation cleaning mechanism comprises a transmission seat (14) arranged at the top end of a support rod (11) above the anode plate (8), docking joints (30) are arranged on both sides of the lower end of the transmission seat (14), a connecting head (29) is installed at the lower end of the docking joint (30), a brush roller (28) is installed at the lower end of the connecting head (29), an asynchronous motor (15) is installed at the upper end of the transmission seat (14), and a guide rail (28) is arranged on one side of the transmission seat (14). 16), the transmission seat (14) is connected to the guide rail (16) through an active slider (27), a servo motor (17) is installed at one end of the guide rail (16), spray pipes (22) are arranged on both sides of the support rod (11) of the anode plate (8), a plurality of branch pipes (23) are arranged at the lower end of the spray pipe (22), and the plurality of branch pipes (23) are equidistant from each other, and the front ends of the spray pipes (22) on both sides are connected through a U-shaped three-way pipe (25).

2. The electrolytic preparation device of chloroauric acid according to claim 1, characterized in that: A screw rod (26) is installed inside the guide rail (16), and the screw rod (26) is transmission-connected to an active slider (27); an output end of the servo motor (17) passes through and extends into the inside of the guide rail (16), and is transmission-connected to the screw rod (26).

3. The electrolytic preparation device of chloroauric acid according to claim 2, characterized in that: A guide column (18) is provided on the other side of the transmission seat (14), and both ends of the guide column (18) are fixedly connected to the preparation pool (1) via a support (19), and the transmission seat (14) is slidably connected to the guide column (18) via a driven slider (20).

4. The electrolytic preparation device of chloroauric acid according to claim 3, characterized in that: A first bearing (21) is installed at the connection between the driven slider (20) and the guide column (18).

5. The electrolytic preparation device of chloroauric acid according to claim 1, characterized in that: A docking groove (36) is provided inside the docking joint (30), and limiting holes (34) are provided on both sides of the docking joint (30), and the limiting holes (34) are communicated with the docking joint (30). Contraction grooves (37) are provided inside both sides of the connecting head (29), and springs (38) are installed inside the contraction grooves (37). A clamping block (35) is installed at the end of the spring (38), and the connecting head (29) is clamped and connected with the limiting holes (34) on the docking joint (30) through the clamping block (35).

6. The electrolytic preparation device of chloroauric acid according to claim 5, characterized in that: The upper end of the butt joint (30) penetrates and extends into the interior of the transmission seat (14) and is provided with a driven gear (32); the output end of the asynchronous motor (15) penetrates and extends into the interior of the transmission seat (14) and is provided with a driving gear (31); the output end of the asynchronous motor (15) is meshed and transmission-connected with the driven gear (32) via the driving gear (31); and a second bearing (33) is provided at the connection between the butt joint (30) and the transmission seat (14).

7. The electrolytic preparation device of chloroauric acid according to claim 6, characterized in that: A plurality of nozzles (24) are installed on the inner side of the branch pipe (23), and the plurality of nozzles (24) are distributed at equal intervals, and the nozzles (24) are arranged to be tilted downward.

8. The electrolytic preparation device of chloroauric acid according to claim 7, characterized in that: The anode plate (8) is Au, the cathode plate (9) is graphite, and the reference electrode (7) is a saturated calomel electrode.

9. The electrolytic preparation device of chloroauric acid according to claim 8, characterized in that: Fasteners (13) are installed at the connection points between the two ends of the support rod (11) and the bracket (12).

10. The electrolytic preparation device of chloroauric acid according to claim 8, characterized in that: The four corners of the flange plate frame (4) are flange-connected to the central partition plate (3) via bolts (6).

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