Palladium chloride electrolytic preparation device and preparation process

Abstract

The invention discloses a palladium chloride electrolytic preparation device and a preparation process, and specifically relates to the field of palladium chloride preparation. The device comprises a frame, wherein a liquid inlet manifold and a liquid outlet manifold are respectively provided on both sides of the frame. A plurality of electrolysis units are provided on the frame, wherein the electrolysis units comprise a unit plate and electrode plates located on both sides of the unit plate, wherein the electrode plates cooperate with each other to form an electrode chamber, wherein the unit plate is provided with a liquid inlet joint and a liquid outlet joint communicating with the electrode chamber, and further comprises a liquid distribution component and a pressure regulation component. The device provides the electrode chamber with a plurality of vertical liquid outlets by arranging the liquid distribution component, the pressure regulation component and the electrolysis units, and maintains substantially the same initial velocity of the plurality of liquid outlets by arranging movable plates, elastic members and sealing columns, and during use, a user can adjust the liquid inlet pressure of the liquid inlet manifold according to the distribution of metal palladium on the electrode plates, so as to make the liquid distribution in the electrode chamber more uniform.

Description

Technical Field

[0001] The present invention relates to the technical field of palladium chloride preparation, and more particularly to a palladium chloride electrolytic preparation device and a preparation process. Background Art

[0002] Palladium chloride, also known as palladium dichloride, is the main raw material for the preparation of palladium-containing catalysts and other palladium compounds. It is often used as a palladium catalyst for reactions such as hydrogenation, dehydrogenation, oxidation, and reforming. It can also be used as an analytical reagent for the detection of metallic mercury and iodide.

[0003] With the improvement of environmental awareness and the increasing demand for efficient utilization of resources, the method of recovering palladium from palladium-containing materials such as waste palladium catalysts and electronic waste and converting it into palladium chloride is becoming increasingly important.

[0004] As one of the mainstream methods for purifying palladium metal, electrolysis can deposit palladium on the cathode by precisely controlling the electrolysis conditions while minimizing the co-deposition of other metals, thereby obtaining high-purity palladium.

[0005] Ion exchange membrane electrolyzer is a common electrolytic purification equipment, which consists of multiple electrolytic units with a structure similar to that of a filter press. The electrolyte is introduced into the multiple electrolytic units through the liquid inlet pipes on both sides. The electrolytic units are separated into the anode chamber and the cathode chamber by the anode plate, the cathode plate and the ion membrane. Since the anode chamber and the cathode chamber have only one liquid inlet, it is easy to cause the problem of uneven liquid distribution. The existing method is to use a distribution pipe to improve the effect of uniform distribution of the liquid in the electrode chamber, but the problem of uneven liquid distribution still exists.

[0006] In the prior art, in order to improve the uniform distribution of liquid in the electrode chamber, a distribution pipe is used; however, the length of the distribution pipe is relatively long, and affected by pressure, flow rate and resistance, there are large differences in the liquid flow rate of each liquid outlet, which makes the liquid flow rate on the side of the electrode chamber away from the liquid inlet lower, while more metal palladium will be deposited on the electrode plate with large liquid flow; the uneven distribution of liquid will not only cause uneven current density in different parts of the electrode, but also cause strong electrode reaction in areas with high current density and accelerated loss of electrode material. In areas with low electrolyte flow, the number of ions participating in the electrolysis reaction is relatively small, which slows down the precipitation rate of metal palladium.

[0007] At the same time, in order to provide support and protection for the ion membrane and the electrode plate, multiple reinforcing ribs are set in the electrode chamber. However, during the electrolytic purification of waste palladium, the impurities or suspended matter generated will adhere to the reinforcing ribs. These impurities will not only cause corrosion to the reinforcing ribs and reduce the structural strength of the reinforcing ribs, but the impurities will also precipitate and precipitate together with the palladium ions at the cathode, forming a co-deposition phenomenon, which reduces the purity of the electrolyzed metallic palladium.

[0008] Therefore, the present invention proposes a palladium chloride electrolytic preparation device and preparation process to solve the above problems. Summary of the Invention

[0009] In order to overcome the above-mentioned defects of the prior art, the embodiments of the present invention provide a palladium chloride electrolytic preparation device and preparation process, which solves the problems raised in the above-mentioned background technology by providing a liquid distribution component, a pressure regulating component and an auxiliary mechanism.

[0010] To achieve the above object, the present invention provides the following technical solution: a palladium chloride electrolytic preparation device, comprising a frame, wherein a liquid inlet pipe and a liquid outlet pipe are respectively provided on both sides of the frame, and a plurality of electrolytic units are provided on the frame, wherein the electrolytic units include a unit plate and electrode plates located on both sides of the unit plate, wherein the electrode plates cooperate with the unit plates to form an electrode chamber, wherein the unit plate is provided with a liquid inlet joint and a liquid outlet joint communicating with the electrode chamber, and further comprising:

[0011] The liquid distribution assembly is provided in multiple pieces and is located in each electrode chamber, including a liquid inlet pipe connected to the liquid inlet joint, a plurality of equally spaced connectors are provided on the circumferential side of the liquid inlet pipe, a distribution pipe is rotatably connected to the connector, and a liquid outlet is opened on the circumferential side of the distribution pipe;

[0012] The pressure regulating assembly is provided with multiple components and is respectively located in the connecting head, including a movable plate that slides up and down in the connecting head, a fixed plate is fixedly connected in the connecting head, an elastic member is provided between the movable plate and the fixed plate, the movable plate is rotatably connected to the distribution pipe, a sealing column coaxially arranged with the distribution pipe is fixedly connected to the fixed plate, and a through hole matching the sealing column is opened at the end of the distribution pipe.

[0013] Preferably, the liquid inlet joint and the liquid outlet joint in the same electrode chamber are arranged diagonally, and the liquid inlet joint and the liquid outlet joint are respectively connected to the liquid inlet main pipe and the liquid outlet main pipe through hoses.

[0014] Preferably, a plurality of the connecting heads are fixedly connected with reinforcing ribs, the two sides of the reinforcing ribs are respectively in contact with the inner wall of the pole chamber and the side wall of the pole plate, and a plurality of equally spaced notches are respectively provided on both sides of the reinforcing ribs, a connecting groove is provided in the reinforcing ribs, the distribution pipe is located in the connecting groove, and the two sides of the connecting groove are arc surfaces and in contact with the outer wall of the distribution pipe.

[0015] Preferably, the movable plate is an annular structure, and a connecting ring is fixedly connected to the side of the movable plate away from the elastic member, an annular groove matching the connecting ring is opened at the end of the distribution pipe close to the movable plate, and a plurality of guide blades are fixedly connected to the inner wall of the distribution pipe close to the connecting head.

[0016] Preferably, the liquid outlet holes are provided in plurality and are evenly distributed along the length direction of the distribution pipe, and the liquid outlet holes are in a spiral shape.

[0017] Preferably, an auxiliary mechanism is further included, which is located in the movable plate and the distribution pipe. After the electrolyte is introduced into the liquid inlet pipe, part of the electrolyte enters the annular groove through the auxiliary mechanism, reducing the friction between the annular groove and the connecting ring.

[0018] Preferably, the auxiliary mechanism includes a liquid inlet groove opened at the bottom of the movable plate, the connecting ring includes a connecting strip and a connecting plate, a movable gap is formed between the annular groove and the connecting plate, and a plurality of circumferentially evenly distributed flow channels are opened on the movable plate, the connecting strip and the connecting plate, one end of the flow channel is connected to the movable gap, and the other end is connected to the liquid inlet groove.

[0019] Preferably, a filter is provided in the liquid inlet tank, and a plurality of circumferentially evenly distributed cleaning components are fixedly connected to the bottom of the distribution pipe. The cleaning component includes a connecting rod fixedly connected to the distribution pipe, and an arc-shaped scraper is provided on the side of the connecting rod close to the filter, and a scraper is provided on one side of the scraper.

[0020] A process for preparing palladium chloride comprises the following steps:

[0021] Step 1: waste pretreatment, crushing and grinding the palladium-containing waste to reduce its particle size;

[0022] Step 2: Dissolving: According to the properties of the palladium waste, the pretreated waste is added to aqua regia solution and stirred to convert the palladium into palladium ions to obtain a palladium-containing solution;

[0023] Step 3: Remove nitric acid from the palladium solution by evaporating it to a syrupy state, adding concentrated hydrochloric acid and repeatedly evaporating it to dryness 3-4 times to remove nitric acid from the palladium solution;

[0024] Step 4: removing impurities by using precipitation or ion exchange to remove some impurity ions or insoluble impurities in the palladium-containing solution;

[0025] Step 5: Electrolytic purification: The palladium-containing solution after impurities removal is used as the basis, an appropriate amount of conductive salt is added, and the pH value of the solution is adjusted to 1-2 with acid or alkali to obtain an electrolyte. The crude palladium is used as a soluble anode, and a high-purity palladium plate or titanium plate is used as a cathode. The electrolyte is continuously injected into the anode chamber and the cathode chamber respectively, so that the electrolyte circulates in the chamber;

[0026] Step 6: Collecting the metallic palladium: removing the cathode plate from the electrolytic cell and stripping the palladium layer deposited on the cathode plate mechanically or chemically to obtain crude palladium;

[0027] Step 7: Refining the crude palladium, using chemical refining methods to remove residual impurities and obtain pure palladium powder;

[0028] Step 8: Prepare palladium chloride by placing pure palladium powder into a reactor and dissolving it in aqua regia or using a hydrochloric acid-chlorine method to obtain a palladium chloride solution;

[0029] Step 9: Crystallization and drying: concentrate the palladium chloride solution to saturation, cool it to precipitate palladium chloride crystals, filter it, and then dry it at 100-120° C. to obtain palladium chloride.

[0030] Preferably, the conductive salt in step five is sodium chloride or ammonium sulfate.

[0031] Technical effects and advantages of the present invention:

[0032] 1. The present invention provides a plurality of vertical liquid outlets in the electrode chamber through the arrangement of a liquid distribution component, a pressure regulating component and an electrolysis unit, and maintains a substantially consistent initial velocity of the plurality of liquid outlets through the arrangement of a movable plate, an elastic member and a sealing column. At the same time, during use, the user can adjust the liquid inlet pressure of the liquid inlet main pipe according to the distribution of the metal palladium on the electrode plate, so that the liquid distribution in the electrode chamber is more uniform under appropriate pressure.

[0033] 2. The present invention is provided with guide vanes, distribution pipes, reinforcing ribs and liquid outlet holes. The distribution pipe rotates under the action of the guide vanes and the electrolyte, thereby preventing impurities or suspended matter from adhering to the distribution pipe. At the same time, the liquid sprayed from the liquid outlet hole can also flush the reinforcing ribs on both sides of the distribution pipe to prevent suspended matter from adhering to the reinforcing ribs, thereby improving or even avoiding the corrosion of the distribution pipe and reinforcing ribs by impurities, and also improving the problem of impurity co-deposition caused by impurity precipitation, thereby improving the purity of metallic palladium.

[0034] 3. The present invention uses auxiliary mechanisms, cleaning mechanisms and filters to allow part of the electrolyte to enter the active gap to act as a lubricant, reducing the friction between the distribution pipe and the movable plate. A filter is provided to further filter the electrolyte to prevent fine particles carried in the electrolyte from entering the active gap. At the same time, the scraper and blade rotate with the rotation of the distribution pipe, and clean the filter during the rotation process to achieve a self-cleaning effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention.

[0036] Figure 2 It is a schematic diagram of the planar structure of the present invention.

[0037] Figure 3 Schematic diagram of the coordination between the electrolysis unit, the liquid inlet manifold and the liquid outlet manifold in the present invention.

[0038] Figure 4 Schematic diagram of the disassembly of the electrolysis unit of the present invention.

[0039] Figure 5 This is a schematic diagram of the liquid distribution component of the present invention located in the electrode chamber.

[0040] Figure 6 It is a schematic structural diagram of the liquid distribution component of the present invention.

[0041] Figure 7 For the present invention Figure 6 Enlarged view of the structure of part A in the middle.

[0042] Figure 8 For the present invention Figure 7 Enlarged view of the structure of part B.

[0043] Figure 9 It is a three-dimensional schematic diagram of the distribution pipe of the present invention.

[0044] Figure 10 This is a schematic diagram of the coordination between the distribution pipe and the reinforcement ribs of the present invention.

[0045] Figure 11 It is a structural schematic diagram of the cleaning component of the present invention.

[0046] The accompanying drawings are:

[0047] 1. Frame;

[0048] 2. Liquid inlet main pipe;

[0049] 3. Liquid outlet pipe;

[0050] 4. Electrolysis unit; 41. Unit plate; 42. Electrode plate; 43. Electrode chamber; 44. Liquid inlet connector; 45. Liquid outlet connector;

[0051] 5. Liquid distribution assembly; 51. Liquid inlet pipe; 52. Connector; 53. Distribution pipe; 531. Annular groove; 532. Guide vane; 54. Liquid outlet;

[0052] 6. Pressure regulating assembly; 61. Movable plate; 62. Fixed plate; 63. Elastic member; 64. Sealing column; 65. Connecting ring; 651. Connecting strip; 652. Connecting plate;

[0053] 7. Reinforcement rib; 71. Notch; 72. Connection groove;

[0054] 8. Auxiliary mechanism; 81. Liquid inlet tank; 811. Filter; 82. Active gap; 83. Flow channel;

[0055] 9. Cleaning assembly; 91. Connecting rod; 92. Scraper; 93. Scraper blade. DETAILED DESCRIPTION

[0056] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0057] Example 1

[0058] Since the existing distribution pipe is relatively long, affected by pressure, flow rate and resistance, there is a large difference in the liquid flow rate of each liquid outlet, which makes the liquid flow rate on the side of the electrode chamber away from the liquid inlet lower, while more metal palladium will be deposited on the electrode plate with large liquid flow rate; the uneven distribution of liquid will not only cause uneven current density in different parts of the electrode, but also cause strong electrode reaction in areas with high current density and faster loss of electrode material. In areas with low electrolyte flow rate, the number of ions participating in the electrolysis reaction is relatively small, which slows down the precipitation rate of metal palladium. This embodiment is specially invented to solve the above problems.

[0059] See also Figures 1 to 11 As shown, a palladium chloride electrolytic preparation device according to an embodiment of the present invention includes a frame 1, with a liquid inlet main pipe 2 and a liquid outlet main pipe 3 respectively provided on both sides of the frame 1, and a plurality of electrolytic units 4 are provided on the frame 1. The electrolytic units 4 include a unit plate 41 and electrode plates 42 located on both sides of the unit plate 41, and an electrode chamber 43 is formed between the electrode plate 42 and the unit plate 41. The unit plate 41 is provided with a liquid inlet joint 44 and a liquid outlet joint 45 connected to the electrode chamber 43, and further includes a liquid distribution component 5 and a pressure regulating component 6.

[0060] See also Figures 4 to 6 As shown, there are multiple liquid distribution components 5 and they are respectively located in each electrode chamber 43. The liquid distribution component 5 includes a liquid inlet pipe 51 connected to the liquid inlet joint 44. A plurality of equally distributed connectors 52 are provided on the circumferential side of the liquid inlet pipe 51. A distribution pipe 53 is rotatably connected in the connector 52, and a liquid outlet hole 54 is opened on the circumferential side of the distribution pipe 53.

[0061] See also Figures 6 to 8 As shown, there are multiple pressure regulating assemblies 6 and they are respectively located in the connecting head 52. The pressure regulating assembly 6 includes a movable plate 61 that slides up and down in the connecting head 52. A fixed plate 62 is fixedly connected in the connecting head 52. An elastic member 63 is provided between the movable plate 61 and the fixed plate 62. The movable plate 61 is rotatably connected to the distribution pipe 53. A sealing column 64 coaxially arranged with the distribution pipe 53 is fixedly connected to the fixed plate 62, and a through hole matching the sealing column 64 is opened at the end of the distribution pipe 53.

[0062] See also Figure 5As shown, the liquid inlet connector 44 and the liquid outlet connector 45 in the unified electrode chamber 43 are arranged diagonally, and the liquid inlet connector 44 and the liquid outlet connector 45 are respectively connected to the liquid inlet main pipe 2 and the liquid outlet main pipe 3 through hoses.

[0063] See also Figure 5 and Figure 10 As shown, multiple connectors 52 are fixedly connected with reinforcing ribs 7, and the two sides of the reinforcing ribs 7 are respectively in contact with the inner wall of the pole chamber 43 and the side wall of the pole plate 42, and multiple equidistant notches 71 are respectively provided on both sides of the reinforcing ribs 7. A connecting groove 72 is provided in the reinforcing rib 7, and the distribution pipe 53 is located in the connecting groove 72. The two sides of the connecting groove 72 are arc surfaces and are in contact with the outer wall of the distribution pipe 53.

[0064] During use, when the electrolysis device is in a shutdown state, the movable plate 61 and the distribution pipe 53 are in the initial position under the action of the elastic member 63, and the sealing column 64 and the distribution pipe 53 are in a sealed state. When the electrolyte enters the liquid inlet pipe 51 from the liquid inlet main pipe 2, the hose and the liquid inlet connector 44, the electrolyte gradually fills the liquid inlet pipe 51 and gradually increases the pressure until the pressure in the liquid inlet pipe 51 breaks through the elastic force of the elastic member 63. The movable plate 61 and the distribution pipe 53 move upward under the action of the liquid pressure. At this time, the sealing column 64 and the distribution pipe 53 are unsealed, and the electrolyte gradually enters the distribution pipe 53 and is sprayed out through the liquid outlet 54.

[0065] During the circulation of the electrolyte, the electrolyte in the electrode chamber 43 enters the liquid outlet main pipe 3 through the liquid outlet connector 45 and the hose at the top of the unit plate 41. During the electrolytic purification of palladium waste, the electrolyte circulates continuously.

[0066] It should be noted that, during use of the electrolysis device, the liquid inlet pressure of the liquid inlet main pipe 2 may be appropriately increased to adjust the maximum effective height of the electrolyte in the distribution pipe 53 .

[0067] In summary, through the arrangement of the liquid distribution component 5, the pressure regulating component 6 and the electrolysis unit 4, the electrode chamber 43 is provided with a plurality of vertical liquid outlets, and through the arrangement of the movable plate 61, the elastic member 63 and the sealing column 64, the initial velocities of the plurality of liquid outlets are kept basically consistent. At the same time, during use, the user can adjust the liquid inlet pressure of the liquid inlet main pipe 2 according to the distribution of the metal palladium on the electrode plate 42, so that the liquid distribution in the electrode chamber 43 is more uniform under appropriate pressure.

[0068] Example 2

[0069] In actual use, it was found that since multiple reinforcing ribs 7 were provided in the electrode chamber 43, impurities or suspended matter generated during the electrolytic purification of scrap palladium would adhere to the reinforcing ribs 7. These impurities would not only corrode the reinforcing ribs 7 and reduce the structural strength of the reinforcing ribs 7, but the impurities would also precipitate and precipitate together with palladium ions at the cathode, forming a co-deposition phenomenon, which would reduce the purity of the electrolyzed metallic palladium. Further improvements were made on the basis of the above embodiments.

[0070] See also Figure 7 and Figure 8 As shown, the movable plate 61 is an annular structure, and a connecting ring 65 is fixedly connected to the side of the movable plate 61 away from the elastic member 63. An annular groove 531 matching the connecting ring 65 is provided at the end of the distribution pipe 53 close to the movable plate 61, and a plurality of guide blades 532 are fixedly connected to the inner wall of the distribution pipe 53 close to the connecting head 52.

[0071] On the basis of the above embodiment, during use, when the liquid pressure in the liquid inlet pipe 51 breaks through the restriction of the elastic part 63, the electrolyte enters the distribution pipe 53, and during the flow of the electrolyte, the guide vanes 532 are affected by the fluid and cause the distribution pipe 53 to rotate. During the circulation of the electrolyte, the distribution pipe 53 continues to rotate, and the rotation speed is related to the flow speed of the electrolyte. The greater the flow rate, the faster the rotation speed.

[0072] To sum up, through the arrangement of the guide blades 532, the distribution pipe 53, the reinforcing ribs 7 and the liquid outlet 54, the distribution pipe 53 rotates under the action of the guide blades 532 and the electrolyte, thereby preventing impurities or suspended matter from adhering to the distribution pipe 53. At the same time, the liquid sprayed from the liquid outlet 54 can also flush the reinforcing ribs 7 on both sides of the distribution pipe 53 to prevent suspended matter from adhering to the reinforcing ribs 7, thereby improving or even avoiding the corrosion of the distribution pipe 53 and the reinforcing ribs 7 by impurities, and also improving the problem of impurity co-deposition caused by the precipitation of impurities, thereby improving the purity of metallic palladium.

[0073] Example 3

[0074] In order to reduce the friction between the distribution pipe 53 and the movable plate 61 and make the distribution pipe 53 rotate more smoothly, further improvements are made on the basis of the above embodiment.

[0075] See also Figure 8 As shown, it also includes an auxiliary mechanism 8, which is located in the movable plate 61 and the distribution pipe 53. After the electrolyte is introduced into the liquid inlet pipe 51, part of the electrolyte enters the annular groove 531 through the auxiliary mechanism 8, reducing the friction between the annular groove 531 and the connecting ring 65.

[0076] The auxiliary mechanism 8 includes a liquid inlet groove 81 opened at the bottom of the movable plate 61, the connecting ring 65 includes a connecting strip 651 and a connecting plate 652, a movable gap 82 is formed between the annular groove 531 and the connecting plate 652, and a plurality of circumferentially evenly distributed flow channels 83 are opened on the movable plate 61, the connecting strip 651 and the connecting plate 652, one end of the flow channel 83 is connected to the movable gap 82, and the other end is connected to the liquid inlet groove 81.

[0077] See also Figure 8 and Figure 11 As shown, a filter screen 811 is provided in the liquid inlet tank 81, and a plurality of circumferentially evenly distributed cleaning components 9 are fixedly connected to the bottom of the distribution pipe 53. The cleaning component 9 includes a connecting rod 91 fixedly connected to the distribution pipe 53. An arc-shaped scraper 92 is provided on the side of the connecting rod 91 close to the filter screen 811, and a scraper blade 93 is provided on one side of the scraper 92.

[0078] During use, after the electrolyte enters the liquid inlet pipe 51, part of the electrolyte enters the movable gap 82 through the liquid inlet groove 81 and the flow channel 83. When the distribution pipe 53 and the movable plate 61 move upward under the push of the liquid, the electrolyte will be used as a lubricating liquid in the movable gap 82, thereby reducing the friction that needs to be overcome when the distribution pipe 53 rotates.

[0079] Although the scrap palladium has been pre-treated during electrolysis, some granular impurities will inevitably remain in the electrolyte. In order to prevent impurities from accumulating in the active gap 82, a filter 811 is set in the liquid inlet tank 81, and the electrolyte is further filtered through the filter 811. At the same time, combined with the rotation of the distribution pipe 53, a cleaning component 9 is set at the bottom of the distribution pipe 53, so that the scraper 92 and the scraper 93 clean the filter 811 as the distribution pipe 53 rotates.

[0080] To sum up, through the settings of the auxiliary mechanism 8, the cleaning mechanism and the filter 811, part of the electrolyte enters the movable gap 82 to act as a lubricating liquid, reducing the friction between the distribution pipe 53 and the movable plate 61, and the filter 811 is provided to further filter the electrolyte to prevent fine particles carried in the electrolyte from entering the movable gap 82. At the same time, the scraper 92 and the scraper 93 rotate with the rotation of the distribution pipe 53, and clean the filter 811 during the rotation process to achieve a self-cleaning effect.

[0081] Example 4

[0082] A process for preparing palladium chloride comprises the following steps:

[0083] Step 1: Waste pretreatment: crush and grind the palladium-containing waste to reduce its particle size.

[0084] Step 2: Dissolution. According to the properties of the palladium waste, the pretreated waste is added to aqua regia solution and stirred to convert the palladium into palladium ions to obtain a palladium-containing solution.

[0085] Step 3: Remove nitric acid. Evaporate the palladium-containing solution to a syrupy state. Add concentrated hydrochloric acid and evaporate repeatedly for 3-4 times to remove nitric acid from the palladium-containing solution.

[0086] Step 4: Impurity removal: using precipitation or ion exchange to remove some impurity ions or insoluble impurities in the palladium-containing solution.

[0087] Step 5: Electrolytic purification: Use the palladium-containing solution after impurities removal as the basis, add an appropriate amount of conductive salt, and adjust the pH value of the solution to 1-2 with acid or alkali to obtain an electrolyte. Use crude palladium as a soluble anode and a high-purity palladium plate or titanium plate as a cathode. Continuously inject the electrolyte into the anode chamber and cathode chamber respectively to circulate the electrolyte in the chamber.

[0088] Step 6: Collection of metallic palladium: Remove the cathode plate from the electrolytic cell and use mechanical or chemical methods to peel off the palladium layer deposited on the cathode plate to obtain crude palladium.

[0089] Step 7: Refining the crude palladium, using chemical refining methods to remove residual impurities and obtain pure palladium powder.

[0090] Step 8: Prepare palladium chloride. Place pure palladium powder into a reactor and dissolve it in aqua regia or use the hydrochloric acid-chlorine method to obtain a palladium chloride solution.

[0091] Step 9: Crystallization and drying: concentrate the palladium chloride solution to saturation, cool it to precipitate palladium chloride crystals, filter it, and then dry it at 100-120° C. to obtain palladium chloride.

[0092] The conductive salt in step five is sodium chloride or ammonium sulfate.

[0093] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A palladium chloride electrolytic preparation device, comprising a frame, a liquid inlet manifold and a liquid outlet manifold are respectively provided on both sides of the frame, and a plurality of electrolysis units are provided on the frame, characterized in that: The electrolysis unit includes a unit plate and electrode plates located on both sides of the unit plate, wherein an electrode chamber is formed between the electrode plates and the unit plate, and the unit plate is provided with a liquid inlet joint and a liquid outlet joint communicating with the electrode chamber, and further includes: The liquid distribution assembly is provided in multiple pieces and is located in each electrode chamber, including a liquid inlet pipe connected to the liquid inlet joint, a plurality of equally spaced connectors are provided on the circumferential side of the liquid inlet pipe, a distribution pipe is rotatably connected to the connector, and a liquid outlet is opened on the circumferential side of the distribution pipe; A pressure regulating assembly is provided with multiple components and is respectively located in the connecting head, including a movable plate that slides up and down in the connecting head, a fixed plate is fixedly connected in the connecting head, an elastic member is provided between the movable plate and the fixed plate, the movable plate is rotatably connected to the distribution pipe, a sealing column coaxially arranged with the distribution pipe is fixedly connected to the fixed plate, and a through hole matching the sealing column is opened at the end of the distribution pipe; A connecting ring is fixedly connected to the side of the movable plate away from the elastic member, and an annular groove matching the connecting ring is formed at one end of the distribution pipe close to the movable plate; It also includes an auxiliary mechanism, which is located in the movable plate and the distribution pipe. After the electrolyte is introduced into the liquid inlet pipe, part of the electrolyte enters the annular groove through the auxiliary mechanism, thereby reducing the friction between the annular groove and the connecting ring. The auxiliary mechanism includes a liquid inlet groove opened at the bottom of the movable plate, the connecting ring includes a connecting strip and a connecting plate, a movable gap is formed between the annular groove and the connecting plate, and a plurality of circumferentially evenly distributed flow channels are opened on the movable plate, the connecting strip and the connecting plate, one end of the flow channel is connected to the movable gap, and the other end is connected to the liquid inlet groove.

2. palladium chloride electrolysis preparation device according to claim 1, is characterized in that, The liquid inlet joint and the liquid outlet joint in the same electrode chamber are arranged diagonally, and the liquid inlet joint and the liquid outlet joint are respectively connected to the liquid inlet main pipe and the liquid outlet main pipe through hoses.

3. palladium chloride electrolysis preparation device according to claim 2, is characterized in that, Reinforcing ribs are fixedly connected to the multiple connecting heads, and the two sides of the reinforcing ribs are respectively in contact with the inner wall of the pole chamber and the side wall of the pole plate, and a plurality of equally spaced notches are respectively provided on both sides of the reinforcing ribs. A connecting groove is provided in the reinforcing ribs, and the distribution pipe is located in the connecting groove. The two sides of the connecting groove are arc surfaces and in contact with the outer wall of the distribution pipe.

4. palladium chloride electrolysis preparation device according to claim 3, is characterized in that, The movable plate is an annular structure, and a plurality of guide vanes are fixedly connected to the inner wall of the distribution pipe on the side close to the connector.

5. palladium chloride electrolysis preparation device according to claim 4, is characterized in that, The liquid outlet holes are provided in plurality and are distributed equidistantly along the length direction of the distribution pipe, and the liquid outlet holes are in a spiral shape.

6. palladium chloride electrolysis preparation device according to claim 5, is characterized in that, A filter is provided in the liquid inlet tank, and a plurality of circumferentially evenly distributed cleaning components are fixedly connected to the bottom of the distribution pipe. The cleaning component includes a connecting rod fixedly connected to the distribution pipe, and an arc-shaped scraper is provided on the side of the connecting rod close to the filter, and a scraper is provided on one side of the scraper.

7. A palladium chloride preparation process, according to the palladium chloride electrolytic preparation device according to any one of claims 1-6, characterized in that, The following steps are involved: Step 1: waste pretreatment, crushing and grinding the palladium-containing waste to reduce its particle size; Step 2: Dissolving: According to the properties of the palladium waste, the pretreated waste is added to aqua regia solution and stirred to convert the palladium into palladium ions to obtain a palladium-containing solution; Step 3: Remove nitric acid from the palladium solution by evaporating it to a syrupy state, adding concentrated hydrochloric acid and repeatedly evaporating it to dryness 3-4 times to remove nitric acid from the palladium solution; Step 4: removing impurities by using precipitation or ion exchange to remove some impurity ions or insoluble impurities in the palladium-containing solution; Step 5: Electrolytic purification: The palladium-containing solution after impurities removal is used as the basis, an appropriate amount of conductive salt is added, and the pH value of the solution is adjusted to 1-2 with acid or alkali to obtain an electrolyte. The crude palladium is used as a soluble anode, and a high-purity palladium plate or titanium plate is used as a cathode. The electrolyte is continuously injected into the anode chamber and the cathode chamber respectively, so that the electrolyte circulates in the chamber; Step 6: Collecting the metallic palladium: removing the cathode plate from the electrolytic cell and stripping the palladium layer deposited on the cathode plate mechanically or chemically to obtain crude palladium; Step 7: Refining the crude palladium, using chemical refining methods to remove residual impurities and obtain pure palladium powder; Step 8: Prepare palladium chloride by placing pure palladium powder into a reactor and dissolving it in aqua regia or using a hydrochloric acid-chlorine method to obtain a palladium chloride solution; Step 9: Crystallization and drying: concentrate the palladium chloride solution to saturation, cool it to precipitate palladium chloride crystals, filter it, and then dry it at 100-120° C. to obtain palladium chloride.

8. palladium chloride preparation technology according to claim 7, is characterized in that, The conductive salt in step five is sodium chloride or ammonium sulfate.

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