CN109468657B - Preparation method of anode plate for electrolyzing manganese dioxide - Google Patents
Preparation method of anode plate for electrolyzing manganese dioxide Download PDFInfo
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- CN109468657B CN109468657B CN201811547313.3A CN201811547313A CN109468657B CN 109468657 B CN109468657 B CN 109468657B CN 201811547313 A CN201811547313 A CN 201811547313A CN 109468657 B CN109468657 B CN 109468657B
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Abstract
The invention belongs to the technical field of preparation of anode plates for electrolysis, and discloses a preparation method of an anode plate for electrolyzing manganese dioxide, which comprises the following steps: 1) Coating metal powder on the surface of the titanium plate; 2) After sintering, the titanium plate forms intermediate titanium and a composite anode strip with an alloy coating on the surface; 3) Shaping the composite anode strip obtained in the step 2); 4) And (3) reprocessing the plurality of composite anode strips obtained in the step 3) to obtain the anode plate. The prepared anode plate can be corrected and shaped. Therefore, external force is applied to four points of the cast aluminum cross arm, the whole electrode plate generates pretension, the anode plate is corrected and shaped, and the plane torsion degree of the whole anode plate is controlled to be +/-3 mm after shaping is completed.
Description
Technical Field
The invention belongs to the technical field of preparation of anode plates for electrolysis, and particularly relates to a preparation method of an anode plate for manganese dioxide electrolysis and a method for correcting and shaping the anode plate.
Background
With the continuous demand for new energy, the battery industry at home and abroad is developed at a high speed, and the production of high-performance mercury-free alkaline zinc-manganese batteries is the key development point of the battery industry. Manganese dioxide, as an anode material of batteries, directly affects the development of the battery industry. Processes for preparing manganese dioxide can be classified into Natural Manganese Dioxide (NMD), electrolytic Manganese Dioxide (EMD), and Chemical Manganese Dioxide (CMD). In the early days, natural manganese dioxide is often used for preparing manganese dioxide, but along with the increasing exhaustion of resources, the difficulty in the preparation process is large and the crystal form is not good, so that Electrolytic Manganese Dioxide (EMD) and Chemical Manganese Dioxide (CMD) become the mainstream for preparing manganese dioxide at present, but in the process of producing and preparing manganese dioxide by a large-scale electrolytic method, the selection of an electrolytic anode material becomes a key point.
The anode material goes through the development process of graphite, lead-silver alloy, pure titanium, titanium-manganese-chromium-iron quaternary alloy and titanium-manganese alloy coating anodes, and the graphite and the lead-silver alloy are completely eliminated at present.
Pure titanium anodes are highly susceptible to passivation when used at slightly higher current densities or at slightly lower electrolysis temperatures, resulting in increased cell voltage and increased power consumption.
The anode plate made of the titanium-manganese-chromium-iron quaternary alloy has poor welding performance and cannot meet the requirement of large-scale production at present.
The titanium manganese alloy coating anode (Chinese utility model patent 87216402) is applied to industrial production in scale from 1990, and has excellent passivation resistance and long service life. Because a plurality of composite anode strips are welded, assembled and processed by the cast aluminum cross arm to obtain the anode plate, the shape of the anode strips is distorted in the production process, although the anode strips are shaped, the anode plate is not in the same plane, and the anode plate is greatly distorted again due to uneven knocking stress of heating and discharging in the electrolytic use process, so that the electrolytic process is seriously influenced.
Disclosure of Invention
The invention provides a method for preparing, correcting and shaping an anode plate for electrolytic manganese dioxide, aiming at the defects in the production and preparation of a titanium-manganese alloy coating anode plate, which comprises the following steps:
the method comprises the steps of coating a layer of metal mixed powder on the surface of a titanium plate, carrying out high-temperature argon protection, lifting and sintering on the titanium plate coated with the metal mixed powder to form a composite anode strip with middle titanium and a metal alloy coating on the surface, shaping the anode strip, riveting, assembling, welding, assembling and processing an aluminum casting cross arm to obtain an anode plate, and finishing correction and shaping work by applying four-point external force to the aluminum casting cross arm to form the anode plate for electrolytic manganese dioxide.
The specific steps of coating the metal mixed powder on the surface of the titanium plate are as follows: the metal mixed powder comprises titanium and manganese, and the weight percentage of each component is as follows: titanium: 30-70%, manganese: 30 to 70 percent. The metal mixed powder and the polyvinyl alcohol glue are mixed to form slurry, the slurry is placed in a spray gun storage tank, is pressurized by high-pressure gas, is sprayed out from a gun nozzle, and finally is uniformly attached to the surface of the titanium strip.
The method comprises the following specific steps of high-temperature argon protection lifting sintering: the titanium plate coated with the metal mixed powder slurry on the surface is naturally dried and then placed in a normal-temperature vacuum storage tank, and the vacuum storage tank is vacuumized to 10 DEG -3 And introducing argon for protection after Pa, then carrying out lifting, heating the titanium plate coated with the metal mixed powder on the surface by a constant-temperature heating furnace directly above the vacuum storage tank, rapidly carrying out lifting to a cold well directly above the constant-temperature heating furnace after heating, rapidly downwards placing the titanium plate into the storage tank through the constant-temperature heating furnace after cooling, and thus completing vacuum sintering to form a composite anode strip with titanium in the middle and a metal alloy coating on the surface.
The specific steps of shaping the anode strip are as follows: the anode strip after sintering can produce the distortion of different degree, inserts the one end of anode strip in the fixed trough clamp of a 1cm width, and the other end makes the anode strip take place to warp again through applying the moment of torsion of variation in size, reduces the holistic distortion degree of anode strip to within 3mm through the plastic.
The riveting and assembling method comprises the following specific steps: and placing a plurality of composite anode strips on a special die platform according to the requirements of a drawing, fixing all the anode strips by using a clamping plate after all the composite anode strips are placed in place, and riveting the copper busbar and the composite anode strips together by using rivets.
The welding assembly comprises the following specific steps: the lower end of the shaped composite anode strip is vertically welded with the pure titanium rib plate, the back surface of the shaped composite anode strip is protected by argon filled with an argon protective cover during welding, the front surface of the shaped composite anode strip is welded by argon arc welding, and the front surface and the back surface of the shaped composite anode strip are welded discontinuously. In order to ensure the welding quality, the metal components in the welding area are controlled, and 5-15 mm of non-coating is reserved at one end of the composite anode strip welded with the titanium rib plate.
The method comprises the following specific steps of: an anode plate prototype formed by a plurality of composite anode strips which are assembled by riveting and welding is vertically placed in an aluminum casting cross arm mould with a conductive bus bar below, the mould is assembled in place, 600-650 ℃ 6063 aluminum alloy solution is poured, the mould is naturally cooled to 200 ℃ and is demoulded, then the mould is naturally cooled to normal temperature, redundant burrs are removed, and the aluminum casting cross arm is finished.
The anode plate correcting and shaping method comprises the following specific steps: firstly, vertically hanging an anode plate cast aluminum cross arm on a detection frame, determining the deformation of a subsequent cast aluminum cross arm according to the offset corresponding to a detection scale, then placing the anode plate on a shaping platform, applying an external force corresponding to the previous deformation to enable the cast aluminum cross arm to reach the predicted deformation, finally hanging the anode plate on the detection frame again, detecting the deformation, and finishing shaping if the deformation is within +/-3 mm; if the deformation is larger than +/-3 mm, the steps are repeated to continue the rectification and the reshaping until the deformation is within +/-3 mm.
The invention has the beneficial effects that: the method applies external force to four points of the cast aluminum cross arm during correction and shaping to generate pretension force on the whole electrode plate, thereby correcting and shaping the anode plate, generating deformation on each anode strip and finally ensuring that the plane torsion of the whole anode plate is within +/-3 mm. The electrolytic manganese dioxide anode plate prepared by the method has extremely strong corrosion resistance, the bath pressure is lower than that of a pure titanium anode by more than 0.5-1V, and the electrolytic manganese dioxide anode plate does not need to be subjected to passivation treatment after each electrolysis cycle in the process of producing manganese dioxide by electrolysis and can be repeatedly used. The anode plate which is shaped and corrected by applying an external force to four points of the cast aluminum cross arm shortens the plate manufacturing period, has high integral strength, stable geometric shape and uniform electrolytic current distribution, is convenient for loading, unloading and stripping products, improves the yield of manganese dioxide in each electrolytic period and prolongs the service life of the anode plate, and the shaping method can be used for multiple times and maintains the flatness of the anode plate for a long time. Therefore, the invention is an ideal method for preparing and shaping the anode plate for electrolyzing manganese dioxide.
Drawings
FIG. 1 is a schematic structural diagram of a titanium manganese alloy anode plate according to the invention.
FIG. 2 is a schematic view of the shaping and correction of the titanium-manganese alloy anode plate by adopting a method of applying an external force by a cast aluminum cross arm at four points.
Detailed Description
The invention is further illustrated with reference to the following figures and examples:
example 1
The metal mixed powder comprises titanium and manganese, and the weight percentage of each component is as follows: titanium: 50%, manganese: 50 percent of metal powder and polyvinyl alcohol glue are mixed to form slurry, the slurry is placed in a storage tank of a spray gun, is pressurized by high-pressure gas and is sprayed out from a gun nozzle, and finally is uniformly attached to the surface of the titanium strip.
The titanium plate coated with the metal mixed powder slurry on the surface is naturally dried and then placed in a normal-temperature vacuum storage tank, and the vacuum storage tank is vacuumized to 10 DEG -3 And (2) introducing argon gas for protection after Pa, then pulling the titanium plate coated with the metal powder to pass through a constant temperature heating furnace (furnace temperature of 1300 ℃) positioned right above the vacuum storage tank for heating at the pulling speed of 10cm/min, quickly pulling the titanium plate to a cold well right above the constant temperature heating furnace after heating, quickly downwards placing the titanium plate to the storage tank through the constant temperature heating furnace after cooling for 5min, thereby completing vacuum sintering and forming the composite anode strip with the middle part being titanium and the surface being the metal alloy coating.
The anode strip after sintering can produce the distortion of different degree, inserts the one end of anode strip in the 1cm wide fixed slot clamp, and the other end makes the anode strip take place to warp again through applying the moment of torsion of variation in size, reduces the holistic distortion degree of anode strip to within 3mm through the plastic.
And placing a plurality of composite anode strips on a special die platform according to the requirements of a drawing, fixing all the anode strips by using a clamping plate after all the composite anode strips are placed in place, and riveting the copper busbar and the composite anode strips together by using rivets.
The lower end of the composite metal strip is vertically welded with the pure titanium rib plate, the back surface of the composite metal strip is protected by argon filled with an argon protective cover during welding, the front surface of the composite metal strip is welded by argon arc welding, and the front surface and the back surface of the composite metal strip are welded discontinuously. In order to ensure the welding quality and control the metal components in the welding area, 5-15 mm of non-coating is reserved at one end of the composite anode strip welded with the titanium rib plate.
An anode plate prototype formed by a plurality of composite anode strips which are assembled by riveting, welding and assembling is arranged below a conductive busbar and is vertically placed in an aluminum casting cross arm mould, the mould is assembled in place, 600-650 ℃ 6063 aluminum alloy solution is poured, the aluminum casting cross arm mould is naturally cooled to 200 ℃ and is demoulded, then the aluminum casting cross arm mould is naturally cooled to normal temperature, redundant burrs are removed, and the aluminum casting cross arm is finished.
And vertically hanging the anode plate cast aluminum cross arm on a detection frame, and determining the deformation of the anode plate cast aluminum cross arm according to the offset corresponding to the detection scale, wherein the deformation is within +/-25 mm. The deformation of the anode plate is trimmed by bending a single anode strip, and the optimal deformation can be adjusted within +/-10 mm.
The titanium manganese alloy anode plate is used under the normal industrial electrolysis condition, and the current density is 60A/m 2 The voltage of the electrolytic manganese dioxide reaches the level of mercury-free alkaline manganese battery level and can be used by manufacturers. After 10 cycles (10 days per cycle), the deformation of the anode plate is increased to +/-35 mm, the requirement of the electrolysis process cannot be met, a single anode strip needs to be bent to trim the deformation of the anode plate, and the optimal deformation can be adjusted to be within +/-10 mm.
The reconditioned titanium-manganese alloy anode plate is used under the normal industrial electrolysis condition, and the current density is 60A/m 2 The voltage of the electrolytic manganese dioxide reaches the level of mercury-free alkaline manganese battery level and can be used by manufacturers. After 10 cycles of use (10 days per cycle), the deformation of the anode plate is increased to +/-35 mm, the requirement of the electrolytic process cannot be met, and the deformation of the anode plate needs to be trimmed again.
The reconditioned titanium-manganese alloy anode plate is used under the normal industrial electrolysis condition, and the current density is 60A/m 2 The voltage of the electrolytic manganese dioxide reaches the level of mercury-free alkaline manganese battery level and can be used by manufacturers. After 9 cycles of use (10 days per cycle), the deformation of the anode plate increases to +/-35 mm,the requirement of the electrolytic process cannot be met, and the deformation of the anode plate needs to be trimmed again.
Example 2
And other process conditions are the same as those of the embodiment 1, the anode plate cast aluminum cross arm is vertically hung on a detection frame, the deformation of the anode plate cast aluminum cross arm is determined according to the offset corresponding to the detection scale, and the deformation is within +/-25 mm.
Placing the anode plate on the shaping platform, applying external force corresponding to the previous deformation, and bearing the force according to the attached figure 2. In the figure: f1 and F2 are adjusting external forces applied to two ends of the cast aluminum cross arm; f3 and F4 are external forces applied to the cast aluminum cross arm by the shaping platform. Adopting a method of applying an external force by four points on the cast aluminum cross arm to enable the cast aluminum cross arm to reach the expected deformation, finally hanging the anode plate on the detection frame again, detecting the deformation, and finishing the correction and shaping if the deformation is within +/-3 mm; if the deformation is larger than +/-3 mm, the steps are repeated to continue the rectification and the reshaping until the deformation is within +/-3 mm.
The titanium manganese alloy anode plate is used under the normal industrial electrolysis condition, and the current density is 60A/m 2 The voltage of the electrolytic manganese dioxide reaches the level of mercury-free alkaline manganese battery level and can be used by manufacturers. After 40 cycles (10 days per cycle), the deformation of the anode plate is increased to +/-35 mm, the requirement of the electrolytic process is not met, and the deformation of the anode plate needs to be trimmed again.
The titanium-manganese alloy anode plate which is corrected and finished by adopting a method of applying external force at four points on the cast aluminum cross arm is used under the normal industrial electrolysis condition, and the current density is 60A/m 2 The voltage of the electrolytic manganese dioxide reaches the level of mercury-free alkaline manganese battery level and can be used by manufacturers. After 40 cycles (10 days per cycle), the deformation of the anode plate is increased to +/-35 mm, the requirement of the electrolytic process is not met, and the deformation of the anode plate needs to be trimmed again.
The corrected and trimmed titanium-manganese alloy anode plate is used under the normal industrial electrolysis condition by adopting a method of applying an external force by a cast aluminum cross arm at four points again, and the current density is 60A/m 2 The voltage of the electrolytic manganese dioxide reaches the level of mercury-free alkaline manganese battery level and can be used by manufacturers. After 39 cycles (10 days per cycle), the deformation of the anode plate is increased to +/-35 mm, the requirement of the electrolytic process cannot be met, and the deformation of the anode plate needs to be trimmed again.
The above embodiments describe the technical solutions of the present invention in detail. It will be clear that the invention is not limited to the described embodiments. Based on the embodiments of the present invention, those skilled in the art can make various changes, but any changes equivalent or similar to the present invention are within the protection scope of the present invention.
Claims (7)
1. The preparation method of the anode plate for electrolyzing manganese dioxide is characterized by comprising the following steps of:
1) Coating metal powder on the surface of a titanium plate;
2) After sintering, the titanium plate forms a composite anode strip with intermediate titanium and an alloy coating on the surface;
3) Shaping the composite anode strip obtained in the step 2); the shaping comprises the following steps: inserting one end of the composite anode strip into a groove-shaped fixture, and applying torque to the other end of the composite anode strip to deform the composite anode strip so as to reduce the overall distortion degree to be within +/-3 mm;
4) Reprocessing the plurality of composite anode strips obtained in the step 3) to obtain an anode plate; then also comprises
Step 5), correcting and shaping the obtained anode plate; the method comprises the following specific steps: firstly, detecting an anode plate, determining subsequent deformation according to the offset, then placing the anode plate on a shaping platform, applying external force to four points of the cast aluminum cross arm to enable the whole electrode plate to generate a pretension force, so that the anode plate is corrected and shaped, each anode strip generates deformation, and shaping is completed when the deformation is detected to be within +/-3 mm; if the deformation is greater than + -3 mm, the above operation is repeated.
2. The method according to claim 1, wherein the step of coating the surface of the titanium plate with the metal powder in step 1) is as follows: the metal powder comprises a mixture of titanium and manganese, and the weight percentages of the components are as follows: titanium: 30-70%, manganese: 30% -70%; and mixing the metal powder with polyvinyl alcohol glue to form slurry, and spraying the slurry to be attached to the surface of the titanium plate through a spray gun.
3. The method according to claim 1, wherein the sintering in step 2) comprises the steps of: and (2) pulling the titanium plate obtained in the step 1) under the protection of argon, heating the titanium plate by using a constant-temperature heating furnace, pulling the titanium plate to a cold well for cooling after heating, and then sintering the titanium plate by using the constant-temperature heating furnace to form a composite anode strip with titanium in the middle and an alloy metal coating on the surface.
4. The method of claim 1, wherein the reprocessing in step 4) comprises: riveting, assembling, welding, assembling and casting an aluminum cross arm; the riveting and assembling method comprises the following specific steps: and fixing and riveting a plurality of composite anode strips on the template platform, and riveting the copper busbar and each composite anode strip together.
5. The method according to claim 4, wherein the welding assembly comprises the following specific steps: and (3) vertically welding the lower end of the composite anode strip with the pure titanium rib plate, wherein the back surface is protected by argon gas during welding, the front surface is welded by argon arc welding, and the front surface and the back surface are intermittently welded.
6. The method according to claim 5, wherein a 5-15 mm uncoated coating is reserved at one end of the composite anode strip welded with the titanium rib plate.
7. The method of claim 4, wherein the steps of casting the aluminum cross arm are as follows: placing an anode plate prototype formed by a plurality of composite anode strips which are riveted, assembled and welded in an aluminum casting cross arm mould, pouring 600-650 ℃ 6063 aluminum alloy solution, cooling to 200 ℃ for demoulding, and cooling to normal temperature after demoulding to obtain the aluminum casting cross arm.
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| CN103173784A (en) * | 2011-12-20 | 2013-06-26 | 北京有色金属研究总院 | Large full-immersion Ti-Mn alloy coat anode plate for manganese dioxide electrolysis, and its making method |
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