CN114807978A - Method for producing electrolytic manganese dioxide by wet method - Google Patents
Method for producing electrolytic manganese dioxide by wet method Download PDFInfo
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- CN114807978A CN114807978A CN202210449112.XA CN202210449112A CN114807978A CN 114807978 A CN114807978 A CN 114807978A CN 202210449112 A CN202210449112 A CN 202210449112A CN 114807978 A CN114807978 A CN 114807978A
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/21—Manganese oxides
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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Abstract
The invention belongs to the technical field of electrolytic manganese dioxide production, and discloses a method for producing electrolytic manganese dioxide by a wet method. The time prompting module, the temperature control module and the grinding module can be jointly used with other modules, so that the time control and temperature control functions of the time prompting module, the temperature control module and the grinding module on the other modules are realized. The preparation method of the electrolytic manganese dioxide is simple, the modularization of the workflow method is realized, the coupling among modules is low, and the manganese dioxide product is obtained through a series of modularized operations.
Description
Technical Field
The invention belongs to the technical field of electrolytic manganese dioxide production, and particularly relates to a method for producing electrolytic manganese dioxide by a wet method.
Background
At present, two technological methods are generally adopted domestically and internationally for carrying out deep processing treatment on manganese: firstly, the manganese alloy product can be directly produced by adopting a pyrometallurgy process for rich ores with low harmful impurities (such as phosphorus and sulfur); secondly, for most of manganese carbonate and part of manganese oxide ore, a series of salt products of manganese are generally produced by adopting a hydrometallurgy technology, and then electrolytic manganese dioxide is produced by electrolyzing the salt products. In the prior art, the process method mainly adopted in the process of producing electrolytic manganese dioxide is used for reducing and roasting manganese oxide ore and then leaching the manganese oxide ore to prepare solution, and has the defects of long process flow, high production cost, easy pollution to the surrounding environment of a plant area and the like. In another method, manganese dioxide ore and a reducing agent pyrite are used for leaching to prepare a solution, and a deep purification process is rarely adopted for deeply removing impurities from the prepared manganese sulfate solution, so that the purity of the electrolyte is low, the impurity content in the electrolyte is high, the quality of an electrolytic manganese dioxide product is influenced, and more importantly, the quality of the electrolytic manganese dioxide product is influenced.
The method for producing electrolytic manganese dioxide by a wet method with application number 201310730548.7 in Chinese patent comprises the steps of leaching, pretreatment, purification, standing, filtering, heating, electrolysis and post-treatment, and adopts heat conducting oil to preheat a manganese sulfate solution before electrolysis, so that the heating temperature of the solution can be controlled, the solution can be electrolyzed better, and the electrolysis efficiency is improved. Meanwhile, the invention adopts the diaphragm electrolytic cell of which the plurality of cathode areas correspond to one anode area to carry out electrolysis, thereby not only saving the cost and avoiding the precipitated manganese dioxide from being polluted, but also controlling the flow of the electrolyte by the constant current pump, replenishing the electrolyte in time and realizing the output rate of one-time electrolysis to the maximum extent. The technology solves the technical problems mentioned above to a certain extent, but the technology has inaccurate problems in the aspects of time and heating temperature in a hearth in the specific implementation, the sulfuric acid is used for stirring and processing the solution at the beginning, the subsequent standing heating causes the loss of the sulfuric acid, the cost is too high, the technical flow limit in the technology is not clear, and the time and the temperature defined in each operation step are easy to be confused.
Through the above analysis, the problems and defects of the prior art are as follows:
(1) in the specific embodiment, the current technology has the problem of inaccuracy in the control of time and heating temperature in the hearth;
(2) in the prior art, sulfuric acid is used for stirring and treating the solution in the initial step, and the subsequent standing and heating also causes the loss of the sulfuric acid, so the cost is too high;
(3) the boundary of the operation flow in the current technology is not clear, and the time and the temperature defined in each operation step are easy to be confused.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for producing electrolytic manganese dioxide by a wet method.
The invention is realized in this way, the method for producing electrolytic manganese dioxide by wet method, the method includes time prompt module, temperature control module, grinding module, manganese sulfate solution preparation module, manganese sulfate solution processing module, manganese sulfate solution heating electrolysis module and manganese dioxide processing module;
the time prompting module presets time required to operate when each unit is operated, and when the corresponding unit is selected, the time prompting unit can also give a plurality of possible used time, and then the corresponding time is selected or newly set;
the temperature control module is used for controlling the combustion temperature of the combustion furnace;
the grinding module comprises a powder mesh tester, and is used for grinding the high-phosphorus high-iron manganese ore and the pyrite into powder by a grinder respectively, and the powder mesh tester detects that the ground powder mesh reaches about 200 meshes;
the manganese sulfate solution preparation module comprises a primary manganese sulfate solution unit, a secondary manganese sulfate solution unit and a tertiary manganese sulfate solution unit;
the primary manganese sulfate solution unit is used for mixing high-phosphorus high-iron manganese ore powder and pyrite powder in proportion, wherein the mass of the high-phosphorus high-iron manganese ore powder is five times that of the pyrite powder, and the high-phosphorus high-iron manganese ore powder is put into a beaker; determining firing time and firing temperature, placing a beaker on a combustion furnace for firing, pouring water into the beaker after firing, mixing the water with the fired mixture, fully stirring and standing the mixture, and sucking the upper layer part of the standing mixed solution serving as a primary manganese sulfate solution into an operation bottle;
the secondary manganese sulfate solution unit is used for adding a small amount of electrolytic waste liquid into the remaining mixture solution, fully stirring, standing, and sucking the upper solution into an operation bottle;
in the third manganese sulfate solution unit, a small amount of sulfuric acid is added into the remaining mixture solution, the mixture solution is stirred and placed still, and then all the mixture solution is introduced into an operation bottle;
the manganese sulfate solution treatment module is used for sequentially adding calcium carbonate to remove iron ions, barium sulfide to remove heavy metal ions, sodium ferulate and hydrogen peroxide into an operation bottle containing a manganese sulfate solution, stirring and standing, then adding a potassium permanganate solution, stirring and standing, and finally adding activated carbon to realize high-purity purification; the manganese sulfate solution treatment module also comprises a solution pH value detector unit, selenium dioxide and ammonium sulfate solution are used for neutralizing and titrating the manganese sulfate solution, the pH value of the solution is controlled within a preset range, then the solution is kept stand, and finally the solution is subjected to superfine filtration to be placed in a heating container;
the manganese sulfate solution heating and electrolysis module is combined with a temperature control unit to set the temperature, the heating solution filled with the pure manganese sulfate solution is placed on a combustion furnace to be heated, then the pure manganese sulfate solution maintained at the temperature is conveyed into a cathode area of an electrolytic cell through a guide pipe, a sulfuric acid-manganese sulfate electrolysis system is used, manganese dioxide is obtained from an anode area, and finally, electrolysis waste liquid after electrolysis is output and recovered through a corresponding guide pipe;
the manganese dioxide processing module is used for crushing the obtained manganese dioxide by using the grinding module, washing with water, drying and distilling, adding a certain amount of an active agent for alkali washing, drying and distilling, washing with water again, and grinding after drying and distilling to obtain electrolytic manganese dioxide.
Preferably, the ignition time in the primary manganese sulfate solution unit is about 3.5 hours, the ignition temperature is about 600 ℃, the volume of water required to be added when water and the ignition mixture are mixed is 5 times of that of the mixture, and the standing time after stirring is 2 hours; the standing time in the secondary manganese sulfate solution unit is 1.5 hours; and the standing time in the third-stage manganese sulfate solution unit is 1 hour.
Preferably, the manganese sulfate solution treatment module needs to neutralize the pH value of the manganese sulfate solution within the range of 6-7, and the manganese sulfate solution treatment module needs to be kept still for 12 hours.
Preferably, the heating temperature of the manganese sulfate solution in the heating electrolysis module is 100 ℃.
In combination with the technical solutions and the technical problems to be solved, please analyze the advantages and positive effects of the technical solutions to be protected in the present invention from the following aspects:
first, aiming at the technical problems existing in the prior art and the difficulty in solving the problems, the technical problems to be solved by the technical scheme of the present invention are closely combined with the technical scheme to be protected and the results and data in the research and development process, and some creative technical effects brought after the problems are solved are analyzed in detail and deeply. The specific description is as follows:
in the process of preparing manganese dioxide, the limited time of each step and the temperature control of the heating of the combustion furnace are accurately controlled, and the quality of the finally obtained manganese dioxide is technically guaranteed. And when the initial mixed solution is prepared, water is used for dissolving the mixture, and only the vector sulfuric acid solution is added in the last link for mixing reaction, so that the use amount of sulfuric acid is greatly reduced, and the technical implementation cost is reduced. And each operation flow is modularized, and the operation steps are orderly carried out with the aid of a time prompt module, a temperature control module and a grinding module, so that the high-quality electrolytic manganese dioxide product is finally obtained.
Secondly, considering the technical scheme as a whole or from the perspective of products, the technical effect and advantages of the technical scheme to be protected by the invention are specifically described as follows:
the preparation method of the electrolytic manganese dioxide is simple, the modularization of the workflow method is realized, the coupling among modules is low, and the manganese dioxide product is obtained through a series of modularization operations.
Drawings
Fig. 1 is a flow chart of a method for producing electrolytic manganese dioxide by a wet process according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
First, an embodiment is explained. This section is an explanatory embodiment expanding on the claims so as to fully understand how the present invention is embodied by those skilled in the art.
As shown in fig. 1, the method for producing electrolytic manganese dioxide by a wet process includes a time prompt module, a temperature control module, a grinding module, a manganese sulfate solution preparation module, a manganese sulfate solution treatment module, a manganese sulfate solution heating electrolysis module and a manganese dioxide treatment module;
the time prompting module presets time required to operate when each unit is operated, and when the corresponding unit is selected, the time prompting unit can also give a plurality of possible used time, and then the corresponding time is selected or newly set;
the temperature control module is used for controlling the combustion temperature of the combustion furnace;
the grinding module comprises a powder mesh tester, and is used for grinding the high-phosphorus high-iron manganese ore and the pyrite into powder by a grinder respectively, and the powder mesh tester detects that the ground powder mesh reaches about 200 meshes;
the manganese sulfate solution preparation module comprises a primary manganese sulfate solution unit, a secondary manganese sulfate solution unit and a tertiary manganese sulfate solution unit;
the primary manganese sulfate solution unit is used for mixing high-phosphorus high-iron manganese ore powder and pyrite powder in proportion, wherein the mass of the high-phosphorus high-iron manganese ore powder is five times that of the pyrite powder, and the high-phosphorus high-iron manganese ore powder is put into a beaker; determining firing time and firing temperature, placing a beaker on a combustion furnace for firing, pouring water into the beaker after firing, mixing the water with the fired mixture, fully stirring and standing the mixture, and sucking the upper layer part of the standing mixed solution serving as a primary manganese sulfate solution into an operation bottle;
the secondary manganese sulfate solution unit is used for adding a small amount of electrolytic waste liquid into the remaining mixture solution, fully stirring, standing, and sucking the upper solution into an operation bottle;
in the third manganese sulfate solution unit, a small amount of sulfuric acid is added into the remaining mixture solution, the mixture solution is stirred and placed still, and then all the mixture solution is introduced into an operation bottle;
the manganese sulfate solution treatment module is used for sequentially adding calcium carbonate to remove iron ions, barium sulfide to remove heavy metal ions, sodium ferulate and hydrogen peroxide into an operation bottle containing a manganese sulfate solution, stirring and standing, then adding a potassium permanganate solution, stirring and standing, and finally adding activated carbon to realize high-purity purification; the manganese sulfate solution treatment module also comprises a solution pH value detector unit, selenium dioxide and ammonium sulfate solution are used for neutralizing and titrating the manganese sulfate solution, the pH value of the solution is controlled within a preset range, then the solution is kept stand, and finally the solution is subjected to superfine filtration to be placed in a heating container;
the manganese sulfate solution heating and electrolysis module is combined with a temperature control unit to set the temperature, the heating solution filled with the pure manganese sulfate solution is placed on a combustion furnace to be heated, then the pure manganese sulfate solution maintained at the temperature is conveyed into a cathode area of an electrolytic cell through a guide pipe, a sulfuric acid-manganese sulfate electrolysis system is used, manganese dioxide is obtained from an anode area, and finally, electrolysis waste liquid after electrolysis is output and recovered through a corresponding guide pipe;
the manganese dioxide processing module is used for crushing the obtained manganese dioxide by using the grinding module, washing with water, drying and distilling, adding a certain amount of an active agent for alkali washing, drying and distilling, washing with water again, and grinding after drying and distilling to obtain electrolytic manganese dioxide.
The burning time in the primary manganese sulfate solution unit is about 3.5 hours, the burning temperature is about 600 ℃, the volume of water required to be added when water and the burning mixture are mixed is 5 times of that of the mixture, and the standing time after stirring is 2 hours; the standing time in the secondary manganese sulfate solution unit is 1.5 hours; and the standing time in the third-stage manganese sulfate solution unit is 1 hour.
The manganese sulfate solution treatment module needs to neutralize the pH value of the manganese sulfate solution within the range of 6-7, and the time required for standing is 12 hours.
The heating temperature of the manganese sulfate solution in the heating electrolysis module is 100 ℃.
The working principle is as follows: according to the invention, a primary manganese sulfate solution unit, a secondary manganese sulfate solution unit and a tertiary manganese sulfate solution unit of a manganese sulfate solution preparation module are combined with a time prompt module, a temperature control module and a grinding module to prepare a manganese sulfate solution, then impurity removal, purification and filtration of the manganese sulfate solution are realized through a manganese sulfate solution treatment module combined time prompt module, then electrolysis is realized through a manganese sulfate solution heating and electrolysis module combined with the temperature control module to obtain untreated manganese dioxide, and finally a high-purity manganese dioxide product is obtained through manganese dioxide treatment module combined grinding module treatment.
And II, application embodiment. In order to prove the creativity and the technical value of the technical scheme of the invention, the part is an application example of the technical scheme of the claims to a specific product or related technology.
Grinding high-phosphorus high-iron manganese ore and pyrite into powder with the mesh number of about 200 meshes, then mixing the two kinds of powder according to a proportion, firing, preparing into an aqueous solution after firing, fully stirring and mixing, standing for a period of time, sucking the upper part of the solution into an operation bottle, adding water into the rest part of the solution, stirring to prepare a solution, sucking the upper part of the solution into the operation bottle after standing, adding sulfuric acid into the rest part of the solution, stirring and standing, and then completely pouring the solution into the operation bottle, thus preparing the manganese sulfate solution. And then removing impurities from the solution, purifying, filtering and neutralizing with acid and alkali to obtain a pure neutral solution, then heating the solution again to electrolyze to obtain manganese dioxide, and finally grinding the manganese dioxide and then performing water washing, alkali washing and water washing to obtain a high-purity manganese dioxide product.
It should be noted that the embodiments of the present invention can be realized by hardware, software, or a combination of software and hardware. The hardware portion may be implemented using dedicated logic; the software portions may be stored in a memory and executed by a suitable instruction execution system, such as a microprocessor or specially designed hardware. Those skilled in the art will appreciate that the apparatus and methods described above may be implemented using computer executable instructions and/or embodied in processor control code, such code being provided on a carrier medium such as a disk, CD-or DVD-ROM, programmable memory such as read only memory (firmware), or a data carrier such as an optical or electronic signal carrier, for example. The apparatus and its modules of the present invention may be implemented by hardware circuits such as very large scale integrated circuits or gate arrays, semiconductors such as logic chips, transistors, or programmable hardware devices such as field programmable gate arrays, programmable logic devices, etc., or by software executed by various types of processors, or by a combination of hardware circuits and software, e.g., firmware.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. The method for producing the electrolytic manganese dioxide by the wet method is characterized by comprising a time prompting module, a temperature control module, a grinding module, a manganese sulfate solution preparation module, a manganese sulfate solution treatment module, a manganese sulfate solution heating electrolysis module and a manganese dioxide treatment module;
the time prompting module presets time required to operate when each unit is operated, and when the corresponding unit is selected, the time prompting unit can also give a plurality of possible used time, and then the corresponding time is selected or newly set;
the temperature control module is used for controlling the combustion temperature of the combustion furnace;
the grinding module comprises a powder mesh tester, and is used for grinding the high-phosphorus high-iron manganese ore and the pyrite into powder by a grinder respectively, and the powder mesh tester detects that the ground powder mesh reaches about 200 meshes;
the manganese sulfate solution preparation module comprises a primary manganese sulfate solution unit, a secondary manganese sulfate solution unit and a tertiary manganese sulfate solution unit;
the primary manganese sulfate solution unit is used for mixing high-phosphorus high-iron manganese ore powder and pyrite powder in proportion, wherein the mass of the high-phosphorus high-iron manganese ore powder is five times that of the pyrite powder, and the high-phosphorus high-iron manganese ore powder is put into a beaker; determining firing time and firing temperature, placing a beaker on a combustion furnace for firing, pouring water into the beaker after firing, mixing the water with the fired mixture, fully stirring and standing the mixture, and sucking the upper part of the standing mixed solution serving as a primary manganese sulfate solution into an operation bottle;
the secondary manganese sulfate solution unit is used for adding a small amount of electrolytic waste liquid into the remaining mixture solution, fully stirring, standing, and sucking the upper solution into an operation bottle;
in the third manganese sulfate solution unit, a small amount of sulfuric acid is added into the remaining mixture solution, the mixture solution is stirred and placed still, and then all the mixture solution is introduced into an operation bottle;
the manganese sulfate solution treatment module is used for sequentially adding calcium carbonate to remove iron ions, barium sulfide to remove heavy metal ions, sodium ferulate and hydrogen peroxide into an operation bottle containing a manganese sulfate solution, stirring and standing, then adding a potassium permanganate solution, stirring and standing, and finally adding activated carbon to realize high-purity purification; the manganese sulfate solution treatment module also comprises a solution pH value detector unit, selenium dioxide and ammonium sulfate solution are used for neutralizing and titrating the manganese sulfate solution, the pH value of the solution is controlled within a preset range, then the solution is kept stand, and finally the solution is subjected to superfine filtration to be placed in a heating container;
the manganese sulfate solution heating and electrolysis module is combined with a temperature control unit to set the temperature, the heating solution filled with the pure manganese sulfate solution is placed on a combustion furnace to be heated, then the pure manganese sulfate solution maintained at the temperature is conveyed into a cathode area of an electrolytic cell through a guide pipe, a sulfuric acid-manganese sulfate electrolysis system is used, manganese dioxide is obtained from an anode area, and finally, electrolysis waste liquid after electrolysis is output and recovered through a corresponding guide pipe;
the manganese dioxide processing module is used for crushing the obtained manganese dioxide by using the grinding module, washing with water, drying and distilling, adding a certain amount of an active agent for alkali washing, drying and distilling, washing with water again, and grinding after drying and distilling to obtain electrolytic manganese dioxide.
2. The wet process for producing electrolytic manganese dioxide according to claim 1, wherein the ignition time in the primary manganese sulfate solution unit is about 3.5 hours, the ignition temperature is about 600 ℃, the volume of water to be added when mixing water and the ignition mixture is 5 times that of the mixture, and the standing time after stirring is 2 hours; the standing time in the secondary manganese sulfate solution unit is 1.5 hours; and the standing time in the third-stage manganese sulfate solution unit is 1 hour.
3. The method for wet-producing electrolytic manganese dioxide according to claim 1, wherein the manganese sulfate solution treatment module is configured to neutralize the manganese sulfate solution within a pH range of 6 to 7 for a period of 12 hours.
4. The method for wet-producing electrolytic manganese dioxide of claim 1, wherein the heating temperature of the manganese sulfate solution in the heated electrolytic module is 100 ℃.
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| CN202210449112.XA CN114807978A (en) | 2022-04-27 | 2022-04-27 | Method for producing electrolytic manganese dioxide by wet method |
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| CN202210449112.XA CN114807978A (en) | 2022-04-27 | 2022-04-27 | Method for producing electrolytic manganese dioxide by wet method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194767A (en) * | 2013-04-16 | 2013-07-10 | 中南大学 | Method for preparing manganese sulfate electrolyte by using high-iron and high-phosphor manganese ores |
| CN103695636A (en) * | 2013-12-24 | 2014-04-02 | 柳州豪祥特科技有限公司 | Preparation method of electrolytic manganese dioxide |
| CN103710540A (en) * | 2013-12-24 | 2014-04-09 | 柳州豪祥特科技有限公司 | Method for preparing manganese sulfate electrolyte |
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- 2022-04-27 CN CN202210449112.XA patent/CN114807978A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194767A (en) * | 2013-04-16 | 2013-07-10 | 中南大学 | Method for preparing manganese sulfate electrolyte by using high-iron and high-phosphor manganese ores |
| CN103695636A (en) * | 2013-12-24 | 2014-04-02 | 柳州豪祥特科技有限公司 | Preparation method of electrolytic manganese dioxide |
| CN103710540A (en) * | 2013-12-24 | 2014-04-09 | 柳州豪祥特科技有限公司 | Method for preparing manganese sulfate electrolyte |
Non-Patent Citations (1)
| Title |
|---|
| 宁孝生，尹淑贤，陈本忠: "氧化锰矿还原浸出研究" * |
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