CN114480886A - Method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity - Google Patents
Method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity Download PDFInfo
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- CN114480886A CN114480886A CN202111586461.8A CN202111586461A CN114480886A CN 114480886 A CN114480886 A CN 114480886A CN 202111586461 A CN202111586461 A CN 202111586461A CN 114480886 A CN114480886 A CN 114480886A
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- magnesium
- manganese
- carbonate ore
- manganese carbonate
- producing electrolytic
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B47/00—Obtaining manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/10—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of chromium or manganese
Abstract
The invention discloses a method for producing electrolytic manganese metal by using manganese carbonate ore with high magnesium impurity, which comprises the following steps: s1: crushing high-magnesium impurity manganese carbonate ore, inputting the crushed high-magnesium impurity manganese carbonate ore into a chemical combination barrel, adding sulfuric acid into the chemical combination barrel, and leaching under the condition of high temperature and high acid generated by the sulfuric acid for 25-35 min; s2: after the anode solution is reduced in the step S1, replenishing the anode solution to a specified liquid level, continuing leaching for 2-3 hours, and controlling the residual acid to be 1-2 g/L; s3: adding manganese oxide ore powder into the leachate obtained in the step S2 to remove iron, adding ammonia water to adjust the pH value of the solution to 4.0-5.0, and then performing filter pressing; s4: and removing magnesium from the obtained filter pressing. The method has the advantages of high magnesium removal rate, no influence on an electrolytic manganese electrolyte system, no need of adding special equipment, normal combination and purification temperature, simple and convenient operation under the condition of normal atmospheric pressure and strong operability.
Description
Technical Field
The invention relates to the technical field of electrode material preparation, in particular to a method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity.
Background
The electrolytic manganese metal is widely applied to the fields of metallurgy, medicine, electronics, communication and the like. At present, the main method for producing electrolytic manganese metal in China is to use manganese carbonate ore or roasted manganese powder as a main raw material. Because the domestic manganese carbonate ore resources are limited and the grade is limitedThe reduction year by year, in addition, the magnesium content of manganese carbonate ore is higher in some places, and Mn is generated when the electrolyte is prepared2+And Mg2+Meanwhile, the leaching causes that Mg is accumulated in the electrolyte repeatedly and is difficult to remove, and influences are brought to the development of electrolytic manganese metal industry. Therefore, the production of electrolytic manganese metal by utilizing manganese carbonate ore with high magnesium impurity is an urgent problem to be solved.
The manganese carbonate ore is abundant in China, and is an ideal ore source for producing electrolytic manganese metal. However, manganese carbonate ore used for electrolyzing manganese metal in China, particularly manganese carbonate ore produced in Sichuan, Shaanxi and Gansu parts, has the magnesium content of 3-6 percent, and a large amount of Mg is generated while electrolyte is prepared2+Impurities associated with Mn2+Leaching together, and because of the similarity of the chemical properties of the two, there is no good way to leach Mg2+And (4) effectively removing. Mg (magnesium)2+Electrical negative ratio of Mn2+Is small, so Mg2+The electrode reaction does not generally occur to produce magnesium metal, but rather Mg in the electrolyte over time as the anolyte returns to the leaching process2+The continuous accumulation can generally reach about 35g/L, and the highest accumulation can even reach about 50 g/L. According to the study of Mg2+The leaching rate of manganese can be obviously reduced by increasing the concentration, and Mg in the leaching tank2+When the concentration is 50g/L, the leaching rate of manganese is only about 75 percent, and along with the circulation of the anode solution, Mg in the leaching solution is recycled every time2+The amount of the catalyst is increased by 2-3 g/L. The concentration of magnesium ions in the manganese electrolyte is higher, and the manganese electrolyte is mainly damaged by the following points:
(1)Mg2+is easy to react with Mn in solution2+、NH4+And SO42-The crystallization is carried out together, so that compact and hard double salt crystals are formed on the inner wall of the equipment and are attached to the inner wall of an electrolytic bath and the inner wall of a pipeline, a solution channel is easily blocked, the conveying speed of the solution is reduced, the heat conduction performance of the pipeline is reduced, and the heat transfer efficiency is obviously reduced. Affecting the normal production of manganese.
(2) The density, viscosity and conductivity of the manganese electrolyte are increased, the surface tension is reduced, the filtration is difficult and difficult to remove, and the voltage and resistance of the electrolytic cell are increased to cause the reduction of the current efficiency, thereby reducing the electrolytic efficiency.
(3)Mg2+Occupying ionic gaps in a sulfuric acid system, and indirectly reducing the leaching rate of manganese ore.
(4)Mg2+"too high concentration affects Mn2+The mass transfer process finally reduces the current efficiency, and when the current is lower, the manganese metal grows in a remarkable dendritic shape, so that the compactness of the metal is reduced, and the quality is reduced.
The enrichment of magnesium in an electrolyte system in electrolytic manganese production is a difficult problem in the electrolytic manganese industry, and many manufacturers face the problem only to different degrees. How to thoroughly solve the problem is only reported by some research properties, the existing fluoride salt precipitation method, carbonate salt precipitation method, saturation degree crystallization method and solvent extraction method respectively have some obvious disadvantages, such as high production cost, complex operation, high energy consumption, poor magnesium separation effect and the like, and the problem is not formally reported when the industrial scale is carried out.
Disclosure of Invention
The invention provides a method for producing electrolytic manganese metal by using manganese carbonate ore with high magnesium impurity, which aims to solve the technical problems that: the enrichment of magnesium in an electrolyte system in the production of electrolytic manganese.
In view of the above problems of the prior art, according to one aspect of the present disclosure, the following technical solutions are adopted in the present invention:
a method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity comprises the following steps:
s1: crushing high-magnesium impurity manganese carbonate ore, inputting the crushed high-magnesium impurity manganese carbonate ore into a combination barrel, adding sulfuric acid into the combination barrel, leaching the high-magnesium impurity manganese carbonate ore powder and the sulfuric acid according to a mineral acid weight ratio of 1: 0.8-0.88 by using a high-temperature and high-acid condition generated by the sulfuric acid, wherein the leaching time is 25-35 min;
s2: after the anode solution is reduced in the step S1, replenishing the anode solution to a specified liquid level, continuing leaching for 2-3 hours, and controlling the residual acid to be 1-2 g/L;
s3: adding manganese oxide ore powder into the leachate obtained in the step S2 to remove iron, adding ammonia water to adjust the pH value of the solution to 4.0-5.0, and then performing filter pressing;
s4: and removing magnesium from the obtained filter pressing, firstly controlling the concentration of ammonium sulfate in a manganese sulfate solution to be 70-140 g/L, the concentration of magnesium ions to be 20-50 g/L and the initial temperature to be 30-90 ℃, then adding a magnesium removing agent, standing for a period of time to obtain a magnesium precipitate, and then filtering to remove magnesium.
In order to better realize the invention, the further technical scheme is as follows:
further, in the step S4, the magnesium removing agent is added twice, the magnesium removing agent A is added firstly, and after the reaction is carried out for 30min to 120min, the magnesium removing agent B is added, and the reaction is carried out for 30min to 120 min.
Furthermore, the addition amount of the magnesium removing agent A is 20-200 g/L.
Furthermore, the addition amount of the magnesium removing agent B is 40-180 g/L.
Further, after the magnesium removing agent B is added and reacts, standing for 2-5 h.
Further, the liquid obtained after filtration in the step S4 was neutralized to PH 7.0.
Further, SDD was added to the neutralized liquid to pH7.0, followed by filtration to remove heavy metal impurities.
Further, a purifying agent is added to the liquid from which the heavy metal impurities are removed, and then filtered, and the filtered liquid is sent to an electrolysis shop for electrolysis.
Compared with the prior art, the invention has the following beneficial effects:
1) compared with the method for removing magnesium ions by a crystallization method, the method for producing electrolytic manganese metal by using manganese carbonate ore with high magnesium impurity has the advantages of short treatment period, almost no loss of ammonium and manganese in an electrolyte system, no addition of extra equipment, no blockage of pipelines and low cost of manpower and material resources;
2) compared with the method for removing magnesium ions by an extraction method, the method has the advantages of low treatment cost and no secondary pollution;
3) compared with other precipitation methods for removing magnesium ions, the method has the advantages that the influence on the electrolysis of electrolytic manganese metal is not introduced, and ammonium and manganese in an electrolyte system are hardly lost;
4) the invention has wide application range, is suitable for most of electrolytic manganese industries, and does not have the problem of use limitation;
5) the method and the parameter control have better magnesium removal effect.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
A method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity comprises the following steps:
s1: crushing high-magnesium impurity manganese carbonate ore, inputting the crushed high-magnesium impurity manganese carbonate ore into a combination barrel, adding sulfuric acid into the combination barrel, leaching the high-magnesium impurity manganese carbonate ore powder and the sulfuric acid according to a mineral acid weight ratio of 1: 0.8-0.88 by using a high-temperature and high-acid condition generated by the sulfuric acid, wherein the leaching time is 25-35 min;
s2: after the anode solution is reduced in the step S1, replenishing the anode solution to a specified liquid level, continuing leaching for 2-3 hours, and controlling the residual acid to be 1-2 g/L;
s3: adding manganese oxide ore powder into the leachate obtained in the step S2 to remove iron, adding ammonia water to adjust the pH value of the solution to 4.0-5.0, and then performing filter pressing;
s4: and removing magnesium from the obtained filter pressing, firstly controlling the concentration of ammonium sulfate in a manganese sulfate solution to be 70-140 g/L, the concentration of magnesium ions to be 20-50 g/L and the initial temperature to be 30-90 ℃, then adding a magnesium removing agent, standing for a period of time to obtain a magnesium precipitate, and then filtering to remove magnesium.
Wherein, in order to improve the magnesium removal effect, the magnesium removing agent can be added twice, the magnesium removing agent A is firstly added, the magnesium removing agent B is added after the reaction is carried out for 30min to 120min, and the reaction is carried out for 30min to 120 min.
The addition amount of the magnesium removing agent A can be 20-200g/L, and the addition amount of the magnesium removing agent B can be 40-180 g/L. After the magnesium removing agent B is added and reacts, standing for 2-5 h, and then filtering to remove precipitates.
The liquid filtered in step S4 may be neutralized to PH7.0, SDD added to the neutralized PH7.0 liquid, and then filtered to remove heavy metal impurities.
Then adding a purifying agent into the liquid to remove the heavy metal impurities, then filtering, and sending the filtered liquid into an electrolysis workshop for electrolysis.
Example 1
And (3) taking the solution obtained in the step S3, firstly measuring the concentration of ammonium sulfate in the solution to be 100g/L, the concentration of magnesium ions to be 30g/L, the concentration of manganese ions to be 36g/L, the initial temperature to be 50 ℃, adding 50g/L of a magnesium removing agent A, after reacting for 30min, adding 50g/L of a magnesium removing agent B, reacting for 30min, standing for 2h to obtain magnesium precipitate, filtering, and measuring the residual magnesium in the solution to be 21 g/L.
Example 2
Example 2 is different from example 1 in that 90g/L of magnesium removing agent A is added, 50g/L of magnesium removing agent B is added after 30min of reaction, the reaction is carried out for 30min, and the mixture is kept stand for 2h to obtain magnesium precipitate, filtered and the residual magnesium of the solution is measured to be 14 g/L.
Example 3
This example differs from example 1 in that the initial temperature was 30 ℃ and the residual magnesium of the solution was measured at 19 g/L.
Example 4
Example 4 differs from example 1 in that the ammonium sulfate concentration of the solution from which magnesium is to be removed is 70g/L, and the residual magnesium of the solution is measured as 19 g/L.
Example 5
This example differs from example 1 in that 19g/L of magnesium remained in the solution after the reaction for 60min after the addition of the magnesium removing agent A.
Example 6
This example differs from example 1 in that the reaction is carried out for 60min after addition of the magnesium-removing agent B. The residual magnesium in the solution was measured at 19 g/L.
Example 7
This example differs from example 1 in that the magnesium removing agent B was added and left to stand for 240 min. The residual magnesium in the solution was measured at 19 g/L.
Example 8
The difference between the example and the example 1 is that the concentration of magnesium ions in the solution to be removed is 45g/L, and the residual magnesium in the solution is measured to be 32 g/L.
In the case of the example 9, the following examples are given,
the difference between the example and the example 1 is that the concentration of manganese ions in the solution to be removed is 30g/L, and the residual magnesium in the solution is measured to be 20 g/L.
The following results were obtained by testing the residual magnesium content of the magnesium-removed solution obtained by the magnesium removal method described in examples 1 to 9 of the present invention:
in conclusion, the method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity has high magnesium removal rate, does not influence an electrolytic manganese electrolyte system, does not need to add special equipment, has normal combination and purification temperature and strong operability under normal atmospheric pressure, and is simple and convenient to operate.
The invention has small negative influence on the prior electrolytic manganese production process, simple equipment, easy realization of industrialization, capability of meeting the process production requirement, economy and feasibility, no pollution to an electrolytic manganese system, capability of promoting the benign development of the electrolytic manganese industry and great significance to the electrolytic manganese industry.
The embodiments are described in a progressive manner in the specification, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
Reference throughout this specification to "one embodiment," "another embodiment," "an embodiment," etc., means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment described generally in this application. The appearances of the same phrase in various places in the specification are not necessarily all referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is submitted that it is within the scope of the invention to effect such feature, structure, or characteristic in connection with other embodiments.
Although the invention has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure. More specifically, various variations and modifications are possible in the component parts and/or arrangements of the subject combination arrangement within the scope of the disclosure and claims of this application. In addition to variations and modifications in the component parts and/or arrangements, other uses will also be apparent to those skilled in the art.
Claims (8)
1. A method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity is characterized by comprising the following steps:
s1: crushing the manganese carbonate ore with high magnesium impurity, inputting the crushed manganese carbonate ore with high magnesium impurity into a combination barrel, adding sulfuric acid into the combination barrel, leaching the manganese carbonate ore powder with high magnesium impurity and the sulfuric acid according to the weight ratio of 1: 0.8-0.88 of mineral acid, and leaching for 25-35min under the condition of high temperature and high acid generated by the sulfuric acid;
s2: after the anode solution is reduced in the step S1, replenishing the anode solution to a specified liquid level, continuing leaching for 2-3 hours, and controlling the residual acid to be 1-2 g/L;
s3: adding manganese oxide ore powder into the leachate obtained in the step S2 to remove iron, adding ammonia water to adjust the pH value of the solution to 4.0-5.0, and then performing filter pressing;
s4: and removing magnesium from the obtained filter pressing, firstly controlling the concentration of ammonium sulfate in a manganese sulfate solution to be 70-140 g/L, the concentration of magnesium ions to be 20-50 g/L and the initial temperature to be 30-90 ℃, then adding a magnesium removing agent, standing for a period of time to obtain a magnesium precipitate, and then filtering to remove magnesium.
2. The method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity content according to claim 1, wherein the magnesium removing agent A is added in the step S4 twice, the magnesium removing agent A is added firstly, the reaction lasts for 30-120 min, then the magnesium removing agent B is added, and the reaction lasts for 30-120 min.
3. The method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity content according to claim 2, wherein the addition amount of the magnesium removing agent A is 20-200 g/L.
4. The method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity content according to claim 2, wherein the addition amount of the magnesium removing agent B is 40-180 g/L.
5. The method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity content according to claim 2, wherein the magnesium removing agent B is added and allowed to stand for 2-5 hours after the reaction is completed.
6. The method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity content according to any one of claims 1 to 5, wherein the liquid obtained after filtration in the S4 step is neutralized to pH 7.0.
7. The method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity content as claimed in claim 6, characterized in that SDD is added to the liquid neutralized to pH7.0, and then filtered to remove heavy metal impurities.
8. The method for producing electrolytic manganese metal from manganese carbonate ore with high magnesium impurity content as claimed in claim 7, wherein a purifying agent is added to the liquid from which heavy metal impurities are removed, and then the liquid is filtered, and the filtered liquid is sent to an electrolysis shop for electrolysis.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3900385A (en) * | 1973-09-20 | 1975-08-19 | Mitsui Mining & Smelting Co | Method for continuous production of electrolytic manganese dioxide |
| CN101508467A (en) * | 2008-11-18 | 2009-08-19 | 湖北开元化工科技股份有限公司 | Preparation of high purity manganese sulfate |
| CN102134731A (en) * | 2011-01-21 | 2011-07-27 | 重庆武陵锰业有限公司 | Method for removing magnesium via cycle of ethanol in electrolytic manganese machining process |
| CN104404568A (en) * | 2014-12-15 | 2015-03-11 | 中信大锰矿业有限责任公司大新锰矿分公司 | Method for producing electrolytic manganese metal with manganese carbonate ore |
| CN104928469A (en) * | 2015-07-08 | 2015-09-23 | 长沙矿冶研究院有限责任公司 | Method for removing magnesium in sulfuric acid leaching process of rhodochrosite |
| CN112813273A (en) * | 2021-01-05 | 2021-05-18 | 南通北新新能源科技有限公司 | Method for recycling cobalt, nickel and manganese in ternary battery positive electrode waste |
-
2021
- 2021-12-23 CN CN202111586461.8A patent/CN114480886A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3900385A (en) * | 1973-09-20 | 1975-08-19 | Mitsui Mining & Smelting Co | Method for continuous production of electrolytic manganese dioxide |
| CN101508467A (en) * | 2008-11-18 | 2009-08-19 | 湖北开元化工科技股份有限公司 | Preparation of high purity manganese sulfate |
| CN102134731A (en) * | 2011-01-21 | 2011-07-27 | 重庆武陵锰业有限公司 | Method for removing magnesium via cycle of ethanol in electrolytic manganese machining process |
| CN104404568A (en) * | 2014-12-15 | 2015-03-11 | 中信大锰矿业有限责任公司大新锰矿分公司 | Method for producing electrolytic manganese metal with manganese carbonate ore |
| CN104928469A (en) * | 2015-07-08 | 2015-09-23 | 长沙矿冶研究院有限责任公司 | Method for removing magnesium in sulfuric acid leaching process of rhodochrosite |
| CN112813273A (en) * | 2021-01-05 | 2021-05-18 | 南通北新新能源科技有限公司 | Method for recycling cobalt, nickel and manganese in ternary battery positive electrode waste |
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