CN111647911B - Process for removing magnesium ions in electrolytic manganese anolyte - Google Patents
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- CN111647911B CN111647911B CN202010232044.2A CN202010232044A CN111647911B CN 111647911 B CN111647911 B CN 111647911B CN 202010232044 A CN202010232044 A CN 202010232044A CN 111647911 B CN111647911 B CN 111647911B
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Abstract
The invention relates to a process for removing magnesium ions in electrolytic manganese anolyte, belonging to the field of non-ferrous metallurgy. Adding concentrated sulfuric acid into electrolytic manganese anolyte, performing heat exchange and precooling on the electrolytic manganese anolyte by adopting crystallization mother liquor, and adding the electrolytic manganese anolyte into a primary crystallization reactor; an external cooler is adopted for heat exchange and temperature reduction to 0-5 ℃, and the mixture is stirred for 15-45 min under heat preservation; then pumping into a secondary crystallization reactor, adopting an external cooler to continuously exchange heat and reduce the temperature to-10-0 ℃, and keeping the temperature and stirring for 45-120 min. After the reaction is finished, a magnesium-containing solid product is separated by filtering through a centrifugal machine, the obtained crystallization mother liquor is returned to the precooling step to be used as a precooling medium, and the obtained crystallization mother liquor is returned to the manganese ore powder leaching process after precooling heat exchange and cold recovery.
Description
Technical Field
The invention relates to a process for removing magnesium ions in electrolytic manganese anolyte, belonging to the technical field of nonferrous metallurgy.
Background
In the electrolytic manganese production process, magnesium-containing minerals in manganese ores are dissolved by sulfuric acid and enter leaching liquid in the leaching stage, and magnesium ions are difficult to remove in subsequent purification, electrolysis and other links, so that continuous cyclic enrichment of the magnesium ions is caused in the process of recycling electrolytic manganese anolyte, and finally the magnesium ions in the electrolytic manganese anolyte reach 22-35 g/L. The high-concentration magnesium ions cause the adverse effects of pipeline blockage, increased power consumption, reduction of the purity of the electrolytic manganese and the like, and bring much harm to the production of the electrolytic manganese.
The currently reported methods for removing magnesium from electrolytic manganese solution include fluoride salt precipitation, ion exchange adsorption, solvent extraction and the like. For example, patent application No. 2010503168.6 provides a method for reducing the concentration of magnesium ions in an electrolytic manganese anolyte by adding ammonium carbonate solids to the electrolytic manganese anolyte, then adding ammonium fluoride and aluminum sulfate, respectively, and separating the magnesium-containing solids by settling and filtering. Patent application No. 201110024249.2 provides a method for recycling ethanol to remove magnesium in electrolytic manganese processing technology, which comprises adding ethanol into electrolytic manganese anolyte to precipitate magnesium sulfate, filtering to remove magnesium sulfate, distilling the filtrate to recover ethanol, and returning to electrolytic manganese processing technology. The patent with the patent application number of 2015103948104 provides a method for removing magnesium from electrolytic manganese anolyte, which comprises the steps of adding the electrolytic manganese anolyte produced in the electrolytic manganese industry into a crystallization tank, adding concentrated sulfuric acid into the crystallization tank while introducing liquid ammonia, continuously adjusting the introduction amount of the liquid ammonia and controlling the pH value of a solution system in the crystallization tank to be close to neutral; after all the reaction raw materials are added, naturally cooling to separate out composite salt crystals, and after a period of crystallization, carrying out solid-liquid separation; the separated supernatant is circularly used for electrolytic manganese chemical leaching. Patent application No. 201510703592.8 provides a method for removing magnesium ions from magnesium sulfate solution by adsorption method, which comprises adsorbing with adsorbent, regenerating, and preparing by-product from magnesium-containing product. The patent with the application number of 201810313444.9 provides a method for reducing calcium and magnesium ions in electrolytic manganese qualified liquid by solvent extraction.
Although the existing magnesium removal methods are various and various methods can remove magnesium ions in the electrolytic manganese anolyte to a certain extent, the method still has some defects and cannot meet the requirement of the actual production of electrolytic manganese. In the actual production process of the electrolytic manganese enterprises at present, how to effectively remove high-concentration magnesium ions in solution is still a technical problem to be further solved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a process for removing magnesium ions in electrolytic manganese anolyte. The process of the invention separates magnesium in the form of magnesium sulfate salt by increasing the concentration of sulfuric acid in the electrolytic manganese anolyte and controlling the technical conditions of the process, thereby achieving the purpose of removing magnesium ions in the solution. The invention is realized by the following technical scheme.
The invention relates to a process for removing magnesium ions in electrolytic manganese anolyte, which comprises the steps of supplementing concentrated sulfuric acid into the electrolytic manganese anolyte, carrying out heat exchange precooling on the electrolytic manganese anolyte by adopting crystallization mother liquor, and adding the electrolytic manganese anolyte into a primary crystallization reactor; cooling to A deg.C by heat exchange with an external cooler, and stirring for at least 10 min; pumping into a secondary crystallization reactor, continuously performing heat exchange by using an external cooler to reduce the temperature to B ℃, and keeping the temperature and stirring for at least 30 min; after the reaction is finished, filtering and separating a magnesium-containing solid product by using a centrifugal machine, returning the obtained crystallization mother liquor to a precooling step to be used as a precooling medium, and returning to a manganese ore powder leaching process after precooling heat exchange and cold recovery, wherein the value of A is less than or equal to 5; the value of B is less than or equal to 0; and B is less than A.
Preferably, the process of the invention comprises the following steps:
(1) adding concentrated sulfuric acid: and adding concentrated sulfuric acid into the electrolytic manganese anolyte to adjust the sulfuric acid concentration of the solution to be 45-120 g/L, so as to obtain the acidity-adjusted solution.
(2) Pre-cooling: and (3) carrying out heat exchange and precooling on the electrolytic manganese anolyte to 10-20 ℃ by using the crystallization mother liquor produced in the previous round of magnesium removal process step (5) to obtain a precooling liquid.
(3) Primary crystallization: pumping the pre-cooled liquid produced in the step (2) into a first-stage crystallization reactor, starting stirring, continuously performing heat exchange and cooling through an external cooler by adopting a coil or a jacket heat exchange device, reducing the temperature of the solution to 0-5 ℃, and performing heat preservation reaction for 15-45 min.
(4) Secondary crystallization: pumping the primary crystallization slurry produced in the step (3) into a secondary crystallization reactor, starting stirring, continuously performing heat exchange and cooling through an external cooler by adopting a coil or a jacket heat exchange device, reducing the temperature of the solution to-10-0 ℃, and performing heat preservation reaction for 45-120 min.
(5) Separation by a centrifuge: and (4) after the reaction in the step (4) is finished, quickly separating the separated magnesium-containing solid product by using a centrifugal machine, returning the obtained crystallization mother liquor to a precooler to be used as a precooling medium, and returning to the leaching process after precooling heat exchange.
Optimally, the stirring speed in the step (3) and the step (4) is 30-150 rpm.
As a preferred scheme, the process for removing magnesium ions in the electrolytic manganese anolyte defines the concentration of free sulfuric acid in the electrolytic manganese anolyte as Cg/L; then, after adding concentrated sulfuric acid, obtaining a liquid after acidity adjustment; the concentration of free sulfuric acid in the acidity adjusted solution is Dg/L, and D/C is more than or equal to 2.
As a preferable scheme, the concentration of the concentrated sulfuric acid is more than or equal to 45 g/L.
According to the process for removing the magnesium ions in the electrolytic manganese anolyte, the loss of Mn element is less than or equal to 1.5% before and after treatment, and the loss can be less than or equal to 1% after optimization.
The electrolytic manganese production comprises main process processes of leaching, impurity removal, electrolysis and the like, manganese ore powder is leached to obtain leachate, the leachate is purified and impurity removed to obtain qualified electrolyte, the qualified electrolyte is added into an electrolytic cell, manganese ions are separated out through cathodic electrodeposition after a certain period of electrolysis to obtain metal manganese, the electrolyte passes through a diaphragm cloth to enter an anode chamber, oxygen is separated out at an anode, meanwhile, sulfuric acid-containing anolyte is produced, the anolyte is obtained through a false bottom overflow electrolytic cell, and then the anolyte returns to the manganese ore powder for leaching. The anolyte produced in the manganese electrolysis process contains 35-40 g/L of sulfuric acid, and the manganese content is 13-15g/L, which is a main leaching agent for leaching manganese ore powder, but because the manganese ore powder contains a certain amount of calcium, magnesium and other impurity elements in the production process, calcium sulfate precipitate and magnesium sulfate salt are formed in the leaching process, so that the consumption loss of sulfuric acid is caused. Thus, the lixiviant used in manganese ore fines leaching is usually supplemented with a certain amount of concentrated sulphuric acid in addition to the anolyte returned by electrolysis to maintain the acid balance of the system. The method is combined with the electrolytic manganese production process, concentrated sulfuric acid which needs to be supplemented in the leaching process is added into the anolyte before the magnesium removal in advance, and the magnesium ions are promoted to be precipitated and separated out in the form of magnesium sulfate salt by increasing the acidity of the solution and controlling the relevant process technical conditions, so that the selective removal of the magnesium ions in the solution is realized. The high-acid anolyte after the removal of magnesium ions is returned to the manganese ore powder leaching process for recycling.
The invention has the beneficial effects that:
(1) the process can effectively remove magnesium ions in the electrolytic manganese anolyte, eliminate adverse effects of pipeline blockage, power consumption increase, electrolytic manganese purity reduction and the like caused by high-concentration magnesium ions in the electrolytic manganese process, ensure that the electrolytic manganese operation is more smooth, reduce the energy consumption and improve the purity of the electrolytic manganese.
(2) The process does not need to add ammonia water, liquid ammonia and other chemical reagents in the magnesium removal process, does not need to carry out neutralization reaction in the magnesium removal process, does not introduce new impurity ions and pollution sources, and has no potential negative influence on the electrolytic manganese production process.
(3) Compared with the prior art of fluoride salt precipitation magnesium removal method, ion exchange adsorption magnesium removal method, solvent extraction magnesium removal method and the like, the process of the invention does not need to use an additional reagent, does not need to add a magnesium removal agent or use an organic reagent, has simple process and no wastewater output, and has the advantages of less reagent consumption, low operation cost, clean and environment-friendly process, less Mn loss and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
10L of anolyte taken from an electrolytic manganese factory, wherein the temperature of the anolyte is 40 ℃, and the anolyte mainly comprises the following chemical components: 25.0g/L of magnesium, 16.0g/L of manganese, 35g/L of free sulfuric acid, and the balance of ammonium sulfate, water and the like. The specific operation steps are as follows:
(1) and slowly replenishing concentrated sulfuric acid, and stopping adding acid when the concentration of free sulfuric acid in the electrolytic manganese anolyte is adjusted to 45g/L to obtain the acidity-adjusted solution.
(2) And (3) carrying out heat exchange and precooling on the electrolytic manganese anolyte to 20 ℃ by using a heat exchanger and utilizing the crystallization mother liquor with the temperature of-5 ℃ to obtain precooling liquid.
(3) Pumping the pre-cooled liquid produced in the step (2) into a first-stage crystallization reactor, starting stirring, controlling the stirring speed to be 150rpm, adopting a jacket heat exchange device to continuously exchange heat and reduce the temperature through external cooling, reducing the temperature of the solution to 0 ℃, and carrying out heat preservation reaction for 15 min.
(4) Pumping the primary crystallization slurry produced in the step (3) into a secondary crystallization reactor, starting stirring, controlling the stirring speed to be 150rpm, adopting a jacket heat exchange device to continuously exchange heat and reduce the temperature through an external cooler, reducing the temperature of the solution to-5 ℃, and carrying out heat preservation reaction for 120 min.
(5) And (4) after the reaction in the step (4) is finished, rapidly separating the separated magnesium-containing solid product by using a centrifugal machine, returning 9.6L of crystallization mother liquor obtained to a precooler to serve as a precooling medium, and returning to the manganese ore powder leaching process after precooling and heat exchange.
The main chemical components of the obtained magnesium-removed liquid are 16.5g/L magnesium, 15.8g/L manganese and 44.0g/L sulfuric acid. 1120g of magnesium-containing solid product containing 8.2% of magnesium was obtained.
Example 2
10L of anolyte taken from an electrolytic manganese factory, wherein the temperature of the anolyte is 39 ℃, and the anolyte mainly comprises the following chemical components: 30.0g/L of magnesium, 15.0g/L of manganese, 38.2g/L of free sulfuric acid, and the balance of ammonium sulfate, water and the like. The specific operation steps are as follows:
(1) and slowly replenishing concentrated sulfuric acid, adjusting the concentration of free sulfuric acid in the electrolytic manganese anolyte to 80g/L, and stopping adding acid to obtain the acidity-adjusted liquid.
(2) And (3) exchanging heat and precooling the electrolytic manganese anolyte to 15 ℃ by using the crystallization mother liquor at the temperature of-8 ℃ by using a heat exchanger to obtain precooling liquid.
(3) Pumping the pre-cooled liquid produced in the step (2) into a first-stage crystallization reactor, starting stirring, controlling the stirring speed to be 60rpm, adopting a jacket heat exchange device to continuously exchange heat and reduce the temperature through external cooling, reducing the temperature of the solution to-2 ℃, and carrying out heat preservation reaction for 30 min.
(4) Pumping the primary crystallization slurry produced in the step (3) into a secondary crystallization reactor, starting stirring, controlling the stirring speed to be 60rpm, adopting a jacket heat exchange device to continuously exchange heat and reduce the temperature through an external cooler, reducing the temperature of the solution to-8 ℃, and carrying out heat preservation reaction for 90 min.
(5) And (4) after the reaction in the step (4) is finished, rapidly separating the separated magnesium-containing solid product by using a centrifugal machine to obtain 9.3L of crystallization mother liquor, returning the crystallization mother liquor to a precooler to be used as a precooling medium, and returning the crystallization mother liquor to the manganese ore powder leaching process after precooling and heat exchange.
The main chemical components of the obtained magnesium-removed liquid are 14.2g/L magnesium, 14.9g/L manganese and 79.3g/L sulfuric acid. Thus, 2090g of a magnesium-containing solid product and 8.0% of magnesium were obtained.
Example 3
10L of anolyte taken from an electrolytic manganese factory, wherein the temperature of the anolyte is 38 ℃, and the anolyte mainly comprises the following chemical components: 35.0g/L of magnesium, 14.0g/L of manganese, 40.0g/L of free sulfuric acid, and the balance of ammonium sulfate, water and the like. The specific operation steps are as follows:
(1) and slowly replenishing concentrated sulfuric acid, adjusting the concentration of free sulfuric acid in the electrolytic manganese anolyte to 120g/L, and stopping adding acid to obtain the acidity-adjusted liquid.
(2) And (3) carrying out heat exchange on the electrolytic manganese anolyte by using a crystallization mother liquor with the temperature of-10 ℃ by using a heat exchanger, and precooling to 10 ℃ to obtain a precooling liquid.
(3) Pumping the pre-cooled liquid produced in the step (2) into a first-stage crystallization reactor, starting stirring, controlling the stirring speed to be 30rpm, adopting a jacket heat exchange device to continuously exchange heat and reduce the temperature through external cooling, reducing the temperature of the solution to-6 ℃, and carrying out heat preservation reaction for 45 min.
(4) Pumping the primary crystallization slurry produced in the step (3) into a secondary crystallization reactor, starting stirring, controlling the stirring speed to be 30rpm, continuously exchanging heat and cooling through an external cooler by adopting a jacket heat exchange device, reducing the temperature of the solution to-10 ℃, and carrying out heat preservation reaction for 60 min.
(5) And (4) after the reaction in the step (4) is finished, rapidly separating the separated magnesium-containing solid product by using a centrifugal machine to obtain 9.1L of crystallization mother liquor, returning the crystallization mother liquor to a precooler to be used as a precooling medium, and returning the crystallization mother liquor to the manganese ore powder leaching process after precooling and heat exchange.
The main chemical components of the obtained magnesium-removed liquid are 13.0g/L magnesium, 13.9g/L manganese and 119.7g/L sulfuric acid. 3160g of magnesium-containing solid product and 7.3% of magnesium are obtained.
Comparative example 1
The other conditions were the same as in example 3 except that: the sulfuric acid is not supplemented, namely the concentration of the sulfuric acid in the system is 40g/L when the first stage and the second stage are cooled; the main chemical components of the obtained magnesium-removed liquid are 22.5g/L magnesium, 13.9g/L manganese and 39.8g/L sulfuric acid.
Comparative example 2
The other conditions were the same as in example 3 except that: omitting the step (3): after the pre-cooling liquid is obtained, the pre-cooling liquid is directly cooled to-10 ℃, and the heat preservation reaction is carried out for 105 min. The main chemical components of the obtained magnesium-removed liquid are 17.8g/L magnesium, 13.5g/L manganese and 118.0g/L sulfuric acid.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (5)
1. A process for removing magnesium ions in electrolytic manganese anolyte is characterized in that: the process comprises the following steps:
(1) adding concentrated sulfuric acid: adding concentrated sulfuric acid into the electrolytic manganese anolyte to adjust the sulfuric acid concentration of the solution to be 45-120 g/L, and obtaining a liquid after acidity adjustment;
(2) pre-cooling: carrying out heat exchange and precooling on the electrolytic manganese anolyte to 10-20 ℃ by using the crystallization mother liquor produced in the previous round of magnesium removal process step (5) to obtain precooling liquid;
(3) primary crystallization: pumping the pre-cooled liquid produced in the step (2) into a primary crystallization reactor, starting stirring, continuously performing heat exchange and cooling through an external cooler by adopting a coil or a jacket heat exchange device, reducing the temperature of the solution to A ℃, wherein the value of A is 0-5 or-2 or-6, and performing heat preservation reaction for 15-45 min;
(4) secondary crystallization: pumping the primary crystallization slurry produced in the step (3) into a secondary crystallization reactor, starting stirring, continuously performing heat exchange and cooling through an external cooler by adopting a coil or a jacket heat exchange device, reducing the temperature of the solution to B ℃, and performing heat preservation reaction for 45-120 min; the value of B is-5, -8 or-10; and B is less than A;
(5) separation by a centrifuge: and (5) after the reaction in the step (4) is finished, quickly separating the separated magnesium-containing solid product by adopting a centrifugal machine, returning the obtained crystallization mother liquor to a precooler to be used as a precooling medium, and returning to the leaching process after precooling heat exchange.
2. The process for removing magnesium ions from an electrolytic manganese anolyte as defined in claim 1, wherein: and the stirring speed in the step (3) and the step (4) is 30-150 rpm.
3. The process for removing magnesium ions from an electrolytic manganese anolyte as claimed in claim 1, characterized in that: defining the concentration of free sulfuric acid in the electrolytic manganese anolyte as Cg/L; then, after adding concentrated sulfuric acid, obtaining a liquid after acidity adjustment; the concentration of free sulfuric acid in the acidity adjusted solution is Dg/L, and D/C is more than or equal to 2.
4. The process for removing magnesium ions from an electrolytic manganese anolyte as claimed in claim 3, characterized in that: the concentration of free sulfuric acid is 80-130 g/L.
5. The process for removing magnesium ions from an electrolytic manganese anolyte as defined in claim 1, wherein: the loss of Mn element before and after the treatment is less than or equal to 1.5%.
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| JP2011195878A (en) * | 2010-03-18 | 2011-10-06 | Sumitomo Metal Mining Co Ltd | Method for recovering copper from copper sulfide |
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| FI110268B (en) * | 2001-03-09 | 2002-12-31 | Outokumpu Oy | Process for removing calcium from sulfate solutions in a zinc process |
| CN104058429A (en) * | 2014-07-04 | 2014-09-24 | 中节能六合天融环保科技有限公司 | Method for magnesium sulfate continuous crystallization |
| CN105040038B (en) * | 2015-07-08 | 2017-07-07 | 长沙矿冶研究院有限责任公司 | The method for carrying out demagging to electrolytic manganese anolyte using ammonium sulfate |
| CN104947154B (en) * | 2015-07-08 | 2017-09-12 | 长沙矿冶研究院有限责任公司 | A kind of method that demagging is carried out to electrolytic manganese anolyte |
| CN105154916B (en) * | 2015-08-13 | 2017-09-12 | 长沙矿冶研究院有限责任公司 | A kind of method of impurity content of magnesium in fractional precipitation reduction electrolytic manganese system |
| CN109761800B (en) * | 2018-12-25 | 2022-04-08 | 兄弟科技股份有限公司 | Method for removing oxalic acid by continuous crystallization in glyoxylic acid production process |
| CN109628745B (en) * | 2019-01-03 | 2020-11-24 | 昆明理工大学 | Method for removing magnesium ions from waste electrolyte of zinc hydrometallurgy |
| CN109680300B (en) * | 2019-01-31 | 2021-06-15 | 贵州大学 | Method for removing magnesium in manganese sulfate solution by double salt crystallization method |
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