CN105154916A - Method for reducing impurity magnesium content in electrolytic manganese system through fractional precipitation - Google Patents
Method for reducing impurity magnesium content in electrolytic manganese system through fractional precipitation Download PDFInfo
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Abstract
The invention discloses a method for reducing the impurity magnesium content in an electrolytic manganese system through fractional precipitation. The method includes the following steps that 1, liquid ammonia is added to an electrolytic manganese anode solution or a qualified solution to adjust the pH value of the solution to be 6.5 to 9, and then magnesium precipitation additives are added for the reaction; 2, solid and liquid separation is conducted on reaction slurry obtained after the step 1, magnesium precipitation residues and a solution obtained after magnesium precipitation are obtained, and the magnesium precipitation residues are returned to an electrolytic manganese chemical combination workshop; 3, liquid ammonia is added to the solution obtained after magnesium precipitation to adjust the pH value of the solution to be 6 to 10, and then magnesium precipitation additives are added for the reaction; and 4, solid and liquid separation is conducted on reaction slurry obtained after the step 3, magnesium precipitation residues and a solution obtained after magnesium precipitation are obtained, and the solution obtained after magnesium precipitation is directly returned to the electrolytic manganese production system. According to the process, manganese and magnesium in the electrolytic manganese system are separated through a fractional precipitation method according to the solubility product difference between manganese carbonate and magnesium carbonate, manganese carbonate is reused, magnesium carbonate is discharged out of the system, and the purpose of reducing impurity magnesium in the electrolytic manganese system is achieved.
Description
Technical field
The invention belongs to metallurgical technology field, particularly relate to the removal methods of impurity magnesium in a kind of electrolytic manganese system.
Background technology
In electrolytic manganese industrial production, magnesium, as main accompanying elements a kind of in manganese ore, enters solution and generates magnesium sulfate in leaching process.Because magnesium and manganese character is between the two close, be isolated more difficult, cause in the metallurgical system of manganese that magnesium cannot effective elimination.And in conventional manganese metallurgical process, manganese electrolyte is that closed cycle utilizes, therefore the accumulation of magnesium sulfate in solution can be caused, and produce a series of harm thus: 1) along with magnesium density in solution raises, system can produce ammonium magnesium sulfate crystallization, especially, when temperature reduces, whole production system there will be big area disordered crystalline.A large amount of ammonium magnesium sulfate forms fine and close crystallization in equipment surface, and blocking solution channel, worsens production operation environment, jeopardizes equipment and produces normal operation.2) the ammonium magnesium sulfate crystallization of crystallization causes the loss of the effective constituent such as manganese, ammonium, and production cost is increased.3) in electrolytic process, magnesium crystallization can increase voltage and the resistance of electrolyzer, reduces electrolytic cell currents efficiency, increases the production cost of electrolyzer energy consumption and manganese.Therefore, in electrolytic manganese production process magnesium addition remove the important factor day by day becoming and affect manganese Metallurgical Industry Development.
In order to eliminate the harm that impurity magnesium is produced electrolytic metal Mn, large quantity research is carried out to the separation of magnesium in electrolytic manganese production process both at home and abroad, mainly comprise: 1) ammonium magnesium sulfate crystallization process, by suitably increasing ammonium sulfate concentrations or reduction system solution temperature in solution, ammonium magnesium sulfate complex salt crystal is concentrated separate out, reach the object of magnesium ion content in reduction system.The method long processing period, solution causes structure deteriorate, and needs very large man power and material's cost.2) chemical precipitation method, mainly application and magnesium can form the method that magnesium removes by the less precipitation agent of solubleness from solution.Conventional precipitation agent has oxalate, phosphoric acid salt and compound precipitants etc., and it is high that the method mainly exists precipitation agent cost, easily introduces the problems such as new foreign ion.3) extraction process, mainly selects suitable extraction agent to carry out extracting and separating to the magnesium in electrolytic manganese anolyte or qualifying liquid, but the method exists cost better and pollute the problems such as larger, is still in theoretical research stage at present, not industrialization.Therefore, aforesaid method all thoroughly can not solve the impact that electrolytic manganese system magnesium addition content overproof brings, and there is not yet method effective and feasible in actual production so far.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, provides a kind of fractional precipitation to reduce the method for impurity Mg content in electrolytic manganese system.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is:
Fractional precipitation reduces a method for impurity magnesium in electrolytic manganese system, comprises the following steps:
1) in electrolytic manganese anolyte or qualifying liquid, add liquefied ammonia regulator solution pH value to 6.5 ~ 9, then add heavy manganese additive and constantly stir and react, the Mn wherein in heavy manganese additive and electrolytic solution or qualifying liquid
2+mol ratio be 0.9 ~ 1.2;
2) carry out solid-liquid separation to the reacting slurry after step 1), obtain the solution after heavy manganese slag and heavy manganese, heavy manganese slag returns to electrolytic manganese chemical combination workshop and replaces dry powder and ammonia neutralization to leach the spent acid of terminal;
3) to step 2) add liquefied ammonia regulator solution pH value to 6 ~ 10 in solution after heavy manganese, then add heavy magnesium additive and constantly stir and react, the Mg in the solution wherein after heavy magnesium additive and heavy manganese
2+mol ratio be 0.5 ~ 3;
4) carry out solid-liquid separation to the reacting slurry after step 3), obtain the solution after heavy magnesium slag and heavy magnesium, the solution after heavy magnesium is mainly ammoniumsulphate soln, directly returns electrolytic manganese production system, and heavy magnesium slag enters slag storehouse and stores up.
Above-mentioned fractional precipitation reduces the method for impurity Mg content in electrolytic manganese system, and preferably, in described step 1), in pending electrolytic manganese anolyte, Mn ionic concn is 10 ~ 17g/L, Mg ionic concn is 25 ~ 40g/L, (NH
4)
2sO
4concentration 70g/L ~ 90g/L.
Above-mentioned fractional precipitation reduces the method for impurity Mg content in electrolytic manganese system, and preferably, in described step 1), in pending electrolytic manganese qualifying liquid, Mn ionic concn is 30 ~ 45g/L, Mg ionic concn is 25 ~ 40g/L, (NH
4)
2sO
4concentration 70g/L ~ 90g/L.
Above-mentioned fractional precipitation reduces the method for impurity Mg content in electrolytic manganese system, and preferably, in described step 1), heavy manganese additive is one or several in carbonic acid gas, volatile salt, bicarbonate of ammonia.Heavy manganese additive abundant raw material source, low price.Especially carbonic acid gas is as the waste gas in chemical combination workshop in electrolytic manganese production process, can also realize process gas and reduce discharging, have the advantage reduced costs with protection of the environment concurrently while utilizing its heavy manganese.Heavy manganese additive generates manganous carbonate with the Mn ionic reaction in solution and separates out from solution under ammoniacal liquor exists, and heavy manganese additive utilization ratio is high, and speed of reaction is fast, and heavy manganese efficiency is high, and its reaction is: Mn
2++ HCO
3 -+ NH
3h
2o=MnCO
3+ NH
4 ++ H
2o.Heavy manganese additive can not introduce other foreign ions simultaneously, does not affect electrolytic manganese solution system.Adopt liquefied ammonia regulator solution pH value, liquefied ammonia must be controlled in this process and add speed, if add excessive velocities, a large amount of Mn ion in topical solutions can be caused to be Mn (OH)
2separate out, affect separation and the recycling of follow-up heavy manganese slag, then slowly add heavy manganese additive, react certain hour at a set temperature and sink manganese, continue to add liquefied ammonia simultaneously and ensure solution ph in the reasonable scope.
Above-mentioned fractional precipitation reduces the method for impurity Mg content in electrolytic manganese system, and preferably, in described step 1), controlling temperature of reaction in heavy manganese reaction process is 30 ~ 60 DEG C, and the reaction times is 10 ~ 120min.
Above-mentioned fractional precipitation reduces the method for impurity Mg content in electrolytic manganese system, and preferably, in described step 3), heavy magnesium additive is one or several in carbonic acid gas, volatile salt, bicarbonate of ammonia.
Above-mentioned fractional precipitation reduces the method for impurity Mg content in electrolytic manganese system, and preferably, in described step 3), controlling temperature of reaction in heavy reactive magnesium process is 30 ~ 60 DEG C, and the reaction times is 10 ~ 120min.
Above-mentioned fractional precipitation reduces the method for impurity Mg content in electrolytic manganese system, preferably, and described step 2) in, in the solution after heavy manganese, Mn ionic concn is lower than 3g/L; In described step 4), in the solution after heavy magnesium, Mg ionic concn is lower than 20g/L, and ammonium sulfate concentrations is 110g/L ~ 155g/L.
Above-mentioned fractional precipitation reduces the method for impurity Mg content in electrolytic manganese system, preferably, and described step 2) in, the main component of heavy manganese slag is manganous carbonate.
Principle of the present invention is: according to MnCO at the standard conditions
3and MgCO
33H
2the solubility product of O is respectively 1.8 × 10
-11with 2.14 × 10
-5, and Mg in anolyte handled by the present invention and qualifying liquid
2+concentration and Mn
2+concentration is more or less the same, within 10 times.After adding precipitation agent carbonate, because carbonate concentration is identical, and manganous carbonate solubility product is lower, therefore generates the Mn needed for manganous carbonate precipitation
2+concentration is than the Mg generated needed for carbonic acid magnesium precipitate
2+low 6 orders of magnitude, namely manganous carbonate first precipitates, along with manganous carbonate precipitation is constantly separated out, Mn in solution
2+continuous reduction, manganous carbonate precipitation is separated out to continue, carbonate concentration in solution must be made constantly to increase, when carbonate concentration be increased to magnesiumcarbonate start precipitate needed for concentration time, then manganous carbonate and magnesiumcarbonate precipitate simultaneously, but now can calculate according to the solubility product of hydrocarbonate of magnesia, the Mn in solution when magnesiumcarbonate starts to precipitate
2+theoretical concentration be 10
-6mol/L, i.e. Mn
2+what precipitated is very complete.Therefore, according to the difference of manganous carbonate and hydrocarbonate of magnesia solubility product, under the same conditions, the fractional precipitation of manganese in solution, magnesium can be realized completely, reach the object removing impurity Mg content in electrolytic manganese system.Isolated manganous carbonate recycle, and magnesiumcarbonate is discharged system, reach the object reducing impurity magnesium in electrolytic manganese system.
Compared with prior art, the invention has the advantages that:
1) technique of the present invention is according to the solubility product difference of manganese, magnesium carbonate, adopts the method for fractional precipitation to be separated manganese and magnesium in electrolytic manganese system, manganous carbonate reuse, and magnesiumcarbonate is discharged system, reach the object reducing impurity magnesium in electrolytic manganese system; The heavy manganese adopted in technological process and heavy magnesium additive abundant raw material, be cheaply easy to get, and heavy manganese and heavy magnesium efficiency high.
2) the heavy manganese slag obtained in technological process of the present invention can be directly used in the neutralizing agent in electrolytic manganese production manganese ore leaching process, thus realizes manganese and all recycle.
3) the demagging slag stability obtained in technological process of the present invention is better, and without the need to further process, directly can enter slag storehouse and stack, the ammoniumsulphate soln after heavy magnesium directly can return electrolytic manganese production system and recycle.
4) technique of the present invention is combined closely with existing electrolytic manganese production process, simple, is easy to realize suitability for industrialized production.
5) produce without hazardous and noxious substances in technological process of the present invention, damage can not be caused to production unit, more can not to environment.
Accompanying drawing explanation
Fig. 1 is the method process flow sheet that fractional precipitation of the present invention reduces impurity Mg content in electrolytic manganese system.
Embodiment
For the ease of understanding the present invention, hereafter will do to describe more comprehensively, meticulously to the present invention in conjunction with Figure of description and preferred embodiment, but protection scope of the present invention is not limited to following specific embodiment.
Unless otherwise defined, hereinafter used all technical terms are identical with the implication that those skilled in the art understand usually.The object of technical term used herein just in order to describe specific embodiment is not be intended to limit the scope of the invention.
Apart from special instruction, all ingredients used in the present invention, raw material are can commodity commercially or can by the obtained product of known method.
embodiment 1:
Fractional precipitation of the present invention reduces a method for impurity Mg content in electrolytic manganese system, and its process flow sheet as shown in Figure 1, comprises the following steps:
1) at electrolytic manganese anolyte, (Mn concentration is 10g/L, Mg concentration is 25g/L, (NH
4)
2sO
4concentration 70g/L) add liquefied ammonia regulator solution pH value to 6.5, then add the bicarbonate of ammonia (Mn in bicarbonate of ammonia and anolyte
2+mol ratio be 0.9), and continuing to add liquefied ammonia, to maintain the pH value of solution constant, and continuous stirring reaction 10min, control temperature of reaction is 30 DEG C simultaneously.
2) carry out settlement separate to the reacting slurry after step 1), obtain the solution after heavy manganese slag and heavy manganese.Heavy manganese slag main component is manganous carbonate, returns to electrolytic manganese chemical combination workshop and replaces dry powder and ammonia neutralization to leach the spent acid of terminal.In in solution after heavy manganese, Mn concentration is 2.36g/L.
3) to step 2) add liquefied ammonia regulator solution pH value to 6.0 in solution after heavy manganese, then add the bicarbonate of ammonia (Mg in the solution after bicarbonate of ammonia and heavy manganese
2+mol ratio be 0.5), adding liquefied ammonia, to maintain pH value constant, and continuous stirring reaction 10min, and control temperature of reaction is 30 DEG C simultaneously.
4) press filtration is carried out to the reacting slurry after step 3), obtain the solution after heavy magnesium slag and heavy magnesium.In solution after heavy magnesium, Mg concentration is 16.83g/L, and ammonium sulfate concentrations is 113.88g/L, and the solution after heavy magnesium directly returns electrolytic manganese production system.Heavy magnesium slag is mainly magnesium carbonate hydrate, directly can enter slag storehouse and store up, realize the open circuit of Mg in electrolytic manganese system.
embodiment 2:
Fractional precipitation of the present invention reduces a method for impurity Mg content in electrolytic manganese system, and its process flow sheet as shown in Figure 1, comprises the following steps:
1) at electrolytic manganese anolyte, (Mn concentration is 17g/L, Mg concentration is 40g/L, (NH
4)
2sO
4concentration 90g/L) add liquefied ammonia regulator solution pH value to 9, then add the volatile salt (Mn in volatile salt and anolyte
2+mol ratio be 1.2), continue to add liquefied ammonia maintenance system pH value constant, continuous stirring reaction 100min, control temperature of reaction is 60 DEG C simultaneously.
2) carry out settlement separate to the reacting slurry after step 1), obtain the solution after heavy manganese slag and heavy manganese.Heavy manganese slag main component is manganous carbonate, returns to electrolytic manganese chemical combination workshop and replaces dry powder and ammonia neutralization to leach the spent acid of terminal.In in solution after heavy manganese, Mn concentration is 0.20g/L.
3) to step 2) add liquefied ammonia regulator solution pH value to 10 in solution after heavy manganese, then add the bicarbonate of ammonia (Mg in the solution after volatile salt and heavy manganese
2+mol ratio be 3), continue to add liquefied ammonia maintenance system pH value constant, continuous stirring reaction 120min, control temperature of reaction is 70 DEG C simultaneously.
4) press filtration is carried out to the reacting slurry after step 3), obtain the solution after heavy magnesium slag and heavy magnesium.In solution after heavy magnesium, Mg concentration is 4.98g/L, and ammonium sulfate concentrations is 143.81g/L, and the solution after heavy magnesium directly returns electrolytic manganese production system.Heavy magnesium slag is mainly magnesium carbonate hydrate, directly can enter slag storehouse and store up, realize the open circuit of Mg in electrolytic manganese system.
embodiment 3:
Fractional precipitation of the present invention reduces a method for impurity Mg content in electrolytic manganese system, and its process flow sheet as shown in Figure 1, comprises the following steps:
1) at electrolytic manganese qualifying liquid, (Mn concentration is 30g/L, Mg concentration is 25g/L, (NH
4)
2sO
4concentration 70g/L) add liquefied ammonia regulator solution pH value to 7, then pass into CO
2gas (CO
2with the Mn in qualifying liquid
2+mol ratio be 0.9), continuing to add liquefied ammonia, to maintain solution ph constant, then continuous stirring reaction 100min, and control temperature of reaction is 60 DEG C simultaneously.
2) carry out settlement separate to the reacting slurry after step 1), obtain the solution after heavy manganese slag and heavy manganese.Heavy manganese slag main component is manganous carbonate, returns to electrolytic manganese chemical combination workshop and replaces dry powder and ammonia neutralization to leach the spent acid of terminal.In in solution after heavy manganese, Mn concentration is 3.20g/L.
3) to step 2) add liquefied ammonia regulator solution pH value to 7 in solution after heavy manganese, then pass into CO
2(CO
2with the Mg in the solution after heavy manganese
2+mol ratio be 0.5), add liquefied ammonia and regulate slurry pH value constant, then continuous stirring reaction 10min, control temperature of reaction is 30 DEG C simultaneously.
4) press filtration is carried out to the reacting slurry after step 3), obtain the solution after heavy magnesium slag and heavy magnesium.In solution after heavy magnesium, Mg concentration is 19.91g/L, and ammonium sulfate concentrations is 120.67g/L, and the solution after heavy magnesium directly returns electrolytic manganese production system.Heavy magnesium slag is mainly magnesium carbonate hydrate, directly can enter slag storehouse and store up, realize the open circuit of Mg in electrolytic manganese system.
embodiment 4:
Fractional precipitation of the present invention reduces a method for impurity Mg content in electrolytic manganese system, and its process flow sheet as shown in Figure 1, comprises the following steps:
1) at electrolytic manganese qualifying liquid, (Mn concentration is 45g/L, Mg concentration is 40g/L, (NH
4)
2sO
4concentration 90g/L) add liquefied ammonia regulator solution pH value to 9, then add volatile salt and bicarbonate mixture (the wherein mol ratio 1:1 of volatile salt and bicarbonate of ammonia, the Mn in volatile salt and bicarbonate mixture and qualifying liquid
2+mol ratio be 1.2), it is constant to add liquefied ammonia maintenance system pH, and continuous stirring reaction 100min, and control temperature of reaction is 60 DEG C simultaneously.
2) carry out settlement separate to the reacting slurry after step 1), obtain the solution after heavy manganese slag and heavy manganese.Heavy manganese slag main component is manganous carbonate, returns to electrolytic manganese chemical combination workshop and replaces dry powder and ammonia neutralization to leach the spent acid of terminal.In in solution after heavy manganese, Mn concentration is 1.00g/L.
3) to step 2) add liquefied ammonia regulator solution pH value to 10 in solution after heavy manganese, then add volatile salt and bicarbonate mixture (the wherein mol ratio 1:1 of volatile salt and bicarbonate of ammonia, the Mg in the solution after volatile salt and bicarbonate mixture and heavy manganese
2+mol ratio be 3), continuing to add liquefied ammonia, to maintain the pH value of solution constant, and continuous stirring reaction 120min, and control temperature of reaction is 70 DEG C simultaneously.
4) press filtration is carried out to the reacting slurry after step 3), obtain the solution after heavy magnesium slag and heavy magnesium.In qualifying liquid after demagging, Mg concentration is 11.23g/L, and ammonium sulfate concentrations is 152.72g/L, directly returns electrolytic manganese production system.Heavy magnesium slag is mainly magnesium carbonate hydrate, directly can enter slag storehouse and store up, realize the open circuit of Mg in electrolytic manganese system.
Claims (9)
1. fractional precipitation reduces a method for impurity Mg content in electrolytic manganese system, it is characterized in that, comprises the following steps:
1) in electrolytic manganese anolyte or qualifying liquid, add liquefied ammonia regulator solution pH value to 6.5 ~ 9, then add heavy manganese additive and constantly stir and react, wherein Mn in heavy manganese additive and electrolytic solution or qualifying liquid
2+mol ratio be 0.9 ~ 1.2;
2) carry out solid-liquid separation to the reacting slurry after step 1), obtain the solution after heavy manganese slag and heavy manganese, heavy manganese slag returns in electrolytic manganese chemical combination workshop and leaches the spent acid of terminal;
3) to step 2) add liquefied ammonia regulator solution pH value to 6 ~ 10 in solution after heavy manganese, then add heavy magnesium additive and constantly stir and react, the Mg in the solution wherein after heavy magnesium additive and heavy manganese
2+mol ratio be 0.5 ~ 3;
4) carry out solid-liquid separation to the reacting slurry after step 3), obtain the solution after heavy magnesium slag and heavy magnesium, the solution after heavy magnesium directly returns electrolytic manganese production system.
2. fractional precipitation as claimed in claim 1 reduces the method for impurity Mg content in electrolytic manganese system, and it is characterized in that, in described step 1), in pending electrolytic manganese anolyte, Mn ionic concn is 10 ~ 17g/L, Mg ionic concn is 25 ~ 40g/L, (NH
4)
2sO
4concentration 70g/L ~ 90g/L.
3. fractional precipitation as claimed in claim 1 reduces the method for impurity Mg content in electrolytic manganese system, and it is characterized in that, in described step 1), in pending electrolytic manganese qualifying liquid, Mn ionic concn is 30 ~ 45g/L, Mg ionic concn is 25 ~ 40g/L, (NH
4)
2sO
4concentration 70g/L ~ 90g/L.
4. fractional precipitation as described in any one of claims 1 to 3 reduces the method for impurity Mg content in electrolytic manganese system, it is characterized in that, in described step 1), heavy manganese additive is one or several in carbonic acid gas, volatile salt, bicarbonate of ammonia.
5. the fractional precipitation as described in any one of claims 1 to 3 reduces the method for impurity Mg content in electrolytic manganese system, it is characterized in that, in described step 1), controlling temperature of reaction in heavy manganese reaction process is 30 ~ 60 DEG C, and the reaction times is 10 ~ 120min.
6. fractional precipitation as described in any one of claims 1 to 3 reduces the method for impurity Mg content in electrolytic manganese system, it is characterized in that, in described step 3), heavy magnesium additive is one or several in carbonic acid gas, volatile salt, bicarbonate of ammonia.
7. the fractional precipitation as described in any one of claims 1 to 3 reduces the method for impurity Mg content in electrolytic manganese system, it is characterized in that, in described step 3), controlling temperature of reaction in heavy reactive magnesium process is 30 ~ 60 DEG C, and the reaction times is 10 ~ 120min.
8. the fractional precipitation as described in any one of claims 1 to 3 reduces the method for impurity Mg content in electrolytic manganese system, it is characterized in that, described step 2) in, in the solution after heavy manganese, Mn ionic concn is lower than 3g/L; In described step 4), in the solution after heavy magnesium, Mg ionic concn is lower than 20g/L, and ammonium sulfate concentrations is 110g/L ~ 155g/L.
9. the fractional precipitation as described in any one of claims 1 to 3 reduces the method for impurity Mg content in electrolytic manganese system, it is characterized in that, described step 2) in, the main component of heavy manganese slag is manganous carbonate.
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| CN111172561A (en) * | 2018-11-13 | 2020-05-19 | 云南创一磷业技术有限公司 | Method for separating magnesium in electrolytic manganese production process |
| CN111647911A (en) * | 2020-03-27 | 2020-09-11 | 昆明理工大学 | Process for removing magnesium ions in electrolytic manganese anolyte |
| CN114212828A (en) * | 2021-12-31 | 2022-03-22 | 湖南烯富环保科技有限公司 | Method for removing impurities from manganese sulfate solution |
| CN114702075A (en) * | 2022-04-11 | 2022-07-05 | 中南大学 | Purification preparation method of manganese sulfate |
| CN115872452A (en) * | 2022-12-27 | 2023-03-31 | 江西赣锋锂业集团股份有限公司 | Method for recovering magnesium and manganese from impurity-removing slag of spodumene leaching solution |
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