CN109052481A - The method that absorption method removes magnesium ion in manganese sulfate solution - Google Patents
The method that absorption method removes magnesium ion in manganese sulfate solution Download PDFInfo
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- CN109052481A CN109052481A CN201811041482.XA CN201811041482A CN109052481A CN 109052481 A CN109052481 A CN 109052481A CN 201811041482 A CN201811041482 A CN 201811041482A CN 109052481 A CN109052481 A CN 109052481A
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- Prior art keywords
- sulfate solution
- manganese sulfate
- manganese
- adsorbent
- magnesium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/10—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses the methods of magnesium ion in a kind of absorption method removal manganese sulfate solution.The present invention has formulated special adsorbent preparation process, the technique position that adsorbent is added, adsorbent amount, the composition of adsorbent, absorption pH, reaction time, reaction temperature etc..Keep it high (removal rate 65~70%) for the removal efficiency of magnesium ion, accumulation of the magnesium in system can be effectively reduced, reduce its normal Influence of production to the system, and it is low in cost, manganese sulfate solution will not be caused the secondary pollution present invention have the characteristics that apparatus and process it is simple, it is low in cost, be easy to automate and be mass produced, the magnesium of absorption is handled in a manner of byproduct simultaneously, and the regeneration rate of adsorbent is 90% or so.The magnesium in manganese sulfate solution can be effectively removed using the present invention, small to the negative effect of existing electrolytic manganese production technology, equipment is simple, easily realizes industrialization, is able to satisfy technique production requirement, by the benign development of positive promotion manganese industry.
Description
Technical field
The present invention relates to chemical technology field, the method for magnesium ion in specially a kind of absorption method removal manganese sulfate solution.
Background technique
Electrolytic manganese is the industrial development of our province regional economy or even the whole nation as a kind of important metallurgy, chemical raw material
It makes a great contribution.On January 22nd, 2016,103 geology group of Guizhou Provincial Geological Prospecting Bureau have found entirely latent in Guizhou pine peach
Highly, general feel manganese ore, three, peach level ground ultra-large type manganese ore deposit, wherein general feel manganese ore deposit newly verifies 1.92 hundred million tons of manganese resource amount,
It is the first to occupy China, Asia first.So far, it is known as the manganese resource amount that the Tongren district Guizhou Province of " manganese is all " possesses and has leapt to China
First, into world forefront.More than 20 family of electrolytic manganese enterprise of our province Tongren Prefecture, Guizhou electrolytic manganese production capacity already take up Chinese electrolysis
25% or so of manganese production capacity.In addition southwest can mine group, Jin Shi flag International Holdings Ltd and Guizhou Province Pan county multiple star source manganese
The successive operation of industry Co., Ltd, Guizhou electrolytic manganese production capacity are expected to occupy 35% or so of China.
Although development is so swift and violent, the work in terms of technological innovation is made considerably less, therefore there are still many in production
Problem, wherein the higher phenomenon of magnesium ion concentration in manganese sulfate solution, causes different degrees of influence to production, it has also become industry
Common problem, cause the highest attention of related scholar, applicant investigates Duo Jia electrolytic manganese enterprise on the spot, from it
Know at person in charge of the technology aspect, the magnesium ion situation in each enterprise's electrolyte is as shown in table 1.
Magnesium ion concentration in 1 electrolytic manganese enterprise electrolyte of table
From table 1 it follows that magnesium ion concentration is 27g/l~30g/l, pine in the manganese sulfate solution of Zun Yi day magnetic manganese industry
Peach three and manganese industry are 24g/l~28g/l, and the Huifeng Song Tao manganese industry is 25g/l~29g/l, Ningxia Tianyuan Meng Ye Co., Ltd
It is 28g/l~32g/l, up to 42g/l when winter is serious, Xinjiang Aketao nation of section manganese industry is 29g/l~33g/l, once
There is the up to record of 40g/l, and manganese ion concentration is only 35g/l or so in the new liquid of electrolytic manganese (leaching tanks inflow), into electricity
Solution liquid is 20g/l or so (electrolysis working solution) after mixing with waste electrolyte.Obvious concentration impurity ion is higher than base metal ion
Concentration, the phenomenon have become the common problem of industry, are just seriously threatening the normal production of electrolytic manganese.
Generally qualitative to think, magnesium ion concentration increase will cause following harm: 1. magnesium sulfate is easy to crystallize together with product,
The greater loss of the effective components such as manganese sulfate and ammonium sulfate is caused, product quality is reduced, increases the density and viscosity of solution,
Filtration difficulty increases the voltage of electrolytic cell and resistance, causes the current efficiency of electrolytic cell to reduce, to reduce the life of electrolytic cell
Produce efficiency.2. forming fine and close hard crystallization on the surface that equipment is contacted with solution, solution channel is blocked, passing through for solution is reduced
Ability causes solution discharge pressure to increase, meanwhile, magnesium crystallization also increases pipeline thermal resistance, influences the heat transfer of liquid, makes heat transfer efficiency
It significantly reduces.3. the ion gap that magnesium ion will occupy in sulfuric acid system, leads to the reduction of Leaching of rhodochrosite ore rate indirectly.4. with
Magnesium ion concentration increases, and will occupy certain position in the solution, and certainly will bring obstruction to the mass transfer of manganese ion, finally influence electric current
Efficiency improves current efficiency in actual production as far as possible, reduces influence of the impurity to system, in most of manganese sulfate electrolytes
Manganese ion concentration maintain low concentration (20g/l), the manganese ion concentration after electrolysis in anolyte be 15g/l~18g/l, two
The difference of person is minimum, and liquid inventory is big, and production efficiency is low.
Removal based on magnesium ion, related scholar have done numerous studies, and there are as below methods: 1. mechanical means method.Manipulator
The advantages of section method is exactly to be handled using mechanical stirring or the means of vibration the device for having formed magnesium crystallization, the method
It is easy to operate, but disadvantage is it is obvious that such as long processing period, will cause the impaired place of equipment inner wall to become rough, make to set
It is standby to be easier to crystallize in later production, and mechanical means needs very big man power and material, then needs to stop production when crystallizing serious
Cleaning；2. chemical precipitation method.Chemical precipitation method is extremely low and higher with manganese formation relative solubility using solubility is formed with magnesium
Compound as the method for separating magnesium manganese after precipitating reagent magnesium sinking.Common precipitating reagent have fluoride, carbonate, phosphate,
Urea and hydroxide precipitating etc..Separately there is researcher into manganese sulfate solution, is passed through carbon dioxide and realizes magnesium, manganese separation.From this
A little precipitation method see that urea method sedimentation effect is bad, and the solubility of carbon dioxide in aqueous solution is limited, and it is heavy to limit carbon dioxide
Shallow lake method, carbonate, hydroxide and phosphate precipitation are required at higher pH, and while removing magnesium, a large amount of manganese also can
It is lost because generating precipitating, from the solubility product of various magnesium salts it is found that villiaumite method is more satisfactory method, but villiaumite method is heavy
Shallow lake product filtration difficulty, the complete fluorine ion of unreacted will cause fatal harm to cathode plate, and the cost of villiaumite is very high, therefore
There are also a distances from industrial application for chemical precipitation method；3. extraction.Extractant is largely organic reagent, certainly will will lead to body
It is the accumulative of organic matter, and organic matter increase will cause secondary pollution to manganese sulfate solution, to the weight such as conductivity, viscosity of solution
Physico-chemical property is wanted to have a negative impact.In addition, magnesium ion is up to 30g/l in manganese sulfate solution, will be brought using extraction huge
Volume processing cost；4. ore method for pretreating.This method is only applicable to pyrolusite, and now electrolytic manganese industry it is most of using
Manganese spar, manganese spar manganese during dilute sulfuric acid processing also can be dissolved out largely and cause to lose, and therefore, this method has one
Surely limitation is used.
In terms of the research of forefathers, the removal means of magnesium ion are more, but there are still respective disadvantages, so far, without work
The demagging means of industry, hinder the sustainable development of electrolytic manganese industry.Therefore, seek a kind of economically feasible, to system without dirt
The magnesium ion minimizing technology and control technique of dye seem very necessary.
There are some metal ions to be handled using absorption method at present, still, the adsorbent used is inhaled for active carbon
Attached principle be physical absorption, it can be effectively removed coloration, stink, can remove secondary effluent in most organic pollutants and certain
A little inorganic matters, but it is unobvious to the removal effect of Mg ion.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides the sides of the magnesium ion in a kind of absorption method removal manganese sulfate solution
Method, it is high for the removal efficiency of magnesium ion, reduces accumulation of the magnesium in system, reduces its normal production shadow to the system
It rings, and low in cost, secondary pollution will not be caused to manganese sulfate solution, with overcome the deficiencies in the prior art.
In order to achieve the above object, the present invention is achieved by the following technical programs: absorption method removes in manganese sulfate solution
Magnesium ion method, the open circuit portions manganese sulfate solution in electrolytic manganese production system, and use specific adsorbent to carry out it
Then adsorption treatment regenerates adsorbent, product containing magnesium prepares byproduct.
The open circuit manganese sulfate solution includes anolyte, a hydraulic fluid, two hydraulic fluids, new liquid and to electrolytic manganese leached mud
Cleaning solution.
The specific adsorbent forms single compound by one or more of Fe, Al, Mn, Ba, Ca or Si element
Or complex compound is raw material.
The specific adsorbent is that raw materials of compound is added in the manganese sulfate solution for opening a way out, is 3.2- in pH
6.5, fabricated in situ is carried out under conditions of reaction time 30-60min, temperature are 45-75 DEG C and is obtained.
Specific adsorbent adsorption process control condition is as follows: the adsorbent that every cube of open circuit portions solution uses is 50-
150kg, absorption pH are 3.5-7.5, and adsorption time 30-120min, adsorption temp is 25-85 DEG C.
Beneficial effect
Compared with prior art, the process part that the present invention has formulated the composition of specific adsorbent and preparation, adsorbent are added
Position, adsorbent amount, absorption pH, reaction time, reaction temperature etc..Formed physics, chemical combined absorption, make its for high magnesium from
The removal efficiency of sub- concentration (25-30g/l) is high (removal rate is 65~70%), effectively reduces accumulation of the magnesium in system, reduces
Its normal Influence of production to the system, and it is low in cost, secondary pollution will not be caused to manganese sulfate solution.The present invention, which has, to be set
Standby simple process, low in cost, the features such as being easy to automate and be mass produced, while the magnesium adsorbed can prepare byproduct, inhale
Attached dose of regeneration rate is 90% or so.The magnesium in manganese sulfate solution can be effectively reduced using the present invention, to existing electrolysis
The negative effect of manganese production technology is small, and equipment is simple, easily realizes industrialization, is able to satisfy technique production requirement, will actively promote manganese work
The benign development of industry.
Specific embodiment
The embodiment of the present invention 1: the method that absorption method removes the magnesium ion in manganese sulfate solution, in electrolytic manganese production system
Middle open circuit portions manganese sulfate solution, used special preparation adsorbent carry out adsorption treatment, then to specific adsorbent into
Row regeneration, product containing magnesium prepare byproduct.The open circuit manganese sulfate solution is anolyte.Specific adsorbent by Fe unification
Conjunction object is raw material, is carried out under conditions of control pH is 4.5 in manganese sulfate solution, reaction time 60min, temperature are 45 DEG C former
Position is synthesized into, and the specific adsorbent dosage of every cube of manganese sulfate solution is 100kg, adsorbs pH are as follows: and 4.5, adsorption time is
60min, adsorption temp are 45 DEG C.It is verified, pass through going for the magnesium ion in the manganese sulfate solution after the method absorption of embodiment 1
Except rate is 25%, the loss late of manganese is 12%.
The embodiment of the present invention 2: the method that absorption method removes the magnesium ion in manganese sulfate solution, in electrolytic manganese production system
Middle open circuit portions manganese sulfate solution, used special preparation adsorbent carry out adsorption treatment, then to specific adsorbent into
Row regeneration, product containing magnesium prepare byproduct.The open circuit manganese sulfate solution is a hydraulic fluid.Specific adsorbent is by Fe, Al and Mn
Complex compound be raw material, in manganese sulfate solution control pH be 6.5, the condition that reaction time 60min, temperature are 65 DEG C
Lower progress fabricated in situ and obtain, the specific adsorbent dosage of every cube of manganese sulfate solution is 100kg, adsorbs pH are as follows: 5.5, absorption
Time is 60min, and adsorption temp is 45 DEG C.It is verified, by the magnesium in the manganese sulfate solution after the absorption of the method for embodiment 2 from
The removal rate of son is 65%, and the loss late of manganese is 15%.
The embodiment of the present invention 3: the method that absorption method removes the magnesium ion in manganese sulfate solution, in electrolytic manganese production system
Middle open circuit portions manganese sulfate solution, used special preparation adsorbent carry out adsorption treatment, then to specific adsorbent into
Row regeneration, product containing magnesium prepare byproduct.The open circuit manganese sulfate solution is new liquid.Specific adsorbent by Al and Mn complexity
Compound is raw material, is carried out under conditions of control pH is 6.8 in manganese sulfate solution, reaction time 60min, temperature are 55 DEG C
Fabricated in situ and obtain, the specific adsorbent dosage of every cube of manganese sulfate solution is 85kg, adsorbs pH are as follows: 5.5, adsorption time is
60min, adsorption temp are 45 DEG C.It is verified, pass through going for the magnesium ion in the manganese sulfate solution after the method absorption of embodiment 3
Except rate is 68%, the loss late of manganese is 5%.
The embodiment of the present invention 4: the method that absorption method removes the magnesium ion in manganese sulfate solution, in electrolytic manganese production system
Middle open circuit portions manganese sulfate solution, used special preparation adsorbent carry out adsorption treatment, then to specific adsorbent into
Row regeneration, product containing magnesium prepare byproduct.The open circuit manganese sulfate solution is leached mud washing lotion.Specific adsorbent is by Fe, Al
Complex compound with Mn is raw material, and control pH is 6.5 in manganese sulfate solution, reaction time 60min, temperature are 65 DEG C
Under the conditions of carry out fabricated in situ and obtain, the specific adsorbent dosage of every cube of manganese sulfate solution is 100kg, absorption pH are as follows: 6.5,
Adsorption time is 60min, and adsorption temp is 55 DEG C.It is verified, by the manganese sulfate solution after the method absorption of embodiment 4
The removal rate of magnesium ion is 30%, and the loss late of manganese is 7%.
The embodiment of the present invention 5: the method that absorption method removes the magnesium ion in manganese sulfate solution, in electrolytic manganese production system
Middle open circuit portions manganese sulfate solution, used special preparation adsorbent carry out adsorption treatment, then to specific adsorbent into
Row regeneration, product containing magnesium prepare byproduct.The open circuit manganese sulfate solution is new liquid.Specific adsorbent by Al and Ba complexity
Compound is raw material, is carried out under conditions of control pH is 6.5 in manganese sulfate solution, reaction time 60min, temperature are 55 DEG C
Fabricated in situ and obtain, the specific adsorbent dosage of every cube of manganese sulfate solution is 120kg, adsorbs pH are as follows: 5.5, adsorption time is
60min, adsorption temp are 65 DEG C.It is verified, pass through going for the magnesium ion in the manganese sulfate solution after the method absorption of embodiment 5
Except rate is 69%, the loss late of manganese is 4.5%.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of method of the magnesium ion in absorption method removal manganese sulfate solution, it is characterised in that: in electrolytic manganese production system
Open circuit portions manganese sulfate solution, and specific adsorbent is used to carry out adsorption treatment to it, then adsorbent is regenerated, contains magnesium
Product prepares byproduct.
2. the method for the magnesium ion in absorption method removal manganese sulfate solution according to claim 1, it is characterised in that: described
The manganese sulfate solution of open circuit be anolyte, a hydraulic fluid, two hydraulic fluids, new liquid and to one of electrolytic manganese leached mud cleaning solution or
Two kinds.
3. the method for the magnesium ion in absorption method removal manganese sulfate solution according to claim 1, it is characterised in that: described
Specific adsorbent forms single compound by one or more of Fe, Al, Mn, Ba, Ca or Si element or complex compound is made
For raw material.
4. the method for the magnesium ion in absorption method removal manganese sulfate solution according to claim 3, it is characterised in that: described
Specific adsorbent be that raw materials of compound is added in the manganese sulfate solution opening a way out, and be 3.2-6.5, reaction time in pH
Fabricated in situ is carried out under conditions of being 45-75 DEG C for 30-60min, temperature and is obtained.
5. according to claim 1, adsorbent described in 3 or 4, the method for removing the magnesium ion in manganese sulfate solution, feature exist
In: the specific adsorbent that the solution of every cube of open circuit uses is 50-150kg, and absorption pH is 3.5-7.5, adsorption time 30-
120min, adsorption temp are 25-85 DEG C.
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| CN201811041482.XA CN109052481A (en) | 2018-09-07 | 2018-09-07 | The method that absorption method removes magnesium ion in manganese sulfate solution |
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| CN201811041482.XA CN109052481A (en) | 2018-09-07 | 2018-09-07 | The method that absorption method removes magnesium ion in manganese sulfate solution |
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Cited By (5)
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|---|---|---|---|---|
| CN109680300A (en) * | 2019-01-31 | 2019-04-26 | 贵州大学 | A kind of method that complex salt crystal method removes magnesium in manganese sulfate solution |
| CN110983039A (en) * | 2019-12-31 | 2020-04-10 | 贵州合众锰业科技有限公司 | Method for removing impurities in pyrolusite sulfur dioxide leaching solution |
| CN114436335A (en) * | 2020-10-30 | 2022-05-06 | 贵州大学 | Method for removing magnesium from manganese sulfate solution |
| CN115724470A (en) * | 2022-09-26 | 2023-03-03 | 广西科技师范学院 | Method for purifying manganese sulfate solution |
| CN115724470B (en) * | 2022-09-26 | 2024-05-07 | 广西科技师范学院 | Purification method of manganese sulfate solution |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN115724470A (en) * | 2022-09-26 | 2023-03-03 | 广西科技师范学院 | Method for purifying manganese sulfate solution |
| CN115724470B (en) * | 2022-09-26 | 2024-05-07 | 广西科技师范学院 | Purification method of manganese sulfate solution |
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