CN108660326A - A method of reduction acidolysis-leaching is simultaneously except iron handles manganese oxide ore - Google Patents
A method of reduction acidolysis-leaching is simultaneously except iron handles manganese oxide ore Download PDFInfo
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- CN108660326A CN108660326A CN201810530591.1A CN201810530591A CN108660326A CN 108660326 A CN108660326 A CN 108660326A CN 201810530591 A CN201810530591 A CN 201810530591A CN 108660326 A CN108660326 A CN 108660326A
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- Prior art keywords
- acidolysis
- manganese
- reduction
- leaching
- iron
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Classifications
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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
-
- 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
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- 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
Abstract
The invention belongs to manganese metallurgical technology fields, disclose a kind of method that reduction acidolysis leaches while removing iron processing oxidized form manganese ore.This method is divided into：It restores acidolysis and leaches while removing iron.The present invention utilizes biomass castoff such as sawdust, stalk etc. to make reducing agent, not only reduce environmental pollution, but also can turn waste into wealth, and reduces production cost.Using reduction acidolysis technology, biomass structure is destroyed using the concentrated sulfuric acid, it is small molecule reduced sugar to make the Substance P hydrolysis such as cellulose therein, hemicellulose, is used for Reduction of manganese ore.Without heating in ageing process, do not increase energy consumption.After ageing, high price manganese oxide is reduced to manganese sulfate, can be directly dissolved in water.Separation of iron in goethite form is used while leaching acidolysis material, and manganese is made to enter solution in the form of manganese sulfate, and iron is with goethite shape Precipitation.It will leach and can shorten technological process except iron is combined together, simplify operation, improve existing biomass and directly leach the problems such as existing extraction temperature is high, and the time is long when manganese oxide ore.
Description
Technical field
The invention belongs to manganese metallurgical technology field, it is related to a kind of reduction acidolysis-leaching while except iron handles oxidized form manganese ore
Method.
Background technology
Manganese is a kind of important strategic resource, is widely used in metallurgy, chemical industry, battery, the multiple fields such as agricultural.With work
Industry produces the increase to manganese product demand, and high-grade manganese ore increasingly depleted is rationally current grind using middle-low grade manganese ore
Study carefully emphasis.Oxidized form manganese ore cannot directly and acid-base reaction, it is necessary to be leached in reduction system.Currently used processing method packet
Include two kinds of reduction roasting-leaching and direct reducing leaching.
Traditional pyrometallurgy technology is mostly used coal and makees reducing agent, is roasted at 800-1000 DEG C.This method is easily operated,
It but due to calcination temperature height, thus can consume larger, and a large amount of flue dust and pernicious gas be will produce in reaction process, to environment
It pollutes.Direct reducing leaching method is directly added into reducing agent in Leaching Systems, converts value Mn to Mn2+Into molten
Liquid.Common reducing agent includes SO2, FeSO4, H2O2, glucose, sucrose etc..Direct reducing leaching method has compared with pyrogenic process roasts
There is the advantages of energy consumption is relatively low, clean environment firendly, but wherein there is also some defects.For example, SO2It is likely to result in environmental pollution；
Ferrous sulfate can cause the iron content in leachate excessively high, come to subsequent solution purification zone difficult；The cost of organic matter it is higher and
Consumption is big, is not suitable for industrial production.
Biomass is a kind of rich reserves, renewable resource cheap and easy to get, can hydrolyze generation reduction under certain condition
Property substance, therefore can be used as reducing agent processing manganese oxide ore.The CO that biomass generates in the process in utilization2But also as photosynthetic work
Raw material is absorbed by plants, and for growth, therefore biomass is a kind of neutral carbon reducing agent, meets environmental requirement.
Domestic scholars have carried out some to the reduction treatment of manganese oxide ore and have studied and applied for related patents.Patent
201210042585.4 disclose it is a kind of making reducing agent with locust tree, the reducing leaching manganese oxide ore in aqueous sulfuric acid medium
Method；Patent 201310185079.5, which is disclosed, answers the lignosulfonates byproduct in paper industry slurrying as reducing agent
Method for pyrolusite reducing leaching；Patent 201210035738.2 discloses a kind of biogas reduction of low grade manganese oxide
The method that mine produces manganese monoxide mineral powder；Patent 200810107428.0 discloses a kind of biomass self-heating reduction of low grade oxygen
Change the method for manganese ore extracting sulfuric acid manganese；Patent 201210042706.5, which discloses a kind of useless tealeaves, to be made reducing agent and is situated between in sulfuric acid
The method of reducing leaching manganese oxide ore in matter；Patent 201510185506.9 discloses a kind of Low grade manganese ore production electrolysis
The liquid method processed of manganese or manganese dioxide；Patent 201010226226.5 discloses a kind of trade waste cassava alcohol waste water leaching
The method for taking semi-manganese oxide ore to prepare manganese sulfate solution；Patent 201510191276.7 discloses a kind of to be handled with carbonaceous reductant
The method that manganese oxide ore produces manganese sulfate；201210156250.5 disclose it is a kind of making reducing agent with Phytolacca acinosa, in sulfuric acid solution
The method of reducing leaching manganese oxide.
There are also the researchs using biomass processes manganese oxide ore in domestic and foreign literature.The scholars such as Hariprasad use dry
Leaf makees reducing agent and leaches manganese oxide ore, and in reducing agent/manganese ore mass ratio 0.5, sulfuric acid concentration 5%, pulp density 10% leaches
8h is leached under conditions of 95 DEG C of temperature, the concentration of manganese in the solution is more than 90g/L；JianrongXue etc. has carried out Phytolacca acinosa sulfuric acid
The research of reduction-oxidation manganese ore in system, in reducing agent/manganese ore mass ratio 4:10, sulfuric acid concentration 1.7mol/L, extraction temperature 95
8h is leached under conditions of DEG C, manganese leaching rate reaches 98% or more；Wheat stalk reduction roasting-the leaching such as Honglei Zhang
Manganese oxide ore.Experiment gained optimal conditions is reducing agent/manganese ore mass ratio 0.1, and powder particle size is less than 0.85mm, calcination temperature
550 DEG C, roasting time 15min.
Although biomass reduction manganese oxide ore has development prospect, there is also some problems.As hydrometallurgy process is straight
It connects when leaching manganese oxide ore using biomass reduction there is reaction temperature height, the time is long, the big problem of acid consumption.In addition mine
The dissolving of iron oxide can clean to subsequent purification and bring difficulty in stone
Invention content
Existing production cost is high when the present invention is for the processing of existing manganese oxide ore, and efficiency is low, it is proposed that a kind of reductic acid
Simultaneously except the manganese oxide ore processing method of iron, this method may be implemented to leach, except iron is carried out at the same time, to simplify technique stream for solution-leaching
Journey, it is easily operated.
It is another object of the present invention to improve, existing leaching when existing biomass directly leaches manganese oxide ore is warm
The problems such as degree is high, and the time is long.
The present invention provides a kind of biomass reduction acidolysis-leachings simultaneously except the method that iron handles manganese oxide ore.This method
It is broadly divided into two parts：It restores acidolysis and leaches while removing iron.
Step 1, acidolysis is restored：First biomass reductant and manganese mineral powder in mass ratio 0.3~0.5 is mixed, is then added
Water and the concentrated sulfuric acid, wherein water/manganese mineral powder ratio (ml/g) is 0.5~1.0, and the concentrated sulfuric acid/manganese mineral powder mass ratio is 0.8~1.0；It fills
Divide after stirring to be placed in seal box and be aged 12-24h, obtains acidolysis material；
Step 2, it leaches while removing iron：Using separation of iron in goethite form, by the way of batch charging, acid is added in calcium oxide
PH value of solution is controlled in solution material, in leaching process in OK range, extraction temperature is 90-95 DEG C, reaction time 1.5-3h.Pass through
The method can make the manganese sulfate generated after reduction acidolysis enter solution, and iron is precipitated as goethite, to realize ferrimanganic point
From.
Further, the manganese oxide ore is the mixture of one or more of pyrolusite, manganite or braunite.
Further, the mass fraction of manganese ore Powder Particle Size used less than 75 μm is not less than 85% in the step 1.
Further, biomass reductant/manganese mineral powder mass ratio is 0.3~0.4 in the step 1.
Further, digestion time is 16~20h in the step 1.
Further, the liquid-solid ratio (ml/g) when being leached in the step 2 while removing iron is 4~8.
Further, pH value of solution is controlled in the step 2 between 2.5~3.0.
Compared with prior art, the present invention advantage is：
(1) present invention utilizes biomass castoff such as sawdust, stalk etc. to make reducing agent, not only reduce environmental pollution, but also energy
Turn waste into wealth, reduces production cost.
(2) using reduction acidolysis technology, biomass structure is destroyed using the concentrated sulfuric acid, makes cellulose therein, hemicellulose
Equal Substance P hydrolysis are small molecule reduced sugar, are used for Reduction of manganese ore.Without heating in ageing process, do not increase energy consumption.
(3) after being aged, high price manganese oxide is reduced to manganese sulfate, can be directly dissolved in water.It is used while leaching acidolysis material
Separation of iron in goethite form makes manganese enter solution in the form of manganese sulfate, and iron is with goethite shape Precipitation.It will leach and remove iron knot
Technological process can be shortened by being combined, and simplify operation.
Description of the drawings
Fig. 1 is present invention process flow chart.
Specific embodiment
The present invention is illustrated by following instance.
Embodiment 1
Manganese grade is about 20% in selected sample ore, and ore is crushed to the mass fraction less than 75 μm and is not less than 85%.Reduction
Agent sawdust is derived from local wood-working factory.
First miberal powder, sawdust are mixed when restoring acidolysis, water and the concentrated sulfuric acid is then added, is sufficiently stirred and is placed in incubator
It is aged 14h.Reducing agent/manganese ore mass ratio is controlled when charging, sulfuric acid/manganese ore mass ratio and water/mine ratio (ml/g) they are respectively 0.3,
0.8,0.5.
It leaches in iron removal simultaneously and uses separation of iron in goethite form.First acidolysis material and calcium oxide are sufficiently mixed, then divided
It criticizes and is added to the water, control pH value of solution=2.5, the leaching 1.5h at 90 DEG C, mixing speed 300rpm leach liquid-solid ratio 4.
It is separated by solid-liquid separation after leaching, the wash water after leached mud washing returns to leaching process and is continuing with.The manganese obtained by this technology
Leaching rate is 84.3%, and iron content is less than 0.028g/L in solution.
Embodiment 2
Manganese content is about 25% in selected sample ore, and ore is crushed to the mass fraction less than 75 μm and is not less than 95%.Reduction
Agent sawdust is derived from local wood-working factory.
First by miberal powder when restoring acidolysis, stalk is sufficiently mixed, and then sequentially adds water and the concentrated sulfuric acid, controls reducing agent/manganese
Mine mass ratio, sulfuric acid/manganese ore mass ratio and water/mine ratio (ml/g) are respectively 0.35,1.0,1.0.It is sufficiently stirred and is placed on sealing
18h is aged in case.
It leaches in iron removal simultaneously and uses separation of iron in goethite form.First acidolysis material and calcium oxide are mixed, then added in batches
Enter in water, control pH value of solution=2.8, the leaching 2h at 95 DEG C, mixing speed 300rpm leach liquid-solid ratio 6.After leaching
It is separated by solid-liquid separation, the wash water after leached mud washing returns to leaching process and is continuing with.
It is 94.3% by the manganese leaching rate that this technology obtains, and iron content is less than 0.0075g/L in solution.
Embodiment 3
Manganese content is about 25% in selected sample ore, and ore is crushed to all less than 75 μm.Reducing agent sawdust is derived from local wood
Material processing factory.
First the miberal powder of certain mass and sawdust are mixed when restoring acidolysis, then sequentially add water and the concentrated sulfuric acid, control is also
Former agent/manganese ore mass ratio, sulfuric acid/manganese ore mass ratio and water/mine ratio (ml/g) are respectively 0.4,0.9,0.8.It is sufficiently stirred postposition
In being aged 16h in incubator.
It leaches in iron removal simultaneously and uses separation of iron in goethite form.First acidolysis material and calcium oxide are sufficiently mixed, then divided
It criticizes and is added to the water, control pH=2.6, the leaching 2h at 95 DEG C, mixing speed 300rpm, leach liquid-solid ratio 5.After leaching
It is separated by solid-liquid separation, the wash water after leached mud washing returns to leaching process and is continuing with.
It is 93.2% by the manganese leaching rate that this technology obtains, and iron content is less than 0.012g/L in solution.
Embodiment 4
Manganese content is about 25% in selected sample ore, and ore is crushed to all less than 75 μm.Reducing agent sawdust is derived from local wood
Material processing factory.
First the miberal powder of certain mass and sawdust are mixed when restoring acidolysis, then sequentially add water and the concentrated sulfuric acid, control is also
Former agent/manganese ore mass ratio, sulfuric acid/manganese ore mass ratio and water/mine ratio (ml/g) are respectively 0.5,1.0,1.0.It is sufficiently stirred postposition
In being aged for 24 hours in incubator.
It leaches in iron removal simultaneously and uses separation of iron in goethite form.First acidolysis material and calcium oxide are sufficiently mixed, then divided
It criticizes and is added to the water, control pH=3.0, the leaching 3h at 95 DEG C, mixing speed 300rpm, leach liquid-solid ratio 8.After leaching
It is separated by solid-liquid separation, the wash water after leached mud washing returns to leaching process and is continuing with.
It is 91.5% by the manganese leaching rate that this technology obtains, and iron content is less than 0.0069g/L in solution.
Claims (8)
1. a kind of reduction acidolysis-leaching is simultaneously except the method for iron processing manganese oxide ore, which is characterized in that include the following steps：
Step 1, acidolysis is restored：First by biomass reductant and manganese mineral powder in mass ratio 0.3~0.5 mix, then be added water and
The concentrated sulfuric acid, wherein water/manganese mineral powder ratio (ml/g) is 0.5~1.0, and the concentrated sulfuric acid/manganese mineral powder mass ratio is 0.8~1.0；Fully stir
It is placed in seal box after mixing and is aged 12-24h, obtain acidolysis material；
Step 2, it leaches while removing iron：By the way of batch charging, calcium oxide is added in acidolysis material, is controlled in leaching process
PH value of solution is in OK range, and extraction temperature is 90-95 DEG C, reaction time 1.5-3h.
2. reduction acidolysis-leaching according to claim 1 is simultaneously except the method for iron processing manganese oxide ore, which is characterized in that
The manganese oxide ore is the mixture of one or more of pyrolusite, manganite or braunite.
3. reduction acidolysis-leaching according to claim 1 or 2 is simultaneously except the method for iron processing manganese oxide ore, feature exists
In the mass fraction of manganese ore Powder Particle Size used less than 75 μm is not less than 85% in the step 1.
4. reduction acidolysis-leaching according to claim 1 or 2 is simultaneously except the method for iron processing manganese oxide ore, feature exists
In biomass reductant/manganese mineral powder mass ratio is 0.3~0.4 in the step 1.
5. reduction acidolysis-leaching according to claim 3 is simultaneously except the method for iron processing manganese oxide ore, which is characterized in that
Biomass reductant/manganese mineral powder mass ratio is 0.3~0.4 in the step 1.
6. reduction acidolysis-leaching according to claims 1 or 2 or 5 is simultaneously except the method for iron processing manganese oxide ore, feature
It is, digestion time is 16~20h in the step 1.
7. reduction acidolysis-leaching according to claims 1 or 2 or 5 is simultaneously except the method for iron processing manganese oxide ore, feature
Liquid-solid ratio (ml/g) when being, leached in the step 2 while removing iron is 4~8.
8. reduction acidolysis-leaching according to claims 1 or 2 or 5 is simultaneously except the method for iron processing manganese oxide ore, feature
It is, pH value of solution is controlled in the step 2 between 2.5~3.0.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109457110A (en) * | 2018-11-27 | 2019-03-12 | 中信大锰矿业有限责任公司 | A kind of acids reduction leaching method of Gabon's manganese oxide ore |
| CN109468458A (en) * | 2018-11-27 | 2019-03-15 | 中信大锰矿业有限责任公司 | A kind of method that Gabon's manganese oxide ore leaches and recycles iron |
| CN110184455A (en) * | 2019-06-20 | 2019-08-30 | 东北大学 | A kind of leaching method of difficult leaching cobalt ore |
| CN110373542A (en) * | 2019-08-29 | 2019-10-25 | 贵州大学 | A kind of method of powdered biomass reduction manganese oxide ore |
| CN111041247A (en) * | 2019-12-11 | 2020-04-21 | 遵义天磁锰业集团有限公司 | Preparation method of normal-temperature ferric oxide desulfurizer based on manganese metal liquid preparation |
| CN111411232A (en) * | 2020-03-11 | 2020-07-14 | 中南大学 | Total recovery method of valuable metal elements in positive pole piece of waste power lithium battery |
| CN114015899A (en) * | 2021-11-08 | 2022-02-08 | 田世超 | Method for treating manganese oxide ore by using hydroxyl combined liquid phase reduction |
| CN114162872A (en) * | 2021-12-31 | 2022-03-11 | 湖南烯富环保科技有限公司 | Method for preparing battery-grade manganese sulfate from manganese oxide ore |
| CN114737068A (en) * | 2022-03-17 | 2022-07-12 | 贵州金瑞新材料有限责任公司 | High-efficiency leaching method of high-grade pyrolusite |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN111041247A (en) * | 2019-12-11 | 2020-04-21 | 遵义天磁锰业集团有限公司 | Preparation method of normal-temperature ferric oxide desulfurizer based on manganese metal liquid preparation |
| CN111411232A (en) * | 2020-03-11 | 2020-07-14 | 中南大学 | Total recovery method of valuable metal elements in positive pole piece of waste power lithium battery |
| CN114015899A (en) * | 2021-11-08 | 2022-02-08 | 田世超 | Method for treating manganese oxide ore by using hydroxyl combined liquid phase reduction |
| CN114162872A (en) * | 2021-12-31 | 2022-03-11 | 湖南烯富环保科技有限公司 | Method for preparing battery-grade manganese sulfate from manganese oxide ore |
| CN114737068A (en) * | 2022-03-17 | 2022-07-12 | 贵州金瑞新材料有限责任公司 | High-efficiency leaching method of high-grade pyrolusite |
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