CN104131182A - Reduction leaching method for separating manganese and silver in manganese silver concentrate - Google Patents
Reduction leaching method for separating manganese and silver in manganese silver concentrate Download PDFInfo
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- CN104131182A CN104131182A CN201410363050.6A CN201410363050A CN104131182A CN 104131182 A CN104131182 A CN 104131182A CN 201410363050 A CN201410363050 A CN 201410363050A CN 104131182 A CN104131182 A CN 104131182A
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Abstract
The invention discloses a reduction leaching method for separating manganese and silver in a manganese silver concentrate, and belongs to the technical field of preparation of manganese sulfate for electrolysis. The reduction leaching method is mainly achieved through the following steps: (1) dissolving a certain amount of sodium metabisulfite into a certain amount of water; and (2) slowly adding the sodium metabisulfite solution into a manganese silver concentrate pulp, stirring and carrying out a reduction reaction in an acidic medium, after completion of the reduction reaction, filtering, carrying out solid-liquid separation, and thus respectively obtaining a manganese-containing solution and a silver-containing ore mud. The subsequent manganese leached solution is subjected to deep purification and impurity removal to prepare a pure manganese sulfate solution, and the sliver-enriched residue is subjected to silver extraction by an ammoniacal thiosulfate method. The selected reducing agent has strong reducibility, the reaction required temperature is low, the output waste residue amount is small, the reaction time is short, the purification and impurity removal cost of the manganese leached solution is low, requirements on equipment are low, and the reaction process is controllable. The clear, environmental-protection and high-efficiency production process is provided for comprehensive utilization of manganese silver ore resources in China.
Description
Technical field
The invention belongs to electrolysis manganous sulfate preparing technical field, relate in particular to and a kind of manganese silver in mn-ag concentrate is carried out to separated acids reduction leaching method.
Background technology
Manganese-silver ore is the potential valuable source of Chinese precious metal industry.The general manganese content 3%～5% of domestic manganese-silver ore raw ore, silver content is tens of to number kg/ton, has verified silver-colored reserves and has added up to nearly ten thousand tons.Manganese-silver ore is one of difficult complicated mineral intergrowth of generally acknowledging, domestic existing enterprise is raw materials used mostly is the mineral (Ag ﹥ 400g/t) higher to silver content, technique mainly be take Extracting Ag by cyanidation as main, but due to isomorphous reason, the rate of recovery of silver is lower, be only 10%～50%, China's manganese carbonate ore resource has faced exhaustion at present, and electrolytic manganese industry will progressively enter the common stage of utilizing of two kinds of resources of manganese carbonate ore and manganese-silver ore.Therefore researching and developing high-efficiency cleaning soaks preparation of manganese China is had to huge environment and economy meaning.
Extract manganese-silver ore object space method and mainly contain pyrogenic process and wet method, because thermal process energy consumption is high, it is large to pollute, seriously less use now of waste.Patents has CN100564551C.Wet processing manganese-silver ore is current main flow technique.Manganese-silver ore Leaching mechanism is fairly simple.Under acidic conditions, utilize the oxidisability of manganese, by adding suitable reductive agent to be reduced leaching.The selection of reductive agent is the emphasis of leaching of manganese.
Existing reductive agent mainly divides two large class, organic reductive agent and mineral-type reductive agents.The advantage of using organic waste to make reductive agent as stalk, waste molasses, bagasse etc. is that environmental protection, cost are low, and shortcoming is that raw material is difficult for transportation, and the manganese sulfate solution of production contains the organism small-particle that is difficult to Ex-all.Patents has CN100451139C.Mineral-type reductive agent has pyrite, sulfurous gas, sulphite, hydrogen peroxide etc.The advantage of using pyrite to make reductive agent is that cost is low, and leaching yield is high, is to apply at present more reductive agent.Shortcoming is that speed of response is slow; Owing to introducing pyrite, increased the foreign matter content that the quantity of slag and manganous sulfate leach liquor, and then increased the cost of later purification removal of impurities; And pyrite can react with sulfuric acid under sour environment, cause acid consumption and follow-up removal of impurities operation reagent consumption to increase, if control improperly, have hydrogen sulfide and overflow.Patents has CN103422118A, CN101845562B, CN101456595A, CN103233119A etc.Use sulfurous gas do reductive agent advantage be Well-recovered, leaching yield is high, shortcoming is that gas is difficult for obtaining, transportation is difficulty comparatively, and sulfurous gas easily overflows and can worsen working condition contaminate environment.Patents has CN1079258A, CN102634819A.
Summary of the invention
The present invention, in order to solve prior art deficiency, provides a kind of manganese silver in mn-ag concentrate has been carried out to separated acids reduction leaching method.Present method is utilized Sodium Pyrosulfite (Na
2s
2o
5) as reductive agent, its reductibility is strong, raw material is easy to get; The method reaction process is controlled, reacts temperature required low; Do not introduce new impurity, the cost of later purification removal of impurities greatly reduces.
For realizing object of the present invention, adopt following methods:
Manganese silver in mn-ag concentrate is carried out to a separated acids reduction leaching method, and step is as follows:
1, preparation metabisulfite solution;
2, to high intensity magnetic separation gained particle diameter, be to add water and the vitriol oil in 200 ± 50 object mn-ag concentrate breezes, stir and form after ore pulp, again the sodium metabisulfite solution preparing is joined in mn-ag concentrate ore pulp, stir reduction reaction occurs, keep slurry pH 2 to 4, slurry temperature is 15 ℃ to 50 ℃, and extraction time is 2 to 5 hours;
Wherein, vitriol oil addition is that breeze per ton adds 60kg to 150kg, the liquid-solid mass ratio of the cumulative volume of the vitriol oil and water and breeze is 2:1 to 5:1, Sodium Pyrosulfite add-on is that breeze per ton adds 100kg to 300kg, and the water of preparation sodium metabisulfite solution is 1:4 to 1:1 with adding the volume ratio of the water in breeze;
3,, after reduction reaction completes, filtration, solid-liquid separation, obtain respectively manganese containing solution and argentiferous sludge.
By aforesaid method, the manganese silver of mn-ag concentrate is carried out to separation, manganese leaching yield is in 95% left and right, and silver loss is no more than 2%.The follow-up manganese liquid that soaks is prepared pure manganese sulfate solution through deep purifying removal of impurities, and rich silver-colored slag is used ammoniac thiosulfate method desilver.
The invention has the advantages that:
1, Sodium Pyrosulfite has plurality of advantages as reductive agent.In chemical property, Sodium Pyrosulfite reductibility is better than sulphite and sulfurous gas, and raw material is easy to get; Reaction process is controlled, reacts temperature required low; In reaction process, can not overflow sulfur dioxide gas; Do not introduce new impurity, the cost of later purification removal of impurities greatly reduces.
2, the inventive method can be carried out effective separation to the manganese silver of mn-ag concentrate, and manganese leaching yield is in 95% left and right, and silver loss is no more than 2%.
3, to react output waste residue amount little in the present invention, and the reaction times is short, soaks manganese liquid purification and impurity removal cost low, to plant and instrument, requires low.For China comprehensive utilization manganese-silver ore Resource Supply a kind of environmental protection, efficient, cost are low is expected to realize industrialized production method.
Embodiment
In following examples, all ingredients is commercial industrial goods.
Embodiment 1
Domestic certain mn-ag concentrate, containing manganese 10.3%, silver-colored 243g/t, mineral grain grade 200 ± 50 orders.
Preparation metabisulfite solution; Get again 10 kilograms of these manganese-silver ore powder, add the vitriol oil and water, stir and form after ore pulp, the sodium metabisulfite solution preparing is joined in ore pulp and stirred, Sodium Pyrosulfite addition is 100 kg/t, vitriol oil addition is 60kg/t, liquid-solid ratio is 2:1, and the water of preparation sodium metabisulfite solution is 1:1 with adding the volume ratio of water in manganese-silver ore powder, keeps slurry pH 3.5 to 4, extraction temperature is 35oC, time 2 h; After reduction reaction completes, filtration, solid-liquid separation, obtain respectively manganese containing solution and argentiferous sludge.
Utilize equipment I CP (inductively coupled plasma spectrum generator) to carry out atomic absorption method detection to manganese containing solution, the leaching yield of manganese reaches 90.3%, and in manganese leach liquor, manganese content is 25.0g/L.
Embodiment 2
Manganese oxide ore is identical with embodiment 1.Domestic certain mn-ag concentrate, containing manganese 10.3%, silver-colored 243g/t, mineral grain grade 200 ± 50 orders.
Preparation metabisulfite solution; Get again 10 kilograms of these manganese-silver ore powder, add the vitriol oil and water, stir and form after ore pulp, sodium metabisulfite solution is joined in ore pulp and stirred, Sodium Pyrosulfite addition is 200kg/t, vitriol oil addition is 105kg/t, liquid-solid ratio is 3.5:1, and the water of preparation sodium metabisulfite solution is 1:2.5 with adding the volume ratio of water in manganese-silver ore powder, keeps slurry pH 3 to 3.5, extraction temperature is 15oC, 3.5 hours time; After reduction reaction completes, filtration, solid-liquid separation, obtain respectively manganese containing solution and argentiferous sludge.
Utilize equipment I CP (inductively coupled plasma spectrum generator) to carry out atomic absorption method detection to manganese containing solution, the leaching yield of manganese can reach 96.5%, and manganese leach liquor manganese content is 30g/L.
Embodiment 3
Domestic certain mn-ag concentrate, containing manganese 20.54%, silver-colored 354g/t, mineral grain grade 200 ± 50 orders.
Preparation metabisulfite solution; Get again 10 kilograms of these manganese-silver ore powder, add the vitriol oil and water, stir and form after ore pulp, sodium metabisulfite solution is joined in ore pulp and stirred, Sodium Pyrosulfite addition is 300kg/t, vitriol oil addition is 150kg/t, liquid-solid ratio is 5:1, and the water of preparation sodium metabisulfite solution is 1:4 with adding the volume ratio of water in manganese-silver ore powder, keeps slurry pH 2 to 2.5, extraction temperature is 50oC, 5 hours time; After reduction reaction completes, filtration, solid-liquid separation, obtain respectively manganese containing solution and argentiferous sludge.
Utilize equipment I CP (inductively coupled plasma spectrum generator) to carry out atomic absorption method detection to manganese containing solution, the leaching yield of manganese can reach 95.5%, and manganese leach liquor manganese content is 36g/L.
Claims (4)
1. manganese silver in mn-ag concentrate is carried out to a separated acids reduction leaching method, it is characterized in that, step is as follows:
Preparation metabisulfite solution; In mn-ag concentrate breeze, add water and the vitriol oil again, stir and form after ore pulp, the sodium metabisulfite solution preparing is joined in ore pulp, stir reduction reaction occurs; After reduction reaction completes, filtration, solid-liquid separation, obtain respectively manganese containing solution and argentiferous sludge.
2. according to claim 1ly a kind of manganese silver in mn-ag concentrate is carried out to separated acids reduction leaching method, it is characterized in that, the particle diameter of mn-ag concentrate breeze is 200 ± 50 orders.
3. according to claim 1ly a kind of manganese silver in mn-ag concentrate is carried out to separated acids reduction leaching method, it is characterized in that, vitriol oil addition is that breeze per ton adds 60kg to 150kg, the liquid-solid mass ratio of the cumulative volume of the vitriol oil and water and breeze is 2:1 to 5:1, Sodium Pyrosulfite add-on is that breeze per ton adds 100kg to 300kg, and the water of preparation sodium metabisulfite solution is 1:4 to 1:1 with adding the volume ratio of the water in breeze.
4. according to claim 1ly a kind of manganese silver in mn-ag concentrate is carried out to separated acids reduction leaching method, it is characterized in that, the condition of described generation reduction reaction is: keep slurry pH 2 to 4, slurry temperature is 15 ℃ to 50 ℃, and extraction time is 2 to 5 hours.
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| CN201410363050.6A CN104131182A (en) | 2014-07-28 | 2014-07-28 | Reduction leaching method for separating manganese and silver in manganese silver concentrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106636667A (en) * | 2016-12-23 | 2017-05-10 | 中南大学 | Method for recycling manganese and silver from manganese-silver ores |
| CN111286603A (en) * | 2020-03-25 | 2020-06-16 | 内蒙古金山矿业有限公司 | Process for recovering silver and co-producing manganese sulfate from manganese-containing silver ore |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1079258A (en) * | 1993-04-07 | 1993-12-08 | 核工业中南地质勘探局230研究所 | Produce manganous sulfate and extract silver-colored method from manganese-silver ore |
| CN101831544A (en) * | 2010-05-18 | 2010-09-15 | 中国地质科学院郑州矿产综合利用研究所 | Method for separating manganese and silver from manganese-silver ore and purifying manganese leaching solution to extract manganese sulfate |
| CN101886168A (en) * | 2010-07-14 | 2010-11-17 | 广西大学 | Extract technology of semi-manganese oxide ore |
| CN103014779A (en) * | 2012-03-18 | 2013-04-03 | 英德佳纳金属科技有限公司 | Multistage ore slurry decomposition-electrodeposition cell and decomposition-electrodeposition combined technique |
| CN103320622A (en) * | 2013-07-18 | 2013-09-25 | 海南金亿新材料股份有限公司 | Technological process for preparing electronic-grade nickel methylsulfonate by utilization of nickel waste material |
| CN103882226A (en) * | 2014-04-14 | 2014-06-25 | 北京矿冶研究总院 | Economic, clean and simple method for leaching cobalt from high-valence cobalt oxide |
-
2014
- 2014-07-28 CN CN201410363050.6A patent/CN104131182A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1079258A (en) * | 1993-04-07 | 1993-12-08 | 核工业中南地质勘探局230研究所 | Produce manganous sulfate and extract silver-colored method from manganese-silver ore |
| CN101831544A (en) * | 2010-05-18 | 2010-09-15 | 中国地质科学院郑州矿产综合利用研究所 | Method for separating manganese and silver from manganese-silver ore and purifying manganese leaching solution to extract manganese sulfate |
| CN101886168A (en) * | 2010-07-14 | 2010-11-17 | 广西大学 | Extract technology of semi-manganese oxide ore |
| CN103014779A (en) * | 2012-03-18 | 2013-04-03 | 英德佳纳金属科技有限公司 | Multistage ore slurry decomposition-electrodeposition cell and decomposition-electrodeposition combined technique |
| CN103320622A (en) * | 2013-07-18 | 2013-09-25 | 海南金亿新材料股份有限公司 | Technological process for preparing electronic-grade nickel methylsulfonate by utilization of nickel waste material |
| CN103882226A (en) * | 2014-04-14 | 2014-06-25 | 北京矿冶研究总院 | Economic, clean and simple method for leaching cobalt from high-valence cobalt oxide |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106636667A (en) * | 2016-12-23 | 2017-05-10 | 中南大学 | Method for recycling manganese and silver from manganese-silver ores |
| CN106636667B (en) * | 2016-12-23 | 2018-10-09 | 中南大学 | A method of recycling manganese and silver from manganese-silver ore |
| CN111286603A (en) * | 2020-03-25 | 2020-06-16 | 内蒙古金山矿业有限公司 | Process for recovering silver and co-producing manganese sulfate from manganese-containing silver ore |
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Application publication date: 20141105 |