CN100537799C - The biological stirring of cobalt-containing sulfur concentrate soaked the cobalt novel process - Google Patents
The biological stirring of cobalt-containing sulfur concentrate soaked the cobalt novel process Download PDFInfo
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- CN100537799C CN100537799C CNB2006101441280A CN200610144128A CN100537799C CN 100537799 C CN100537799 C CN 100537799C CN B2006101441280 A CNB2006101441280 A CN B2006101441280A CN 200610144128 A CN200610144128 A CN 200610144128A CN 100537799 C CN100537799 C CN 100537799C
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Abstract
The present invention relates to biological stirring of cobalt-containing sulfur concentrate and soak the cobalt novel process.Cobalt-containing sulfur concentrate through fine grinding, washing reagent removal, size mixing, operations such as biological agitation leach, solid-liquid separation, deironing, heavy cobalt, obtain the cobaltous sulfide that market can be sold.In leaching process,, need keep 40～55 ℃ of temperature, pH value 1.2～1.8 and certain Fe concentration (1～15g/L) in the system in order to keep the high reactivity of bacterium.This technology can make full use of mineral wealth, improves the mine level of comprehensive utilization, saves cost, improves profit.Be particularly suitable for being applied to the exploitation of the sulphide ores resource that contains cobalt from far-off regions.
Description
Technical field
The present invention relates to a kind of novel process of utilizing moderate thermophile to have a liking for cobalt in the acidleach ore deposit bacterium agitation leach cobalt-containing sulfur concentrate, in the high efficiente callback sulphide ores valency cobalt metal arranged, improve the mine level of comprehensive utilization, belong to the microbial metallurgy technical field.
Background technology
Advantages such as cobalt is a kind of strategy metal, and it has the fusing point height, wear resistance is good, intensity is high, magnetic is good are the important source material of making various superalloys, magneticsubstance, anti-corrosion alloy.Be widely used in industry such as Aeronautics and Astronautics, electrical equipment, machinofacture, chemistry, pottery.China is the country that a cobalt resource lacks, and has the reserves of exploitation meaning only to be 3.9 ten thousand tons, and basic reserves also have only 5.98 ten thousand tons.The cobalt that present China extracts from import cobalt raw material and waste material accounts for 65% of ultimate production.
China's cobalt deposits lean ore is many, rich ore is few, and lacks independent cobalt deposits, and most of symbiosis or association are at present mainly extracted cobalt, as the recovery of Jinchuan company cobalt from the cobalt slag of nickel pyrometallurgical smelting system or import cobalt raw material.But also the cobalt-containing sulfur concentrate of some is put forward cobalt technology because low, the place of production of cobalt grade in remote, industrial foundation under-developed area, adopts traditional sulphur concentrate roasting relieving haperacidity-slag to leach, and sulfuric acid does not have purposes, is difficult to the realization commercial applications.For example, Qinghai Dare Buddhist nun copper cobalt ore is one have been verified to belong to and has contained the large-scale copper deposit of cobalt, is in remote highlands, and useful associated element cobalt wherein is main to coexist with sulphide ores such as pyrite.Copper-sulphide ores wherein adopts floatation process to reclaim, contain cobalt 0.02%～0.1% in the copper flotation tailings, obtain to contain the sulphur concentrate of cobalt 0.1%～1% again through flotation, this concentrate is put forward the cobalt art breading if adopt traditional sulphur concentrate roasting relieving haperacidity-slag to leach, can't solve vitriolic purposes problem, with profitless, still there is not the good plan utilization at present.Therefore,, be necessary to provide the cobalt in a kind of novel process recovery sulphur concentrate, further improve the mineral resources comprehensive utilization level in mine in order efficiently to utilize the cobalt resource in the sulphur concentrate.
Summary of the invention
The purpose of this invention is to provide a kind of from cobalt-containing sulfur concentrate biological agitation leach extract the novel process of cobalt, new technological flow is short, equipment province, simple to operate, energy consumption is lower, do not need through high melt, exhaust emission flue dust and sulfur dioxide gas can not realized the quick leaching and the high efficiente callback of cobalt.
For achieving the above object, the present invention by the following technical solutions: this cobalt-containing sulfur concentrate is biological to be stirred and soaks the cobalt novel process and may further comprise the steps:
(1), cobalt-containing sulfur concentrate is regrinded;
(2), the fine ore after the fine grinding in (1) is washed the reagent removal concentration;
(3), the ore pulp after concentration in (2) is added the sulphur acid for adjusting pH value, improve slurry temperature, inoculated bacteria and add the bacterial growth nutritive medium after pump into biological agitation leach system, carry out bacterial oxidation and leach;
(4), leach liquor constantly circulates, and after the leach liquor cobalt concentration reaches separation requirement, contains the cobalt leach liquor by the pre-deironing of lime carbonate, obtains the cobaltous sulfide product behind the heavy cobalt of sodium sulphite or Sodium sulfhydrate or hydrogen sulfide.
The moderate thermophile that novel process adopts is had a liking for acidleach ore deposit bacterium called after Sulfobacillusthermosulfidooxidans Retech-MTC-1, now deposited and be deposited in China national typical case culture collection center (Wuhan University in the school), preservation registration number CCTCC No:M206029.Preservation date on March 28th, 2006.The original paper that this culture collection is accepted letter of information is called in the application files of " chemistry of moderate thermophilic bacteria and low-grade primary copper sulfide ore and bio combined heap leaching method " for " 200610078976.6 " name at application number.
The pulp density of biological agitation leach is 15%～35%, and slurry pH is 1.2～1.8 in the leaching process, and extraction temperature is controlled between 40～55 ℃, needs in the leaching process to charge in retort to be rich in O
2Air with carbonic acid gas.
Described cobalt-containing sulfur concentrate can be and contains cobalt yellow iron ore concentrate;
Described biological agitation leach ore pulp is after solid-liquid separation, and parting liquid can return the lean solution pond.
Leach liquor in the lean solution pond need carry out lime carbonate preliminary sedimentation iron according to its pH value, iron concentration in leaching working cycle.
The bacterial growth temperature is 40～50 ℃.
In leaching process,, need keep 40～55 ℃ of temperature, pH value 1.2～1.8 and certain Fe concentration (1～15g/L) in the system in order to keep the high reactivity of bacterium.
Current potential mv (SCE) described in the present invention is a reference mode measuring the redox reaction solution potential, and promptly measured potential value is the observed value with respect to saturated calomel electrode.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Fig. 2 is the embodiments of the invention schema
Be the cobalt in the comprehensive utilization cobalt-containing sulfur concentrate, the present invention adopts following design (seeing Fig. 1):
Among Fig. 1, cobalt-containing sulfur concentrate is carried out fine grinding 1 process, so that the mineral disaggregation degree reaches the subsequent treatment worker The requirement of skill;
Cobalt-containing sulfur concentrate after the fine grinding concentrates 2 through concentrator, and overflow enters sewage disposal system, the end after concentrating Flow to into 3 operations of sizing mixing.
The high-concentration ore slurry that is come by concentrator carries out the preconditioning of pH value, preconditioning by adding dilution heat of sulfuric acid After pH value scope between 1.6～1.8, pulp density 20%～40% after regulating. Ore deposit after the preconditioning Add the high concentration bacterial solution of 10%～30% (v/v) in the slurry, the bacteria concentration of high concentration bacterial solution is 107～109/ml; In addition, (for example, ammonium sulfate 1～3g/L) to need to add the nitrogenous source that supplies bacterial growth (for example, potassium dihydrogen phosphate 0.1～0.5g/L) with the phosphorus source. The pan feeding pulp density that connects behind the bacterium of sizing mixing is 15 %～35% (w/w).
Cobalt-containing sulfur concentrate after sizing mixing enters biological stirring leaching system 4, carries out bacterial oxidation and soaks the cobalt processing. The pH of each leaching tanks is controlled between 1.2～1.8 in the leaching process, pulp potential be controlled at 450mv～600mv (SCE), slurry temperature remains on 40 ℃～50 ℃ by cooling or mode of heating, in the ore pulp Oxyty keeps〉4mg/L, the carbon dioxide solubility amount keeps〉15mg/L. In addition, also need the periodic monitoring ore pulp In bacterial concentration, make bacterial concentration by adjusting pH value, temperature or throughput〉106Individual/ml.
Bacterial oxidation soaks ore pulp behind the cobalt through concentrating underflow 7 operations after filtration again after 5, realizes Separation of Solid and Liquid, Filter residue enters the tailingspile; Concentrate overflow and filtrate and all enter lean solution pond 8.
Liquid in the lean solution pond is for containing bacteria liquid, and partially liq returns and sizes mixing, inoculation system, carries out bacterium and stirs Mix oxidation and soak the cobalt circulation. After the cobalt concentration in the lean solution pond reached processing requirements, extracting wherein, liquid entered richness Liquid pool 9; Cobalt-carrying solution in the rich solution pond carries out deironing 10, heavy cobalt 11 is processed; Contain the cobalt sediment through solid-liquid Obtain the cobalt product that can sell after the separation, parting liquid returns lean solution pond 8.
Cobalt content in the above-described cobalt-containing sulfur concentrate〉0.1%, the mog of cobalt-containing sulfur concentrate is less than 76 Micron concentrates the underflow solid concentration greater than 50% (w/w), and the part of sizing mixing bacterial load is 10%～30 % (v/v), the pulp density that biological stirring leaches is 15%～35% (w/w), biological stirring leaches Time is 3～10 days, cobalt leaching rate 〉=80%, and the leachate of producing the cobalt product contains cobalt 〉=2g/L. Adopt carbonic acid Calcium is deironing in advance, and the vulcanized sodium precipitate cobalt obtains the cobalt sulfide product that can sell in market.
Embodiment
The invention will be further described below in conjunction with embodiment.
For example, western certain copper mine of China is the sulfuration mineral deposit that contains a large amount of pyrite, association little cobalt, and the The copper thing is a chalcopyrite, and secondary copper sulfide mineral and copper oxide ore content are less; The process mineralogy analysis revealed does not have independently cobalt mineralss in the ore, element cobalt is sneaked in the pyrites with the isomorph form.This ore deposit copper average content is 1.6%, and the sulphur average content is 36%, and the cobalt average content is 0.1%, and main gangue mineral is quartz, feldspar, chlorite, sericite and carbonate minerals.
(1) as shown in Figure 2, the raw ore of mining behind the copper in the recovery ore, obtains the mine tailing A that high-sulfur contains cobalt through operations such as broken grinding flotations.The mine tailing that high-sulfur is contained cobalt carries out sulphur flotation 13 with flotation machine, obtains containing the sulphur concentrate C of cobalt 1%; Flotation tailings B sends into the mine tailing storehouse.
(2) according to the size-grade distribution situation and the ore grinding testing data of cobalt-containing sulfur concentrate, carry out ball mill ore grinding 2 and handle, make the granularity of cobalt-containing sulfur concentrate less than 38 microns.
(3) cobalt-containing sulfur concentrate concentrates overflow E and enters Sewage treatment systems after three-tray thickener countercurrent washing reagent removal concentrates 2 behind the ore grinding, and the pulp density that concentrates underflow D reaches 65% and enters the pond of sizing mixing and size mixing 3.
(4) concentrate underflow D and in the pond 3 of sizing mixing, cultivate the bacterium leach liquor that contains that bacterium liquid F, the lean solution pond 8 of cultivating in workshop 12 returns and mix, obtain pH1.2～1.8 with dilute sulphuric acid, bacteriotrophy liquid, bacterium, solids concn be about 20% contain the bacterium ore pulp.
(5) contain the bacterium ore pulp and enter in the biological agitation leach jar and leach 4, through plural serial stage bioaeration agitation leach 5 days, the leaching yield of cobalt reached 95%.The ore pulp that bacterium is leached after finishing is sent into three-tray thickener concentrated 5.In the biological agitation leach process, need in monitoring slurry pH, pulp potential, ore pulp dissolved oxygen amount, ore pulp carbonic acid gas meltage, slurry temperature and the ore pulp parameters such as bacteria content.The pH value of ore pulp is controlled between 1.2～1.8, pulp potential is controlled at 450mv～600mv (SCE), slurry temperature remains on 40 ℃～50 ℃ by cooling or type of heating, oxyty in the ore pulp keeps〉4mg/L, the carbonic acid gas meltage keeps〉15mg/L, make the interior bacterium of agitation leach jar keep higher oxidation activity and growth activity, finally obtain high cobalt leaching yield.
(6) leach ore pulp after thickener concentrates 5, overflow H enters lean solution pond 8, and underflow G enters pressure filter and filters 7.
(7) pressure filter filters the 7 filter cake I that produce and sends into the tailings area, and filtrate J returns lean solution pond 8, and the bacterium ore leachate that contains in the lean solution pond 8 returns the pond of sizing mixing.
(8) after the cobalt concentration in the lean solution pond 8 reaches 2g/L, extract its liquid and enter rich solution pond 9.Solution in the rich solution pond obtains the cobaltous sulfide product through Na2S precipitation operation 11 again through precipitation of calcium carbonate iron removal step 10.The cobaltous sulfide product contains cobalt and reaches more than 10%.
(9) ore immersion bacterial culture that adopted of the biological agitation leach novel process of this cobalt-containing sulfur concentrate is that culture of isolated is come out the bacterial classification behind the domestication and improvement of laboratory from certain high-sulfur mining area pit water.Confirming as the moderate thermophile acidophilic bacteria through biological assay, is the Sulfobacillus class.The inorganic salt composition of the substratum of this bacterium is: (NH
1)
2SO
40.5g/L, KCl 0.1g/L, K
2HPO
40.2g/L, MgSO
47H
2O 0.5g/L, Ca (NO
3)
20.01g/L, yeast extract 0.02%; Energy matrix is: simple substance S.The domestication of bacterium is to add granularity less than 76 microns cobalt-containing sulfur concentrate breeze in containing the tap water of above-mentioned nutritive substance, and adding the pulp density that forms behind the ore powder is 1～20% weight percent, and the pH value is between 1.5～2.5; The redox potential of domestication bacterium liquid is 550～650mV (SCE), and bacterial concentration is 10
7～10
9Individual/ml; Described bacterial growth temperature is 4～55 ℃, 45～50 ℃ of optimum growth temps.The moderate thermophile that is adopted in the present embodiment is had a liking for acidleach ore deposit bacterium called after Sulfobacillus thermosulfidooxidans Retech-MTC-1, now deposited and be deposited in China national typical case culture collection center (Wuhan University in the school), preservation registration number CCTCC No:M206029.Preservation date on March 28th, 2006.
Effect of the present invention is: open up the New Process for Treatment of cobalt-containing sulfur concentrate, take full advantage of the cobalt of remote districts Resource improves the mineral resources comprehensive utilization level, reduces environmental pollution, increases economic efficiency. Spy of the present invention Be not fit to be applied to the exploitation of the sulphide ore resource that contains cobalt of remote districts, the western plateau of China.
Claims (9)
1, the biological stirring of a kind of cobalt-containing sulfur concentrate soaked the cobalt novel process, and it is characterized in that: it may further comprise the steps:
(1), cobalt-containing sulfur concentrate is regrinded;
(2), the fine ore after the fine grinding in (1) is washed the reagent removal concentration;
(3), the ore pulp after concentration in (2) is added the sulphur acid for adjusting pH value, improve slurry temperature, inoculated bacteria and add the bacterial growth nutritive medium after pump into biological agitation leach system, carry out bacterial oxidation and leach;
(4), leach liquor constantly circulates, and after the leach liquor cobalt concentration reaches separation requirement, contains the cobalt leach liquor by the pre-deironing of lime carbonate, obtain sulfuration behind the heavy cobalt of sodium sulphite or Sodium sulfhydrate or hydrogen sulfide and bore product.
2, the biological stirring of cobalt-containing sulfur concentrate according to claim 1 soaked the cobalt novel process, it is characterized in that: used bacterium is that moderate thermophile is had a liking for acidleach ore deposit bacterium, its called after sulfobacillus thermosulfidooxidansRetech-MTC-1, now deposited and be deposited in China national typical case culture collection center, the address: Wuhan University in the school, preservation registration number CCTCC No:M206029, preservation date on March 28th, 2006, it is that culture of isolated is come out from the pit water of high-sulfur mining area that this moderate thermophile is had a liking for acidleach ore deposit bacterium, and the bacterial classification behind the domestication and improvement of laboratory, the inorganic salt composition of the substratum of this bacterium is: (NH
4)
2SO
40.5g/L, KCl 0.1g/L, K
2HPO
40.2g/L, MgSO
47H
2O 0.5g/L, Ca (NO
3)
20.01g/L, yeast extract0.02%; Energy matrix is: simple substance S; The domestication of bacterium is to add granularity less than 76 microns cobalt-containing sulfur concentrate breeze in containing the tap water of above-mentioned nutritive substance, and the pulp density that adds behind the cobalt-containing sulfur concentrate breeze is the 1-20% weight percent, and the pH value is between 1.5～2.5; The redox potential of domestication bacterium liquid is 550～650mV, and with respect to the observed value of saturated calomel electrode, bacterial concentration is 10
7～10
9Individual/ml; Described bacterial growth temperature is 4～55 ℃.
3, the biological stirring of cobalt-containing sulfur concentrate according to claim 1 and 2 soaked the brill novel process, it is characterized in that: the pulp density of its biological agitation leach is 15%～35%, slurry pH is 1.2～1.8 in the leaching process, extraction temperature is controlled between 40～55 ℃, needs in the leaching process to charge in retort to be rich in O
2Air with carbonic acid gas.
4, bore biological stirring of sulphur concentrate and soak the cobalt novel process according to claim 1 and 2 containing, it is characterized in that: described cobalt-containing sulfur concentrate is for containing cobalt yellow iron ore concentrate.
5, the biological stirring of cobalt-containing sulfur concentrate according to claim 1 and 2 soaked the brill novel process, and it is characterized in that: cobalt contents is greater than 0.1% in the described cobalt-containing sulfur concentrate.
6, the biological stirring of cobalt-containing sulfur concentrate according to claim 1 and 2 soaked the brill novel process, and it is characterized in that: described cobalt-containing sulfur concentrate is after fine grinding, and the granularity of its ore grinding is less than 76 microns.
7, the biological stirring of cobalt-containing sulfur concentrate according to claim 1 and 2 soaked the cobalt novel process, and it is characterized in that: described biological agitation leach ore pulp is after solid-liquid separation, and parting liquid returns the lean solution pond.
8, the biological stirring of cobalt-containing sulfur concentrate according to claim 1 and 2 soaked the cobalt novel process, and it is characterized in that: the leach liquor in the lean solution pond need carry out lime carbonate preliminary sedimentation iron according to its pH value, iron concentration in leaching working cycle.
9, the biological stirring of cobalt-containing sulfur concentrate according to claim 2 soaked the cobalt novel process, it is characterized in that described bacterial growth temperature is 40～50 ℃.
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| CN102173399B (en) * | 2011-03-08 | 2012-11-21 | 武汉工程大学 | Method for dissolving mid-low-grade rock phosphate by utilizing thermoacidophile |
| CN102618720B (en) * | 2012-04-28 | 2014-05-21 | 长沙有色冶金设计研究院有限公司 | Method for backwash leaching and washing mineral leached materials |
| CN102764692A (en) * | 2012-07-13 | 2012-11-07 | 北京科技大学 | Superfine tailing fluidized mining and bacterial leaching system and technology |
| CN103397181B (en) * | 2013-08-07 | 2015-03-04 | 中国地质科学院矿产综合利用研究所 | Recovery process of associated metal elements in iron ore |
| CN103572048B (en) * | 2013-11-19 | 2015-07-01 | 东北大学 | Method of cobalt leaching with activated carbon catalysis bacteria |
| CN103572049B (en) * | 2013-11-19 | 2015-07-01 | 东北大学 | Bacterium agitation leaching method of cobalt concentrate |
| CN103572050B (en) * | 2013-11-19 | 2015-11-11 | 东北大学 | A kind of biological selectivity leaching method of low-grade copper cobalt ore |
| CN107739822A (en) * | 2017-10-17 | 2018-02-27 | 辽宁石油化工大学 | A kind of method of silver ion catalysis copper cobalt sulfide ore Bioleaching |
| CN107739823A (en) * | 2017-10-17 | 2018-02-27 | 辽宁石油化工大学 | A kind of method of surfactant and silver ion concerted catalysis copper cobalt sulfide ore Bioleaching |
| CN108998396B (en) * | 2018-08-28 | 2019-07-30 | 中南大学 | A kind of cultural method of iron oxidation leaching microbacteria |
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Non-Patent Citations (2)
| Title |
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| 低品位矿石微生物浸出作用机理研究. 尹升华，吴爱祥，苏永定.矿冶，第15卷第2期. 2006 |
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