CN100595297C - Gold extraction process with low pollution and high recovery for refractory gold concentrate - Google Patents
Gold extraction process with low pollution and high recovery for refractory gold concentrate Download PDFInfo
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- CN100595297C CN100595297C CN200810050799A CN200810050799A CN100595297C CN 100595297 C CN100595297 C CN 100595297C CN 200810050799 A CN200810050799 A CN 200810050799A CN 200810050799 A CN200810050799 A CN 200810050799A CN 100595297 C CN100595297 C CN 100595297C
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Abstract
The invention relates to a process for extracting gold of refractory gold concentrates with low pollution and high recovery rate, belonging to the metallurgical process class. The process proposal which combines organically the bacterial oxidation technology with the microwave irradiation technology comprises the following steps of: oxidizing and decomposing sulfide minerals by means of the bacterial oxidation technology first; exposing and dissociating sufficiently the gold; oxidizing a large part of sulfur and arsenic to enter a liquid-phase; carrying out the neutralization treatment to theoxidizing liquid and returning to use; roasting oxidizing slag with microwave at the low temperature; and removing organic carbon in ore. The process solves completely the problem of absorbing the gold in the subsequent cyaniding gold extraction work. The process has high recovery rate of the gold and less environment pollution, is easy to automatically control and saves energy.
Description
Technical field
The present invention relates to a kind of technology of refractory gold ore, particularly a kind of golden ore concentrate hard to treat gold extraction technology of low pollution and high recovery.
Background technology
As everyone knows, along with the fast development of gold industry, be easy to the gold ore resource exhaustion day by day that direct cyaniding is extracted, the difficult-treating gold mine resource has become the main raw material of gold industry from now on.This type of ore shared proportion in explored gold geologic reserve is increasing, extensively is distributed in areas such as the Liao Dynasty, Hunan, osmanthus, Guizhou Province, sweet, river, Anhui, Ji.Its distinguishing feature is exactly that golden form with microfine and parcel is present in pyrite or the arsenopyrite lattice, and contain more interference and leach element, clay class mineral as arsenic, sulphur, antimony, organic carbon or other ADSORPTION OF GOLD cyano complexs, leach the gold that can not reclaim effectively wherein with traditional cyaniding, a difficult problem has become international.Therefore, seeking new refractory gold ore and carry technology for gold and accomplish that resource and environment is unified mutually, is the task of top priority of gold industry.
The development and use of China's difficult-treating gold mine have obtained very big progress in recent years; wherein oxidizing roasting and bio-oxidation pre-treatment indissoluble gold ore deposit have obtained application industrial; but along with the increasingly stringent of various countries to environmental protection requirement; adopt traditional this part gold ore resource of fire metallurgy process technical finesse; reason owing to ore and technology itself; the inevitable sulfurous gas that produces; obnoxious flavour such as arsenic oxide arsenoxide and mercuryvapour; have a strong impact on ecotope; the requirement of protection is difficult to conform; and merely adopt bio-oxidation technology can not solve organic carbon in the ore " robbing gold " effectively; therefore seek new refractory mineral gold extraction technology; fundamentally eliminating environmental pollution, is the gold industry urgent problem.
Summary of the invention
The object of the present invention is to provide a kind of golden ore concentrate hard to treat gold extraction technology of low pollution and high recovery, not only solved the problem of oxidation of sulfide, charcoal material; Gold is fully exposed to be dissociated, make that sulphur, arsenic are most of to enter liquid phase after oxidized, thoroughly solved the problem of ADSORPTION OF GOLD in the follow-up cyaniding operation, this technology has improved the golden rate of recovery, reduced environmental pollution, be easy to automatization control, thereby this part difficult-treating gold mine resource can be made full use of.
Technical scheme of the present invention is: bio-oxidation technology and microwave irradiation technology in the gold metallurgy are combined, utilize bio-oxidation technology earlier, the oxygenolysis sulfide mineral, gold is fully exposed to be dissociated, sulphur, enter liquid phase after the arsenic major part is oxidized, material for next step operation output cleaning, oxidation liquid returns use through neutralizing treatment, oxidation sludge adopts the microwave low-temperature bake, remove the organic carbon in the ore, thoroughly solved the problem of ADSORPTION OF GOLD in the subsequent oxidation operation, therefore this technology has improved the golden rate of recovery, reduced again the pollution of environment and easily automatization control, thereby this part unmanageable gold ore resource is fully used, turned waste into wealth.
Know-why of the present invention is:
1, bio-oxidation ultimate principle:
The parcel gold mineral is mainly metallic sulfides such as pyrite and arsenopyrite in the refractory gold ore; The biological oxidation gold extraction technology utilizes leaching microbacteria that metallic sulfide oxidation is decomposed exactly, and enters liquid phase with the form of soluble sulphate; Main pollution-producing arsenic in the ore utilizes lime iron salt method neutralizing treatment after entering liquid phase with the ionic form again, forms the precipitation of stable ferric arsenate, and qualified discharge can not pollute environment;
The used bacterial species of bio-oxidation is a lot, and their common feature is to be that carbon source is grown, bred as the energy, with the carbonic acid gas with oxidation pyrite, white pyrite, pyrrhotite, mispickel and other metallic sulfides; It can finally be oxidized to ferric iron, sulphur finally is oxidized to sulfuric acid and vitriol, arsenic finally is oxidized to pentavalent arsenic at the iron in the suitable following mineral of condition; It also can be oxidized to sulfuric acid or vitriol to the elementary sulfur that occurs, thiosulphate (reduced sulfur) in chemical reaction, be oxidation of divalent ferric iron; These oxidizing reactions are called direct oxidation;
The product Fe of bacterial oxidation
+++And H
2SO
4Can also and make its decomposition with the metallic sulfide reaction; This chemical reaction is called indirect oxidation; In the product of indirect oxidation, do not reach the maximum valency, can be reached the maximum valency by bacterial oxidation again;
Bacterial oxidation does not need carrying the gold mineral complete oxidation and entering solution, gold is come out and don't skeleton structure that completely destroy carries gold mineral, more helps next step solid-liquid separation and cyaniding operation; Because the chemical reaction velocity of bacterial oxidation is slower, long reaction time is compared the easier control of oxidation depth with pressurization preoxidation with the roasting pre-oxidation process;
(1) direct oxidation
Direct oxidation is meant that bacterium direct oxidation on mineral surface decomposes mineral and continue intermediate oxidation product, makes As, Fe, S all be oxidized to chemical maxivalence; Can bacterium direct oxidation decompose mineral on mineral surface, these chemical equations can be regarded as the net result of bacterial oxidation reaction;
(2) indirect oxidation
Indirect oxidation is meant that sulfide mineral is not decomposed by the bacterium direct oxidation, but by the product Fe of bacterial oxidation
3+And H
2SO
4Oxygenolysis; In bio-oxidation process, the oxygenolysis of sulfide mineral mainly (or all being) is finished by indirect oxidation; These chemical equations have:
FeS
2+3Fe
2(SO
4)
3+3H
2O＝6FeSO
4+FeS
2O
3+3H
2SO
4
4FeAsS+4Fe
2(SO
4)
3+6H
2O+3O
2＝12FeSO
4+4H
3AsO
3+4S
FeS+Fe
2(SO
4)
3＝3FeSO
4+S
(3) bacterial oxidation Fe
++With unsaturated attitude sulphur, arsenic
The topmost effect of bacterial oxidation is an Oxidation of Fe
2+With unsaturated attitude sulphur, arsenic; This oxidation rate than do not have under the situation of bacterium fast a lot; In bio-oxidation process, the effect of bacterium is mainly reflected in the following chemical equation:
At present, the arsenic-containing acid waste water that biological oxidation gold extraction technology produces generally adopts lime (or Wingdale) to carry out the two-stage neutralizing treatment, under based on the prerequisite of iron arsenic in the waste water, make arsenic in the waste water form stable ferric arsenate precipitation and reach the purpose of improvement than Fe/As＞3; Generally, need to adopt measures such as oxygenation or adding strong oxidizer to make the trivalent arsenic and the ferrous iron that exist in the waste water be converted into pentavalent arsenic and ferric iron, to guarantee the stability of final purpose product.
2, microwave irradiation technology principle:
Microwave is that a kind of frequency is at 300MHz～300GHz, the wavelength hertzian wave between 1～1000mm; Micro-wave energy is used as a kind of energy, add thermal material by waste of energy selectivity in material inside, have homogeneous heating, thermo-efficiency height, cleanliness without any pollution, start and stop to heat very fast and even can improve the incomparable advantages of traditional way such as material property, have clear superiority enhancing productivity and improve aspects such as working condition;
Carbon is a kind of extraordinary microwave absorbing material, can be in a short period of time by the microwave oxidation, therefore, microwave irradiation technology and bio-oxidation technology are organically combined, promptly utilize microwave radiation bio-oxidation slag to reach the purpose that selectivity is eliminated organic carbon, so on the one hand since the sulfide content in the oxidation sludge seldom, in the microwave radiation process, can not produce dusty gass such as a large amount of sulfurous gas and arsenic oxide arsenoxide, contained organic carbon has thoroughly been solved the problem of ADSORPTION OF GOLD in the follow-up cyaniding operation by rapid heated volatile in the oxidation sludge on the other hand; Like this, can handle nearly all difficult separation concentrate resource by bio-oxidation-microwave radiation process integration;
In addition, when Gold Ore being carried out pre-treatment, because microwave is to the selectivity heating of mineral with microwave radiation, can make some mineral generation chemical reaction or phase transition in the ore, make the sulfide decomposition that gold is formed parcel, gold is exposed to be dissociated, and is easy to cyaniding and leaches; And, by the control of calcination atmosphere and the application of solidifying agent, sulphur, arsenic in the mineral are produced respectively with the solidified form, comprehensive recovering effect is good, and is friendly more to environment.
The chemical reaction that microwave radiation takes place is as follows:
4FeS
2+11O
2＝2Fe
2O
3+8SO
2
2FeAsS+5O
2＝Fe
2O
3+As
2O
3+2SO
2
C+O
2＝CO
2
CaCO
3/MgCO
3＝CaO/MgO+CO
2
2CaO+2SO
2+O
2＝2CaSO
4
3CaCO
3+As
2O
3+O
2＝Ca
3(AsO
4)
2+3CO
2
In sum, operational path of the present invention is an ore grinding, and---bio-oxidation---microwave radiation---is cyanidation gold-extracted; Utilize bio-oxidation technology earlier, carry out the oxygenolysis sulfide mineral, gold is fully exposed dissociate, sulphur, the most of oxidized liquid phase that enters of arsenic are the material of next step operation output cleaning, and oxidation liquid returns use through neutralizing treatment; Oxidation sludge adopts the microwave low-temperature bake, removes the organic carbon in the ore, has thoroughly solved the problem of ADSORPTION OF GOLD in the follow-up cyanidation gold-extracted operation; This technology had both improved the golden rate of recovery, had reduced the pollution to environment again, the easy automatization control of technological process; The step of this technology is as follows:
(1) gold ore ore grinding and dense reagent removal:
Different Gold Ores, because it is also inequality that the size composition and the occurrence status difference of gold, grinding particle size are formed, generally between-0.045mm content 90%～0.037mm content 95%, carry out dense reagent removal then and adjust the concentration of ore pulp, generally 15%～25%;
(2) bio-oxidation:
Step (1) is adjusted certain density ore pulp feed biological oxidation system, guaranteeing under 35 ℃～45 ℃ of temperature, dissolved oxygen amount 3mg/l～5mg/l, substratum consumption 3kg/t～5kg/t, 5～10 days the processing condition of oxidization time, microbiological oxidation, decomposition sulfide mineral, gold is fully exposed to be dissociated, bio-oxidation rear oxidation washings is through in one-level neutralization and the secondary and after the arsenic removal, make solid-liquid separation, in and slag discharging, neutralizer returns washing and changes into oxidation sludge through press filtration, xeraphium again, enters the next step microwave radiation;
(3) microwave radiation:
The oxidation rinsing liquid of step (2) bio-oxidation is through neutralization back solid-liquid separation, the neutralizer that returns is again through washing, press filtration, dry atomizing oxidation sludge, enter microwave radiation, maintain the temperature at 450 ℃～600 ℃, constant temperature time 15min～25min, oxidation of coal in the ore is removed, and the flue gas of generation is through purifying the back qualified discharge; Calcining through shrend, sizing mixing enters cyanidation gold-extracted step;
(4) cyanidation gold-extracted:
It is 25%～45% that the calcining of step (3) is sized mixing after shrend, pH value 10～11, alkaline purification time 2～6h, NaCN concentration 5 * 10
-4～25 * 10
-4, average blowing-in burden(ing) density 15～25kg/m
3, soak and inhale 5～10 sections of hop counts, soak suction time 60～120h, producing gold mud through above-mentioned processing condition is ingot through refining, filter residue is delivered to tailings reservoir for piling, sizes mixing before filtrate returning soaked.
The invention has the advantages that: utilize bio-oxidation technology, oxidation, decomposition sulfide mineral fully expose gold and dissociate, sulphur, arsenic are most of to enter liquid phase after oxidized, be the material of next step output cleaning, oxidation liquid returns use through neutralizing treatment, reduces the pollution to environment; Oxidation sludge adopts microwave radiation, carry out low-temperature bake, remove the organic carbon in the ore, eliminated " robbing gold " problem of organic carbon, because low-temperature bake, avoided the secondary parcel of low melting point oxide to gold, so the gold recovery height, also reduced the pollution to environment simultaneously, technological process is easy to automatization control.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment:
As shown in Figure 1, be process flow sheet of the present invention.
Certain golden ore concentrate hard to treat, the ore multielement analysis the results are shown in Table 1
The analysis of table 1 golden ore concentrate multielement
| Element | Au(g/t) | Ag(g/t) | Cu | Pb | Zn | As | Fe | S |
| Content (%) | 44.18 | 5.03 | 0.03 | 0.03 | 0.04 | 0.75 | 17.29 | 16.58 |
| Element | C | Sb | Bi | CaO | MgO | Al 2O 3 | SiO 2 | |
| Content (%) | 4.09 | 1.34 | 0.01 | 5.45 | 1.21 | 5.51 | 38.69 |
According to the research of ore process mineralogy, to main harmful element has carried out material phase analysis in the ore, the sulphur material phase analysis the results are shown in Table 2; The arsenic material phase analysis the results are shown in Table 3; The carbon material phase analysis the results are shown in Table 4; The conventional charcoal of gold ore soaks test-results and sees Table 5.
Table 2 concentrate sulphur material phase analysis
| Separate | S/ vitriol | S/ sulfide | Full sulphur |
| Absolute content (%) | 0.41 | 15.97 | 16.58 |
| Relative content (%) | 2.47 | 96.32 | 100.00 |
Table 3 concentrate arsenic material phase analysis
| Separate | The As/ oxide compound | As/ sulfide | Full arsenic |
| Absolute content (%) | 0.15 | 0.59 | 0.75 |
| Relative content (%) | 20.00 | 78.67 | 100.00 |
Table 4 concentrate carbon material phase analysis
| Separate | C/ carbonate | C/ is organic | C/ graphite | Full carbon |
| Absolute content (%) | 1.78 | 1.24 | 1.07 | 4.09 |
| Relative content (%) | 41.52 | 30.32 | 26.16 | 100.00 |
The conventional charcoal of table 5 gold ore soaks test-results
| Concentrate gold grade (g/t) | Soak slag gold grade (g/t) | Leaching yield (%) |
| 44.18 | 41.89 | 0.66 |
Soaking test-results by concentrate multielement analysis and conventional charcoal can find out, this ore belongs to typical trickle dip-dye type carbonaceous refractory gold ore.
Embodiment 1:
(1) gold ore ore grinding and dense reagent removal:
Be-0.045mm content 95% that carrying out dense reagent removal then and adjusting pulp density is 16% with above-mentioned golden ore concentrate hard to treat ore grinding to grinding particle size;
(2) bio-oxidation:
Step (1) is adjusted certain density ore pulp feed biological oxidation system, guaranteeing under 40 ℃ of temperature, dissolved oxygen amount 4mg/l, substratum consumption 4kg/t, 8 days the processing condition of oxidization time, microbiological oxidation, decomposition sulfide mineral, gold is fully exposed to be dissociated, bio-oxidation rear oxidation washings makes solid-liquid separation through in one-level neutralization and the secondary and after the arsenic removal, in and the slag discharging, neutralizer returns washing and changes into oxidation sludge through press filtration, xeraphium again, enters the next step microwave radiation;
(3) microwave radiation:
The oxidation rinsing liquid of step (2) bio-oxidation is through neutralization back solid-liquid separation, the neutralizer that returns is again through washing, press filtration, dry atomizing oxidation sludge, enter microwave radiation, maintain the temperature at 480 ℃, constant temperature time 20min, oxidation of coal in the ore is removed, and the flue gas of generation is through purifying the back qualified discharge; Calcining through shrend, sizing mixing enters cyanidation gold-extracted step;
(4) cyanidation gold-extracted:
It is 33% that the calcining of step (3) is sized mixing after shrend, pH value 10, alkaline purification time 3h, NaCN concentration 6 * 10
-4, average blowing-in burden(ing) density 20kg/m
3, soak and inhale 7 sections of hop counts, soak suction time 84h, producing gold mud through above-mentioned processing condition is ingot through refining, filter residue is delivered to tailings reservoir for piling, sizes mixing before filtrate returning soaked.
Test-results: carbon removal rate: 96.39%
Sulphur evaporation rate: 9.18%
Arsenic curing degree: 95.39%
Gold leaching rate: 95.84%
Embodiment 2:
(1) gold ore ore grinding and dense reagent removal:
Be-0.045mm content 95% that carrying out dense reagent removal then and adjusting pulp density is 16% with above-mentioned difficult-treating gold mine stone ore to grinding particle size;
(2) bio-oxidation:
Step (1) is adjusted certain density ore pulp feed biological oxidation system, guaranteeing under 40 ℃ of temperature, dissolved oxygen amount 5mg/l, substratum consumption 4kg/t, 7 days the processing condition of oxidization time, microbiological oxidation, decomposition sulfide mineral, gold is fully exposed to be dissociated, bio-oxidation rear oxidation washings makes solid-liquid separation through in one-level neutralization and the secondary and after the arsenic removal, in and the slag discharging, neutralizer returns washing and changes into oxidation sludge through press filtration, xeraphium again, enters the next step microwave radiation;
(3) microwave radiation:
The oxidation rinsing liquid of step (2) bio-oxidation is through neutralization back solid-liquid separation, the neutralizer that returns is again through washing, press filtration, dry atomizing oxidation sludge, enter microwave radiation, maintain the temperature at 450 ℃, constant temperature time 18min, oxidation of coal in the ore is removed, and the flue gas of generation is through purifying the back qualified discharge; Calcining through shrend, sizing mixing enters cyanidation gold-extracted step;
(4) cyanidation gold-extracted:
It is 33% that the calcining of step (3) is sized mixing after shrend, pH value 10.5, alkaline purification time 5h, NaCN concentration 15 * 10
-4, average blowing-in burden(ing) density 20kg/m
3, soak and inhale 7 sections of hop counts, soak suction time 84h, producing gold mud through above-mentioned processing condition is ingot through refining, filter residue is delivered to tailings reservoir for piling, sizes mixing before filtrate returning soaked.
Test-results: carbon removal rate: 90.17%
Sulphur evaporation rate: 11.09%
Arsenic curing degree: 95.03%
Gold leaching rate: 89.02%
Embodiment 3:
(1) gold ore ore grinding and dense reagent removal:
Be-0.045mm content 95% that carrying out dense reagent removal then and adjusting pulp density is 16% with above-mentioned difficult-treating gold mine stone ore to grinding particle size;
(2) bio-oxidation:
Step (1) is adjusted certain density ore pulp feed biological oxidation system, guaranteeing under 38 ℃ of temperature, dissolved oxygen amount 5mg/l, substratum consumption 4kg/t, 8 days the processing condition of oxidization time, microbiological oxidation, decomposition sulfide mineral, gold is fully exposed to be dissociated, bio-oxidation rear oxidation washings makes solid-liquid separation through in one-level neutralization and the secondary and after the arsenic removal, in and the slag discharging, neutralizer returns washing and changes into oxidation sludge through press filtration, xeraphium again, enters the next step microwave radiation;
(3) microwave radiation:
The oxidation rinsing liquid of step (2) bio-oxidation is through neutralization back solid-liquid separation, the neutralizer that returns is again through washing, press filtration, dry atomizing oxidation sludge, enter microwave radiation, maintain the temperature at 500 ℃, constant temperature time 22min, oxidation of coal in the ore is removed, and the flue gas of generation is through purifying the back qualified discharge; Calcining through shrend, sizing mixing enters cyanidation gold-extracted step;
(4) cyanidation gold-extracted:
It is 33% that the calcining of step (3) is sized mixing after shrend, pH value 11, alkaline purification time 6h, NaCN concentration 25 * 10
-4, average blowing-in burden(ing) density 20kg/m
3, soak and inhale 7 sections of hop counts, soak suction time 84h, producing gold mud through above-mentioned processing condition is ingot through refining, filter residue is delivered to tailings reservoir for piling, sizes mixing before filtrate returning soaked.
Test-results: carbon removal rate: 96.77%
Sulphur evaporation rate: 10.23%
Arsenic curing degree: 95.13%
Gold leaching rate: 94.34%.
Claims (1)
1, a kind of golden ore concentrate hard to treat gold extraction technology of low pollution and high recovery, it is characterized in that: step is as follows:
One, gold ore ore grinding and dense reagent removal:
Different Gold Ores, because the size composition and the occurrence status difference of gold, it is also inequality that grinding particle size is formed, and between-0.045mm content 90%～0.037mm content 95%, carries out dense reagent removal then and adjust the concentration of ore pulp, 15%～25%;
Two, bio-oxidation:
Step 1 is adjusted certain density ore pulp feed biological oxidation system, guaranteeing under 35 ℃～45 ℃ of temperature, dissolved oxygen amount 3mg/l～5mg/l, substratum consumption 3kg/t～5kg/t, 5～10 days the processing condition of oxidization time, microbiological oxidation, decomposition sulfide mineral, gold is fully exposed to be dissociated, bio-oxidation rear oxidation washings is through in one-level neutralization and the secondary and after the arsenic removal, make solid-liquid separation, in and slag discharging, neutralizer returns washing and changes into oxidation sludge through press filtration, xeraphium again, enters the next step microwave radiation;
Three, microwave radiation:
The oxidation rinsing liquid of step 2 bio-oxidation is through neutralization back solid-liquid separation, the neutralizer that returns is again through washing, press filtration, dry atomizing oxidation sludge, enter microwave radiation, maintain the temperature at 450 ℃～600 ℃, constant temperature time 15min～25min, oxidation of coal in the ore is removed, and the flue gas of generation is through purifying the back qualified discharge; Calcining through shrend, sizing mixing enters cyanidation gold-extracted step;
Four, cyanidation gold-extracted:
It is 25%～45% that the calcining of step 3 is sized mixing after shrend, pH value 10～11, alkaline purification time 2～6h, NaCN concentration 5 * 10
-4～25 * 10
-4, average blowing-in burden(ing) density 15～25kg/m
3, soak and inhale 5～10 sections of hop counts, soak suction time 60～120h, producing gold mud through above-mentioned processing condition is ingot through refining, filter residue is delivered to tailings reservoir for piling, sizes mixing before filtrate returning soaked.
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| 难处理金矿石的细菌氧化机理及影响因素. 杨少华，杨凤丽，余新阳.湿法冶金，第25卷第2期. 2006 * |
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| 难浸金矿预处理技术及其应用. 周丽，文书明，李华伟.云南冶金，第33卷第4期. 2004 * |
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