CN1683573A - Poisonless low cost refining method for noble metals - Google Patents
Poisonless low cost refining method for noble metals Download PDFInfo
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- CN1683573A CN1683573A CN 200510033706 CN200510033706A CN1683573A CN 1683573 A CN1683573 A CN 1683573A CN 200510033706 CN200510033706 CN 200510033706 CN 200510033706 A CN200510033706 A CN 200510033706A CN 1683573 A CN1683573 A CN 1683573A
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Abstract
The poison-less noble metal refining process includes the following steps: superfine treating ore material to nanometer level; setting nanometer level ore powder and water into high pressure reactor, heating and pressurizing to make water reach supercritical state, introducing high pressure oxygen containing gas to oxidize ore material fully; decompressing to evaporate water, and screening remainder solid to obtain required noble metal. Owing to the superfine treatment of the ore material, the coated gold and other accompanied minerals are separated physically, and serial chemical reactions are completed under nanometer size to raise the reaction rate to several times or decades times. Therefore, the present invention has greatly raised yield, greatly lowered cost, no environmental pollution, recovery of heat energy and high comprehensive utility.
Description
[technical field]
The present invention relates to the refinement of precious metal, be specifically related to a kind of poisonless low cost refining method of precious metal.
[background technology]
The difficult separation ore is exactly the ore that can not extract gold from traditional Process for the cyanation, and the card beautiful jade type gold mine of the U.S. is exactly typical indissoluble gold.Cyanide process is since 1880s is applied to gold production, west industrialized country has adopted the gold deposit of many easy cyanidings in the period of over one hundred, it is that the cyanide process processing is inconvenient that early discovery still has most mineral deposits of extraction value many, can not effectively carry gold with cyanide process.These ores are " difficulty is soaked " why, is to contain the organism that carbon etc. can ADSORPTION OF GOLD because of them, causes gold to run off with mine tailing, or the goldc grains embedding is distributed between the crystal of carrier mineral (being mainly arsenic, the antimony sulfides) and in the crack, makes that the rate of recovery of gold is not high.The present gold leaching yield of China has only 60%, that is to say that 40% is wasted.
At present the main extraction process process of gold is: at first sub-elect coarse-grained gold by the heavy sand method, select gold than particulate by flotation process then, leach by cyanide process at last and extract.Also have some to leach methods of extracting in addition as biological bacterium oxidation leaching, high-pressure oxidation leaching, roasting oxidation leaching, microwave oxidation leaching etc.
The carbonaceous refractory gold ore that depolarization is fine still lacks outside the effective treating method, and at present, the ultimate production of world's gold existing about 1/3 is to originate from the indissoluble gold ore deposit.Since indissoluble gold ore resources development technique and the technological process research of the seventies in last century, be that gold extracts the most noticeable, the most active and the most sharp field of endeavouring the popular feeling, research aspect in the world.It is by oxidizing reaction, makes the gold element in the indissoluble gold ore deposit dissociate out, extracts with ordinary method thereafter, dissimilar difficulties is soaked or the difficult separation ore resources is effectively developed.21st century, the basic pretreatment process of refractory gold ore mainly contained roasting method, hot-press method and bacterial oxidation method, they have the refractory gold ore oxygenolysis are become golden sulfide mineral, destroy the sulfide mineral crystalline structure gold that is wrapped is exposed, be beneficial to cyanidation gold-extracted denominator.Now developed treatment technologies such as hot-pressure oxidation, microbiological oxidation and roasting oxidation, these The Application of Technology provide feasibility for the processing of refractory mineral, but certain limitation and drawback are all arranged, and development haves much room for improvement.For example, roasting method changes responsive to operating parameters and feed composition, cause burning or underburnt easily, causes the leaching yield of gold to descend, and can produce sulfurous gas and white arsenic during roasting, comprehensively reclaims when ineffective, can severe contamination atmosphere and environment; The hot-pressure oxidation method is very high to the corrosion protection design and the material safety requirements of equipment, and the initial cost expense is higher, has only the large-scale plant of the day output of construction more than 1200 tons, economically just relatively rationally; The oxidization time of bacterial oxidation method is long, and pulp density is low, needs big volumetrical steel basin, and the cooling cooling that requires the expenditure of energy particularly occurs " mishandle ", and bacterium may be dead, needs the time in several weeks could recover the biomass of bacterium.
China is the world important gold producing country, through exploitation for many years, easily select the smelting gold resource constantly to reduce, the situation that reserved resources is in short supply is more outstanding, but, be distributed widely in geographic difficult-treating gold mines such as southwest, northwest and northeast, reserves account for 30% of national gold deposit geology reserves, and its prospective reserves is more considerable.Be necessary that the research and development operational condition is relatively gentle, method investment cost and productive expense are few, be more suitable for national conditions, the easier refractory gold ore pretreatment process of applying at home.In addition, existing Gold Ore selects most of industrial flows of smelting also to exist and uses the hypertoxicity medicament or produce, discharge radioactive substance on stream, contaminate environment is serious, and long flow path and complexity, the rate of recovery is low, cost is high shortcoming, therefore, demand that research and development rate of recovery height, cost are low urgently, asepsis environment-protecting, can replace the method that extracts gold from of cyanide process.
The supercritical water technology is one of popular research topic in the world in recent years, now is applied to chemical industry, environmental protection, medicine, mining and metallurgy field in various degree.Supercritical water is meant the water when temperature and pressure surpasses 374.3 ℃ of critical temperatures and emergent pressure 22.1MPa respectively, and it has the unexistent peculiar property of standard state water.The density of supercritical water can change continuously by changing temperature and pressure, and various materials solubleness therein all increases with density.Supercritical water can dissolve each other fully with many organic compound materials, also can dissolve each other with gases such as air, oxygen, carbonic acid gas.And the solubleness of inorganic salt and heavy metal is extremely low under high temperature and high pressure, is easy to Separation and Recovery in step-down separates.But existing supercritical water oxidation method is carried gold, has the slow shortcoming of speed of response.
[summary of the invention]
The objective of the invention is to propose a kind of cyanide process that replaces, the poisonless low cost refining method of the precious metal of totally nontoxic, efficient, low basis, environmental protection.
The technical scheme that realizes above-mentioned purpose is: the poisonless low cost refining method of precious metal comprises the steps:
1) mineral aggregate for the treatment of refinement carries out the ultra micro thinning processing, makes its fineness reach submicron to nanometer scale;
2) mineral aggregate after the ultra micro thinning processing and water are added in the autoclave, heating and pressurizing makes water reach supercritical state, and feeds the high pressure oxygen-containing gas, makes the abundant oxidation of mineral aggregate;
3) decompression, transpiring moisture screens remaining solid, obtains required precious metal.
Described ultra micro thinning processing can be realized by the process that comprises the steps:
1a) earlier mineral aggregate tentatively is broken into the powder that fineness meets ultra-fine equipment charging requirement;
1b) above-mentioned powder is made the slurry of solid content 50～70%;
1c) use ultra-fine equipment that slurry is ground, make that powder granularity is 90nm～1500nm.
Preferably, in step 2) reaction in also add heavy calcium carbonate.
Described heavy calcium carbonate preferably fineness is higher than 6000 purpose micropowder of dense calcium carbonate.
The add-on of described micropowder of dense calcium carbonate is preferably 3 times of mole number of institute's sulfur-bearing in the mineral aggregate.
At step 1a) in can use Raymond mill or high pressure roll-in mill as corase grind equipment, raw material is made the powder that granularity is 0.044mm～0.13mm.
The ultra-fine evaluation method selecting optimal equipment that is adopted has the ultra-fine mill of medium.
It is further preferably, described that the ultra-fine mill of medium is arranged is the eddy flow mill that stirs mill or arrange with series system.
Adopt technique scheme, beneficial technical effects of the present invention is: 1) owing among the present invention ore has been carried out nano level ultra-fine processing, the gold that is wrapped is separated with physical form with its associated mineral, this is that present traditional technology is not available; And make that a series of subsequently high-temperature chemical reactions carry out under nanoscale, because the existence of nano effect, can make that speed of reaction improves several times to tens times, output capacity improves greatly, cost greatly reduces, its treatment time is short, the efficient height, can be with carbon, arsenic, exhaustive oxidations such as sulphur, and disposable separation carries gold, needn't cyaniding handle, and production cost is low, non-environmental-pollution, but heat energy recycle also, calcium sulfate, female salt and silicon can reclaim separately, has higher comprehensive benefit, its result effectively improves the extraction yield of gold, particularly for " refractory gold ore ", finally is implemented in the extraction of the gold under the low cost.2) add in ore pulp that an amount of (content according to sulphur in the ore decides add-on, require preferably 3 times of mole number of sulphur of add-on) heavy calcium carbonate, can solve the pollution problem of the sulfurous gas that generates after the sulphur oxidation and sulfuric acid simultaneously to atmosphere and environment, because supercritical water can dissolve each other fully with gases such as organism and air, nitrogen, carbonic acid gas, sulfurous gas, therefore, the sulfurous gas that forms after the sulphur oxidation is soluble in water with water-ground limestone fully reaction to take place, generating water-fast calcium sulfate is gypsum, eliminates the pollution of its discharging back to air.3) select for use fineness to be higher than 6000 purpose micropowder of dense calcium carbonate, because its fine size, specific surface area is very big, makes sufficient reacting and rapidly, can eliminate this pollutent of sulfurous gas more rapidly and thoroughly.
[embodiment]
A kind of poisonless low cost refining method of precious metal, its technical process is:
1) mineral aggregate of at first treating refinement carries out the ultra micro thinning processing, makes its fineness reach nanometer scale.Generally speaking, because the most granularities of mineral aggregate are bigger, therefore preferably roughly grind through ball mill such as Raymond mill or high pressure roll-in mill earlier, to make ultra-fine equipment acceptable powder, according to the requirement of existing general ultra-fine equipment, the granularity of charging powder all allows between 0.044mm～0.13mm.In addition, according to the difference of the mode of operation of ultra-fine equipment, also powder to be made the slurry that meets its requirement for the equipment of wet grinding, general solid content all suits between 50～70%, when the slurry solid content is 100%, then be suitable for the ultra-fine equipment of dry grinding.As for the selection of ultra-fine equipment, can carry out according to the characteristics of treatment capacity and concrete raw material, ultra-fine equipment such as general optional stirring mill, vibration mill, airflow milling, the present invention preferably has the eddy flow mill of the ultra-fine mill of medium class as stirring mill or arranging with series system.After ultra-fine equipment ground, the discharging powder granularity was controlled between 90nm～1500nm and all is fit to.
2) then nano level mineral aggregate and water are added in the autoclave, heating and pressurizing makes water reach supercritical state, and feeds the high pressure oxygen-containing gas, and for example air makes the abundant oxidation of mineral aggregate.In this process, also can add fineness and be higher than 6000 purpose micropowder of dense calcium carbonate, solving after the sulphur oxidation to atmospheric pollution problem, preferably in the mineral aggregate 3 times of the mole number of institute's sulfur-bearing of its add-ons.Supercritical water is under the effect of oxygen, gold trioxide ore preferably, under high temperature and high pressure, can produce spontaneous combustion under the effect of the sulphur in the ore pulp, arsenic, carbon oxygen in air, and the spontaneous oxidation heat release elevates the temperature to 400～600 ℃ the oxidation rapidly of materials such as the sulphur more than 99.9%, arsenic, carbon quilt.Gold, other heavy metals, iron, the solubleness of inorganic salts in supercritical water are extremely low, after the decompression can with precipitation separation rapidly such as water vapour, the gold and silver of Bao Luing, iron, silicon etc. are separated together simultaneously, carbon, sulphur and arsenic are oxidized to CO
2Form innoxious discharging and separate with inorganic salts.And the high pressure-temperature saturated vapo(u)r that supercritical water produces when step-down can drive turbo-generator and is used for generating, and the overbottom pressure steam of generation can be used for producing and life.
3) decompression at last, transpiring moisture screens remaining solid, obtains required precious metal.Screening remaining solid can take by proportion the method that the solid that stays carries out gravity treatment is isolated gold.
Specific embodiment: 200 kilograms of the card beautiful jade type Gold Ores that the first Gold Content that the Guizhou gold mine is produced is 15.03 gram/tons, drop in the WG3 type high pressure roll-in mill that Shenzhen big male mechanical means company limited produces and be broken into breeze, cross 100 mesh sieves, again described breeze is added water and add 35 kilogram of 6000 order water-ground limestone, make solid content and be 60% ore pulp.(this ultrafine eddy flow attitude grinding machine has been applied for Chinese patent then described ore pulp to be dropped into the WXA5 type ultrafine eddy flow attitude grinding machine that Shenzhen big male mechanical means company limited produces, number of patent application is 200410081580.8) in be processed into the ore pulp that granularity is a nanometer scale with 10 fens clock times are ultra-fine, then with ore pulp by being pumped in the homemade autoclave of South China Science ﹠ Engineering University, heat then to 407 ℃ and emergent pressure 23.1MPa supercritical state, feed high-pressure air by 60～160 liters/minute simultaneously, after 75 seconds, stop bubbling air, emit slurry simultaneously, water evaporates in a large number, the solid that stays carries out gravity treatment by proportion, isolates gold.
Isolated gold, putting into the baking oven temperature is 110 ℃ of oven dry down, is weighed as 2.987 grams, the rate of recovery is up to 99.3%.
Present technique also can be used for the extraction of other precious metal.Above content be in conjunction with concrete preferred implementation to further describing that the present invention did, can not be interpreted as concrete enforcement of the present invention and be confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to the scope of patent protection that the present invention is determined by claims of being submitted to.
Claims (8)
1, passes through the poisonless low cost refining method of metal, comprise the steps:
1) mineral aggregate for the treatment of refinement carries out the ultra micro thinning processing, makes its fineness reach submicron to nanometer scale;
2) mineral aggregate after the ultra micro thinning processing and water are added in the autoclave, heating and pressurizing makes water reach supercritical state, and feeds the high pressure oxygen-containing gas, makes the abundant oxidation of mineral aggregate;
3) decompression, transpiring moisture screens remaining solid, obtains required precious metal.
2, the poisonless low cost refining method of precious metal according to claim 1 is characterized in that: described ultra micro refinement is handled and is comprised following steps:
1a) earlier mineral aggregate tentatively is broken into the powder that fineness meets ultra-fine equipment charging requirement;
1b) above-mentioned powder is made the slurry of solid content 50～70%;
1c) use ultra-fine equipment that slurry is ground, make that powder granularity is 90nm～1500nm.
3, the poisonless low cost refining method of precious metal according to claim 1 is characterized in that: in step 2) reaction in also add heavy calcium carbonate.
4, the poisonless low cost refining method of precious metal according to claim 3 is characterized in that: described heavy calcium carbonate is that fineness is higher than 6000 purpose micropowder of dense calcium carbonate.
5, the poisonless low cost refining method of precious metal according to claim 4 is characterized in that: the add-on of described micropowder of dense calcium carbonate is 3 times of mole number of institute's sulfur-bearing in the mineral aggregate.
6, according to the poisonless low cost refining method of any described precious metal of claim 2～5, it is characterized in that: at step 1a) in use Raymond mill or high pressure roll-in mill as corase grind equipment, raw material is made the powder that granularity is 0.044mm～0.13mm.
7, according to the poisonless low cost refining method of any described precious metal of claim 2～5, it is characterized in that: described ultra-fine equipment is that the ultra-fine mill of medium is arranged.
8, the poisonless low cost refining method of precious metal according to claim 7 is characterized in that: described the ultra-fine mill of medium is arranged is the eddy flow mill that stirs mill or arrange with series system.
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| CNB2005100337069A CN1308470C (en) | 2005-03-15 | 2005-03-15 | Poisonless low cost refining method for noble metals |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451187A (en) * | 2014-10-09 | 2015-03-25 | 厦门紫金矿冶技术有限公司 | Superfine milling pretreatment method of refractory gold concentrate |
| CN110331277A (en) * | 2019-07-02 | 2019-10-15 | 长春黄金研究院有限公司 | A method of oxidation carries golden sulfide mineral |
| US11319613B2 (en) | 2020-08-18 | 2022-05-03 | Enviro Metals, LLC | Metal refinement |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10167202B2 (en) | 2016-02-23 | 2019-01-01 | King Abdullah University Of Science And Technology | Enhanced metal recovery through oxidation in liquid and/or supercritical carbon dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9407892D0 (en) * | 1994-04-21 | 1994-06-15 | British Nuclear Fuels Plc | Solvent extraction of metal containing species |
| GB0010241D0 (en) * | 2000-04-28 | 2000-06-14 | Johnson Matthey Plc | Improvements in precious metal refining |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451187A (en) * | 2014-10-09 | 2015-03-25 | 厦门紫金矿冶技术有限公司 | Superfine milling pretreatment method of refractory gold concentrate |
| CN110331277A (en) * | 2019-07-02 | 2019-10-15 | 长春黄金研究院有限公司 | A method of oxidation carries golden sulfide mineral |
| US11319613B2 (en) | 2020-08-18 | 2022-05-03 | Enviro Metals, LLC | Metal refinement |
| US11578386B2 (en) | 2020-08-18 | 2023-02-14 | Enviro Metals, LLC | Metal refinement |
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