CN101314815A - Atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate - Google Patents

Atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate Download PDF

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Publication number
CN101314815A
CN101314815A CNA2008100389391A CN200810038939A CN101314815A CN 101314815 A CN101314815 A CN 101314815A CN A2008100389391 A CNA2008100389391 A CN A2008100389391A CN 200810038939 A CN200810038939 A CN 200810038939A CN 101314815 A CN101314815 A CN 101314815A
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ozone
oxidation method
catalytic oxidation
atmosphere
arsenic
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CN101314815B (en
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李登新
李青翠
钱方珺
戴尚飞
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Donghua University
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Donghua University
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Priority to CN2008100389391A priority Critical patent/CN101314815B/en
Priority to PCT/CN2008/001924 priority patent/WO2009149590A1/en
Priority to CA2722494A priority patent/CA2722494C/en
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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
    • 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
    • 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
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • 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
    • C22B11/00—Obtaining noble metals
    • C22B11/08—Obtaining noble metals by cyaniding
    • 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
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Catalysts (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a normal-atmosphere catalytic oxidation method of refractory high-sulfur high-arsenic gold concentrates, which comprises the steps as follows: (1) right amount of core samples, solid catalysts, and acid and water are added in a reaction kettle provided with a stirrer to form refractory gold ore slurry; (2) under the condition that the temperature ranges from 60 to 100 DEG C, gas oxidants that are ozone and oxygen or the ozone and air are continuously pumped in the slurry, and oxidized ore pulp is formed after continuous mixing; the reaction time is 6 to 18 hours, and then filter liquor and filter residues are obtained through filtration after the oxidized ore pulp is cooled to the room temperature; (3) based on the traditional extraction technology, the filter residues and calcium hydroxide solution are mixed, the pH value ranges from 11 to 12, sodium cyanide is added, the mixed solution is filtered after being stirred for 24 hours, and noble metals are extracted from the filter liquor. The normal-atmosphere catalytic oxidation method has the advantages that the extraction rate of the noble metals such as aurum, silver, etc. and the multipurpose utilization rate of other elements are increased; the environmental pollution is reduced at the same time during the extraction process; in addition, the technology is simple, and the facility cost is lower.

Description

A kind of atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate
Technical field
The present invention relates to a kind of atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate.
Background technology
The high-sulfur high-arsenic hard washing golden ore concentrate treatment process mainly contains pretreatment processs such as roasting oxidation method, pressure oxidation method, atmospheric pressure oxidation method, bacterial oxidation method, nitric acid catalytic oxidation.Main drawback is that the extraction yield of precious metals such as gold and silver in the hard washing golden ore concentrate, platinum, palladium is lower; Other element comprehensive utilization ratios are also lower; In extracting the precious metal process, environment is polluted; And complex process, the cost height.
If a kind of catalyzer is arranged can regenerate in gas phase, solubleness in water is very high again, its cathode potential when sulfuration bed surface reduction is also high, then can significantly reduce required temperature of sulphide ores oxidation acid leaching and oxygen and press, and this is an important directions of hydrometallurgy research work.
Summary of the invention
The objective of the invention is to improve extraction yield and other element comprehensive utilization ratios of precious metals such as gold and silver in the hard washing golden ore concentrate, platinum, palladium; In leaching process, reduce environmental pollution simultaneously; And technology is simple, and equipment cost is lower.
In order to achieve the above object, the invention provides a kind of atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate.Its principle of work is: since the chemical combination bond energy of most of molecules be 25～35 kilocalories/rub, and the redox-potential of ozone approximately is 2.07V, the chemical combination bond energy be 47 kilocalories/rub, therefore ozone is enough to open the chemical combination key of most molecules, break the pyrite and the mispickel that wrap up precious metals such as gold and silver, make precious metal expose out, iron, copper, several elements of manganese can play katalysis and promote oxygen and ozone to dissolve and transformation in water in addition.
Key of the present invention is to have used oxygenant and catalyzer, and its reactions steps is as follows:
O 3+ O 2+ go back ortho states [solid catalyst] → O+ oxidation state [solid catalyst]
O+ oxidation state [solid catalyst]+FeS 2→ FeSO 4+ go back ortho states [solid catalyst]
Wherein going back ortho states [solid catalyst] can be by oxidation again and recycle, and improves dioxygen oxidation speed indirectly.
Concrete steps of the present invention are as follows:
1. an amount of sample ore of disposable adding, solid catalyst and water in having the reactor of agitator, solid catalyst concentration is 151～280 grams per liters, the weight ratio of sample ore and water is 1: 6～1: 10, adds acid to pH value 1～3, is configured to the slurries of refractory gold ore.
2. under 60～100 ℃ temperature condition, in slurries, feed gaseous oxidant continuously, be ozone and oxygen, wherein ozone is that 0.8～1.2 Grams Per Hour and oxygen are 0.1～1.0 cubic metre/hour, or ozone and air, wherein ozone is that 0.8～1.2 Grams Per Hour and air are 0.1～1.0 cubic metre/hour, successively stir, form the oxidation ore pulp, the reaction times is 6～18 hours, reduces to then that room temperature filters to get filtrate and filter residue.
3. according to traditional extraction technique, filter residue mixes with aqua calcis, transfers to pH value 11～12, adds sodium cyanide and stirs 24 hours after-filtration, extracts precious metal from filtrate.
The preparation technology of described solid catalyst is: with industrial iron, copper, hydrochloric acid or chlorine, manganese oxide, aluminum oxide, silicon oxide under normal temperature, condition of normal pressure, evenly stir, mix, in this process, if use chlorine, then feed chlorine continuously, make the composition quality per-cent of its finished product be respectively iron 30%, chlorine 30%, oxygen 15%, copper 10%, manganese 5%, silicon 5% and aluminium 5%.
The acid that the slurries of described refractory gold ore can comprise is hydrochloric acid and sulfuric acid.
Advantage of the present invention is: extraction yield and other element comprehensive utilization ratios of having improved precious metals such as gold and silver in the hard washing golden ore concentrate; In leaching process, reduce environmental pollution simultaneously; And technology is simple, and equipment cost is lower.Measure according to GB, the leaching yield of gold and silver is respectively 68～98.5% and 80～96%, and is respectively less than 40% and 50～60% without the corresponding leaching yield of the direct cyaniding of foregoing invention step.
Embodiment
Below in conjunction with embodiment the present invention is done to set forth in further detail.
Embodiment 1
With reference to figure 1, be high-sulfur high-arsenic hard washing golden ore concentrate atmosphere-pressure catalytic oxidation process flow sheet, disposable adding sample ore, water and solid catalyst in having the reactor of agitator, and sulfuric acid, solid catalyst concentration is 151 grams per liters, the weight ratio of sample ore and water is 1: 10, add sulfuric acid to pH be 1, be configured to the slurries of refractory gold ore.Wherein the preparation technology of solid catalyst is: with industrial iron, copper, manganese oxide, aluminum oxide, silicon oxide under normal temperature, condition of normal pressure, evenly mix, in this process, feed chlorine continuously, make the composition quality per-cent of its finished product be respectively iron 30%, chlorine 30%, oxygen 15%, copper 10%, manganese 5%, silicon 5% and aluminium 5%.
Under 90 ℃ temperature condition, in slurries, feed continuously ozone and oxygen, its feeding amount is respectively 0.8 Grams Per Hour and 0.1 cubic metre/hour, successively stirs, and forms the oxidation ore pulp; Reaction times is 8 hours, reduces to then that room temperature filters to get filtrate and filter residue; According to traditional extraction technique, filter residue is mixed with aqua calcis, transfer to pH value 11, add sodium cyanide and stir 24 hours after-filtration, from filtrate, extract precious metal, to measure according to GB, the leaching yield of gold is 82.65%, the leaching yield of silver is 88.77%.
Embodiment 2
Adopt 1 identical step operation with embodiment, wherein the preparation technology of solid catalyst is: with industrial iron, copper, hydrochloric acid, manganese oxide, aluminum oxide, silicon oxide under normal temperature, condition of normal pressure, evenly mix and close, make the composition quality per-cent of its finished product be respectively iron 30%, chlorine 30%, oxygen 15%, copper 10%, manganese 5%, silicon 5% and aluminium 5%.
Wherein solid catalyst concentration is 280 grams per liters, the weight ratio of sample ore and water is 1: 10, add hydrochloric acid to pH be 1, under 100 ℃ temperature condition, in slurries, feed continuously ozone and air, its feeding amount is respectively 1.2 Grams Per Hours and 0.4 cubic metre/hour, reaction times is 16 hours, according to traditional extraction technique, filter residue is mixed with aqua calcis, transfer to pH value 12, add sodium cyanide and stir 24 hours after-filtration.Measure according to GB, the leaching yield of gold is 98.45%, and the leaching yield of silver is 95.27%.
Embodiment 3
Adopt 1 identical step operation with embodiment, wherein the preparation technology of solid catalyst is: with industrial iron, copper, hydrochloric acid, manganese oxide, aluminum oxide, silicon oxide under normal temperature, condition of normal pressure, evenly mix, make the composition quality per-cent of its finished product be respectively iron 30%, chlorine 30%, oxygen 15%, copper 10%, manganese 5%, silicon 5% and aluminium 5%.
Wherein solid catalyst concentration is 170 grams per liters, the weight ratio of sample ore and water is 1: 6, add sulfuric acid to pH be 3, under 70 ℃ temperature condition, in slurries, feed continuously ozone and air, its feeding amount is respectively 1.0 Grams Per Hours and 0.8 cubic metre/hour, reaction times is 12 hours, according to traditional extraction technique, filter residue is mixed with aqua calcis, transfer to pH value 11, add sodium cyanide and stir 24 hours after-filtration.Measure according to GB, the leaching yield of gold is 68.32%, and the leaching yield of silver is 81.02%.
Embodiment 4
Adopt 1 identical step operation with embodiment, wherein the preparation technology of solid catalyst is: with industrial iron, copper, chlorine, manganese oxide, aluminum oxide, silicon oxide under normal temperature, condition of normal pressure, evenly mix, in this process, feed chlorine continuously, make the composition quality per-cent of its finished product be respectively iron 30%, chlorine 30%, oxygen 15%, copper 10%, manganese 5%, silicon 5% and aluminium 5%.
Wherein solid catalyst concentration is 230 grams per liters, the weight ratio of sample ore and water is 1: 8, add hydrochloric acid to pH be 3, under 100 ℃ temperature condition, in slurries, feed continuously ozone and oxygen, its feeding amount is respectively 0.9 Grams Per Hour and 1.0 cubic metres/hour, reaction times is 8 hours, according to traditional extraction technique, filter residue is mixed with aqua calcis, transfer to pH value 12, add sodium cyanide and stir 24 hours after-filtration.Measure according to GB, the leaching yield of gold is 76.25%, and the leaching yield of silver is 92.19%.

Claims (3)

1. an atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate is characterized in that comprising the steps:
Step 1, in having the reactor of agitator an amount of sample ore of disposable adding, solid catalyst, acid and water, solid catalyst concentration is 151～280 grams per liters, the weight ratio of sample ore and water is 1: 6～1: 10, adds acid to pH value 1～3, is configured to the slurries of refractory gold ore;
Step 2, under 60～100 ℃ temperature condition, in slurries, feed continuously gaseous oxidant: ozone and oxygen, wherein ozone is that 0.8～1.2 Grams Per Hour and oxygen are 0.1～1.0 cubic metre/hour; Or ozone and air, wherein ozone is that 0.8～1.2 Grams Per Hour and air are 0.1～1.0 cubic metre/hour, successively stirs, and forms the oxidation ore pulp, the reaction times is 6～18 hours, reduces to then that room temperature filters to get filtrate and filter residue;
Step 3, according to traditional extraction technique, filter residue mixes with aqua calcis, transfers to pH value 11～12, adds sodium cyanide and stirs 24 hours after-filtration, extracts precious metal from filtrate.
2. a kind of atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate according to claim 1 is characterized in that, the acid described in the step 1 is hydrochloric acid or sulfuric acid.
3. a kind of atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate according to claim 1, it is characterized in that, the preparation technology of the solid catalyst described in the step 1 is: with industrial iron, copper, hydrochloric acid or chlorine, manganese oxide, aluminum oxide, silicon oxide under normal temperature, condition of normal pressure, evenly mix, in this process, if use chlorine, then feed chlorine continuously, make the composition quality per-cent of its finished product be respectively iron 30%, chlorine 30%, oxygen 15%, copper 10%, manganese 5%, silicon 5% and aluminium 5%.
CN2008100389391A 2008-06-13 2008-06-13 Atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate Expired - Fee Related CN101314815B (en)

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CN2008100389391A CN101314815B (en) 2008-06-13 2008-06-13 Atmosphere-pressure catalytic oxidation method for high-sulfur high-arsenic hard washing golden ore concentrate
PCT/CN2008/001924 WO2009149590A1 (en) 2008-06-13 2008-11-25 Atmospherically catalyzing and oxidizing method of refractory gold concentrate with high arsenic and high sulfur
CA2722494A CA2722494C (en) 2008-06-13 2008-11-25 A method for catalytic oxidation of refractory gold concentrate with high contents of sulfur and arsenic under ordinary pressure

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102115814A (en) * 2010-12-14 2011-07-06 哈尔滨工业大学（威海） Normal pressure catalytic oxidation method for refractory polymetallic gold sulfide concentrate
WO2012151721A1 (en) * 2011-05-10 2012-11-15 长春黄金研究院 Wet process for pretreating carbonaceous refractory gold concentrate ore
CN104445076A (en) * 2013-09-12 2015-03-25 气体产品与化学公司 Integrated process for production of ozone and oxygen
CN105349797A (en) * 2014-08-20 2016-02-24 中国科学院过程工程研究所 Method for carrying out pre-treatment desilication gold leaching of gold-containing tailings or cyanidation tailings
CN108034836A (en) * 2017-11-30 2018-05-15 广西大学 The method for pre-oxidizing of sulfide type Gold Concentrate under Normal Pressure

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104313343B (en) * 2014-11-11 2016-02-24 南华大学 A kind of high arsenic leaches gold extracting method containing gold sulfur concentrate oxidizing roasting-microwave-assisted

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4647307A (en) * 1983-01-18 1987-03-03 Rein Raudsepp Process for recovering gold and silver from refractory ores
CN1004426B (en) * 1987-06-22 1989-06-07 中国科学院化工冶金研究所 Catalytic oxidation acid method for pretreating refractory gold concentrate
US5071477A (en) * 1990-05-03 1991-12-10 American Barrick Resources Corporation of Toronto Process for recovery of gold from refractory ores
CN100371478C (en) * 2006-02-11 2008-02-27 欧华北 Wet preprocessing method for difficult-to-treat gold ore containing arsenic and antimony
CN100404707C (en) * 2006-08-03 2008-07-23 山东国大黄金股份有限公司 Method of extracting gold and silver from arsenic containing aurin ore

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102115814A (en) * 2010-12-14 2011-07-06 哈尔滨工业大学（威海） Normal pressure catalytic oxidation method for refractory polymetallic gold sulfide concentrate
CN102115814B (en) * 2010-12-14 2016-04-13 哈尔滨工业大学（威海） The atmosphere-pressure catalytic oxidation method of difficult Gold Concentrates Together With Complicated Metals Sulphides
WO2012151721A1 (en) * 2011-05-10 2012-11-15 长春黄金研究院 Wet process for pretreating carbonaceous refractory gold concentrate ore
CN104445076A (en) * 2013-09-12 2015-03-25 气体产品与化学公司 Integrated process for production of ozone and oxygen
US9371228B2 (en) 2013-09-12 2016-06-21 Air Products And Chemicals, Inc. Integrated process for production of ozone and oxygen
CN105349797A (en) * 2014-08-20 2016-02-24 中国科学院过程工程研究所 Method for carrying out pre-treatment desilication gold leaching of gold-containing tailings or cyanidation tailings
CN105349797B (en) * 2014-08-20 2018-05-22 中国科学院过程工程研究所 A kind of method containing golden tailing or cyanidation tailings pretreatment desiliconization leaching gold
CN108034836A (en) * 2017-11-30 2018-05-15 广西大学 The method for pre-oxidizing of sulfide type Gold Concentrate under Normal Pressure

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CN101314815B (en) 2010-09-08
CA2722494C (en) 2016-04-05
WO2009149590A1 (en) 2009-12-17
CA2722494A1 (en) 2009-12-17

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