CN106222436A - A kind of microwave extract method of magnetic iron ore - Google Patents

A kind of microwave extract method of magnetic iron ore Download PDF

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Publication number
CN106222436A
CN106222436A CN201610715820.8A CN201610715820A CN106222436A CN 106222436 A CN106222436 A CN 106222436A CN 201610715820 A CN201610715820 A CN 201610715820A CN 106222436 A CN106222436 A CN 106222436A
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iron ore
magnetic iron
microwave
solution
extract method
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袁再六
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TONGREN CITY WANSHANG DISTRICT SHENGHE MINING INDUSTRY Co Ltd
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TONGREN CITY WANSHANG DISTRICT SHENGHE MINING INDUSTRY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/045Leaching using electrochemical processes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention belongs to technical field of wet metallurgy, particularly relate to the microwave extract method of a kind of magnetic iron ore.By in magnetic iron ore pre-treatment step, in solution, redox potential current potential is controlled, the loss rate making gold is less than one thousandth, and further in leaching operation, utilizes the distinctive character of microwave, microwave action is on material molecule, make molecular motion accelerate and mutually friction occurs, producing amount of heat, thus accelerate reaction, substantially reduce the response time, improve production efficiency.And substantially increase the leaching rate of gold.

Description

A kind of microwave extract method of magnetic iron ore
Technical field
The present invention relates to technical field of wet metallurgy, it particularly relates to the microwave extract method of a kind of magnetic iron ore.
Background technology
Gold is accompanied by mineral and gives birth to, and such as sulfide gold mine, particularly may be divided into pyrite, magnetic iron ore, arsenical pyrite Etc. ore resource.Further, gold existing forms predominantly submicron-sized particulate in Ore is combined closely with iron mine, and this ultra micro Particulate is tiny to time micro-grade, and then most gold is embedded in the molecular grating of Ore, is formed with Ore and dissolves each other Body;This feature makes Ore when by mechanical lapping or pulverizing, is crushed to maximum fineness in time and is also difficult to make gold from Ore Coming out, the especially gold in magnetic iron ore is more difficult to come out in being attracted to crystal inside grid, and then is difficult to shape Become the gold grain of Free Surface, when causing taking solution leach so that liquid medicine is difficult to contact with golden surface, be the most just difficult to and The biochemical reaction of golden hair and dissolved.
To this end, there is researcher just by research, by exposed for the gold in sulfide ore outside, i.e. pass through pre-treatment step By exposed for gold out, but when taking such measure, the technology often using redox reaction is carried out, at solution In will form potential, and according to general knowledge, different potential will draw different reaction results, or draws Product and consumption of raw materials thing are the most different, and how by Ore, especially magnetic iron ore Ore carries out pretreatment so that big The gold of amount is extracted golden crucial problem by exposed out becoming from magnetic iron ore.It addition, prior art is extracted from solution Au plasma rate is relatively low, is 80~90%, and substantial amounts of gold element is drained off with waste liquid, causes waste.
Based on above-mentioned technical problem, this researcher, in the research of early stage, enters for extracting the technique of gold from magnetic iron ore Row new selection and exploratory development, for enable the gold in magnetic iron ore substantial amounts of by exposed out, and then be follow-up leaching, Enrichment, separation offer basis, and then reduction are extracted the cost of gold from magnetic iron ore and are provided one preprocess method.The present invention Purpose be to study further on the basis of early-stage Study, improve Au plasma rate.
Summary of the invention
In view of this, the present invention, by being optimized technique above, to improve Au plasma rate, obtains bigger warp Ji benefit.
The present invention solves above-mentioned technical problem by the following technical programs:
The microwave extract method of a kind of magnetic iron ore, comprises the following steps:
(1) pretreatment: it is 80~200 mesh that magnetic iron ore is crushed to fineness, it is thus achieved that magnetic iron ore powder is sent in reactive tank, In reactive tank, add magnetic iron ore powder 1~the salpeter solution of 3 times of weight, and to use the mixing speed of agitator be 40~70r/ Min stir process 1~2h, then it is added thereto to salpeter solution 0.7~the sodium nitrite of 0.9 times of weight, and continue stir process After 20~30min, being placed on temperature is that in 60~70 DEG C, standing processes 10~20min, then is added thereto to hydrogen peroxide, its The consumption of middle hydrogen peroxide is 1~1.3 times of sodium nitrite weight, and controls after solution temperature is 50~60 DEG C, then with calomel Electrode as reference electrode, the potential in measuring point solution, and the potential in solution is adjusted and control≤ 450mV so that it is after sustained response 3~4h, it is thus achieved that pretreatment slip, stand-by;
(2) leach: the hydrochloric acid of 1~2 times of addition slip weight in the slip that pretreatment obtains, add again after stirring Enter the 4 of slip weight~the calcium hypochlorite of 6%, then send in microwave reaction kettle and carry out microwave treatment 20~40min, the most quiet Filter after putting process 20~40min, it is thus achieved that containing gold filtrate;
(3) enrichment: the filtrate containing gold obtained is sent in agitator tank, and in agitator tank, add hydrochloric acid consumption 1~2 times Basic anionic resin solution, and to use mixing speed be to filter after 50~60r/min stir process 1~3h, it is thus achieved that containing gold filter Slag;
(4) separate: gold filtering residue will be contained and send in parsing groove, and be added thereto to containing gold filtering residue weight 1~the thiourea of 3 times Solution, and after using mixing speed to be 60~80r/min stir process 30~60min, then it is added thereto to reducing agent, adjust and solve Temperature in analysis groove is 80~90 DEG C, after being 80~90r/min stir process 20~30min with mixing speed, filters, will The filtering residue obtained is dried, and obtains bronze.
The concentration of described salpeter solution is 2~3mol/L.
Described sodium nitrite is the powder of 300~400 mesh.
Described calcium hypochlorite is the powder of 300~400 mesh.
The molar concentration of described hydrochloric acid is 1.5~2.5mol/L.
During described microwave treatment, the power of microwave is 2~8kw.
Described basic anionic resin solution is-N (CH3) 3OH.
The molar concentration of described-N (CH3) 3OH is 1~3mol/L.
The molar concentration of described thiourea solution is 1~2mol/L.
Described reducing agent is white phosphorus.
The consumption of described white phosphorus is 10~30% containing gold filtering residue weight.
The beneficial effects of the present invention is:
First, by magnetic iron ore pre-treatment step, in solution, redox potential current potential is controlled so that molten Redox potential in liquid maintains below 450mv, and then Surface of Pyrrhotite material is reached by extrusion rate More than 85%, also reduce the gold loss rate in pre-treatment step less than one thousandth simultaneously, and then ensure that from magnetic yellow Iron mine extracts Au plasma rate.
Secondly, the present invention by, in leaching operation, utilizing the distinctive character of microwave, microwave action on material molecule, Make molecular motion accelerate and mutually friction occurs, producing amount of heat, thus accelerate reaction, substantially reduce the response time, carry High production efficiency.And substantially increase the leaching rate of gold, reach more than 97%.
Again, by the strict control of technological parameter in each step so that Au plasma rate reaches more than 96%.
Detailed description of the invention
Those skilled in the art understands for convenience, and below in conjunction with embodiment, the present invention will be further described. Embodiment is only the illustration to this invention, is not limitation of the invention, does not makees the step illustrated in embodiment It is all prior art, is not described in detail at this.
Embodiment one
The microwave extract method of a kind of magnetic iron ore, comprises the following steps:
(1) pretreatment: it is 80 mesh that magnetic iron ore is crushed to fineness, it is thus achieved that magnetic iron ore powder is sent in reactive tank, to instead Answering the concentration adding 1 times of weight of magnetic iron ore powder in groove is 2mol/L salpeter solution, and uses the mixing speed of agitator to be 40r/min stir process 1h, then it is added thereto to the sodium nitrite that fineness is 300 mesh of 0.7 times of weight of salpeter solution, and continue After stir process 20min, being placed on temperature is that in 60 DEG C, standing processes 10min, then is added thereto to hydrogen peroxide, wherein mistake The consumption of hydrogen oxide is 1 times of sodium nitrite weight, and controls after solution temperature is 50 DEG C, then using calomel electrode as reference electricity Pole, the potential in measuring point solution, and the potential in solution is adjusted and controls at≤450mV so that it is sustained response After 3h, it is thus achieved that pretreatment slip, stand-by;
(2) leach: the salt that molar concentration is 1.5mol/L of 1 times of addition slip weight in the slip that pretreatment obtains Acid, add after stirring slip weight 4% the calcium hypochlorite that fineness is 300 mesh, then send in microwave reaction kettle Carrying out microwave treatment, the power of microwave is 2kw, and the process time is 20min, filters after then standing processes 20min, it is thus achieved that containing gold Filtrate;
(3) enrichment: the filtrate containing gold obtained is sent in agitator tank, and adds rubbing of hydrochloric acid consumption 1 times in agitator tank Your concentration is-N (CH3) the 3OH solution of 1mol/L, and to use mixing speed be to filter after 50r/min stir process 1h, it is thus achieved that contain Gold filtering residue;
(4) separate: gold filtering residue will be contained and send in parsing groove, and be added thereto to the molar concentration containing gold filtering residue weight 1 times For the thiourea solution of 1mol/L, and after using mixing speed to be 60r/min stir process 30min, then it is added thereto to white phosphorus, in vain The consumption of phosphorus is 10% containing gold filtering residue weight, and adjusting the temperature resolved in groove is 80 DEG C, stirs with mixing speed for 80r/min After processing 20min, filter, the filtering residue obtained is dried, obtains bronze.
Through test, using this programme Au plasma rate is 96.1%.
Embodiment two
The microwave extract method of a kind of magnetic iron ore, comprises the following steps:
(1) pretreatment: it is 200 mesh that magnetic iron ore is crushed to fineness, it is thus achieved that magnetic iron ore powder is sent in reactive tank, to instead Answering the concentration adding 3 times of weight of magnetic iron ore powder in groove is 3mol/L salpeter solution, and uses the mixing speed of agitator to be 70r/min stir process 2h, then the fineness being added thereto to 0.9 times of weight of salpeter solution is 400 mesh sodium nitrite, and continue to stir After mixing process 30min, being placed on temperature is that in 70 DEG C, standing processes 20min, then is added thereto to hydrogen peroxide, wherein peroxide Change consumption is sodium nitrite weight 1.3 times of hydrogen, and control after solution temperature is 60 DEG C, then using calomel electrode as reference electricity Pole, the potential in measuring point solution, and the potential in solution is adjusted and controls at≤450mV so that it is sustained response After 4h, it is thus achieved that pretreatment slip, stand-by;
(2) leach: the salt that molar concentration is 2.5mol/L of 2 times of addition slip weight in the slip that pretreatment obtains Acid, add after stirring slip weight 6% the calcium hypochlorite that fineness is 400 mesh, then send in microwave reaction kettle Carrying out microwave treatment, the power of microwave is 8kw, and the process time is 40min, filters after then standing processes 40min, it is thus achieved that containing gold Filtrate;
(3) enrichment: the filtrate containing gold obtained is sent in agitator tank, and adds rubbing of hydrochloric acid consumption 2 times in agitator tank Your concentration is-N (CH3) the 3OH solution of 3mol/L, and to use mixing speed be to filter after 60r/min stir process 3h, it is thus achieved that contain Gold filtering residue;
(4) separate: gold filtering residue will be contained and send in parsing groove, and be added thereto to the molar concentration containing gold filtering residue weight 3 times For the thiourea solution of 2mol/L, and after using mixing speed to be 80r/min stir process 60min, then it is added thereto to white phosphorus, in vain The consumption of phosphorus is 10~30% containing gold filtering residue weight, and adjusting the temperature resolved in groove is 90 DEG C, with mixing speed as 90r/min After stir process 30min, filter, the filtering residue obtained is dried, obtains bronze.
Through test, using this programme Au plasma rate is 96.5%.
Embodiment three
The microwave extract method of a kind of magnetic iron ore, comprises the following steps:
(1) pretreatment: it is 120 mesh that magnetic iron ore is crushed to fineness, it is thus achieved that magnetic iron ore powder is sent in reactive tank, to instead Answering the concentration adding 2 times of weight of magnetic iron ore powder in groove is 2.5mol/L salpeter solution, and uses the mixing speed of agitator to be 50r/min stir process 1.5h, then the fineness being added thereto to 0.8 times of weight of salpeter solution is 350 mesh sodium nitrite, and continue After stir process 25min, being placed on temperature is that in 65 DEG C, standing processes 15min, then is added thereto to hydrogen peroxide, wherein mistake The consumption of hydrogen oxide is 1.2 times of sodium nitrite weight, and controls after solution temperature is 55 DEG C, then using calomel electrode as reference Electrode, the potential in measuring point solution, and the potential in solution is adjusted and controls at≤450mV so that it is continue anti- After answering 3.5h, it is thus achieved that pretreatment slip, stand-by;
(2) leach: the salt that molar concentration is 2mol/L of 1.5 times of addition slip weight in the slip that pretreatment obtains Acid, add after stirring slip weight 5% the calcium hypochlorite that fineness is 350 mesh, then send in microwave reaction kettle Carrying out microwave treatment, the power of microwave is 5kw, and the process time is 30min, filters after then standing processes 30min, it is thus achieved that containing gold Filtrate;
(3) enrichment: the filtrate containing gold obtained is sent in agitator tank, and adds hydrochloric acid consumption 1.5 times in agitator tank Molar concentration is-N (CH3) the 3OH solution of 2mol/L, and to use mixing speed be to filter after 55r/min stir process 2h, it is thus achieved that Containing gold filtering residue;
(4) separate: gold filtering residue will be contained and send in parsing groove, and be added thereto to the molar concentration containing gold filtering residue weight 2 times For the thiourea solution of 1.5mol/L, and after using mixing speed to be 70r/min stir process 40min, then it is added thereto to white phosphorus, The consumption of white phosphorus is 20% containing gold filtering residue weight, and adjusting the temperature resolved in groove is 85 DEG C, stirs with mixing speed for 85r/min After mixing process 25min, filter, the filtering residue obtained is dried, obtains bronze.
Through test, using this programme Au plasma rate is 96.8%.

Claims (10)

1. the microwave extract method of a magnetic iron ore, it is characterised in that comprise the following steps:
(1) pretreatment: it is 80~200 mesh that magnetic iron ore is crushed to fineness, it is thus achieved that magnetic iron ore powder is sent in reactive tank, to instead Answer and groove adds magnetic iron ore powder 1~the salpeter solution of 3 times of weight, and to use the mixing speed of agitator be 40~70r/min Stir process 1~2h, then be added thereto to salpeter solution 0.7~the sodium nitrite of 0.9 times of weight, and continue stir process 20~ After 30min, being placed on temperature is that in 60~70 DEG C, standing processes 10~20min, then is added thereto to hydrogen peroxide, wherein mistake The consumption of hydrogen oxide is 1~1.3 times of sodium nitrite weight, and controls after solution temperature is 50~60 DEG C, then with calomel electrode As reference electrode, the potential in measuring point solution, and the potential in solution is adjusted and controls, at≤450mV, to make After its sustained response 3~4h, it is thus achieved that pretreatment slip, stand-by;
(2) leach: the hydrochloric acid of 1~2 times of addition slip weight in the slip that pretreatment obtains, after stirring, add material 4~the calcium hypochlorite of 6% of slurry weight, then sends in microwave reaction kettle and carries out microwave treatment 20~40min, then at standing Filter after reason 20~40min, it is thus achieved that containing gold filtrate;
(3) enrichment: the filtrate containing gold obtained is sent in agitator tank, and adds hydrochloric acid consumption 1~the alkalescence of 2 times in agitator tank Resin anion (R.A.) solution, and to use mixing speed be to filter after 50~60r/min stir process 1~3h, it is thus achieved that containing gold filtering residue;
(4) separate: gold filtering residue will be contained and send in parsing groove, and be added thereto to containing gold filtering residue weight 1~the thiourea solution of 3 times, And after using mixing speed to be 60~80r/min stir process 30~60min, then it is added thereto to reducing agent, adjust and resolve groove In temperature be 80~90 DEG C, after being 80~90r/min stir process 20~30min with mixing speed, filter, will obtain Filtering residue dry, obtain bronze.
2. the microwave extract method of magnetic iron ore as claimed in claim 1, it is characterised in that: the concentration of described salpeter solution It is 2~3mol/L.
3. the microwave extract method of magnetic iron ore as claimed in claim 1, it is characterised in that: described sodium nitrite is 300 ~400 powder of mesh.
4. the microwave extract method of magnetic iron ore as claimed in claim 1, it is characterised in that: described calcium hypochlorite is 300 ~400 powder of mesh.
5. the microwave extract method of magnetic iron ore as claimed in claim 1, it is characterised in that: the molar concentration of described hydrochloric acid is 1.5~2.5mol/L.
6. the microwave extract method of magnetic iron ore as claimed in claim 1, it is characterised in that: during described microwave treatment, microwave Power be 2~8kw.
7. the microwave extract method of magnetic iron ore as claimed in claim 1, it is characterised in that: described basic anionic resin Solution is-N (CH3) 3OH, and its molar concentration is 1~3mol/L.
8. the microwave extract method of magnetic iron ore as claimed in claim 1, it is characterised in that: described thiourea solution mole Concentration is 1~2mol/L.
9. the microwave extract method of magnetic iron ore as claimed in claim 1, it is characterised in that: described reducing agent is white phosphorus.
10. the microwave extract method of magnetic iron ore as claimed in claim 9, it is characterised in that: the consumption of described white phosphorus is for containing The 10~30% of gold filtering residue weight.
CN201610715820.8A 2016-08-24 2016-08-24 A kind of microwave extract method of magnetic iron ore Pending CN106222436A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107385208A (en) * 2017-07-31 2017-11-24 中南大学 A kind of microwave radiation technology, which is strengthened, soaks golden method
CN109957661A (en) * 2019-04-29 2019-07-02 中南大学 A kind of microwave reinforced method for recycling chromium from nickel-iron smelting slag and preparing light heat-insulating material
CN110898987A (en) * 2019-11-13 2020-03-24 鞍钢集团矿业有限公司 Oxidation desulfurization method of high-sulfur magnetite concentrate

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CN105036431A (en) * 2015-08-05 2015-11-11 铜仁市万山区盛和矿业有限责任公司 Method for treating mine iron-containing wastewater
CN105084395A (en) * 2015-08-05 2015-11-25 铜仁市万山区盛和矿业有限责任公司 Method for producing soluble potassium through potassium feldspar

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103343224A (en) * 2013-07-29 2013-10-09 沈少波 Method for quickly extracting gold from gold-containing material
CN103552996A (en) * 2013-10-21 2014-02-05 东北大学 Method for reclaiming tellurium from copper anode slime by microwave acid leaching
CN104263962A (en) * 2014-09-23 2015-01-07 铜仁市万山区盛和矿业有限责任公司 Method for extracting gold from pyrrhotite
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107385208A (en) * 2017-07-31 2017-11-24 中南大学 A kind of microwave radiation technology, which is strengthened, soaks golden method
CN107385208B (en) * 2017-07-31 2019-05-17 中南大学 A kind of microwave-assisted golden method of reinforcing leaching
CN109957661A (en) * 2019-04-29 2019-07-02 中南大学 A kind of microwave reinforced method for recycling chromium from nickel-iron smelting slag and preparing light heat-insulating material
CN109957661B (en) * 2019-04-29 2020-11-20 中南大学 Method for recovering chromium from ferronickel smelting slag and preparing light heat-insulating material by microwave reinforcement
CN110898987A (en) * 2019-11-13 2020-03-24 鞍钢集团矿业有限公司 Oxidation desulfurization method of high-sulfur magnetite concentrate

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