CN102021340B - Deep impurity removal technology for coarse gold powder - Google Patents

Deep impurity removal technology for coarse gold powder Download PDF

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CN102021340B
CN102021340B CN2010105727508A CN201010572750A CN102021340B CN 102021340 B CN102021340 B CN 102021340B CN 2010105727508 A CN2010105727508 A CN 2010105727508A CN 201010572750 A CN201010572750 A CN 201010572750A CN 102021340 B CN102021340 B CN 102021340B
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hydrolysis
deionized water
volume
cooling
blowing
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CN102021340A (en
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陈大林
赵彦才
潘从明
李明
张燕
许银风
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Jinchuan Group Co Ltd
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Jinchuan Group Co Ltd
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    • 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
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Abstract

The invention provides a deep impurity removal technology for coarse gold powder, which comprises the following steps: putting the coarse gold powder into a chloridizing leaching reactor according to the liquid-solid ratio of (14-16):1, controlling the acidity of solution to be 3mol/L by adding industrial hydrochloric acid, and leaching by introducing chlorine after the temperature reaches 80-85 DEG C for 10-14 hours; then cooling, discharging and filtering, heating and boiling a filtrate and concentrating the volume to be 25% to 37.5% of the original volume, adding deionized water to the original volume after cooling, stirring for 30-60 minutes, standing for 2 hours and then discharging and filtering; and after hydrolysis, repeatedly operating steps of concentrating, deionized water adding, stirring, standing and filtering to remove impurities by hydrolysis, carrying out gold reduction after 2 to 3 times of hydrolysis treatment, and intensively storing hydrolysis residues. Through the process, the impurity content in the solution not subject to the gold reduction is effectively reduced, and especially the contents of Ag, Sb, Pb and Bi are decreased by 95% or so.

Description

Thick bronze deep impurity-removing technology
Technical field
The present invention relates to hydrometallurgy process in the field of metallurgy, particularly effectively remove the thick bronze deep impurity-removing technology of the impurity elements such as most of silver-colored and antimony in the thick bronze chlorated liquid.
Background technology
The thermal process that adopt are processed copper anode mud more both at home and abroad, my company also was successfully applied to production in 2000 with this technique, mainly be that thick bronze by parting process output is through electrolysis output gold, it is assorted that principle technique is that copper anode mud sulfurization roasting-acidleach divides copper-alkali to soak a minute tellurium-chlorination parting-reduce thick bronze-liquid making electrolysis-electrolyzing gold plate-boil eccysis, this gold production process is tediously long, the requirement of impurity content is high to reducing in the thick bronze, and particularly impurity element silver is difficult to control in the electrolyzing gold plate.Because the in recent years significantly rising of impurity element in the copper raw material, soak operation and produce thick bronze quality and obviously descend so that process the roasting of copper anode mud, being mainly the impurity contents such as argentiferous, lead, antimony, bismuth increases, and finally causes the gold product difficult quality of electrolysis output up to standard.For this reason, having adopted a kind of new wet processing to replace electrolytic process that thick bronze is carried out refining principle technique is that removal of impurities is boiled in thick bronze aqueous solution chlorination-oxalic acid reduction-acid, but the too high levels owing to silver and antimony in the thick bronze, the bronze quality that restores still can not reach the requirement of GB IC-Au99.99, therefore, the novel process of seeking a kind of thick bronze deep impurity-removing has seemed very urgent.
Summary of the invention
Purpose of the present invention will be eliminated above-mentioned the deficiencies in the prior art and shortcoming exactly, provides a kind of energy can effectively remove the thick bronze deep impurity-removing technology of the impurity elements such as most of silver-colored and antimony in the thick bronze chlorated liquid.
In order to achieve the above object, the invention provides a kind of thick bronze deep impurity-removing technology of a kind of thick bronze deep impurity-removing technology, thick bronze is dropped in the chlorination leaching kettle, the ratio of the volume of liquid-solid ratio 14-16:1(liquid and the quality of solid, wherein liquid volume unit is for rising, solid masses unit is kilogram), adding technical hydrochloric acid control solution acidity is 3mol/L, temperature is that 80~85 ℃ of laggard chlorine that work leach, time 10~14h, then cooling off blowing filters, the intensification of above-mentioned filtrate is boiled, concentrated volume fills into deionized water to the stoste volume to original volume 25%~37.5% after the cooling, stir 30~60min, blowing filters after leaving standstill 2h, concentrated after the hydrolysis-as to add deionized water-stir-leave standstill to filter the repeatable operation like this removal of impurities that is hydrolyzed, after 2~3 times hydrolysis treatment repeatedly, can carry out gold and reduce, hydrolysis residue is left concentratedly.
Sb, Bi are amphiprotic substance, and be unstable in acidic solution, and facile hydrolysis generates precipitation.In hydrolytic process, add deionized water, [H in the solution +] reduce, the pH value increases, the SbCl in the solution 3, BiCl 3Be hydrolyzed, form flaxen throw out:
SbCl 3+H 2O?SbOCl↓+2HCl
BiCl 3+H 2O?BiOCl↓+2HCl
When chlorination was leached, most Pb entered in the insoluble slag with the insolubles form and separates with Au, but had the Pb of trace in the solution 2+Unstable, meeting and steeping in water for reconstitution unboiled water solution, the throw out of formation lead hydroxide:
Pb 2++2H 2O?Pb(OH) 2↓+2H +
Simultaneously, after adding deionized water, [the Cl in the solution -] and [AgCl 2 -] reduce, and the former reduction amplitude is larger, and balance is moved to the left side, AgCl in the chlorated liquid 2 -Be converted into the AgCl white precipitate:
AgCl+?Cl ?AgCl 2
Owing to raise with temperature, the solubleness of silver chloride increases, so hydrolytic process is carried out at normal temperatures.
Through this technique, effectively reduced before the gold reduction in the liquid content of foreign matter content, especially Ag, Sb, Pb, Bi about 95%.
Beneficial effect of the present invention:
Figure 2010105727508100002DEST_PATH_IMAGE002
. the invention provides a kind of to the be hydrolyzed technique of deep impurity-removing of thick bronze chloridizing leach solution, the present invention has carried out the deep purifying removal of impurities to refinery practice in the thick bronze and has improved, thick bronze is behind aqueous solution chlorination, adopted the hydrolysis impurity removal process, utilize acidity and ionic concn to change, remove the impurity elements such as wherein a large amount of Ag, Pb, Sb, Bi.
Figure 2010105727508100002DEST_PATH_IMAGE004
. the present invention can make the most of impurity content in the thick bronze chlorated liquid reduce widely, and especially silver reduces more than 95% with antimony; Behind the hydrolysis deep impurity-removing, the impurity of impact reduction reduces in a large number in the chlorated liquid, is conducive to subsequent handling; Chlorated liquid is purified through reduction again, and directly output meets the gold product of GB IC-Au99.99.
Embodiment
Embodiment 1:
Thick bronze drops in the chlorination leaching kettle, control liquid-solid ratio 14:1, and adding technical hydrochloric acid control solution acidity is 3mol/L, and volume is 800L, and temperature is that 80 ℃ of laggard chlorine that work leach, and then time 12h cools off blowing and filters.Filtrate is changed in the hydrolysis kettle, intensification is boiled, concentrated volume is to 200L, cooling fills into deionized water to stoste volume 800L, stirs 30min, blowing filters after leaving standstill 2h, after the hydrolysis liquid changes in the hydrolysis kettle concentrated-add that deionized water-stir-leaving standstill filtration carries out gold reduction after 3 times hydrolysis treatment so repeatedly, hydrolysis residue is left concentratedly, silver, lead, antimony, bi content reduction by 94.2%.
Embodiment 2:
Thick bronze drops in the chlorination leaching kettle, control liquid-solid ratio 15:1, and adding technical hydrochloric acid control solution acidity is 3mol/L, and volume is 800L, and temperature is that 85 ℃ of laggard chlorine that work leach, and then time 10h cools off blowing and filters.Filtrate is changed in the hydrolysis kettle, intensification is boiled, concentrated volume is to 300L, cooling fills into deionized water to stoste volume 800L, stirs 60min, blowing filters after leaving standstill 2h, after the hydrolysis liquid changes in the hydrolysis kettle concentrated-add that deionized water-stir-leaving standstill filtration carries out gold reduction after 2 times hydrolysis treatment so repeatedly, hydrolysis residue is left concentratedly, silver, lead, antimony, bi content reduction by 95.1%.
Embodiment 3:
Thick bronze drops in the chlorination leaching kettle, control liquid-solid ratio 16:1, and adding technical hydrochloric acid control solution acidity is 3mol/L, and volume is 800L, and temperature is that 83 ℃ of laggard chlorine that work leach, and then time 14h cools off blowing and filters.Filtrate is changed in the hydrolysis kettle, intensification is boiled, concentrated volume is to 260L, cooling fills into deionized water to stoste volume 800L, stirs 50min, blowing filters after leaving standstill 2h, after the hydrolysis liquid changes in the hydrolysis kettle concentrated-add that deionized water-stir-leaving standstill filtration carries out gold reduction after 3 times hydrolysis treatment so repeatedly, hydrolysis residue is left concentratedly, silver, lead, antimony, bi content reduction by 94.7%.
Embodiment 4:
Thick bronze drops in the chlorination leaching kettle, control liquid-solid ratio 14:1, and adding technical hydrochloric acid control solution acidity is 3mol/L, and volume is 800L, and temperature is that 81 ℃ of laggard chlorine that work leach, and then time 13h cools off blowing and filters.Filtrate is changed in the hydrolysis kettle, intensification is boiled, concentrated volume is to 220L, cooling fills into deionized water to stoste volume 800L, stirs 40min, blowing filters after leaving standstill 2h, after the hydrolysis liquid changes in the hydrolysis kettle concentrated-add that deionized water-stir-leaving standstill filtration carries out gold reduction after 3 times hydrolysis treatment so repeatedly, hydrolysis residue is left concentratedly, silver, lead, antimony, bi content reduction by 95.3%.
Above-described only is preferred embodiment of the present invention; should be understood that for the person of ordinary skill of the art, under technology enlightenment provided by the present invention, as the common practise of this area; other equivalent modifications and improvement can also be made, also protection scope of the present invention should be considered as.

Claims (1)

1. thick bronze deep impurity-removing method, it is characterized in that: thick bronze drops in the chlorination leaching kettle, add technical hydrochloric acid control solution acidity and temperature and lead to the chlorine leaching, reacting complete rear cooling blowing filters, filtrate is hydrolyzed, it is concentrated to heat up, filling into deionized water to stoste volume after the cooling stirs, leaving standstill rear blowing filters, concentrated after the hydrolysis-as to add deionized water-stir-leave standstill to filter the repeatable operation like this removal of impurities that is hydrolyzed, through repeatedly carrying out the gold reduction after 2~3 times hydrolysis treatment, hydrolysis residue is left concentratedly, and specific embodiment and processing parameter are as follows:
A. thick bronze is dropped in the chlorination leaching kettle liquid-solid ratio 14-16 liter: 1 kilogram, adding technical hydrochloric acid control solution acidity is 3mol/L, and temperature is that 80~85 ℃ of laggard chlorine that work leach, and then time 10~14h cools off blowing and filter;
B. filtrate among the step a is heated up and boiled, concentrated volume fills into deionized water to the stoste volume to original volume 25%~37.5% after the cooling, stir 30~60min, leave standstill 2h after blowing filter;
C. carry out the gold reduction behind the repeating step b 2~3 times, hydrolysis residue is left concentratedly.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107576754A (en) * 2017-07-27 2018-01-12 长春黄金研究院 A kind of Cupper determination method in thick gold
CN107604176A (en) * 2017-07-28 2018-01-19 云南铜业股份有限公司 A kind of method that high-purity bronze is extracted from copper anode mud and high-purity bronze
CN110205500B (en) * 2019-06-18 2021-09-17 山东黄金冶炼有限公司 Method for removing impurities in reduced gold powder

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1442498A (en) * 2003-04-11 2003-09-17 山东黄金集团有限公司焦家金矿 Method of crude gold purification
CN101570830A (en) * 2009-06-10 2009-11-04 宋裕华 Extraction method of high-purity gold

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1442498A (en) * 2003-04-11 2003-09-17 山东黄金集团有限公司焦家金矿 Method of crude gold purification
CN101570830A (en) * 2009-06-10 2009-11-04 宋裕华 Extraction method of high-purity gold

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