CN102618885A - Auxiliary reagent suitable for rapid electrorefining of high-silver alloyed gold - Google Patents
Auxiliary reagent suitable for rapid electrorefining of high-silver alloyed gold Download PDFInfo
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- CN102618885A CN102618885A CN2012101087520A CN201210108752A CN102618885A CN 102618885 A CN102618885 A CN 102618885A CN 2012101087520 A CN2012101087520 A CN 2012101087520A CN 201210108752 A CN201210108752 A CN 201210108752A CN 102618885 A CN102618885 A CN 102618885A
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- auxiliary reagent
- silver
- electrorefining
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Abstract
The invention relates to the field of gold electrorefining purification, in particular to an auxiliary reagent suitable for rapid electrorefining of high-silver alloyed gold. The auxiliary reagent QJ-D-1 for gold electrolysis is a mixture composed of 15-80% of ammonium chloride, 15-80% of potassium chloride, and 0.5-5% of sodium methylene dinaphthalene disulfonate serving as a dispersing agent. According to the invention, the severe anodic passivation phenomenon in the electrolysis process of the high-silver alloyed gold is reduced, the electrolysis efficiency of the high-silver sample is improved, the concentration of hydrochloric acid in the electrolyte is reduced to lower than 2 mol/L, and the environmental pollution is reduced. Alloyed gold with Ag content of 5-10% is directly electrolyzed, the quality of the product obtained after one-time electrolysis meets the requirements of national 1# standard gold and 2# standard gold, the yield of cathode gold within 40 hours is approximate to 70%, the residual anode rate is less than 20%, and the metal balance recovery rate is 99.92%.
Description
Technical field
The present invention relates to the field that a kind of gold electrorefining is purified, particularly relate to the silver-colored gold containing material quick electrolysis of a kind of suitable height purified auxiliary reagent.
Background technology
The method of gold purification is a lot, wherein mainly comprises pyrogenic process oxidation refining, chlorination refining method, electrolytic refining process, chemical refining method, solvent refined method etc.Wherein, electrolytic process has that technology is simple, the advantage of constant product quality, and Production Flow Chart is long, the gold problem that excessive inventory but exist simultaneously.In order to overcome the deficiency that the traditional electrical solution exists, development in recent years quick electrolysis technology, make the electrolytic efficiency of gold obtain raising by a relatively large margin.But the most deleterious composition is a silver in the electrolytic process anode gold, and the silver in the anode gold becomes the Silver monochloride shell and sticks on the positive plate, and electrolytic efficiency is reduced significantly; When if the silver amount is too high, make the anode gold produce passivation, hinder the continuation dissolving of anode gold, and make anode separate out chlorine, cause gold ion dilution in the electrolytic solution simultaneously, production rate slows down.In order to solve the harm of silver, at present when the electrorefining of gold toward electrolyzer in input AC electricity in the input dc power, the pulsatory current of formation imparity; Perhaps adopt automatic commutation technology of cycle, make negative switching of electric current of positive plate, make and produce a large amount of gases on the anode, the Silver monochloride shell receives gas percussion to become loose, can reduce the anode passivation degree to a certain extent, improves the electrolytic efficiency of high silver anode gold.In addition, improve the concentration of hydrochloric acid in the electrolytic solution, make part A gCl deposition form AgCl
2 -Also can improve the electrolytic efficiency of high silver anode gold to a certain extent.
But no matter take which kind of technology at present, in electro deposition gold process, the content of silver is controlled in 5% (m/m) usually in the anode gold, and silver measures too that Gao Zehui makes electrolysing period long, and production efficiency is low.In addition, select high acidity condition electrolysis usually in order to improve electrolytic efficiency, the concentration of hydrochloric acid is generally 4-6molL in the electrolytic solution
-1, because higher electrolyte acidity, stronger volatility is arranged in electrolytic process, there are problems such as environmental pollution and Working environment be relatively poor.
Summary of the invention
In order to overcome the deficiency that prior art exists, the present invention provides a kind of high silver-colored gold containing material quick electrolysis purified auxiliary reagent that is suitable for.
It is following that the present invention solves the technical scheme that its technical problem underlying takes: a kind ofly be suitable for high silver-colored gold containing material quick electrolysis purified auxiliary reagent, golden electrolysis auxiliary reagent QJ-D-1 is by ammonia chloride (NH
4Cl), the compounding substances formed of Repone K (KCl) and diffusant methylene-bis bitter edible plant sodium sulfonate (NNO), the massfraction proportional range of this each component of electrolysis auxiliary reagent: NNO:0.5-5%, NH
4Cl:15-80%, KCl:15-80%.
The concentration of gold electrolysis auxiliary reagent QJ-D-1 in electrolytic solution is 80-120gL
-1
The invention has the beneficial effects as follows, adopt golden electrolysis auxiliary reagent QJ-D-1 can effectively improve the content of silver in the electro deposition gold desired raw material gold containing material, effectively eliminate anode passivation phenomenon and raising electrolytic efficiency that Silver monochloride causes; Adding golden electrolysis auxiliary reagent QJ-D-1 simultaneously can make electrolyte acidity by traditional 4-5molL
-1HCl is reduced to 2molL
-1Below, reduced the consumption and the environmental pollution of reagent, significant environmental benefit is arranged.
In order to solve adhering in a large number owing to silver nitride precipitation on the anode in the high silver anode gold electrolytic process; Cause the serious passivation of anode; Make the significantly reduced problem of electrode efficiency, the present invention has taked in electrolytic process, in electrolytic solution, to add the technical scheme of a certain amount of diffusant methylene-bis bitter edible plant sodium sulfonate.NNO is a kind of macromole salt of processable, and its negatively charged ion is for having surface-active macromole negatively charged ion.This diffusant is added electrolytic solution, can form one deck macromole anionic membrane on the gold anode surface on the one hand, stop the Silver monochloride shell and fine and close adhesion of anode gold that produce in the electrolytic process to cause anode passivation; The existence of diffusant can make silver nitride precipitation become loose on the other hand, is beneficial to attached to the Silver monochloride on the anode gold freely to come off.So anode passivation degree obviously reduces, and has improved the electrolytic efficiency of high silver anode gold.
In order to solve the environmental pollution that causes in the high acidity electrolytic solution electrolytic process, the mixing salt with ammonia chloride and Repone K in electrolytic process substitutes the hydrochloric acid in the part electrolytic solution.On the one hand the concentration of hydrochloric acid in the electrolytic solution is effectively reduced, reduce the environmental pollution that the volatilization of hydrochloric acid causes in the electrolytic process; Add chloride salt on the other hand, because a large amount of cl ionss and " salt effect " of existence are provided, the solubleness of silver nitride precipitation is increased, the formation speed of having slowed down silver nitride precipitation on the anode gold has improved electrolytic efficiency.
Embodiment
Embodiment one: the electrolysis of argentiferous about 5% (m/m) gold containing material
Choose gold containing material, wherein contain Au 93.5%, Ag 4.8%, and Cu 0.56%, and Ni 0.92%, and Fe 0.13%, and Pb 0.02%, and the content of 12 elements such as Zn, As, Sb, Cr, Mn, Sn, Mg carries out electrolysis all less than 0.005%.
Drop into woollen weight 32Kg, amounting to Cheng Chunchong is 29.8Kg, gold ion concentration 90-120gL in the preparing electrolyte
-1, concentration of hydrochloric acid 1.5-2molL
-1, electrolysis auxiliary reagent QJ-D-1 consists of 1.0%NNO+19% NH
4Cl+80%KCl, the concentration of golden electrolysis auxiliary reagent QJ-D-1 in electrolytic solution is 80gL
-1, electrolyte temperature 45-55 ℃, electrolysis time 36h.
The electrolysis concrete steps are following:
The first step: preparation chlorauric acid solution
Greater than 99.95% bronze 5000-6000g, place double-layer glass reaction kettle with purity, in airtight negative pressure system, use 6molL
-1HCl and 14molL
-1HNO
3Dissolving preparation electrolyte.
Described Au, HCl and HNO
3Ratio be: 4: 16: 1, the quality of Au wherein for dropping into, unit be kilogram (Kg); The volume of HCl for dropping into, unit is for rising (L), and concentration is 6molL
-1HNO
3Be the volume that drops into, unit is for rising (L), and concentration is 14molL
-1
Gold plaque and bronze are for once drop in batches, and hydrochloric acid is for once add in batches, and nitric acid takes controlled stream slowly to drip, and rate of addition is 5-20mlmin
-1
The type of heating that dissolution process is selected is the hot water circulation heating of glass reaction still middle layer, and Heating temperature is 80-100 ℃.Whole dissolution process needs constantly to stir with stirrer.
Second step: drive the oxynitride in the chlorauric acid solution
After the bronze dissolving fully, residual in the solution have a certain amount of NO
3 -, NO
2 -The oxidisability ion, the existence of these oxynitride can influence the later stage electrolytic process, therefore need drive these materials, is commonly called as " catching up with nitre ".
Drip 200-400ml ethanolic soln and constantly stirring in the chlorauric acid solution solution that in the glass reaction still, has prepared, and further heating concentrates chlorauric acid solution 1-2h.
Described concentrating is under negative pressure state, to carry out, and the intravital pressure of still is 50-70KPa, and type of heating can be selected the water cycle heating, adds 95-100 ℃ of temperature; Also can select the oil bath heating, add about 300 ℃ of temperature.
The 3rd step: preparing electrolyte
In the plastic containers of the chlorauric acid solution suction 60-80mL that dissolving is good, add golden electrolysis auxiliary reagent QJ-D-14-6Kg, and add a certain amount of water it is fully dissolved.It is about 50L that further a certain amount of hydrochloric acid of adding and water make the final volume of electrolytic solution, and the concentration of hydrochloric acid is 1.5-2molL
-1
The 4th step: casting Jinyang pole plate
The gold containing material raw material is cast as Jinyang pole plate, and positive plate is of a size of, 200mmx250mmx6mm, and the weight of every Jinyang pole plate is 5-5.8Kg;
The 5th step: electrolysis
The electrolytic solution that the 3rd step was prepared is evacuated in the electrolyzer; Jinyang pole plate is suspended on the anode conducting rod, as negative plate, opens electrolysis power with the high purity titanium plate; The employing cycle, automatic commutation technology was carried out electrolysis, and the time ratio of forward and reversible circulation chooses 8: 1-15: 1.Electrolysis time 30-40h.
The 6th step: sampling detects and casting standard ingot
Electrolysis is taken off the negative electrode proof gold from negative plate after finishing, and boils with 6molL-1 hydrochloric acid and washes 2-4h, cleans 2-3 time with zero(ppm) water then, in baking oven, dries.With intermediate frequency furnace dissolving negative electrode gold, adopt the vacuum sampling system to get test sample after treating to dissolve fully and carry out quality test.Use 3 kilograms of standard gold die casting Au2 then
#The standard ingot is if the check product meets Au1
#Standard ingot standard then further is cast into the Au99.99%1 of every 1Kg
#The standard ingot.
Electrolysis gained data are following: obtain meeting the proof gold 21.46Kg of Au99.99% standard-required, each impurity content is seen table 1 in the product, productive rate 72.0%; Anode scrap 4.63Kg, residual anode ratio 14.5%; Anode bronze 4.16Kg.Through the metal balance analysis, golden comprehensive recovery 99.92%, whole process loss 0.08%.
Table 1: argentiferous about 5% (m/m) gold containing material electrorefining product quality analysis result
Through analyzing, the amount of each impurity element is all less than the requirement of GB to Au99.99% in the product, and the content of gold surpasses 99.995%.
Embodiment two: the electrolysis of argentiferous about 7% (m/m) gold containing material
Choose gold containing material, wherein contain Au 92.1%, Ag 7.2%, and Cu 0.46%, and the content of 15 elements such as Ni, Fe, Pb, Zn, As, Sb, Cr, Mn, Sn, Mg carries out electrolysis all less than 0.005%.The electrolysis concrete steps are identical with embodiment one.
Drop into woollen weight 31.7Kg, amounting to Cheng Chunchong is 29.20Kg, gold ion concentration 90-120gL in the electrolytic solution
-1, concentration of hydrochloric acid 1.5-2molL
-1, electrolysis auxiliary reagent QJ-D-1 consists of 2.0%NNO+43% NH
4Cl+55% KCl, the concentration of golden electrolysis auxiliary reagent QJ-D-1 in electrolytic solution is 100gL
-1, electrolyte temperature 45-55 ℃, electrolysis time 38h.
Electrolysis gained data are following: obtain meeting the proof gold 20.92Kg of Au99.99% standard-required, each impurity content is seen table 2 in the product, productive rate 71.64%; Anode scrap 5.78Kg, residual anode ratio 18.23%; Anode bronze 3.06Kg.Through the metal balance analysis, golden comprehensive recovery 99.92%, whole process loss 0.08%.
Table 2: argentiferous about 7% (m/m) gold containing material electrorefining product quality analysis result
Through analyzing, the amount of each impurity element is all less than the requirement of GB to Au99.99% in the product, and the content of gold surpasses 99.993%.
Embodiment three: the electrolysis of argentiferous about 10% (m/m) gold containing material
Choose gold containing material, wherein contain Au 89.82%, Ag 9.58%, Cu0.36%, and Ni 0.15%, and the content of 14 elements such as Fe, Pb, Zn, As, Sb, Cr, Mn, Sn, Mg carries out electrolysis all less than 0.005%.The electrolysis concrete steps are identical with embodiment one.
Drop into woollen weight 30.12Kg, amounting to Cheng Chunchong is 27.04Kg, gold ion concentration 90-120gL in the electrolytic solution
-1, concentration of hydrochloric acid 1.5-2molL
-1, electrolysis auxiliary reagent QJ-D-1 consists of 3.0%NNO+52% NH
4Cl+45% KCl, the concentration of golden electrolysis auxiliary reagent QJ-D-1 in electrolytic solution is 120gL
-1, electrolyte temperature 45-55 ℃, electrolysis time 40h.
Electrolysis gained data are following: obtain meeting the proof gold 18.51Kg of Au99.95% standard-required, each impurity content is seen table 3 in the product, productive rate 68.45%; Anode scrap 5.59Kg, residual anode ratio 18.60%; Anode bronze 4.07Kg.Through the metal balance analysis, golden comprehensive recovery 99.93%, whole process loss 0.07%.
Table 3: argentiferous about 10% (m/m) gold containing material electrorefining product quality analysis result
Through analyzing, the amount of each impurity element is all less than the requirement of GB to Au99.95% in the product, and the content of gold surpasses 99.98%.
Claims (2)
1. one kind is suitable for high silver-colored gold containing material quick electrolysis purified auxiliary reagent, and it is characterized by: golden electrolysis auxiliary reagent QJ-D-1 is by ammonia chloride (NH
4C1), the compounding substances formed of Repone K (KCl) and diffusant methylene-bis bitter edible plant sodium sulfonate (NNO), the massfraction proportioning of described golden each component of electrolysis auxiliary reagent QJ-D-1 is following: NNO:0.5-5%, NH4Cl:15-80%, KCl:15-80%.
2. a kind of high silver-colored gold containing material quick electrolysis purified auxiliary reagent that is suitable for according to claim 1, it is characterized by: the concentration of golden electrolysis auxiliary reagent QJ-D-1 in electrolytic solution is 80-120gL
-1
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|---|---|---|---|
| CN201210108752.0A CN102618885B (en) | 2012-04-13 | 2012-04-13 | Auxiliary reagent suitable for rapid electrorefining of high-silver alloyed gold |
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| CN102618885B CN102618885B (en) | 2014-08-27 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103311572A (en) * | 2013-06-13 | 2013-09-18 | 苏州诺信创新能源有限公司 | Novel lithium-ion battery electrolyte |
| CN109312481A (en) * | 2016-03-09 | 2019-02-05 | 托尔斯滕·科拉斯公司 | The electrorefining of thick gold |
| CN113774433A (en) * | 2021-09-30 | 2021-12-10 | 励福(江门)环保科技股份有限公司 | Preparation method of high-purity gold |
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Cited By (5)
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| CN109312481B (en) * | 2016-03-09 | 2020-10-16 | 托尔斯滕·科拉斯公司 | Electrolytic purification of crude gold |
| EA036684B1 (en) * | 2016-03-09 | 2020-12-08 | Торстен Корас | Electrolytic refinement of raw gold |
| CN113774433A (en) * | 2021-09-30 | 2021-12-10 | 励福(江门)环保科技股份有限公司 | Preparation method of high-purity gold |
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