CN102618885B - 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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- CN102618885B CN102618885B CN201210108752.0A CN201210108752A CN102618885B CN 102618885 B CN102618885 B CN 102618885B CN 201210108752 A CN201210108752 A CN 201210108752A CN 102618885 B CN102618885 B CN 102618885B
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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 auxiliary reagent of the silver-colored gold containing material quick electrolysis of a kind of applicable height refining.
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 advantages of that technique is simple, constant product quality, but exist simultaneously, Production Flow Chart is long, the gold problem that excessive inventory.For overcome traditional electrical solution exist deficiency, development in recent years quick electrolysis technique, make golden electrolytic efficiency obtain raising by a relatively large margin.But in electrolytic process anode gold, the most harmful composition is silver, and the silver in anode gold becomes silver chloride shell and sticks on positive plate, and electrolytic efficiency is significantly reduced; If when silver amount is too high, make anode gold produce passivation, hinder the continuation of anode gold to dissolve, and make anode separate out chlorine, cause gold ion dilution in electrolytic solution simultaneously, production rate slows down.In order to solve silver-colored harm, at present in the time of golden electrorefining toward input AC electricity in input dc power in electrolyzer, form the pulsatory current of asymmetry; Or automatic commutation technology of employing cycle, makes the negative switching of electric current of positive plate, make to produce a large amount of gas on anode, silver chloride shell is subject to gas percussion to become loose, can reduce to a certain extent anode passivation degree, improves the electrolytic efficiency of high silver anode gold.In addition, improve the concentration of hydrochloric acid in electrolytic solution, make part AgCl precipitation form AgCl
2 -also can improve to a certain extent the electrolytic efficiency of high silver anode gold.
But no matter take at present which kind of technology, in use electrolytic process refining of gold process, in anode gold, the content of silver is controlled in 5% (m/m) conventionally, and silver is measured too Gao Zehui makes electrolysing period long, and production efficiency is low.In addition, conventionally select high acidity condition electrolysis in order to improve electrolytic efficiency, in electrolytic solution, the concentration of hydrochloric acid is generally 4-6molL
-1, due to higher electrolyte acidity, in electrolytic process, there is stronger volatility, there is the problems such as environmental pollution and Working environment be poor.
Summary of the invention
The deficiency existing in order to overcome prior art, the invention provides a kind of auxiliary reagent that is suitable for the refining of high silver-colored gold containing material quick electrolysis.
It is as follows that the present invention solves the technical scheme that its technical problem underlying takes: a kind of auxiliary reagent that is suitable for the refining of high silver-colored gold containing material quick electrolysis, golden electrolysis auxiliary reagent QJ-D-1 is by ammonia chloride (NH
4cl), the compounding substances of Repone K (KCl) and diffusant methylene-bis bitter edible plant sodium sulfonate (NNO) composition, the massfraction proportional range of the each component of this 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 electro deposition gold desired raw material gold containing material, effectively eliminate anode passivation phenomenon and raising electrolytic efficiency that silver chloride causes; Add golden electrolysis auxiliary reagent QJ-D-1 can make electrolyte acidity by traditional 4-5molL simultaneously
-1hCl is reduced to 2molL
-1below, reduce consumption and the environmental pollution of reagent, had significant environmental benefit.
In order to solve adhering in a large number due to silver nitride precipitation on anode in 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 to add the technical scheme of a certain amount of diffusant methylene-bis bitter edible plant sodium sulfonate in electrolytic solution.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 to electrolytic solution, can form on gold anode surface on the one hand one deck macromole anionic membrane, stop the silver chloride shell and fine and close adhesion of anode gold that in electrolytic process, produce to cause anode passivation; The existence of diffusant can make silver nitride precipitation become loose on the other hand, is beneficial to the silver chloride free dropping being attached on anode gold.So anode passivation degree obviously reduces, and has improved the electrolytic efficiency of high silver anode gold.
In order to solve the environmental pollution causing in high acidity electrolytic solution electrolytic process, the hydrochloric acid in electrolytic process in the mixing salt Substitute For Partial electrolytic solution of use ammonia chloride and Repone K.Can make the concentration of hydrochloric acid in electrolytic solution effectively be reduced on the one hand, reduce the environmental pollution that in electrolytic process, the volatilization of hydrochloric acid causes; Add on the other hand chloride salt, due to a large amount of chlorions and " salt effect " of existence being provided, the solubleness of silver nitride precipitation is increased, slowed down the formation speed of silver nitride precipitation on anode gold, improved electrolytic efficiency.
Embodiment
Embodiment mono-: argentiferous 5% left and right (m/m) gold containing material electrolysis
Choose gold containing material, wherein contain Au 93.5%, Ag 4.8%, Cu 0.56%, Ni 0.92%, Fe 0.13%, Pb 0.02%, the content of 12 elements such as Zn, As, Sb, Cr, Mn, Sn, Mg is all less than 0.005%, carries out electrolysis.
Drop into woollen weight 32Kg, amounting to Cheng Chunchong is 29.8Kg, gold ion concentration 90-120gL in preparation electrolytic solution
-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 DEG C, electrolysis time 36h.
Electrolysis concrete steps are as follows:
The first step: prepare chlorauric acid solution
Be greater than 99.95% bronze 5000-6000g by purity, be placed in double-layer glass reaction kettle, in airtight negative pressure system, use 6molL
-1hCl and 14molL
-1hNO
3electrolyte is prepared in dissolving.
Described Au, HCl and HNO
3ratio be: 4: 16: 1, wherein Au be drop into quality, unit is kilogram (Kg); HCl is the volume dropping into, and unit is for rising (L), and concentration is 6molL
-1; HNO
3for the volume dropping into, unit is for rising (L), and concentration is 14molL
-1.
Gold plaque and bronze are for once dropping in batches, and hydrochloric acid is for once adding in batches, and nitric acid takes controllable flow slowly to drip, and rate of addition is 5-20mlmin
-1.
The type of heating that dissolution process is selected is glass reaction still middle layer hot water circulation heated, and Heating temperature is 80-100 DEG C.Whole dissolution process need constantly stir with stirrer.
Second step: drive the oxynitride in chlorauric acid solution
Bronze remains a certain amount of NO after dissolving completely in solution
3 -, NO
2 -dithizone, the existence of these oxynitride can affect later stage electrolytic process, therefore needs to drive these materials, is commonly called as " catching up with nitre ".
In the chlorauric acid solution solution having prepared in glass reaction still, drip 200-400ml ethanolic soln and constantly stir, and the further concentrated chlorauric acid solution 1-2h of heating.
Described concentrated be to carry out under negative pressure state, the pressure in kettle is 50-70KPa, type of heating can be selected water cycle heating, adds temperature 95-100 DEG C; Also can select oil bath heating, add 300 DEG C of left and right of temperature.
The 3rd step: preparation electrolytic solution
By in the plastic containers of the chlorauric acid solution suction 60-80mL having dissolved, add golden electrolysis auxiliary reagent QJ-D-14-6Kg, and add a certain amount of water it is fully dissolved.Further adding a certain amount of hydrochloric acid and water to make the final volume of electrolytic solution is 50L left and right, and the concentration of hydrochloric acid is 1.5-2molL
-1.
The 4th step: casting Jinyang pole plate
Gold containing material raw material is cast as to 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 is prepared is evacuated in electrolyzer, Jinyang pole plate is suspended on anode conducting rod, as negative plate, opens electrolysis power with 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
After electrolysis finishes, from negative plate, negative electrode proof gold is taken off, boil and wash 2-4h with 6molL-1 hydrochloric acid, then clean 2-3 time with distilled water, in baking oven, dry.With intermediate frequency furnace dissolving negative electrode gold, adopt until completely dissolved vacuum sampling system to get detection sample and carry out quality test.Then use 3 kilograms of standard gold die casting Au2
#standard ingot, if inspection product meets Au1
#standard ingot standard, is further cast into the Au99.99%1 of every 1Kg
#standard ingot.
Electrolysis the data obtained is as follows: obtain meeting the proof gold 21.46Kg of Au99.99% standard-required, in product each impurity content in table 1, productive rate 72.0%; Anode scrap 4.63Kg, residual anode ratio 14.5%; Anode bronze 4.16Kg.Through metal balance analysis, golden comprehensive recovery 99.92%, whole process loss 0.08%.
Table 1: argentiferous 5% left and right (m/m) gold containing material electrorefining product quality analysis result
By analyzing, in product, the amount of each impurity element is all less than the requirement of GB to Au99.99%, and the content of gold exceedes 99.995%.
Embodiment bis-: argentiferous 7% left and right (m/m) gold containing material electrolysis
Choose gold containing material, wherein contain Au 92.1%, Ag 7.2%, Cu 0.46%, the content of 15 elements such as Ni, Fe, Pb, Zn, As, Sb, Cr, Mn, Sn, Mg is all less than 0.005%, carries out electrolysis.Electrolysis concrete steps are identical with embodiment mono-.
Drop into woollen weight 31.7Kg, amounting to Cheng Chunchong is 29.20Kg, gold ion concentration 90-120gL in 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 DEG C, electrolysis time 38h.
Electrolysis the data obtained is as follows: obtain meeting the proof gold 20.92Kg of Au99.99% standard-required, in product each impurity content in table 2, productive rate 71.64%; Anode scrap 5.78Kg, residual anode ratio 18.23%; Anode bronze 3.06Kg.Through metal balance analysis, golden comprehensive recovery 99.92%, whole process loss 0.08%.
Table 2: argentiferous 7% left and right (m/m) gold containing material electrorefining product quality analysis result
By analyzing, in product, the amount of each impurity element is all less than the requirement of GB to Au99.99%, and the content of gold exceedes 99.993%.
Embodiment tri-: argentiferous 10% left and right (m/m) gold containing material electrolysis
Choose gold containing material, wherein contain Au 89.82%, Ag 9.58%, Cu0.36%, Ni 0.15%, the content of 14 elements such as Fe, Pb, Zn, As, Sb, Cr, Mn, Sn, Mg is all less than 0.005%, carries out electrolysis.Electrolysis concrete steps are identical with embodiment mono-.
Drop into woollen weight 30.12Kg, amounting to Cheng Chunchong is 27.04Kg, gold ion concentration 90-120gL in 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 DEG C, electrolysis time 40h.
Electrolysis the data obtained is as follows: obtain meeting the proof gold 18.51Kg of Au99.95% standard-required, in product each impurity content in table 3, productive rate 68.45%; Anode scrap 5.59Kg, residual anode ratio 18.60%; Anode bronze 4.07Kg.Through metal balance analysis, golden comprehensive recovery 99.93%, whole process loss 0.07%.
Table 3: argentiferous 10% left and right (m/m) gold containing material electrorefining product quality analysis result
By analyzing, in product, the amount of each impurity element is all less than the requirement of GB to Au99.95%, and the content of gold exceedes 99.98%.
Claims (2)
1. an auxiliary reagent that is suitable for the refining of high silver-colored gold containing material quick electrolysis, is characterized by: golden electrolysis auxiliary reagent QJ-D-1 is by ammonia chloride (NH
4cl), the compounding substances of Repone K (KCl) and diffusant sodium methylene bis-naphthalene sulfonate (NNO) composition, the massfraction proportioning of the described each component of golden electrolysis auxiliary reagent QJ-D-1 is as follows: NNO:0.5-5%, NH
4cl:15-80%, KCl:15-80%.
2. a kind of auxiliary reagent that is suitable for the refining of high silver-colored gold containing material quick electrolysis according to claim 1, is characterized by: the concentration of golden electrolysis auxiliary reagent QJ-D-1 in electrolytic solution is 80-120gL
-1.
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|---|---|---|---|
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| CN102618885B true CN102618885B (en) | 2014-08-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017153547A1 (en) * | 2016-03-09 | 2017-09-14 | Thorsten Koras | Electrolytic refinement of raw gold |
Families Citing this family (2)
| 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 |
| 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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| US4139432A (en) * | 1976-08-16 | 1979-02-13 | Ghiringhelli Hugh A | Process for electrochemically recovering precious metals from ores |
| CN2158521Y (en) * | 1993-05-04 | 1994-03-09 | 沈阳黄金学院贵金属材料厂 | Heating equipment for electrolyzing gold |
| CN2359299Y (en) * | 1999-01-26 | 2000-01-19 | 东北大学黄金学院 | 2-pi period change gold electrolytic power |
| CN2443971Y (en) * | 2000-08-23 | 2001-08-22 | 内蒙古乾坤金银精炼股份有限公司 | Apparatus of working up positive mud for electrolysing gold |
| US20080169196A1 (en) * | 2007-01-16 | 2008-07-17 | Patrick Ismail James | Apparatus and method for electrochemical modification of liquid streams |
| JP2012012653A (en) * | 2010-06-30 | 2012-01-19 | Waseda Univ | Method for producing metallic fine particle |
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2012
- 2012-04-13 CN CN201210108752.0A patent/CN102618885B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4139432A (en) * | 1976-08-16 | 1979-02-13 | Ghiringhelli Hugh A | Process for electrochemically recovering precious metals from ores |
| CN2158521Y (en) * | 1993-05-04 | 1994-03-09 | 沈阳黄金学院贵金属材料厂 | Heating equipment for electrolyzing gold |
| CN2359299Y (en) * | 1999-01-26 | 2000-01-19 | 东北大学黄金学院 | 2-pi period change gold electrolytic power |
| CN2443971Y (en) * | 2000-08-23 | 2001-08-22 | 内蒙古乾坤金银精炼股份有限公司 | Apparatus of working up positive mud for electrolysing gold |
| US20080169196A1 (en) * | 2007-01-16 | 2008-07-17 | Patrick Ismail James | Apparatus and method for electrochemical modification of liquid streams |
| JP2012012653A (en) * | 2010-06-30 | 2012-01-19 | Waseda Univ | Method for producing metallic fine particle |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017153547A1 (en) * | 2016-03-09 | 2017-09-14 | Thorsten Koras | Electrolytic refinement of raw gold |
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