CN101701346B - Method for increasing quality of cathode silver power - Google Patents
Method for increasing quality of cathode silver power Download PDFInfo
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- CN101701346B CN101701346B CN2009101176293A CN200910117629A CN101701346B CN 101701346 B CN101701346 B CN 101701346B CN 2009101176293 A CN2009101176293 A CN 2009101176293A CN 200910117629 A CN200910117629 A CN 200910117629A CN 101701346 B CN101701346 B CN 101701346B
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- nitric acid
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Abstract
The invention discloses a method for increasing quality of cathode silver power, aiming to solve the problem that the copper impurity in the cathode silver power exceeds standard. The method comprises the following steps: preparing cathode silver power by controlling the compositions of electrolyte to comprise 90-120g/l of Ag, 8-10g/l of HNO3 and less than 35-60g/l of Cu, and using 20-28g/l of dilute nitric acid to dissolve, soak and rinse the cathode silver power when the copper content in the electrolyte is more than 35g/l, wherein the soaking temperature is 40-50 DEG C, the soaking time is 2h, and the rinsing temperature is 80-90 DEG C. By using the method of the invention, the cost of the 1# cathode silver is reduced and the mass of the product silver ingot is increased. The method has the advantages of low operating intensity, simple equipment, low production cost, capability of not changing the original processing equipment, and the like.
Description
Technical field
The present invention relates to nonferrous metallurgy, chemical metallurgy industry, a kind of specifically method that improves the silver powder quality of production.
Background technology
At present, in the domestic silver-colored refining electrolysis production, improving quality of cathode silver power mainly is the content of metals such as control impurity copper, lead, bismuth, and its method is: 1, reduce anode alloy plate copper content, 2, constantly a large amount of replacings replenishes new electrolytic solution.And, in production practice, have following problem from above two kinds of method researchs;
1), the refined alloy plate is at Ag+Au 〉=97% o'clock, continuing to reduce the copper amount will make refining cycle prolong, energy consumption increases, draw from pyrorefining is actual, when copper in the electrum less than 2% the time, if impurity copper is reduced by 0.2%, electrum plate direct yield will descend 0.5%, the flux energy consumption will increase 2.5%, have the limit of impurities problem simultaneously, and this will directly have influence on gold and silver direct yield and refining cycle.
2), 1# silver is produced, require the electrolytic solution cupric less than 25 grams per liters, when the copper content overproof, electrolytic solution needs all to handle, and liquid making again is because the method for impurity needs constantly a large amount of replacings to replenish new electrolytic solution in this control electrolytic solution, and the liquid making cycle is long again, cost is high, labour intensity is big, 10 batches of electrolysis just need to handle when producing 1# silver, and the Ag electrolyte time will take about 1/3rd of the production time usually, directly influence finishing of production cycle and output task.
Summary of the invention
The object of the invention provides a kind of method that improves quality of cathode silver power, to solve the problem that impurity copper exceeds standard in the electric silver powder.
The present invention includes the following step:
Control electrolytic solution is formed at Ag:90-120g/l, HNO
3: 8-10g/l, Cu: the silver powder of producing under＜35--60g/l the condition, when electrolytic solution cupric during, adopt the dilute nitric acid dissolution of 20--28g/l to soak, embathe greater than 35 grams per liters, soaking temperature 40-50 ℃, soak time 2 hours, wash temperature 80-90 ℃.
Soak solution preferably contains nitric acid 22--26 grams per liter, preferred 40 ℃ of soaking temperature, preferred 80 ℃ of wash temperature.
The present invention adopts rare nitric acid dousing, embathe the method that electric silver powder improves quality of cathode silver power is to produce the later stage at electrorefining of silver.Electrolytic solution impurity Cu is accumulated to 40g/l when above, and the electric silver powder of output mainly is 2# silver, and its impurity mainly is that copper exceeds standard, adopt rare nitric acid dousing electricity silver powder after, can reduce content of copper ion in the silver powder rapidly, make it reach the standard of 1# silver.
The present invention has reduced the cost of producing 1# silver, has improved the quality of product silver ingot.Have that manipulation strength is low, equipment simply, does not change original process equipment, the low advantages such as (soaking 0.1 yuan/kilogram in silver powder) of production cost expense.
The present invention program analyzes:
1), impurity copper content in the anode alloy plate is normally maximum, reaches 2% or more.Enter electrolytic solution with the copper nitrate solution form in the electrolytic process; Because it is above that the electropotential of copper is at half than silver, in salpeter solution, copper can be separated out at negative electrode, and concentration is more and more higher.But under normal electrolytic situation, the possibility that copper is separated out in negative electrode is little.But bad when concentration polarization or electrolytic solution agitation cycle, silver ions acutely sinks, and causes that the ratio of silver-bearing copper content is in the electrolytic solution at 2: 1 o'clock, and copper can be separated out on the top of negative electrode, influences electric silver amount.
2), high cupric ion influences electric silver and separates out
Copper reduction destroys silver-colored dissolving from anode, separate out and destroy the balance in the electrolytic solution on negative electrode, when anode cupric 5%, the silver that negative electrode is separated out has 84% to be silver from anode dissolution, all the other are from negatively charged ion in the electrolytic solution, thereby cause electrolytic solution intermediate ion concentration to reduce.Copper is electrochemical solution on anode, enters in the electrolytic solution with the Cu2+ form, and has following reaction:
Cu
2++e＝Cu
+
The appearance of monovalent ion, not only consumed power also may the output copper powder
2Cu
++e＝Cu
2++Cu↓
Copper powder promptly can pollute the anode sludge, can reduce electric silver amount again, particularly when the high anode of electrolysis cupric, because anode is only separated out silver, and the every dissolving 1 gram cathode of anode is just separated out 3.4 gram silver, so should often extract the high electrolytic solution of part cupric out during the high anode of electrolysis cupric, and mend the high silver nitrate solution of part concentration.
3), experimental program is formulated
If change the technical process situation, from the pyrometallurgical smelting alloy sheets, fall copper or electrolytic solution and handle and fall the copper method and all be difficult to reach standard requirement, still selected the electrolysis rear impurity silver powder that exceeds standard is leached the decopper(ing) test.
Silver powder carries out diluted acid leaching scheme 3.1 cupric exceeds standard
3.1.1 the copper silver powder that exceeds standard is carried out rare nitric acid dousing after hot wash.Grope rare nitric acid solubleness to silver powder under different content.This experiment nitric acid amount of allocating into adds since 5 grams per liters;
3.1.2 soak time is to the influence of decopper(ing) under the understanding grasp differing temps
Observe 3.1.3 regularly stir, sampling and testing silver powder returns molten amount
3.1.4 soaking back silver powder washs with different water temperatures
3.1.5 each experiment former state is cast with monkey, gets standard and send quality inspection place to analyze
3.1.6 determine the rational technology condition of the rare nitric acid dousing of silver powder, strengthen operational administrative simultaneously, avoid improper pollution as far as possible.
4), experimental result
Tens batches of tests through two wheat harvesting periods are groped, and have finished pre-stage test, and experimental data sees Table one
Table one
4.1 experimental analysis is analyzed from table one and is drawn:
The silver powder 4.1.1 rare nitric acid dousing exceeds standard increases with acidity, and the decopper(ing) rate improves.
4.1.2 electric silver powder soaking temperature, soak time is little to decopper(ing) test variable effect.
4.1.3 when nitric acid content during at the 20-28 grams per liter, effect is best, leach decopper(ing) content reduce near half.
Surpass 30 grams per liters 4.1.4 work as acid content, silver powder returns molten amount and increases, and the decopper(ing) rate is obviously change not.
4.2 experiment brief summary
According to above analytical results, we have made the following standard of silver preparing electrolysis process process parameter:
4.2.1 produce the later stage at electrorefining of silver, the electrolytic solution composition is controlled at Ag:90--120 grams per liter, HNO
3: 8--10 grams per liter, Cu＜35--60 grams per liter.
4.2.2, the silver powder of producing is carried out rare nitric acid soaks copper when electrolytic solution cupric during greater than 35 grams per liters.
4.2.3 soak solution contains nitric acid 22--28 grams per liter, and soaking temperature 40-50 ℃, soak time 2 hours, wash temperature 80-90 ℃.
4.2.4 silver powder and rare nitric acid solid-to-liquid ratio are 1: 1.2 (volume ratio).
5), industrial practice
According to experimental result, definite technical qualification, but design and installation one cover sealing and circulating soak the silver powder device, this operation of equipment is simple, leach liquor can be recycled repeatedly, saves nitric acid dosage, energy-conserving and environment-protective.Operation was soaked hundred batches 2 years more, and the decopper(ing) rate on average reaches 32%, and the silver ingot copper content is all fallen 2 percentage points, and 1# silver percentage of product reaches 96%.
6), economic benefit
The impurity silver powder that exceeds standard is carried out after rare nitric acid leaches decopper(ing), 35 batches of silver powder that exceed standard of immersion treatment altogether in the present invention's experiment, the decopper(ing) rate on average reaches 32%, and the silver ingot copper content reduces by 2 percentage points.1# silver percentage of product reaches 96%.The our factory silver electrolyte is handled and is extended to 20 batch processed once for 10 batches by original electrolysis, save 80,000 yuan of the electrolyte reagent expenses of handling year, reduce displacement silver powder and return 10 tons of stove meltings, 100 kilograms of losses are directly received in the minimizing melting, be worth 320,000 yuan, reduce and produce 3 tons in turnover silver powder.50 tons of annual 1# silver volume increase only can many extra earnings be worth 2,500,000 yuan from 1# silver and 2# silver price differential, and annual total benefit reaches 3,500,000 yuan.Lay the foundation for improving 1# silver percentage of product, obtained huge economic benefit and social benefit, have excellent popularization and be worth.
Embodiment
The following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1
In electrorefining of silver was produced, in the silver-colored electrolysis production later stage, production specifications mainly were that the electrolytic solution composition is controlled at Ag:90-120g/l, HNO
3: 8-10g/l, Cu:＜35--60g/l, when the electrolytic solution cupric greater than to 30g/l when above, Cu content will be above 0.0034% in the electric silver powder of separating out, the silver powder of producing under the above-mentioned condition adopts the dilute nitric acid dissolution of 20g/l to soak, embathe, silver powder and rare nitric acid solid-to-liquid ratio are 1: 1.2 (volume ratio), 60 ℃ of soaking temperatures, soak time 4 hours, 80 ℃ of wash temperatures.
Embodiment 2
Production specifications are with embodiment 1, and the silver powder of production adopts the dilute nitric acid dissolution of 20g/l to soak, embathe, and silver powder and rare nitric acid solid-to-liquid ratio are 1: 1 (volume ratio), 40 ℃ of soaking temperatures, soak time 2 hours, 90 ℃ of wash temperatures.
Embodiment 3
Production specifications are with embodiment 1, and the silver powder of production adopts the dilute nitric acid dissolution of 24g/l to soak, embathe, and silver powder and rare nitric acid solid-to-liquid ratio are 1: 1.2 (volume ratio), 50 ℃ of soaking temperatures, soak time 2 hours, 85 ℃ of wash temperatures.
Embodiment 4
Production specifications are with embodiment 1, and the silver powder of production adopts the dilute nitric acid dissolution of 24g/l to soak, embathe, and silver powder and rare nitric acid solid-to-liquid ratio are 1: 1.5 (volume ratio), 40 ℃ of soaking temperatures, soak time 4 hours, 80 ℃ of wash temperatures.
Embodiment 5
Production specifications are with embodiment 1, and the silver powder of production adopts the dilute nitric acid dissolution of 22g/l to soak, embathe, and silver powder and rare nitric acid solid-to-liquid ratio are 1: 1.5 (volume ratio), 40 ℃ of soaking temperatures, soak time 4 hours, 80 ℃ of wash temperatures.
Embodiment 6
Production specifications are with embodiment 1, and the silver powder of production adopts the dilute nitric acid dissolution of 26g/l to soak, embathe, and silver powder and rare nitric acid solid-to-liquid ratio are 1: 1.3 (volume ratio), 40 ℃ of soaking temperatures, soak time 4 hours, 80 ℃ of wash temperatures.
Embodiment 7
Production specifications are with embodiment 1, and the silver powder of production adopts the dilute nitric acid dissolution of 25g/l to soak, embathe, and silver powder and rare nitric acid solid-to-liquid ratio are 1: 1.4 (volume ratio), 60 ℃ of soaking temperatures, soak time 2 hours, 80 ℃ of wash temperatures.
Embodiment 8
Production specifications are with embodiment 1, and the silver powder of production adopts the dilute nitric acid dissolution of 28g/l to soak, embathe, and silver powder and rare nitric acid solid-to-liquid ratio are 1: 1.2 (volume ratio), 40 ℃ of soaking temperatures, soak time 2 hours, 80 ℃ of wash temperatures.
Embodiment 9
Production specifications are with embodiment 1, and the silver powder of production adopts the dilute nitric acid dissolution of 28g/l to soak, embathe, and silver powder and rare nitric acid solid-to-liquid ratio are 1: 1.2 (volume ratio), 40 ℃ of soaking temperatures, soak time 2 hours, 80 ℃ of wash temperatures.
Claims (2)
1. method that improves quality of cathode silver power, it is characterized in that: it comprises the following steps:
Control electrolytic solution is formed at Ag:90-120g/l, HNO
3: 8-10g/l, Cu: produce silver powder under the＜35g/l condition,, adopt the dilute nitric acid dissolution of 20--28g/l to soak, embathe silver powder when electrolytic solution cupric during greater than 35 grams per liters, soaking temperature 40-50 ℃, soak time 2 hours, wash temperature 80-90 ℃.
2. the method for raising quality of cathode silver power according to claim 1 is characterized in that: soak solution contains nitric acid 22--26 grams per liter, 40 ℃ of soaking temperatures, 80 ℃ of wash temperatures.
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| CN2009101176293A CN101701346B (en) | 2009-11-28 | 2009-11-28 | Method for increasing quality of cathode silver power |
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|---|---|---|---|
| CN2009101176293A CN101701346B (en) | 2009-11-28 | 2009-11-28 | Method for increasing quality of cathode silver power |
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| CN101701346B true CN101701346B (en) | 2011-08-17 |
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| CN102605389A (en) * | 2012-03-14 | 2012-07-25 | 云南驰宏锌锗股份有限公司 | Low consumption efficient method for washing and drying of electrolytic silver powder |
| CN105132706A (en) * | 2015-08-31 | 2015-12-09 | 白银有色集团股份有限公司 | Method for removing impurities in electrolytic silver powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940141A (en) * | 2006-09-22 | 2007-04-04 | 江西铜业集团公司贵冶分公司 | Non-copper ionic-silver electrolyzation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940141A (en) * | 2006-09-22 | 2007-04-04 | 江西铜业集团公司贵冶分公司 | Non-copper ionic-silver electrolyzation |
Non-Patent Citations (3)
| Title |
|---|
| 容智梅.银电解过程中杂质行为及其控制.《湖南有色金属》.2003,第19卷(第3期),16-18. * |
| 赵永.提高电银质量的生产实践.《有色冶炼》.2000,第29卷(第5期),24-26. * |
| 陈鹤群.银电解生产工艺的改进.《昆明理工大学学报》.2000,第25卷(第6期),60-63. * |
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Granted publication date: 20110817 Termination date: 20201128 |