CN105274351B - The technique that a kind of organic reducing method reclaims High Purity Gold from the earth of positive pole - Google Patents
The technique that a kind of organic reducing method reclaims High Purity Gold from the earth of positive pole Download PDFInfo
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- CN105274351B CN105274351B CN201510654906.XA CN201510654906A CN105274351B CN 105274351 B CN105274351 B CN 105274351B CN 201510654906 A CN201510654906 A CN 201510654906A CN 105274351 B CN105274351 B CN 105274351B
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Abstract
The present invention relates to the technique that a kind of organic reducing method reclaims High Purity Gold from the earth of positive pole, belong to hydrometallurgy production technical field.Carry out as follows：1. earth of positive pole removal of impurities is embathed with the nitric acid for boiling；2. the nitric acid insoluble slag molten gold of chloroazotic acid；3. 4. the reduction containing golden wang aqueous solution oxalic acid washes through washing, pickling and again leached mud again, obtains meeting the finished product gold of international more than IG Au99.99%.The present invention is improved on traditional oxalic acid reducing process extraction of gold process, not only greatly improves the quality of finished product gold, and eliminates electrolysis process and the follow-up purification of traditional handicraft, shortens the production cycle, saves production cost.
Description
Technical field
The present invention relates to the technique that a kind of organic reducing method reclaims High Purity Gold from the earth of positive pole, belong to hydrometallurgy production skill
Art field.
Background technology
With the development of science and technology, the purposes of gold is more and more wider, and consumption figure is increasing, promotes gold smelting skill
Art is continued to develop, and extraction of gold process occurs in that a revolution.The method that gold is reclaimed from nonferrous heavy metal electrolysis anode sludge has：Grass
Sour reducing process, nitric acid oxidation method, chloroazotic acid method, electrolysis.The fineness of gold that oxalic acid reducing process and nitric acid oxidation method are reclaimed is not high, expensive
Metal synthetical recovery level is not high；Although chloroazotic acid method can produce high-quality gold product, production process needs to carry out
Nitre is caught up with, operating process is complicated, and is suitable only for small-scale production；Electrolysis reclaims gold process from the earth of positive pole, can
To produce 1# ingots.It is more that its major defect is that noble metal overstocks, and the production cycle is more long.
On 04 27th, 1988, Chinese invention patent application publication No. CN87105051A disclosed a kind of separation of gold and silver
New method, the method use three sections of counterflow leaching techniques of chloroazotic acid, restore cake of gold with oxalic acid solution, through founding after containing gold
Proof gold more than 99.9%, eliminates electrolytic process.Although the method process is simple, with short production cycle, production process is also not required to
Carry out catching up with nitre.But chloroazotic acid and hydrochloric acid solution consumption are big, investment of production or larger.
The content of the invention
The technical problem to be solved in the present invention is directed to the shortcoming of prior art, proposes a kind of organic reducing method from the earth of positive pole
The middle technique for reclaiming High Purity Gold, can improve the leaching rate of gold and obtain purity thick bronze higher.
The technical scheme is that：A kind of organic reducing method reclaims the technique of High Purity Gold from the earth of positive pole, by following step
Suddenly carry out：
1. acidleach removal of impurities
The earth of positive pole, control liquid solid product mass ratio 8-12 are embathed with the nitric acid for boiling：1L/kg；Make the part in the earth of positive pole
Oxide, hydroxide and soluble-salt enter solution；Impurity enters solution during avoiding chloroazotic acid parting；It is filtered dry nitric acid not
Molten slag, reclaims silver from nitric acid washing lotion；
2. the molten gold of chloroazotic acid
Add chloroazotic acid, control liquid solid product mass ratio 4-7 in nitric acid insoluble slag：1L/kg；Heating, in 95-100 DEG C of condition
Under, the gold in the earth of positive pole is oxidized and is transferred to solution and is formed containing golden wang aqueous solution；After silver in the earth of positive pole is oxidized and in solution
Chloride binding, formed indissoluble white silver nitride precipitation and enter silver chlorate slag in；Silver chlorate slag send silver-colored workshop to reclaim silver；
3. oxalic acid reduction
Containing golden wang aqueous solution under the conditions of 91-95 DEG C of temperature, oxalic acid reduction is added；Oxalic acid addition is the 125- of theoretical amount
130%；And in reduction process, the alkali lye containing saturation villaumite is added, control pH 1-2, Selectively leaching gold；
4. the leached mud for 3. step being obtained again through washing, pickling and wash again, obtain meeting international IG-Au99.99% with
On finished product gold.
The present invention is set about by design optimization from process modification, is improved on traditional oxalic acid reducing process extraction of gold process,
Before oxalic acid reduction, earth of positive pole nitric acid is boiled into removal of impurities, the impurity such as the copper in the earth of positive pole, lead, bismuth are removed.Reduced with oxalic acid
The finished product gold for meeting international more than IG-Au99.99% is directly obtained, organic chemistry reducing process of the present invention reclaims height from the earth of positive pole
Pure gold technology key is when being reduced with oxalic acid, to add the alkali lye control pH=1-2 containing villaumite.Introduce the purpose of villaumite
It is not change chlorine ion concentration.The present invention not only greatly improves the quality of finished product gold, and eliminates electrolysis process and traditional work
The follow-up purification of skill, shortens the production cycle, saves production cost.The present invention can be interrupted production, and gold backlog is few, money
Gold turnover is fast, and the scattered gold produced in production process is few, is easy to manage and safeguards, particularly suitable medium and small industrial enterprise.
Brief description of the drawings
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Specific embodiment of the invention is elaborated below in conjunction with the accompanying drawings.
Accompanying drawing 1 represents that the processing step that a kind of organic reducing method reclaims High Purity Gold from the earth of positive pole is：
1. acidleach removal of impurities
Acidleach removal of impurities is first carried out before with chloroazotic acid parting, the earth of positive pole, the solid volume mass of control liquid are embathed with the nitric acid for boiling
Than 10：1L/kg；The partial oxide in the earth of positive pole, hydroxide and soluble-salt is set to enter solution；Avoid chloroazotic acid parting mistake
Impurity enters solution in journey；Nitric acid insoluble slag is filtered dry, silver is reclaimed from nitric acid washing lotion；
2. the molten gold of chloroazotic acid
Add chloroazotic acid, control liquid solid product mass ratio 6 in nitric acid insoluble slag：1L/kg；Heating, under the conditions of 100 DEG C, sun
Gold in the mud of pole is oxidized and is transferred to solution and is formed containing golden wang aqueous solution；Chlorine after silver in the earth of positive pole is oxidized and in solution from
Son is combined, and is formed the white silver nitride precipitation of indissoluble and is entered in silver chlorate slag；Silver chlorate slag send silver-colored workshop to reclaim silver；
Main chemical reactions in chloroazotic acid leaching process have：
Au + HNO3 + 4HCl = H[AuCl4] + NO↑+ 2H2O
Ag++CL-=AgCl↓
3. oxalic acid reduction
Under the conditions of 95 DEG C of golden wang aqueous solution temperature, oxalic acid reduction is added；Oxalic acid addition is the 125% of theoretical amount；And
In reduction process, the alkali lye containing saturation villaumite is added, control pH 1-2, Selectively leaching gold；
Main chemical reactions have：
2HAuCl2+3H2C2O4=2Au+8HCl+6CO2↑
4. the leached mud for 3. step being obtained again through washing, pickling and wash again, obtain meeting international IG-Au99.99% with
On finished product gold.
The alkali lye of above-mentioned saturation villaumite is the mixed solution of saturated sodium-chloride and NaOH；Specific mass ratio is chlorination
Sodium：NaOH：Water=1：1:3.85.
Above-mentioned silver chlorate slag send silver-colored workshop to reclaim silver-colored step：Silver chlorate slag is cleaned to neutrality with running water, is passed through
Filter, the leached mud of cleaning, then after dried process, add soda and be well mixed, heating reduction；The addition of soda is theory
The 110%-130% of value；The leached mud being mixed is placed in heating furnace, is to slowly warm up to 500-600 DEG C, constant temperature 20-60 minutes；
Then 1050~1100 DEG C, after constant temperature 10-30 minutes are gradually heated to, ingot casting are carried out and is obtained thick silver ingot.
Claims (2)
1. the technique that a kind of organic reducing method reclaims High Purity Gold from the earth of positive pole, it is characterised in that carry out as follows：
1. acidleach removal of impurities
The earth of positive pole, control liquid solid product mass ratio 8-12 are embathed with the nitric acid for boiling：1L/kg；Make the partial oxidation in the earth of positive pole
Thing, hydroxide and soluble-salt enter solution；Impurity enters solution during avoiding chloroazotic acid parting；It is filtered dry nitric acid insoluble
Slag, reclaims silver from nitric acid washing lotion；
2. the molten gold of chloroazotic acid
Add chloroazotic acid, control liquid solid product mass ratio 4-7 in nitric acid insoluble slag：1L/kg；Heating, under the conditions of 95-100 DEG C, sun
Gold in the mud of pole is oxidized and is transferred to solution and is formed containing golden wang aqueous solution；Chlorine after silver in the earth of positive pole is oxidized and in solution from
Son is combined, and is formed the white silver nitride precipitation of indissoluble and is entered in silver chlorate slag；Silver chlorate slag send silver-colored workshop to reclaim silver；
3. oxalic acid reduction
Containing golden wang aqueous solution under the conditions of 91-95 DEG C of temperature, oxalic acid reduction is added；Oxalic acid addition is the 125- of theoretical amount
130%；And in reduction process, the alkali lye containing saturation villaumite is added, control pH 1-2, Selectively leaching gold；
4. the leached mud for 3. step being obtained is washed through washing, pickling and again again, obtains meeting international more than IG-Au99.99%'s
Finished product gold；
The alkali lye of the saturation villaumite is the mixed solution of saturated sodium-chloride and NaOH；Specific mass ratio is sodium chloride：
NaOH：Water=1：1:3.85.
2. a kind of organic reducing method according to claim 1 reclaims the technique of High Purity Gold from the earth of positive pole, and its feature also exists
In：The silver chlorate slag send silver-colored workshop to reclaim silver-colored step：Silver chlorate slag is cleaned to neutrality with running water, through filtering, clearly
The leached mud washed, then after dried process, add soda and be well mixed, heating reduction；The addition of soda is theoretical value
110%-130%；The leached mud being mixed is placed in heating furnace, is to slowly warm up to 500-600 DEG C, constant temperature 20-60 minutes；Then
1050~1100 DEG C, after constant temperature 10-30 minutes are gradually heated to, ingot casting are carried out and is obtained thick silver ingot.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106222421A (en) * | 2016-08-17 | 2016-12-14 | 北京矿冶研究总院 | Gold mud treatment method |
| CN106119554B (en) * | 2016-08-18 | 2018-01-16 | 紫金矿业集团股份有限公司 | High Purity Gold and the method for being enriched with silver, platinum and palladium are prepared from silver anode slime |
| CN106756047B (en) * | 2016-12-23 | 2018-06-29 | 郴州市金贵银业股份有限公司 | High sundries silver anode slime puies forward the processing method of gold |
| CN107641721B (en) * | 2017-09-29 | 2019-10-18 | 云南驰宏锌锗股份有限公司 | A kind of method of thick gold purification |
| CN110863215A (en) * | 2019-12-27 | 2020-03-06 | 有研亿金新材料有限公司 | Method for preparing gold electrolyte by using gold electrolysis anode mud |
| CN115198096A (en) * | 2022-06-29 | 2022-10-18 | 江西铜业技术研究院有限公司 | Method for preparing gold-tetranine by one-stage chemical reduction refining of silver anode mud |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328541A (en) * | 2008-07-27 | 2008-12-24 | 郴州市金贵银业股份有限公司 | Gold wet purification process |
| CN102373338A (en) * | 2010-08-20 | 2012-03-14 | 沈阳有色金属研究院 | Method for extracting metallic silver from silver chloride sediment |
| CN102703691A (en) * | 2012-06-20 | 2012-10-03 | 四川省天泽贵金属有限责任公司 | New technology for extracting high-purity gold by adopting wet process |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328541A (en) * | 2008-07-27 | 2008-12-24 | 郴州市金贵银业股份有限公司 | Gold wet purification process |
| CN102373338A (en) * | 2010-08-20 | 2012-03-14 | 沈阳有色金属研究院 | Method for extracting metallic silver from silver chloride sediment |
| CN102703691A (en) * | 2012-06-20 | 2012-10-03 | 四川省天泽贵金属有限责任公司 | New technology for extracting high-purity gold by adopting wet process |
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