CN105274351A - Process for recycling high-purity gold from anode slime through organic reduction method - Google Patents
Process for recycling high-purity gold from anode slime through organic reduction method Download PDFInfo
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- CN105274351A CN105274351A CN201510654906.XA CN201510654906A CN105274351A CN 105274351 A CN105274351 A CN 105274351A CN 201510654906 A CN201510654906 A CN 201510654906A CN 105274351 A CN105274351 A CN 105274351A
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Abstract
The invention relates to a process for recycling high-purity gold from anode slime through an organic reduction method and belongs to the technical field of wet-method smelting production. The process includes the following steps that firstly, the anode slime is soaked in and washed through boiled nitric acid so as to remove impurities; secondly, residues insoluble in the nitric acid is dissolved through aqua regia to dissolve gold; thirdly, a gold-contained aqua regia solution is reduced through oxalic acid; and fourthly, leached residues are washed through water, pickled and washed through water again, so that a finished gold product meeting the international IG-Au of over 99.99%. By the adoption of the method, a traditional process for extracting gold through an oxalic acid reduction method is improved, the quality of the finished gold product is greatly improved, an electrolysis process and refinement performed after the traditional process are omitted, a production period is shortened, and production cost is saved.
Description
Technical field
The present invention relates to the technique that a kind of organic reducing method reclaims High Purity Gold from the anode sludge, belong to hydrometallurgy production technical field.
Background technology
Along with the development of science and technology, the purposes of gold is more and more wider, and consumption is increasing, facilitates gold smelting tech development, and a revolution has appearred in gold extraction technology.The method reclaiming gold from nonferrous heavy metal electrolysis anode sludge has: oxalic acid reduction method, nitric acid oxidation method, chloroazotic acid method, electrolytic process.The fineness of gold that oxalic acid reduction method and nitric acid oxidation method reclaim is not high, and precious metal synthetical recovery level is not high; Although chloroazotic acid method can produce high-quality gold product, production process needs to carry out catching up with nitre, makes operating process complicated, and is only suitable for small-scale production; Electrolytic process reclaims gold process from the anode sludge, can produce 1# ingot.It is more that its major defect is that precious metal overstocks, and the production cycle is longer.
On 04 27th, 1988, Chinese invention patent application publication No. CN87105051A discloses a kind of novel method of separation of gold and silver, and the method adopts chloroazotic acid three sections of counterflow leaching techniques, restores cake of gold with oxalic acid solution, after founding containing gold be greater than 99.9% proof gold, eliminate electrolytic process.Although the method technique is simple, with short production cycle, production process does not need to carry out catching up with nitre yet.But chloroazotic acid and hydrochloric acid soln consumption are greatly, and investment of production is still larger.
Summary of the invention
The technical problem to be solved in the present invention is the shortcoming for prior art, proposes the technique that a kind of organic reducing method reclaims High Purity Gold from the anode sludge, can improve the leaching yield of gold and obtain the higher thick bronze of purity.
Technical scheme of the present invention is: a kind of organic reducing method reclaims the technique of High Purity Gold from the anode sludge, carries out as follows:
1. acidleach removal of impurities
Embathe the anode sludge with the nitric acid boiled, control liquid-solid volume mass and compare 8-12:1L/kg; The partial oxide in the anode sludge, oxyhydroxide and soluble salt is made to enter solution; Avoid impurity in chloroazotic acid parting process and enter solution; Be filtered dry nitric acid insoluble slag, recover silver from nitric acid washing lotion;
2. the molten gold of chloroazotic acid
In nitric acid insoluble slag, add chloroazotic acid, control liquid-solid volume mass and compare 4-7:1L/kg; Heating, under 95-100 DEG C of condition, the gold in the anode sludge is oxidized and proceed to solution formation containing golden wang aqueous solution; Chloride binding after silver in the anode sludge is oxidized and in solution, forms the white silver nitride precipitation of indissoluble and enters in silver chloride slag; Silver chloride slag send silver-colored workshop recover silver;
3. oxalic acid reduction
Containing golden wang aqueous solution under temperature 91-95 DEG C of condition, add oxalic acid reduction; Oxalic acid add-on is the 125-130% of theoretical amount; And in reduction process, add the alkali lye containing saturated villaumite, control pH1-2, Selectively leaching gold;
4. the leached mud 3. step obtained, again through washing, pickling with wash, obtains the finished product gold meeting international more than IG-Au99.99% again.
The present invention, by design optimization, sets about from process modification, traditional oxalic acid reduction method gold extraction technology is improved, and before oxalic acid reduction, anode sludge nitric acid is boiled removal of impurities, by impurity removings such as the copper in the anode sludge, lead, bismuths.Directly obtain with oxalic acid reduction the finished product gold meeting international more than IG-Au99.99%, when the technology key that organic chemistry reduction method of the present invention reclaims High Purity Gold from the anode sludge is to reduce with oxalic acid, add the alkali lye control pH=1-2 containing villaumite.The object introducing villaumite is not change chlorine ion concentration.The present invention not only improves the quality of finished product gold greatly, and eliminates electrolysis process and the follow-up purification of traditional technology, shortens the production cycle, saves production cost.The present invention can be interrupted production, and gold backlog is few, and turnover of funds is fast, and the scattered gold produced in production process is few, is convenient to management and defendance, suitable especially medium and small industrial enterprise.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is elaborated.
Accompanying drawing 1 represents that the processing step that a kind of organic reducing method reclaims High Purity Gold from the anode sludge is:
1. acidleach removal of impurities
Before with chloroazotic acid parting, first carry out acidleach removal of impurities, embathe the anode sludge with the nitric acid boiled, control liquid-solid volume mass and compare 10:1L/kg; The partial oxide in the anode sludge, oxyhydroxide and soluble salt is made to enter solution; Avoid impurity in chloroazotic acid parting process and enter solution; Be filtered dry nitric acid insoluble slag, recover silver from nitric acid washing lotion;
2. the molten gold of chloroazotic acid
In nitric acid insoluble slag, add chloroazotic acid, control liquid-solid volume mass and compare 6:1L/kg; Heating, under 100 DEG C of conditions, the gold in the anode sludge is oxidized and proceed to solution formation containing golden wang aqueous solution; Chloride binding after silver in the anode sludge is oxidized and in solution, forms the white silver nitride precipitation of indissoluble and enters in silver chloride slag; Silver chloride slag send silver-colored workshop recover silver;
Main chemical reactions in chloroazotic acid leaching process has:
Au+HNO
3+4HCl=H[AuCl
4]+NO↑+2H
2O
Ag
++CL
-=AgCl↓
3. oxalic acid reduction
Containing under golden wang aqueous solution temperature 95 DEG C of conditions, add oxalic acid reduction; Oxalic acid add-on is 125% of theoretical amount; And in reduction process, add the alkali lye containing saturated villaumite, control pH1-2, Selectively leaching gold;
Main chemical reactions has:
2HAuCl
2+3H
2C
2O
4=2Au+8HCl+6CO
2↑
4. the leached mud 3. step obtained, again through washing, pickling with wash, obtains the finished product gold meeting international more than IG-Au99.99% again.
The alkali lye of above-mentioned saturated villaumite is the mixing solutions of saturated sodium-chloride and sodium hydroxide; Concrete mass ratio is sodium-chlor: sodium hydroxide: water=1:1:3.85.
Above-mentioned silver chloride slag send the step of silver-colored workshop recover silver to be: by the cleaning of silver chloride slag tap water to neutral, after filtration, the leached mud of cleaning, then after drying process, adds soda and mix, heat reduction; The add-on of soda is the 110%-130% of theoretical value; By the leached mud be mixed, be placed in process furnace, be slowly warming up to 500-600 DEG C, constant temperature 20-60 minute; Then be heated to 1050 ~ 1100 DEG C gradually, after constant temperature 10-30 minute, carry out ingot casting and obtain thick silver ingot.
Claims (3)
1. organic reducing method reclaims a technique for High Purity Gold from the anode sludge, it is characterized in that carrying out as follows:
1. acidleach removal of impurities
Embathe the anode sludge with the nitric acid boiled, control liquid-solid volume mass and compare 8-12:1L/kg; The partial oxide in the anode sludge, oxyhydroxide and soluble salt is made to enter solution; Avoid impurity in chloroazotic acid parting process and enter solution; Be filtered dry nitric acid insoluble slag, recover silver from nitric acid washing lotion;
2. the molten gold of chloroazotic acid
In nitric acid insoluble slag, add chloroazotic acid, control liquid-solid volume mass and compare 4-7:1L/kg; Heating, under 95-100 DEG C of condition, the gold in the anode sludge is oxidized and proceed to solution formation containing golden wang aqueous solution; Chloride binding after silver in the anode sludge is oxidized and in solution, forms the white silver nitride precipitation of indissoluble and enters in silver chloride slag; Silver chloride slag send silver-colored workshop recover silver;
3. oxalic acid reduction
Containing golden wang aqueous solution under temperature 91-95 DEG C of condition, add oxalic acid reduction; Oxalic acid add-on is the 125-130% of theoretical amount; And in reduction process, add the alkali lye containing saturated villaumite, control pH1-2, Selectively leaching gold;
4. the leached mud 3. step obtained, again through washing, pickling with wash, obtains the finished product gold meeting international more than IG-Au99.99% again.
2. a kind of organic reducing method according to claim 1 reclaims the technique of High Purity Gold from the anode sludge, is further characterized in that: the alkali lye of described saturated villaumite is the mixing solutions of saturated sodium-chloride and sodium hydroxide; Concrete mass ratio is sodium-chlor: sodium hydroxide: water=1:1:3.85.
3. a kind of organic reducing method according to claim 1 reclaims the technique of High Purity Gold from the anode sludge, be further characterized in that: described silver chloride slag send the step of silver-colored workshop recover silver to be: by the cleaning of silver chloride slag tap water to neutral, after filtration, the leached mud of cleaning, again after drying process, add soda and mix, heat reduction; The add-on of soda is the 110%-130% of theoretical value; By the leached mud be mixed, be placed in process furnace, be slowly warming up to 500-600 DEG C, constant temperature 20-60 minute; Then be heated to 1050 ~ 1100 DEG C gradually, after constant temperature 10-30 minute, carry out ingot casting and obtain thick silver ingot.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106119554A (en) * | 2016-08-18 | 2016-11-16 | 紫金矿业集团股份有限公司 | High Purity Gold the method being enriched with silver, platinum and palladium is prepared from silver anode slime |
CN106222421A (en) * | 2016-08-17 | 2016-12-14 | 北京矿冶研究总院 | Gold mud treatment method |
CN106756047A (en) * | 2016-12-23 | 2017-05-31 | 郴州市金贵银业股份有限公司 | Debris silver anode slime high puies forward the processing method of gold |
CN107641721A (en) * | 2017-09-29 | 2018-01-30 | 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 |
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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 |
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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 |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106222421A (en) * | 2016-08-17 | 2016-12-14 | 北京矿冶研究总院 | Gold mud treatment method |
CN106119554A (en) * | 2016-08-18 | 2016-11-16 | 紫金矿业集团股份有限公司 | High Purity Gold the method being enriched with silver, platinum and palladium is prepared from silver anode slime |
CN106756047A (en) * | 2016-12-23 | 2017-05-31 | 郴州市金贵银业股份有限公司 | Debris silver anode slime high puies forward the processing method of gold |
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 |
CN107641721A (en) * | 2017-09-29 | 2018-01-30 | 云南驰宏锌锗股份有限公司 | A kind of method of thick gold purification |
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 |
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