CN105132694B - Comprehensive recovery method of tailings containing precious metals - Google Patents
Comprehensive recovery method of tailings containing precious metals Download PDFInfo
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- CN105132694B CN105132694B CN201510517284.6A CN201510517284A CN105132694B CN 105132694 B CN105132694 B CN 105132694B CN 201510517284 A CN201510517284 A CN 201510517284A CN 105132694 B CN105132694 B CN 105132694B
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Abstract
The invention discloses a comprehensive recovery method of tailings containing precious metals, which comprises the following steps of firstly introducing oxygen into the tailings for oxidizing roasting, oxidizing and leaching calcine by using sulfuric acid to remove most iron, evaporating and crystallizing a leaching solution to obtain industrial ferric sulfate, chloridizing and leaching the leaching residue by using sulfuric acid and sodium chloride, sending the leaching residue serving as lead-rich slag to a lead smelting enterprise, replacing the leaching solution by using iron powder to obtain a mixture of crude gold and silver, sending the mixture to a precious metal deep processing system, adjusting the pH of the replacement solution by using ammonia water or sodium hydroxide to precipitate iron, and calcining the obtained iron hydroxide to obtain iron oxide red serving as a raw material in the coating industry. The process method of the invention eliminates the influence of long-term stacking of the slag on the environment, has clean and environment-friendly process and does not generate secondary pollution.
Description
Technical field
The invention belongs to melting waste slag comprehensive reutilization field, relates in particular to a kind of to the comprehensive of the tailings containing noble metal
Conjunction utilizes technology.
Background technology
With the utilization of continually developing of mineral resources, available metals resources are fewer and fewer, the secondary money such as mine tailing and tailings
The comprehensive utilization in source increasingly attracts people's attention, and these noble metal tailings parts are the mine tailing of left over by history, and quantity is larger,
At that time due to technology or the factor such as flow and local special weather conditions, so as in its tailings containing gold about in 1g/t
Left and right, argentiferous is in 40g/t or so, and mine tailing is in addition to key component Au, Ag, other elements（Cu、Pb、Zn、）Content is very low, does not reach
The index of comprehensive utilization, harmful element（As、Hg、Sb）Content is all very low, smaller to the influence of extraction of noble metal.The whole nation is yellow at present
Such tailings of golden industry stockpiling has several ten million tons, and about produces t more than 12000 daily now, only with Liang great pans area of China
Exemplified by Henan area and Shandong District, such a tailings t about more than 4000 is about produced daily, and its quantity is big to have some idea of, at present, should
Class tailings the only way out is exactly to sell coloured manufacturing enterprise to use as additive（Its demand is limited）, because tailings produces
Amount is big, will exist in sale and stack（It is outdoor）And the process of long-distance transport, due to wherein containing a variety of harmful elements, for a long time
Surrounding enviroment are brought serious secondary pollution by solar exposure, rain drop erosion, strong wind airborne dust, therefore, are sought more preferably for tailings
Outlet, effectively develop its huge economic value contained, be the task of top priority.
By showing main component repeated detection in tailings and material phase analysis result, the noble metal in tailings is mainly certainly
Right gold, silver, wherein free gold and adhesion gold account for the 85.5% of total amount, and parcel gold only accounts for the 14.5% of total amount.Although correlative study people
Member proposes many processing methods, and the most frequently used method is that tailings regrinds-dump leaching, and its rate of recovery is low, and makes again because of period
With cyanide, the secondary pollution of environment, patent " valuable metal roasting-cyaniding gold-containing tailing synthetical recovery work are easily caused
Skill "（CN 102168176 A）Using it is therein it is iron take ferric chloride purifying agent, asking for product quality and traction be present
Topic.
The content of the invention
The present invention is directed to the deficiency in existing recovery process method, there is provided a kind of integrated treatment tailings containing noble metal recovery
The method utilized.
The present invention is achieved by the following scheme, a kind of comprehensive recovering process of tailings containing noble metal, specifically include with
Lower step：
1）The oxidizing roasting of noble metal tailings：Tailings containing noble metal is taken, is tiled into Muffle furnace, is passed through noble metal tailings matter
Percentage 5-15% oxygen is measured, controls 500-1000 DEG C of sintering temperature, time 0.5-6h, calcining is cooled to 80-150 DEG C；
2）The leaching of calcining：Solid-liquid mass ratio 1 is pressed in calcining：2-8 adds the sulfuric acid that mass fraction is 5-20%, then
Oxidizer 20-50g/L, at 30-100 DEG C, reaction 0.5-6h is leached, filtering, obtains filter residue enrichment slag and filtrate ferric sulfate solution
Liquid, filtrate evaporative crystallization obtain industrial sulphuric acid iron, and solid-liquid mass ratio 1 is pressed in slag is enriched with：It is 6-30%'s that 2-5, which adds mass fraction,
Sulfuric acid, sodium chloride 50-200g/L is then added in the mixed liquor of enrichment slag and sulfuric acid, 30-100 DEG C, reacts 0.5-4h, filtering
Obtain filter residue lead-rich slag and filtrate leachate；
3）The processing of leachate：In step 2）By the solid mass ratio 8-2 of liquid in obtained leachate：1 amount add iron replacement,
Gold, silver mixed precipitation and displacement liquid are filtrated to get, gold, silver mixture send noble metal deep-processing system, and displacement liquid is adjusted with ammoniacal liquor
PH to 6-9, obtain ferric hydroxide precipitate, filter to obtain iron hydroxide, 400-700 DEG C of calcining heat of control is calcined to iron hydroxide
Iron oxide red.
Further, step 2）Described in oxidant be sodium peroxydisulfate or ammonium persulfate.
Further, step 2）In filtrate evaporative crystallization produce the crystalline mother solution or cooling system obtained in industrial sulphuric acid iron
The condensate water circulatory of system uses.
Advantage is the present invention compared with prior art：The tailings that the present invention is handled contains a variety of groups of iron, silicon, calcium, sulphur etc.
Sub-oxide or salts substances, gold, silver etc. by its parcel or are embedded in some impurity, thus extract it is very difficult, for by tail
The purpose that valuable element recycles to greatest extent in slag, the present invention is using oxygen or the method for air oxidation, now by tailings
Oxidizing roasting is carried out, it is oxide to make the cycling of elements such as iron therein, and sulphate of iron, chlorine are taken using sulfuric acid leaching is largely iron
Change after leaching gold, silver, filtrate iron replacement obtains thick gold, silver sediment, and filter residue is sold to lead smelting enterprise as lead-rich slag.This
Inventive method makes system valuable metal effectively be reclaimed, and three wastes self-loopa utilizes, process cleans environmental protection, it is easy to accomplish industrialization
It is the characteristics of production, specific as follows：
（1）Oxidizing roasting of the present invention makes the base metals such as the part iron in tailings be oxidized to the oxide that sulfuric acid is easy to leach
Deng, sulfuric acid leaching major part iron, reduce the reagent consumption of potassium cloride.
（2）Potassium cloride of the present invention adds sodium chloride to form chlorination system in the solution using sulfuric acid, eliminate using hydrochloric acid,
Environmental pollution when chlorine etc. is leached and the health hazard to employee.
（3）The present invention adds ammoniacal liquor and sodium hydroxide regulation pH precipitated irons, and iron hydroxide calcines iron oxide red processed, reduces iron pair
The influence of system, add the recycling purposes of iron.
（4）Pollution-free extraction noble metal：The present invention recycles sulfuric acid to add sodium chloride using iron enrichment gold, silver are leached in advance
System leaches gold, silver, and technological process is shorter, and the leaching rate of gold, silver, iron is more than 95%, without using Cymag in technique
Deng toxic articles, secondary pollution will not be caused.
（5）Cost advantage protrudes compared with iron oxide red traditional processing technology：This technique major product is iron oxide red, with traditional mode of production
Technique is compared, and because raw material sources are in tailings, and realizes the synthetical recovery of a variety of valuable metals, cost advantage is obvious.
（6）Discharged without sewage, solid waste：This process water essentially consists in the press filtration wash water of solid-liquor separation, and evaporator man
Condensed water in sequence, closed cycle.Caused solid waste mostlys come from separation of solid and liquid twice in technique：The filter of separation of solid and liquid
Slag is rich in lead element, and the pyrometallurgical smelting for lead forms metallic lead, thus whole technique produces without solid waste, realizes ring
Protect clean manufacturing.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
Compositional ranges containing noble metal of the invention are Au0.8-5.6g/t, Ag30-135g/t, Fe20-40%, Pb0.8-2.6%.
Embodiment 1：
A kind of comprehensive recovering process of tailings containing noble metal, specifically includes following steps：Take and contain golden tailings 1000g, tile
Into Muffle furnace, 5% oxygen is continually fed into, controls 500 DEG C, time 0.5h of sintering temperature, calcining is cooled to 80 DEG C, calcining cooling
Liquid-solid ratio 2 is leached in control afterwards:1, sulfuric acid mass fraction 5%, sodium peroxydisulfate dosage 20g/L, 60 DEG C of reaction temperature, react 2h, mistake
Filter, filtrate evaporative crystallization obtain ferrum sulfuricum oxydatum solutum, and evaporation mother liquor returns leaching, and liquid-solid ratio 2 is leached in filter residue control:1, sulfuric acid quality point
Number 10%, sodium chloride dosage 20g/L, 80 DEG C of reaction temperature, 4h, filtering are reacted, filter residue is sold as lead-rich slag, filtrate iron powder
Displacement obtains gold, silver mixed sediment and send noble metal deep-processing system, and displacement liquid adjusts PH to 6-9 with ammoniacal liquor, obtains hydroxide
Iron precipitates, and 500 DEG C of calcining heat of control obtains iron oxide red, measures the main metal of iron oxide red and impurity content meets national standard and market demands.
The rate of recovery of calculating is：Gold 90%, silver 92%, iron 96%, lead 97%.
Embodiment 2：
A kind of comprehensive recovering process of tailings containing noble metal, specifically includes following steps：Take and contain golden tailings 1000g, tile
Into Muffle furnace, 15% oxygen is continually fed into, controls 1000 DEG C, time 6h of sintering temperature, calcining is cooled to 150 DEG C, calcining cooling
Liquid-solid ratio 8 is leached in control afterwards:1, sulfuric acid mass fraction 20%, ammonium persulfate dosage 50g/L, 60 DEG C of reaction temperature, react 2h, mistake
Filter, filtrate evaporative crystallization obtain ferrum sulfuricum oxydatum solutum, and evaporation mother liquor returns leaching, and liquid-solid ratio 3 is leached in filter residue control:1, sulfuric acid quality point
Number 30%, sodium chloride dosage 200g/L, 80 DEG C of reaction temperature, 4h, filtering are reacted, filter residue is sold as lead-rich slag, filtrate iron powder
Displacement obtains gold, silver mixed sediment and send noble metal deep-processing system, and displacement liquid adjusts PH to 6 with ammoniacal liquor, obtains iron hydroxide
Precipitation, 700 DEG C of calcining heat of control obtain iron oxide red, measure the main metal of iron oxide red and impurity content meets national standard and market demands.
The rate of recovery of calculating is：Gold 92%, silver 95%, iron 95%, lead 95%.
Embodiment 3：
A kind of comprehensive recovering process of tailings containing noble metal, specifically includes following steps：Tailings containing noble metal is taken, tiling is extremely
In Muffle furnace, the oxygen of noble metal tailings mass percent 8% is passed through, controls 600 DEG C of sintering temperature, time 3h, calcining is cooled to
120℃；Calcining presses solid-liquid mass ratio 1 with the sulfuric acid that mass fraction is 10%：4 add sulfuric acid in calcining, by calcining and sulfuric acid
Add sodium peroxydisulfate 35g/L in mixed liquor, at 90 DEG C, reaction 4h is leached, filtering, obtains filter residue enrichment slag and filtrate ferric sulfate solution
Liquid, filtrate evaporative crystallization obtain industrial sulphuric acid iron, and solid-liquid mass ratio 1 is pressed in slag is enriched with：3 add the sulfuric acid that mass fraction is 20%,
Then sodium chloride 150g/L is added in the mixed liquor of enrichment slag and sulfuric acid, 90 DEG C, 2h is reacted, filters to obtain filter residue lead-rich slag and filter
Liquid leachate；By the solid mass ratio 4 of liquid in obtained leachate：1 amount adds iron replacement, be filtrated to get gold, silver mixed precipitation and
Displacement liquid, gold, silver mixture send noble metal deep-processing system, and displacement liquid adjusts pH to 8 with ammoniacal liquor, obtain ferric hydroxide precipitate,
Iron hydroxide is filtered to obtain, 500 DEG C of calcining heat of control calcines to obtain iron oxide red to iron hydroxide.
Embodiment 4：
A kind of comprehensive recovering process of tailings containing noble metal, specifically includes following steps：Tailings containing noble metal is taken, tiling is extremely
In Muffle furnace, the oxygen of noble metal tailings mass percent 10% is passed through, controls 800 DEG C, time 5h of sintering temperature, calcining cooling
To 100 DEG C；Calcining presses solid-liquid mass ratio 1 with the sulfuric acid that mass fraction is 15%：6 add sulfuric acid in calcining, by calcining and sulfuric acid
Mixed liquor in add oxidant ammonium persulfate 40g/L, at 50 DEG C, reaction 5h is leached, filtering, obtains filter residue enrichment slag and filtrate
Ferrum sulfuricum oxydatum solutum, filtrate evaporative crystallization obtain industrial sulphuric acid iron, and solid-liquid mass ratio 1 is pressed in slag is enriched with：4, which add mass fractions, is
25% sulfuric acid, sodium chloride 180g/L is then added in the mixed liquor of enrichment slag and sulfuric acid, 70 DEG C, 3h is reacted, filters to obtain filter residue
Lead-rich slag and filtrate leachate；By the solid mass ratio 6 of liquid in obtained leachate：1 amount adds iron replacement, is filtrated to get gold, silver
Mixed precipitation and displacement liquid, gold, silver mixture send noble metal deep-processing system, and displacement liquid adjusts pH to 9 with ammoniacal liquor, obtains hydrogen-oxygen
Change iron precipitation, filter to obtain iron hydroxide, 600 DEG C of calcining heat of control calcines to obtain iron oxide red to iron hydroxide.
The preferable case study on implementation of the present invention is the foregoing is only, is not intended to limit the invention, all spirit in the present invention
With any modification, equivalent substitution and improvements made within principle etc., it should be included in the scope of the protection.
Claims (2)
- A kind of 1. comprehensive recovering process of tailings containing noble metal, it is characterised in that：Specifically include following steps：1）The oxidizing roasting of noble metal tailings：Tailings containing noble metal is taken, noble metal compositional ranges are Au0.8-5.6g/t, Ag30- 135g/t, Fe20-40%, Pb0.8-2.6%, tile into Muffle furnace, be passed through noble metal tailings mass percent 5-15% oxygen Gas, controls 500-1000 DEG C of sintering temperature, time 0.5-6h, and calcining is cooled to 80-150 DEG C；2）The leaching of calcining：Solid-liquid mass ratio 1 is pressed in calcining：2-8 adds the sulfuric acid that mass fraction is 5-20%, then oxygenation Agent sodium peroxydisulfate or ammonium persulfate 20-50g/L, at 30-100 DEG C, reaction 0.5-6h is leached, filtering, obtains filter residue enrichment slag With filtrate ferrum sulfuricum oxydatum solutum, filtrate evaporative crystallization obtains industrial sulphuric acid iron, and solid-liquid mass ratio 1 is pressed in slag is enriched with：2-5 adds quality Fraction is 6-30% sulfuric acid, then the addition sodium chloride 50-200g/L in the mixed liquor of enrichment slag and sulfuric acid, 30-100 DEG C, instead 0.5-4h is answered, filters to obtain filter residue lead-rich slag and filtrate leachate；3）The processing of leachate：In step 2）By the solid mass ratio 8-2 of liquid in obtained leachate：1 amount adds iron replacement, mistake Filter obtains gold, silver mixed precipitation and displacement liquid, and gold, silver mixture send noble metal deep-processing system, and displacement liquid adjusts pH with ammoniacal liquor To 6-9, obtain ferric hydroxide precipitate, filter to obtain iron hydroxide, 400-700 DEG C of calcining heat of control calcines to obtain iron to iron hydroxide It is red.
- A kind of 2. comprehensive recovering process of tailings containing noble metal as claimed in claim 1, it is characterised in that：Filtrate evaporative crystallization The condensate water circulatory for producing the crystalline mother solution obtained in industrial sulphuric acid iron or cooling system uses.
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| CN105907980B (en) * | 2016-04-21 | 2018-09-28 | 西北矿冶研究院 | Method for recovering noble metal from antimony-containing soot |
| CN107723473A (en) * | 2017-08-18 | 2018-02-23 | 西北矿冶研究院 | Comprehensive utilization method of high-arsenic-content polymetallic gold ore |
| CN108374093B (en) * | 2018-03-08 | 2019-08-13 | 蒋央芳 | A kind of processing method of sulfide removal of impurities slag |
| CN109082537B (en) * | 2018-07-11 | 2020-09-01 | 开封大学 | Comprehensive utilization method of roasted gold concentrate |
| CN112251603B (en) * | 2020-09-30 | 2021-10-22 | 中国科学院过程工程研究所 | Method for dissociating cyanidation tailings and synchronously recycling iron, gold and silver in cyanidation tailings |
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| CN100404707C (en) * | 2006-08-03 | 2008-07-23 | 山东国大黄金股份有限公司 | Method of extracting gold and silver from arsenic containing aurin ore |
| CN100580109C (en) * | 2007-12-26 | 2010-01-13 | 东华大学 | Method for extracting gold from waste circuit boards |
| CN102936657A (en) * | 2011-08-15 | 2013-02-20 | 江西格林美资源循环有限公司 | Method for metal recovery by ceramic capacitor |
| CN103695646B (en) * | 2013-11-27 | 2015-06-10 | 灵宝金源矿业股份有限公司 | Method for recovery of gold, silver and iron from gold smelting waste residue |
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Effective date of registration: 20190418 Address after: 737100 Gansu Jinchang Economic and Technological Development Zone Gansu Power Investment Yongchang Power Generation Co., Ltd. South Side Patentee after: Gansu Zhongse Oriental Industry and Trade Co., Ltd. Address before: 730900 people's road, Baiyin District, Baiyin, Gansu Province, No. 19 Patentee before: Xibei (Northwest) Academy of Mineral and Metallurgy |
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Address after: 737100 Gansu Jinchang Economic and Technological Development Zone Gansu Power Investment Yongchang Power Generation Co., Ltd. South Side Patentee after: Gansu high energy Zhongse Environmental Protection Technology Co.,Ltd. Address before: 737100 Gansu Jinchang Economic and Technological Development Zone Gansu Power Investment Yongchang Power Generation Co., Ltd. South Side Patentee before: Gansu Zhongse Oriental Industry and Trade Co.,Ltd. |
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