CN104353843B - Method for preparing high-purity superfine silver powder from copper or lead anodic slimes - Google Patents
Method for preparing high-purity superfine silver powder from copper or lead anodic slimes Download PDFInfo
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Abstract
The invention discloses a method for preparing high-purity superfine silver powder from copper or lead anodic slimes. The method comprises the following steps: taking copper or lead anodic slimes as raw material, ball milling, low-temperature oxidation roasting, leaching selenium, copper and tellurium in dilute sulfuric acid, separating out gold through nitric acid dissolution and residue filtering, diluting, precipitating silver through sodium chloride, dissolving in nitric acid, complexing with weak aqua ammonia, and filtering to obtain a high-purity silver ammonia solution; a reductant and a dispersant composite solution are subjected to the reduction reaction to prepare high-purity nanoscale silver powder. The method is simple in operation, low in environmental pollution, high in metal recovery rate, and low in recovery cost, can obtain higher economic benefits, and points the development direction to the industry of non-ferrous metal waste treatment.
Description
Technical field
The present invention relates to a kind of method that utilization copper or lead anode slurry prepare high pure and ultra-fine silver powder, belong to returning for two grades of resources
Receipts utilize field.
Background technology
In the today for the reserving volume of host mineral resource increasingly depleted for being available for extracting, it is considered in the comprehensive of two grades of resources such as slag, mud
Close recycling aspect and increase research dynamics, development environment is friendly, high economic benefit, low cost extract the valuable metals such as lead, tin,
Noble metal is reclaimed, the substantially bulk industrial treatment and effectively utilizes of secondary resource is realized, it has also become two grades of resources and again
Focus in raw cycle art research.
Silver will be the metal that the first is produced totally in human history, and the reserves of silver are under 300,000 tons in 1940
Current about 30,000 ton are dropped to, about 90% is reduced, recovery time only about 12 years.At present the product source of silver is most
Come from the recovery of associated minerals and two grades of resources, silver is in novel energy, electronic circuit board, electromagnetic shielding material, anti-biotic material
Etc. aspect be widely used, this further requirement is for silver and its demand of deep processed product.
One class staple product super fine silver powder of silver has the spy different from massive material at aspects such as electricity, calorifics, catalysis
Different structure and performance, are widely used in each field such as microelectronic product, solar module, automobile glass heating wire, are each
The raw material of field critical function material, and demand is continuously increased, and has important meaning to improving product, element various aspects of performance
Justice, but the single and high cost in super fine silver powder products material source both at home and abroad, limit the production scale and quality of silver powder product.
The research and method that the domestic recovery for Au and Ag to the earth of positive pole is utilized is more, but most techniques are more complicated, reclaim metal
The rate of recovery is not high, and purity is relatively low, and added value of product is low.The byproduct that the earth of positive pole is obtained when being electrorefining lead, copper, containing silver,
The elements such as copper, lead, antimony, arsenic, wherein patent of invention " extraction process of gold, silver is extracted from the anode mud of copper electroplating " (publication number
CN85100108), this patent of invention goes out gold, silver and impurity by nitric acid leaching silver and chloroazotic acid leaching gold by extract and separate, but useless
Liquid and aftertreatment technology are complicated and thorough, easily to environment；The more ripe oxygen-enriched bottom-blowing melting of technology is reclaimed and divided
Silver-colored (number of patent application 200810049459.5), using continuous oxidation Jin Heyin is obtained to silver-colored slag melting, electrolysis, complex process,
The rate of recovery is low and metal purity cannot ensure.
The content of the invention
There is complex process, environmental pollution, metal for the recycling process of two grades of resources of prior art Anodic mud
The rate of recovery is low, the not high defect of metal purity, and it is to provide one kind to make full use of industrial residue efficiently to return that the purpose of the present invention is
Method of the metallic silver for high-purity Nano-class argent is received, the method is simple to operate, environmental pollution is little, metal recovery low cost,
Preferable economic benefit can be obtained, to industry of non-ferrous metal treatment developing direction is specified.
The invention provides a kind of method that utilization copper or lead anode slurry prepare high pure and ultra-fine silver powder, the method includes following
Step：
Step one：Roasting, leaching
After by copper anode mud and/or lead anode slurry ball mill grinding, being placed at a temperature of 320～350 DEG C carries out oxidizing roasting,
Product of roasting is separated by filtration Jing after the sulfuric acid leaching that mass percent concentration is 10～30%；
Step 2：Dissolving, except gold
Step one is separated by filtration into gained filter residue with red fuming nitric acid (RFNA) by solid-liquid mass ratio 1:2～3 mixing, stir at 40～60 DEG C
After mixing reaction, removing is refiltered containing golden filter residue；
Step 3：Dilution, precipitation
After being diluted with water in filtrate obtained by filtering in step 2, excessive sodium chloride reaction is added, until without new heavy
Precipitation goes out, and filters to isolate precipitation, and precipitation is washed with water until washings are in colourless；
Step 4：Complexing, reduction
After step 3 gained precipitation is dissolved using red fuming nitric acid (RFNA), then ammoniacal liquor is slowly added dropwise in lysate, until solution face
Color is unchanged, filters, and obtains silver ammino solution；Gained silver ammino solution is reduced by composite reduction solution, obtains element silver suspension,
Centrifugal sedimentation, drying, obtain nano-scale silver powder；Wherein, described composite reduction solution by polyethylene of dispersing agent pyrrolidones and
Reducing agent ascorbic acid in mass ratio 1:2～4 compositions.
The utilization copper or lead anode slurry of the present invention prepares the method for high pure and ultra-fine silver powder also includes following preferred version：
The mass content of silver in copper anode mud is 5～20% in preferred scheme.
The mass content of the Preparation of Silver From Lead Anodic Slime described in preferred scheme is 12～30%.
Copper anode mud and/or lead anode slurry ball mill grinding to particle diameter are 130 μm～180 μm in preferred scheme.
Oxidizing roasting time is 8～10 hours in preferred scheme.
The stirring reaction time is 1～3h in step 2 in preferred scheme.
Dilution in preferred scheme in step 3 be by step 2 filter obtained by filtrate be diluted with water to the 2 of original volume
～4 times.
Polyvinylpyrrolidone is copper anode mud and/or quality of lead anode slurry in composite reduction solution in preferred scheme
0.08～0.15 times.
The process of composite reduction solution reduction silver ammino solution is in preferred scheme：Composite reduction solution is diluted to into silver-colored ammonia
After 0.8～1.2 times of liquor capacity, in being slowly dropped to silver ammino solution, stirring reaction.
Combining olefin(e) acid leaching by low-temperature bake in preferred scheme can effectively remove copper, selenium and hoof etc..
For commercially available red fuming nitric acid (RFNA), mass percent concentration is 65～69% to the red fuming nitric acid (RFNA) that the present invention is adopted.
After step 3 gained precipitation is scrubbed in preferred scheme, lead, bismuth, palladium, silicon, the iron of precipitation surface etc. are removed solvable
Property salt.
Ammoniacal liquor is the weak aqua ammonia that quality very concentration is 2～4% in preferred scheme.
The special property of complex compound is generated using silver during silver ammino solution is prepared in preferred scheme, by lead, bismuth
Further removed by filtering with other impurity, obtain fine silver ammonia solution.
Beneficial effects of the present invention：The method of the present invention with industrial copper anode mud or lead anode mud as a raw material, by oxidation
The technique perfect adaptation such as roasting, leaching, dissolving, precipitation, complexing, the metal impurities in copper anode mud or lead anode slurry are removed successively
Go, highly purified Nano Silver is finally obtained.The preparation method of the present invention is simple to operate, relative environmental protection, and silver raising recovery rate is high, can obtain
Preferably economic benefit, to industry of non-ferrous metal treatment developing direction is specified.
Description of the drawings
【Fig. 1】For the process flow diagram of the present invention.
【Fig. 2】The XRD diffraction spectrograms of silver powder obtained in embodiment 1.
【Fig. 3】The SEM photograph of silver powder obtained in embodiment 1.
【Fig. 4】The XRD diffraction spectrograms of silver powder obtained in embodiment 2.
【Fig. 5】The SEM photograph of silver powder obtained in embodiment 2.
【Fig. 6】The XRD diffraction spectrograms of silver powder obtained in embodiment 3.
【Fig. 7】The SEM photograph of silver powder obtained in embodiment 3.
Specific embodiment
Following examples are intended to further illustrate present invention, rather than limit the model of the claims in the present invention protection
Enclose.
Embodiment 1
The smelting of copper anode mud
(1) component of copper anode mud is mainly:Gold, silver, copper, antimony, selenium, lead simultaneously contain a small amount of tin, bismuth, palladium；It is wherein silver
Amount fraction typically 13% to 20% or so, according further to the earth of positive pole different meltings when will allocate into minimal amount of sodium carbonate,
The materials such as iron filings.Silver mass fraction is 14% in the example.
Low-temperature oxidation roasting:Take earth of positive pole 300g and be milled to particle diameter and be about 150 μm, then be placed in roasting apparatus,
320 DEG C of temperature low-temperature oxidation roasting 9 hours obtains calcining, and calcining Jing dilute sulfuric acids leach copper selenium hoof.
(1) nitric acid precipitation is except gold：Calcining is placed in leaching equipment, by solid-liquid mass ratio=1:2 add red fuming nitric acid (RFNA), in temperature
Under 40 degrees Celsius of degree, mechanical agitation 2 hours is filtered to remove filter residue gold.
(2) dilute：(1) is obtained into filtrate and adds deionized water, additional proportion is V (red fuming nitric acid (RFNA))：V (deionized water)=1:
2, and mechanical agitation half an hour.
(3) the heavy silver of sodium chloride：(2) by m (earth of positive pole)：M (sodium chloride)=5:Sodium chloride is added under 1 normal temperature, precipitation is clear
Wash, it is colourless to filtrate, bismuth, tin, palladium, iron are removed with filtrate form.
(4) nitric acid dissolving：Red fuming nitric acid (RFNA), 1 hour of mechanical agitation are added in (3) precipitation, until precipitation is completely dissolved.
(5) weak aqua ammonia complexing：3% weak aqua ammonia is slowly added to, becoming cloudy occurs in solution, continuously adds ammoniacal liquor until solution
It is unchanged.
(6) precipitation filters to obtain silver ammino solution：(5) solution is filtered, lead, bismuth and other impurity are further removed, height is obtained
Purity silver ammino solution A.
(7) mixing reducing agent is matched somebody with somebody and is taken：Ascorbic acid and polyvinylpyrrolidone mixing reducing solution are respectively configured, its configuration
Ratio is m (earth of positive pole)：M (polyvinylpyrrolidone)=10:1, the earth of positive pole：Ascorbic acid=5:1, V (mixed solution):V (silver
Ammonia solution)=1:1.
(8) preparation of super fine silver powder：The silver ammino solution A for having configured and mixing reducing solution reaction B liquid are positioned over into constant temperature
Heat in water-bath, until temperature constant, pours B in there-necked flask into and be put in water bath with thermostatic control, A is added into liquid speed with 1 drop/s
Degree is added in A, and is stirred with the rotating speed constant speed of 180r/min, after A is dripped off, continues to stir 5 minutes, centrifugation afterwards,
Filter, spend and each washing 3 times is distinguished in supersonic wave cleaning machine from water and absolute ethyl alcohol, be then placed in constant temperature 50 in drying box
DEG C being dried 8h obtains super fine silver powder, measures silver raising recovery rate and reaches 98.1%.Using X-ray diffractometer and SEM come
Phase structure, purity and pattern, the particle diameter (as shown in Figure 2 and Figure 3) of silver powder are determined and observe, silver powder diffraction maximum is sharp, with standard
Card (04-0783) coincide, without miscellaneous peak, its high purity 99.4%, and measure its particle diameter and be about 0.5 μm.
Embodiment 2
The smelting of lead anode slurry
Lead anode slurry usually contains Au, Ag, Se, Te, Cu, Al2O3、SiO2, Fe, Sn, Pd, Bi and platinum group metal etc. it is valuable
Element, various components have larger fluctuation range, in general, the total amount of the element such as silver, lead, antimony, tin and copper, arsenic
Account for more than the 70% of dry weight, wherein silver mass fraction between 12%～30%, water content generally between 30%～35%, in addition
According to minimal amount of sodium carbonate will be allocated into during the different meltings of the earth of positive pole.Silver mass fraction is 26% in the example.
(1) low-temperature oxidation roasting:Take earth of positive pole 300g and be milled to particle diameter and be about 150 μm, then be placed in roasting apparatus,
Calcining is obtained in 320 DEG C of temperature low-temperature oxidation roasting 9 hours, calcining Jing dilute sulfuric acids leach copper selenium hoof.
(2) nitric acid precipitation is except gold：Calcining is placed in leaching equipment, by solid-liquid mass ratio=1:2.5 add red fuming nitric acid (RFNA),
At 50 degrees Celsius of temperature, mechanical agitation 2 hours is filtered to remove filter residue gold.
(3) dilute：(2) are obtained into filtrate and adds deionized water, additional proportion is V (red fuming nitric acid (RFNA))：V (deionized water)=1:
2, and mechanical agitation half an hour.
(4) the heavy silver of sodium chloride：(3) by m (earth of positive pole)：M (sodium chloride)=5:Sodium chloride is added under 1 normal temperature, precipitation is clear
Wash, it is colourless to filtrate, bismuth, aluminium, palladium, silicon, iron are removed with filtrate form.
(5) nitric acid dissolving：Red fuming nitric acid (RFNA), 1 hour of mechanical agitation are added in (4) precipitation, until precipitation is completely dissolved.
(6) weak aqua ammonia complexing：3% weak aqua ammonia is slowly added to, becoming cloudy occurs in solution, continuously adds ammoniacal liquor until solution
It is unchanged.
(7) precipitation filters to obtain silver ammino solution：(6) solution is filtered, lead, bismuth and other impurity are further removed, height is obtained
Purity silver ammino solution A.
(8) mixing reducing agent is matched somebody with somebody and is taken：Ascorbic acid and polyvinylpyrrolidone mixing reducing solution are respectively configured, its configuration
Ratio is m (earth of positive pole)：M (polyvinylpyrrolidone)=10:1, the earth of positive pole：Ascorbic acid=5:2, V (mixed solutions):V (silver
Ammonia solution)=1:1.
(9) preparation of super fine silver powder：The silver ammino solution A for having configured and mixing reducing solution reaction B liquid are positioned over into constant temperature
Heat in water-bath, until temperature constant, pours B in there-necked flask into and be put in water bath with thermostatic control, A is added into liquid speed with 1 drop/s
Degree is added in A, and is stirred with the rotating speed constant speed of 180r/min, after A is dripped off, continues to stir 5 minutes, centrifugation afterwards,
Filter, spend and each washing 3 times is distinguished in supersonic wave cleaning machine from water and absolute ethyl alcohol, be then placed in constant temperature 50 in drying box
DEG C being dried 8h obtains super fine silver powder, measures silver raising recovery rate for 98.9%.Using X-ray diffractometer and SEM come instrument
To determine and observe phase structure, purity and pattern, the particle diameter (as shown in Figure 4, Figure 5) of silver powder, silver powder diffraction maximum is sharp, with mark
Quasi- card (04-0783) is coincide, without miscellaneous peak, its high purity 99.5%, and measure its particle diameter and be about 0.45 μm.
Embodiment 3
Chemical process
It is known：The main chemical compositions of certain earth of positive pole are as shown in the table:
| Element | Percentage composition % | It is primarily present form |
| Copper | 16.3 | Cu、CuO、CuSO4、Cu2Se、Cu2Te |
| Lead | 7.9 | PbSO4 |
| Bismuth | 0.8 | Bi2O3、(BiO)2SO4 |
| Antimony | 4.2 | Sb2O3 |
| Iron | 0.18 | FeO、FeSO4 |
| Tellurium | 0.19 | Ag2Te、Cu2Te、Au2Te |
| Selenium | 2.9 | Ag2Se、Cu2Se |
| Gold | 0.09 | Au、Au2Te |
| Silver | 17 | Ag2Se、Ag2Te、AgCl |
| Platinum family | Metal or alloy state |
(1) low-temperature oxidation roasting:Take material 300g and be milled to particle diameter and be about 180 μm, then be placed in roasting apparatus,
350 DEG C of temperature low-temperature oxidation roasting 10 hours obtains calcining, and calcining Jing dilute sulfuric acids leach copper selenium hoof.
(2) nitric acid precipitation is except gold：Calcining is placed in leaching equipment, by solid-liquid mass ratio=1:2.5 add red fuming nitric acid (RFNA),
At 50 degrees Celsius of temperature, mechanical agitation 2 hours is filtered to remove filter residue gold.
(3) dilute：(2) are obtained into filtrate and adds deionized water, additional proportion is V (red fuming nitric acid (RFNA))：V (deionized water)=1:
2, and mechanical agitation half an hour.
(4) the heavy silver of sodium chloride：(3) by m (earth of positive pole)：M (sodium chloride)=5:Sodium chloride is added under 1.5 normal temperature, will be precipitated
Cleaning, it is colourless to filtrate, bismuth, aluminium, palladium, silicon, iron are removed with filtrate form.
(5) nitric acid dissolving：Red fuming nitric acid (RFNA), 1 hour of mechanical agitation are added in (4) precipitation, until precipitation is completely dissolved.
(6) weak aqua ammonia complexing：3% weak aqua ammonia is slowly added to, becoming cloudy occurs in solution, continuously adds ammoniacal liquor until solution
It is unchanged.
(7) precipitation filters to obtain silver ammino solution：(6) solution is filtered, lead, bismuth and other impurity are further removed, height is obtained
Purity silver ammino solution A.
(8) mixing reducing agent is matched somebody with somebody and is taken：Ascorbic acid and polyvinylpyrrolidone mixing reducing solution are respectively configured, its configuration
Ratio is m (earth of positive pole)：M (polyvinylpyrrolidone)=10:1, the earth of positive pole：Ascorbic acid=5:2, V (mixed solutions):V (silver
Ammonia solution)=1:1.
(9) preparation of super fine silver powder：The silver ammino solution A for having configured and mixing reducing solution reaction B liquid are positioned over into constant temperature
Heat in water-bath, until temperature constant, pours B in there-necked flask into and be put in water bath with thermostatic control, A is added into liquid speed with 1 drop/s
Degree is added in A, and is stirred with the rotating speed constant speed of 180r/min, after A is dripped off, continues to stir 5 minutes, centrifugation afterwards,
Filter, spend and each washing 3 times is distinguished in supersonic wave cleaning machine from water and absolute ethyl alcohol, be then placed in constant temperature 50 in drying box
DEG C being dried 8h obtains super fine silver powder, after weighing silver raising recovery rate is 99.0%.Using X-ray diffractometer and SEM
Carry out instrument to determine and observe phase structure, purity and pattern, the particle diameter (as shown in Figure 6, Figure 7) of silver powder, silver powder diffraction maximum is sharp,
It coincide with standard card (04-0783), without obvious miscellaneous peak, its high purity 99.4%, and measure its particle diameter and be about 0.4 μm.
Claims (8)
1. a kind of method that utilization copper or lead anode slurry prepare high pure and ultra-fine silver powder, it is characterised in that comprise the following steps：
Step one：Roasting, leaching
After by copper anode mud and/or lead anode slurry ball mill grinding, being placed at a temperature of 320～350 DEG C carries out oxidizing roasting, roasting
Product is separated by filtration Jing after sulfuric acid leaching copper, selenium and tellurium that mass percent concentration is 10～30%；
Step 2：Dissolving, except gold
Step one is separated by filtration into gained filter residue with red fuming nitric acid (RFNA) by solid-liquid mass ratio 1:2～3 mixing, stir anti-at 40～60 DEG C
Ying Hou, refilters removing containing golden filter residue；
Step 3：Dilution, precipitation
After being diluted with water in filtrate obtained by filtering in step 2, excessive sodium chloride reaction is added, until without new precipitation analysis
Go out, filter to isolate precipitation, and precipitation is washed with water until washings are in colourless；
Step 4：Complexing, reduction
Will step 3 gained precipitation using red fuming nitric acid (RFNA) dissolving after, then be slowly added dropwise ammoniacal liquor in lysate, until solution colour without
Change, filters and removes lead, bismuth and other impurity, obtains silver ammino solution；Gained silver ammino solution is reduced by composite reduction solution, is obtained
To element silver suspension, centrifugal sedimentation, drying, nano-scale silver powder is obtained；Wherein, described composite reduction solution is gathered by dispersant
Vinylpyrrolidone and reducing agent ascorbic acid in mass ratio 1:2～4 compositions.
2. the method for claim 1, it is characterised in that the mass content of described silver in copper anode mud is 5～20%；
The mass content of described Preparation of Silver From Lead Anodic Slime is 12～30%.
3. the method for claim 1, it is characterised in that described copper anode mud and/or lead anode slurry ball mill grinding are extremely
Particle diameter is 130 μm～180 μm.
4. the method for claim 1, it is characterised in that oxidizing roasting time is 8～10 hours.
5. the method for claim 1, it is characterised in that the stirring reaction time is 1～3h in step 2.
6. the method for claim 1, it is characterised in that the dilution in step 3 be step 2 is filtered obtained by filtrate
It is diluted with water to 2～4 times of original volume.
7. the method for claim 1, it is characterised in that polyvinylpyrrolidone is copper in described composite reduction solution
0.08～0.15 times of the earth of positive pole and/or quality of lead anode slurry.
8. the method for claim 1, it is characterised in that described composite reduction solution reduces the process of silver ammino solution
For：After composite reduction solution is diluted to into 0.8～1.2 times of silver ammino solution volume, in being slowly dropped to silver ammino solution, stirring is anti-
Should.
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| CN1600477A (en) * | 2003-09-28 | 2005-03-30 | 中国印钞造币总公司 | Method for preparing nano silver powder |
| KR20060018496A (en) * | 2004-08-24 | 2006-03-02 | 한국지질자원연구원 | Composite metal powder manufaturing method of silver and copper |
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| CN1090604A (en) * | 1993-02-06 | 1994-08-10 | 中国有色金属工业总公司昆明贵金属研究所 | Tin anode mud extracts the method for precious metal and valuable metal |
| CN1600477A (en) * | 2003-09-28 | 2005-03-30 | 中国印钞造币总公司 | Method for preparing nano silver powder |
| KR20060018496A (en) * | 2004-08-24 | 2006-03-02 | 한국지질자원연구원 | Composite metal powder manufaturing method of silver and copper |
| CN101254541A (en) * | 2008-01-21 | 2008-09-03 | 中南大学 | Preparation of nano aluminum powder for conducting resin and storage method |
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Effective date of registration: 20180808 Address after: 423000 Nonferrous Metals Science and Technology Industrial Park, Bailu Town, Suxian District, Chenzhou, Hunan, China Patentee after: CHENZHOU XIANGJIN NONFERROUS METALS Co.,Ltd. Address before: 510000 302 of the south side of 8 two Heng Road, Tianhe District, Guangzhou, Guangdong province (for office use only). Patentee before: Guangzhou fortune Intellectual Property Operation Co.,Ltd. Effective date of registration: 20180808 Address after: 510000 302 of the south side of 8 two Heng Road, Tianhe District, Guangzhou, Guangdong province (for office use only). Patentee after: Guangzhou fortune Intellectual Property Operation Co.,Ltd. Address before: 410004 No. two, 960 Wan Li Li South Road, Yuhua District, Changsha, Hunan Patentee before: CHANGSHA University OF SCIENCE AND TECHNOLOGY |
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Effective date of registration: 20211124 Address after: 423000 office building of Chenzhou Xiangjin Nonferrous Metals Co., Ltd., bailutang Town, Suxian District, Chenzhou City, Hunan Province Patentee after: Chenzhou Huacheng new material technology Co.,Ltd. Address before: 423000 Nonferrous Metals Science and Technology Industrial Park, Bailu Town, Suxian District, Chenzhou, Hunan, China Patentee before: CHENZHOU XIANGJIN NONFERROUS METALS Co.,Ltd. |
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