CN104353843A - 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 utilizing copper or lead anode slurry to prepare high pure and ultra-fine silver powder, belong to the recycling field of secondary resource.
Background technology
In today that the host mineral resource reserve that can supply to extract is day by day exhausted, consider to strengthen research dynamics in the comprehensive reutilization of the secondary such as slag, mud resource, development environment close friend, high economic benefit, low cost extract the valuable metals such as lead, tin, reclaim noble metal, realize the process of bulk industrial substantially of secondary resource and effectively utilize, having become the focus in secondary resource and regeneration cycle area research.
Silver will be that in human history, the first is by the metal exploited totally, and the reserves of silver drop to current about 30,000 tons from 1940 300,000 tons, and decrease about 90%, recovery time approximately only has 12 years.The product source of current silver comes from the recovery of associated minerals and secondary resource mostly, silver being widely used in novel energy, electronic circuit board, electromagnetic shielding material, anti-biotic material etc., and this require that the demand for silver and deep processed product thereof further.
One class staple product super fine silver powder of silver has the special construction and performance that are different from massive material in electricity, calorifics, catalysis etc., be widely used in each fields such as microelectronic product, solar module, automobile glass heating wire, it is the raw material of each field critical function material, and demand constantly increases, to raising product, element various aspects of performance important in inhibiting, but domestic and international super fine silver powder products material source is single and cost is high, limits production scale and the quality of silver powder product.
Research and the method for the recovery for Au and Ag utilization of domestic antianode mud are more, but most technique is more complicated, and the Footwall drift rate of recovery is not high, and purity is lower, and added value of product is low.The byproduct that the earth of positive pole obtains when being electrorefining lead, copper, containing elements such as silver, copper, lead, antimony, arsenic, wherein patent of invention " extracts the extraction process of gold, silver " (publication number CN85100108) from the anode mud of copper electroplating, this patent of invention soaks gold by nitric acid leaching silver with chloroazotic acid, gold, silver and impurity is gone out by extract and separate, but waste liquid and aftertreatment technology are complicated and thorough, easily to environment; A point silver (number of patent application 200810049459.5) is reclaimed in the more ripe oxygen-enriched bottom-blowing melting of technology, utilizes continuous oxidation to obtain Jin Heyin to silver-colored slag melting, electrolysis, and the low and metal purity of complex process, the rate of recovery cannot ensure.
Summary of the invention
Recycling process for prior art Anodic mud secondary resource exists that complex process, environmental pollution, metal recovery rate are low, the not high defect of metal purity, the object of the invention is to be that providing a kind of makes full use of the method for industrial residue high efficiente callback metallic silver for high-purity Nano-class argent, the method is simple to operate, environmental pollution is little, metal recovery cost is low, good economic benefit can be obtained, specify developing direction to non-ferrous metal treatment industry.
The invention provides a kind of method utilizing copper or lead anode slurry to prepare high pure and ultra-fine silver powder, the method comprises the following steps:
Step one: roasting, leaching
After copper anode mud and/or lead anode slurry ball mill grinding, under being placed in the temperature of 320 ~ 350 DEG C, carry out oxidizing roasting, product of roasting after the sulfuric acid leaching that mass percent concentration is 10 ~ 30%, isolated by filtration;
Step 2: dissolve, except gold
Step one isolated by filtration gained filter residue is mixed by solid-liquid mass ratio 1:2 ~ 3 with red fuming nitric acid (RFNA), at 40 ~ 60 DEG C after stirring reaction, refilters removing containing golden filter residue;
Step 3: dilution, precipitation
Filter in step 2 after being diluted with water in the filtrate of gained, then add excessive sodium chloride reaction, until without new Precipitation, filter to isolate precipitation, and precipitation is washed with water until washings are colourless;
Step 4: complexing, reduction
After adopting red fuming nitric acid (RFNA) to dissolve step 3 gained precipitation, more slowly drip ammoniacal liquor in lysate, until solution colour is unchanged, filters, obtain silver ammino solution; Gained silver ammino solution is by composite reduction solution reduction, and obtain elemental silver suspension, centrifugal sedimentation, drying, obtain nano-scale silver powder; Wherein, described composite reduction solution is made up of 1:2 ~ 4 in mass ratio polyethylene of dispersing agent pyrrolidones and reducing agent ascorbic acid.
The method utilizing copper or lead anode slurry to prepare high pure and ultra-fine silver powder of the present invention also comprises following preferred version:
In preferred scheme, the mass content of silver in copper anode mud is 5 ~ 20%.
The mass content of the Preparation of Silver From Lead Anodic Slime described in preferred scheme is 12 ~ 30%.
In preferred scheme, copper anode mud and/or lead anode slurry ball mill grinding to particle diameter are 130 μm ~ 180 μm.
In preferred scheme, the oxidizing roasting time is 8 ~ 10 hours.
In preferred scheme, in step 2, the stirring reaction time is 1 ~ 3h.
Dilution in preferred scheme in step 3 is 2 ~ 4 times that the filtrate of step 2 being filtered gained is diluted with water to original volume.
In preferred scheme, in composite reduction solution, polyvinylpyrrolidone is 0.08 ~ 0.15 times of copper anode mud and/or lead anode slurry quality.
In preferred scheme, the process of composite reduction solution reduction silver ammino solution is: by composite reduction solution dilution to after 0.8 ~ 1.2 times of silver ammino solution volume, be slowly added drop-wise in silver ammino solution, stirring reaction.
Leach by low-temperature bake can effectively remove copper, selenium and hoof etc. in conjunction with olefin(e) acid in preferred scheme.
The red fuming nitric acid (RFNA) that the present invention adopts is commercially available red fuming nitric acid (RFNA), and mass percent concentration is 65 ~ 69%.
In preferred scheme, step 3 gained precipitation is after washing, the soluble-salt such as lead, bismuth, palladium, silicon, iron of removing precipitation surface.
In preferred scheme, ammoniacal liquor is percent mass hundred concentration is the weak aqua ammonia of 2 ~ 4%.
Preparing in silver ammino solution process the special character utilizing silver generation complex compound in preferred scheme, by lead, bismuth and other impurity by filtering removing further, obtaining fine silver ammonia solution.
Beneficial effect of the present invention: method of the present invention with the standard copper earth of positive pole or lead anode slurry for raw material, by technique perfect adaptations such as oxidizing roasting, leaching, dissolving, precipitation, complexings, metal impurities in copper anode mud or lead anode slurry are removed successively, final obtained highly purified Nano Silver.Preparation method of the present invention is simple to operate, relative environmental protection, and silver raising recovery rate is high, can obtain good economic benefit, specifies developing direction to non-ferrous metal treatment industry.
Accompanying drawing explanation
[Fig. 1] is process flow diagram of the present invention.
The XRD diffraction spectrogram of the silver powder that [Fig. 2] obtains for embodiment 1.
The SEM photo of the silver powder that [Fig. 3] obtains for embodiment 1.
The XRD diffraction spectrogram of the silver powder that [Fig. 4] obtains for embodiment 2.
The SEM photo of the silver powder that [Fig. 5] obtains for embodiment 2.
The XRD diffraction spectrogram of the silver powder that [Fig. 6] obtains for embodiment 3.
The SEM photo of the silver powder that [Fig. 7] obtains for embodiment 3.
Detailed description of the invention
Following examples are intended to further illustrate content of the present invention, instead of the scope of restriction the claims in the present invention protection.
Embodiment 1
The smelting of copper anode mud
(1) component of copper anode mud is mainly: gold, silver, copper, antimony, selenium, lead are also containing a small amount of tin, bismuth, palladium; Wherein silver-colored mass fraction is generally about 13% to 20%, will allocate the material such as sodium carbonate, iron filings of minute quantity during different melting in addition according to the earth of positive pole into.In this example, silver-colored mass fraction is 14%.
Low-temperature oxidation roasting: get earth of positive pole 300g and be milled to particle diameter and be about 150 μm, then be placed in roasting apparatus, temperature 320 DEG C of low-temperature oxidation roastings 9 hours calcining, calcining leaches copper selenium hoof through dilute sulfuric acid.
(1) nitric acid precipitation is except gold: be placed in by calcining in leaching equipment, add red fuming nitric acid (RFNA) by solid-liquid mass ratio=1:2, and at temperature 40 degrees Celsius, mechanical agitation 2 hours, crosses and filter filter residue gold.
(2) dilute: (1) is obtained 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) add sodium chloride by under m (earth of positive pole): m (sodium chloride)=5:1 normal temperature, precipitation are cleaned, colourless to filtrate, with the removing of filtrate form bismuth, tin, palladium, iron.
(4) nitric acid dissolve: add red fuming nitric acid (RFNA), mechanical agitation 1 hour in (3) precipitation, until precipitation is dissolved completely.
(5) weak aqua ammonia complexing: slowly add the weak aqua ammonia of 3%, solution occurs becoming muddy, continues to add ammoniacal liquor until solution is unchanged.
(6) sedimentation and filtration obtains silver ammino solution: filtered by (5) solution, further except delead, bismuth and other impurity, obtains high-purity silver ammonia solution A.
(7) mix reducing agent to join and get: configure ascorbic acid and polyvinylpyrrolidone mixing reducing solution respectively, its allocation 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 ammino solution)=1:1.
(8) preparation of super fine silver powder: the silver ammino solution A configured and mixing reducing solution reaction B liquid are positioned in water bath with thermostatic control and heat, until temperature constant, B is poured in there-necked flask and puts into water bath with thermostatic control, A is joined in A with the liquid feeding speed of 1/s, and stir with the rotating speed constant speed of 180r/min, after A drips off, continue stirring 5 minutes, centrifugation afterwards, filter, spend and in supersonic wave cleaning machine, distinguish each washing 3 times from water and absolute ethyl alcohol, then put into drying box constant temperature 50 DEG C of dry 8h and obtain super fine silver powder, record silver raising recovery rate and reach 98.1%.X-ray diffractometer and SEM is adopted to measure and observe the phase structure of silver powder, purity and pattern, particle diameter (as shown in Figure 2 and Figure 3), silver powder diffraction maximum is sharp-pointed, coincide with standard card (04-0783), without assorted peak, its high purity 99.4%, and record its particle diameter and be about 0.5 μm.
Embodiment 2
The smelting of lead anode slurry
Lead anode slurry is usually containing Au, Ag, Se, Te, Cu, Al
2o
3, SiO
2, the valuable element such as Fe, Sn, Pd, Bi and platinum group metal, various component has larger fluctuation range, in the ordinary course of things, the total amount of silver, lead, antimony, tin and the element such as copper, arsenic accounts for more than 70% of dry weight, wherein silver-colored mass fraction is between 12% ~ 30%, water content, usually between 30% ~ 35%, will allocate the sodium carbonate of minute quantity into during different melting in addition according to the earth of positive pole.In this example, silver-colored mass fraction is 26%.
(1) low-temperature oxidation roasting: get earth of positive pole 300g and be milled to particle diameter and be about 150 μm, then be placed in roasting apparatus, temperature 320 DEG C of low-temperature oxidation roastings 9 hours calcining, calcining leaches copper selenium hoof through dilute sulfuric acid.
(2) nitric acid precipitation is except gold: be placed in by calcining in leaching equipment, add red fuming nitric acid (RFNA) by solid-liquid mass ratio=1:2.5, and at temperature 50 degrees Celsius, mechanical agitation 2 hours, crosses and filter filter residue gold.
(3) dilute: (2) are obtained 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) add sodium chloride by under m (earth of positive pole): m (sodium chloride)=5:1 normal temperature, precipitation are cleaned, colourless to filtrate, with the removing of filtrate form bismuth, aluminium, palladium, silicon, iron.
(5) nitric acid dissolve: add red fuming nitric acid (RFNA), mechanical agitation 1 hour in (4) precipitation, until precipitation is dissolved completely.
(6) weak aqua ammonia complexing: slowly add the weak aqua ammonia of 3%, solution occurs becoming muddy, continues to add ammoniacal liquor until solution is unchanged.
(7) sedimentation and filtration obtains silver ammino solution: filtered by (6) solution, further except delead, bismuth and other impurity, obtains high-purity silver ammonia solution A.
(8) mix reducing agent to join and get: configure ascorbic acid and polyvinylpyrrolidone mixing reducing solution respectively, its allocation ratio is m (earth of positive pole): m (polyvinylpyrrolidone)=10:1, the earth of positive pole: ascorbic acid=5:2, V (mixed solution): V (silver ammino solution)=1:1.
(9) preparation of super fine silver powder: the silver ammino solution A configured and mixing reducing solution reaction B liquid are positioned in water bath with thermostatic control and heat, until temperature constant, B is poured in there-necked flask and puts into water bath with thermostatic control, A is joined in A with the liquid feeding speed of 1/s, and stir with the rotating speed constant speed of 180r/min, after A drips off, continue stirring 5 minutes, centrifugation afterwards, filter, spend and in supersonic wave cleaning machine, distinguish each washing 3 times from water and absolute ethyl alcohol, then put into drying box constant temperature 50 DEG C of dry 8h and obtain super fine silver powder, recording silver raising recovery rate is 98.9%.X-ray diffractometer and SEM is adopted to carry out instrument to measure and observe the phase structure of silver powder, purity and pattern, particle diameter (as shown in Figure 4, Figure 5), silver powder diffraction maximum is sharp-pointed, coincide with standard card (04-0783), without assorted peak, its high purity 99.5%, and record its particle diameter and be about 0.45 μm.
Embodiment 3
Chemical process
Known: the main chemical compositions of certain earth of positive pole is as shown in the table:
| Element | Percentage composition % | Main existence form |
| Copper | 16.3 | Cu、CuO、CuSO 4、Cu 2Se、Cu 2Te |
| Plumbous | 7.9 | PbSO 4 |
| Bismuth | 0.8 | Bi 2O 3、(BiO) 2SO 4 |
| Antimony | 4.2 | Sb 2O 3 |
| Iron | 0.18 | FeO、FeSO 4 |
| Tellurium | 0.19 | Ag2Te、Cu 2Te、Au 2Te |
| Selenium | 2.9 | Ag 2Se、Cu 2Se |
| Gold | 0.09 | Au、Au 2Te |
| Silver | 17 | Ag 2Se、Ag 2Te、AgCl |
| Platinum family | Metal or alloy state |
(1) low-temperature oxidation roasting: get material 300g and be milled to particle diameter and be about 180 μm, then be placed in roasting apparatus, temperature 350 DEG C of low-temperature oxidation roastings 10 hours calcining, calcining leaches copper selenium hoof through dilute sulfuric acid.
(2) nitric acid precipitation is except gold: be placed in by calcining in leaching equipment, add red fuming nitric acid (RFNA) by solid-liquid mass ratio=1:2.5, and at temperature 50 degrees Celsius, mechanical agitation 2 hours, crosses and filter filter residue gold.
(3) dilute: (2) are obtained 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) add sodium chloride by under m (earth of positive pole): m (sodium chloride)=5:1.5 normal temperature, precipitation are cleaned, colourless to filtrate, with the removing of filtrate form bismuth, aluminium, palladium, silicon, iron.
(5) nitric acid dissolve: add red fuming nitric acid (RFNA), mechanical agitation 1 hour in (4) precipitation, until precipitation is dissolved completely.
(6) weak aqua ammonia complexing: slowly add the weak aqua ammonia of 3%, solution occurs becoming muddy, continues to add ammoniacal liquor until solution is unchanged.
(7) sedimentation and filtration obtains silver ammino solution: filtered by (6) solution, further except delead, bismuth and other impurity, obtains high-purity silver ammonia solution A.
(8) mix reducing agent to join and get: configure ascorbic acid and polyvinylpyrrolidone mixing reducing solution respectively, its allocation ratio is m (earth of positive pole): m (polyvinylpyrrolidone)=10:1, the earth of positive pole: ascorbic acid=5:2, V (mixed solution): V (silver ammino solution)=1:1.
(9) preparation of super fine silver powder: the silver ammino solution A configured and mixing reducing solution reaction B liquid are positioned in water bath with thermostatic control and heat, until temperature constant, B is poured in there-necked flask and puts into water bath with thermostatic control, A is joined in A with the liquid feeding speed of 1/s, and stir with the rotating speed constant speed of 180r/min, after A drips off, continue stirring 5 minutes, centrifugation afterwards, filter, spend and in supersonic wave cleaning machine, distinguish each washing 3 times from water and absolute ethyl alcohol, then put into drying box constant temperature 50 DEG C of dry 8h and obtain super fine silver powder, obtaining silver raising recovery rate after weighing is 99.0%.X-ray diffractometer and SEM is adopted to carry out instrument to measure and observe the phase structure of silver powder, purity and pattern, particle diameter (as shown in Figure 6, Figure 7), silver powder diffraction maximum is sharp-pointed, coincide with standard card (04-0783), without peak of obviously mixing, its high purity 99.4%, and record its particle diameter and be about 0.4 μm.
Claims (8)
1. utilize copper or lead anode slurry to prepare a method for high pure and ultra-fine silver powder, it is characterized in that, comprise the following steps:
Step one: roasting, leaching
After copper anode mud and/or lead anode slurry ball mill grinding, under being placed in the temperature of 320 ~ 350 DEG C, carry out oxidizing roasting, product of roasting after the sulfuric acid leaching that mass percent concentration is 10 ~ 30%, isolated by filtration;
Step 2: dissolve, except gold
Step one isolated by filtration gained filter residue is mixed by solid-liquid mass ratio 1:2 ~ 3 with red fuming nitric acid (RFNA), at 40 ~ 60 DEG C after stirring reaction, refilters removing containing golden filter residue;
Step 3: dilution, precipitation
Filter in step 2 after being diluted with water in the filtrate of gained, then add excessive sodium chloride reaction, until without new Precipitation, filter to isolate precipitation, and precipitation is washed with water until washings are colourless;
Step 4: complexing, reduction
After adopting red fuming nitric acid (RFNA) to dissolve step 3 gained precipitation, more slowly drip ammoniacal liquor in lysate, until solution colour is unchanged, filters, obtain silver ammino solution; Gained silver ammino solution is by composite reduction solution reduction, and obtain elemental silver suspension, centrifugal sedimentation, drying, obtain nano-scale silver powder; Wherein, described composite reduction solution is made up of 1:2 ~ 4 in mass ratio polyethylene of dispersing agent pyrrolidones and reducing agent ascorbic acid.
2. the method for claim 1, is characterized 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, is characterized in that, described copper anode mud and/or lead anode slurry ball mill grinding to particle diameter are 130 μm ~ 180 μm.
4. the method for claim 1, is characterized in that, the oxidizing roasting time is 8 ~ 10 hours.
5. the method for claim 1, is characterized in that, in step 2, the stirring reaction time is 1 ~ 3h.
6. the method for claim 1, is characterized in that, the dilution in step 3 is 2 ~ 4 times that the filtrate of step 2 being filtered gained is diluted with water to original volume.
7. the method for claim 1, is characterized in that, in described composite reduction solution, polyvinylpyrrolidone is 0.08 ~ 0.15 times of copper anode mud and/or lead anode slurry quality.
8. the method for claim 1, is characterized in that, the process of described composite reduction solution reduction silver ammino solution is: by composite reduction solution dilution to after 0.8 ~ 1.2 times of silver ammino solution volume, be slowly added drop-wise in silver ammino solution, stirring reaction.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104860271A (en) * | 2015-06-08 | 2015-08-26 | 东北大学 | Method for leaching tellurium in copper anode mud under normal pressure |
| CN117483781A (en) * | 2023-12-08 | 2024-02-02 | 郴州市三分地环保信息科技有限公司 | Preparation method of superfine silver powder |
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| CN117483781A (en) * | 2023-12-08 | 2024-02-02 | 郴州市三分地环保信息科技有限公司 | Preparation method of superfine silver powder |
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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. |