CN105695750A - Method for removing platinum and palladium out of silver electrolyte and concentrating platinum and palladium - Google Patents
Method for removing platinum and palladium out of silver electrolyte and concentrating platinum and palladium Download PDFInfo
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- CN105695750A CN105695750A CN201610126617.7A CN201610126617A CN105695750A CN 105695750 A CN105695750 A CN 105695750A CN 201610126617 A CN201610126617 A CN 201610126617A CN 105695750 A CN105695750 A CN 105695750A
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- palladium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Life Sciences & Earth Sciences (AREA)
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- General Life Sciences & Earth Sciences (AREA)
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- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for removing platinum and palladium out of a silver electrolyte and concentrating platinum and palladium. The technology of adopting cocoanut charcoal for adsorbing, desorbing and concentrating platinum and palladium in the silver electrolyte is adopted. The method comprises the operation steps that firstly, the commercial-grade cocoanut charcoal with the particle size ranging from 6 mesh to 20 mesh is taken and added to the electrolyte, vibration is carried out for 1 h-2 h, the cocoanut charcoal loaded with platinum and palladium is filtered out, and the adding amount of the cocoanut charcoal ranges from 5 g/L to 50 g/L; secondly, nitric acid is used as a desorption agent, the loaded cocoanut charcoal is added to the desorption agent, a reaction is carried out for 1 h-2 h at the temperature ranging from 35 DEG C to 50 DEG C, the cocoanut charcoal is filtered out, and the concentration of nitric acid ranges from 3 mol/L to 6 mol/L; and thirdly, the first step and the second step are repeated till the cocoanut charcoal loses activity, the cocoanut charcoal which cannot continue to be used returns to an anode mud smelting furnace as an anode mud treatment auxiliary material, and meanwhile precious metal left in the cocoanut charcoal is recycled. The method has the beneficial effects that operation is convenient, the platinum and palladium recovery rate is high, the treatment cost is low, and environmental pollution is low.
Description
Technical field
The present invention relates to precious metals metallurgy technology, be specifically related to from silver electrolyte absorption the method reclaiming platinum, palladium。
Background technology
Copper pyrometallurgy enterprise adopts copper anode mud to produce the noble metals such as Au Ag Pt Pd mostly, current technology flow process is commonly the earth of positive pole through normal pressure or high pressure acidleach decopper(ing) remove impurity, after remove impurity, the earth of positive pole obtains Duo Er alloy then through Kaldo Furnace melting, and after being cast into Ag positive plate, electrolysis obtains argentum powder；Silver electrolysis anode slime obtains product gold through parting-reduction, and after gold reduction, liquid carries out platinum palladium extraction。
Owing to silver and palladium reduction potential are close, in silver electrolytic process, part platinum palladium also can enter electrolyte and precipitate out entrance argentum powder at negative electrode, reducing argentum powder purity on the one hand thus affecting the quality of argentum powder, causing follow-up platinum palladium yield to reduce on the other hand。In production practices, in usual control silver electrolyte, palladium content is less than 50mg/L, platinum content less than 5mg/L, during the two content overproof, namely needs electrolyte is carried out open circuit process；The traditional treatment method of open circuit silver electrolyte is copper powder displacement method, and by platinum, palladium in electrolyte with silver in the lump replacement Treatment, this technique open circuit electrolyte processing cost is higher。
Summary of the invention
It is an object of the invention to provide the elimination from silver electrolyte that a kind of easy to operate, platinum palladium recovery rate is high, processing cost is low, environmental pollution is little the method being enriched with platinum palladium。
For realizing object above, the present invention removes and is enriched with the method for platinum palladium from silver electrolyte and adopts the technique of platinum palladium in coconut husk charcoal Adsorption and desorption, enrichment silver electrolyte；Silver electrolyte composition is mainly nitric acid and silver nitrate, wherein nitric acid 10 ~ 15g/L, and concentration of silver ions is 100 ~ 150g/L, and in silver electrolytic process, electrolyte platinum content is enriched to 5 ~ 15mg/L, and palladium is enriched to 50 ~ 100mg/L, exists with ionic forms in the electrolytic solution；The operating procedure removing and being enriched with platinum palladium from silver electrolyte is as follows:
1. taking the coconut husk charcoal that grain diameter is 6 ~ 20 orders, add in above-mentioned electrolyte, vibrate 1 ~ 2h, filters out the coconut husk charcoal being loaded with platinum palladium, and coconut husk charcoal addition is 5 ~ 50g/L；
2. with nitric acid as strippant, being added by load coconut husk charcoal in strippant, react 1 ~ 2h at 35 ~ 50 DEG C, leach coconut husk charcoal, concentration of nitric acid is 3 ~ 6mol/L；
3. repeat the above steps is 1. 2., until coconut husk charcoal loses activity；The coconut husk charcoal that can not be continuing with is returned earth of positive pole smelting furnace as ANODE SLIME TREATMENT adjuvant, reclaims residual noble metal in coconut husk charcoal simultaneously。
Described coconut husk charcoal is commerical grade coconut husk charcoal, does not add any functional group modifying agent and dressing agent；In open circuit silver electrolyte, the response rate of platinum palladium is above 95%。
The present invention removes and is enriched with the method for platinum palladium from silver electrolyte and has following technical effect that
(1) adopt commercially available, do not carry out the platinum palladium that any surface functional group coconut husk charcoal that is modified and that modify comes in Adsorption For Ag electrolyte, utilize platinum palladium in nitric acid desorbing load coconut husk charcoal, Productive statistics is little；
(2) will through repeatedly Adsorption and desorption, final deactivated coconut husk charcoal returns earth of positive pole smelting furnace as ANODE SLIME TREATMENT adjuvant, can avoid the loss of the incomplete platinum palladium of desorbing on the one hand, can reduce earth of positive pole fusion process coke input amount on the other hand。
(3) compared with conventional silver electrolyte open-circuit copper powder substitution technique, this method is workable, and platinum palladium recovery rate is high, energy-saving and water-saving, and production cost is low, can effectively ensure that the generation of silver electrolytic process high-quality argentum powder。
The above-mentioned method removing and being enriched with platinum palladium from silver electrolyte can be applicable to electrorefining of silver process electrolyte purification system, it is adaptable to adsorbs when electrolyte platinum palladium content is too high, be enriched with, reclaim platinum palladium。The present invention can obviously reduce the loss in silver electrolytic process of the platinum palladium, improves quality of cathode silver simultaneously；Adsorbing material used can Reusability repeatedly, can act also as ANODE SLIME TREATMENT adjuvant Returning smelting stove after inefficacy, reclaim remaining noble metal in coconut husk charcoal further；The method is easy to operate, and platinum palladium recovery rate is high, and environmental pollution is little。
Accompanying drawing explanation
Fig. 1 is the method process flow diagram that the present invention removed and be enriched with platinum palladium from silver electrolyte。
Accompanying drawing labelling: silver electrolyte 1, load coconut husk charcoal 2, platinum palladium rich solution 3, coconut husk charcoal 4, inactivation coconut husk charcoal 5。
Detailed description of the invention
The method that the present invention removes from silver electrolyte below in conjunction with the drawings and specific embodiments and is enriched with platinum palladium is described in further detail。
Being exemplified below six embodiments, operating procedure is in conjunction with Fig. 1；The present invention remove from silver electrolyte and be enriched with platinum palladium method be suitable for process conditions and scope as follows:
Silver electrolyte forms: concentration of nitric acid 10 ~ 15g/L, and concentration of silver ions is 100 ~ 150g/L, platinum content 5 ~ 15mg/L, palladium 50 ~ 100mg/L, exists with ionic forms in the electrolytic solution；Absorption coconut husk carbon granule footpath is 6 ~ 20 orders, adsorbs duration of oscillation 1 ~ 2h, and coconut husk charcoal addition is 5 ~ 50g/L；Desorbing concentration of nitric acid is 3 ~ 6mol/L, desorption temperature 35 ~ 50 DEG C, desorption time 1 ~ 2h；Inactivation coconut husk charcoal returns earth of positive pole smelting furnace and processes。
Embodiment 1
The present embodiment is in variable concentrations platiniferous solution, and coconut husk charcoal is for the mensuration of the saturated adsorption capacity of platinum:
Take the coconut husk charcoal granule 2g that particle diameter is 6 ~ 20 orders quadruplicate, be separately added into four parts of 1000mL and open a way in silver electrolyte, platinum ion concentration respectively 6.28mg/L, 9.41mg/L, 8.17mg/L and 10.85mg/L in electrolyte；Concussion absorption 1h, filters on the oscillator, measures platinum ion concentration in filtrate, calculates the saturated extent of adsorption of coconut husk charcoal under variable concentrations。Result is as shown in table 1:
Variable concentrations platinum ion saturated adsorption capacity in table 1 coconut husk charcoal open-circuit silver electrolyte
Embodiment 2
The present embodiment is in variable concentrations palladium-containing solution, and coconut husk charcoal is for the mensuration of the saturated adsorption capacity of palladium:
Take the coconut husk charcoal granule 3g that grain diameter is 6 ~ 20 orders, in quadruplicate, be separately added into four parts of 500mL and open a way in silver electrolyte, palladium ion concentration respectively 56.75mg/L, 60.85mg/L, 78.50mg/L and 69.53mg/L in electrolyte；Vibration absorption 1.5h, filters on the oscillator, measures palladium ion concentration in filtrate, calculates the saturated extent of adsorption of coconut husk charcoal under variable concentrations。Result is as shown in table 2:
Variable concentrations palladium ion saturated adsorption capacity in table 2 coconut husk charcoal open-circuit silver electrolyte
Embodiment 3
The present embodiment adds the coconut husk charcoal 18g of particle diameter 6 ~ 20 order in open circuit silver electrolyte and adsorbs, silver electrolyte volume is 500mL, wherein platinum ion concentration is 8.25mg/L, palladium ion concentration is 65.38mg/L, and vibration absorption 1.5h, filters on the oscillator, with the nitric acid 50mL that concentration is 3mol/L as strippant, maintaining the temperature at 45 DEG C, desorption time is 2h, and result is following table such as:
Table 3 absorb-elute experiment (1)
As can be seen from Table 3, adsorb the platinum in electrolyte, palladium ion effect with coconut husk charcoal fine, and adsorption rate is higher, but elution amount is less, causes direct yield only respectively 88.7% and 91.8%。
Embodiment 4
The present embodiment adds the coconut husk charcoal 14g that particle diameter is 6 ~ 20 orders in open circuit silver electrolyte, electrolyte volume is 300mL, wherein platinum ion concentration is 9.40mg/L, palladium ion concentration is 73.86mg/L, and vibration absorption 1.5h, filters on the oscillator, with the nitric acid 50mL that concentration is 6mol/L as strippant, maintaining the temperature at 45 DEG C, desorption time is 2h, and result is following table such as:
Table 4 absorb-elute experiment (2)
Embodiment 5
1. road silver electrolyte 300mL is taken away triplicate；
2. weighing the coconut husk charcoal 14g that particle diameter is 6 ~ 20 orders, join in a electrolyte in 1., wherein platinum ion concentration is 9.67mg/L, and palladium ion concentration is 62.55mg/L, and vibration absorption 1.5h, filters out the coconut husk charcoal being loaded with platinum, palladium on the oscillator；
3. with the nitric acid that 50mL concentration is 5mol/L as strippant, maintaining the temperature at 45 DEG C, desorption time is 2h, filters out the coconut husk charcoal after desorbing；
4. being left intact by the coconut husk charcoal being filtrated to get, directly return step 2., process same sample three times continuously, result is as follows:
Table 5 adsorption test (3)
Embodiment 6
1. road silver electrolyte 500mL is taken away quintuplicate；
2. weighing the coconut husk charcoal 20g that particle diameter is 6 ~ 20 orders, join in a electrolyte in 1., wherein platinum ion concentration is 10.18mg/L, and palladium ion concentration is 73.66mg/L, and vibration absorption 2h, filters out the coconut husk charcoal being loaded with platinum, palladium on the oscillator；
3. with the nitric acid that 50mL concentration is 5mol/L as strippant, maintaining the temperature at 45 DEG C, desorption time is 2h, filters out the coconut husk charcoal after desorbing；
4. being left intact by the coconut husk charcoal being filtrated to get, directly return step 2., process same sample five times continuously, result is as follows:
Table 6 adsorption test (4)
As seen from the above table, with after a coconut husk charcoal Reusability 5 times, in open circuit silver electrolyte, platinum, palladium concentration are down to 0.1 ~ 0.3mg/L, and adsorption rate more than 90%, adsorption effect is better。But the access times being as coconut husk charcoal increase, and the elution amount of metal reduces, and direct yield declines comparatively obvious。
The above-mentioned continuous coconut husk charcoal processing open circuit silver electrolyte five times and filter paper are placed in crucible and burn, residue aqua regia dissolution after burning, filters, the content of platinum, palladium in detection filtrate, then together with merging with platinum palladium in washing liquid, calculates total amount of metal and the response rate。Result is in Table 7:
Table 7 metal balance table
As seen from the above table, using coconut husk charcoal to carry out 5 absorption, and burned by the coconut husk charcoal used after 5 times, reclaim the platinum of non-eluting, palladium on coconut husk charcoal and filter paper, then combine with platinum, palladium in washing liquid in this example, platinum, palladium recovery rate are all more than 95%。
Major effect parameter of the present invention is coconut husk charcoal addition and desorption process concentration of nitric acid。When coconut husk charcoal addition can cause the absorption of platinum in silver electrolyte, palladium not exclusively lower than lower limit；When desorption process concentration of nitric acid can cause platinum in coconut husk charcoal, palladium desorbing incomplete lower than lower limit, coconut husk charcoal cyclic utilization rate is low。
The application of the present invention is not limited to above-mentioned citing; for those of ordinary skills; under the premise without departing from the principles of the invention, it is also possible to improved according to the above description or modify, all these improve or modify in the protection domain that all should fall into the claims in the present invention。
Claims (2)
1. the method removed from silver electrolyte and be enriched with platinum palladium, is characterized in that: adopt the technique of platinum palladium in coconut husk charcoal Adsorption and desorption, enrichment silver electrolyte；Silver electrolyte composition is mainly nitric acid and silver nitrate, wherein nitric acid 10 ~ 15g/L, and concentration of silver ions is 100 ~ 150g/L, and in silver electrolytic process, electrolyte platinum content is enriched to 5 ~ 15mg/L, and palladium is enriched to 50 ~ 100mg/L, exists with ionic forms in the electrolytic solution；The operating procedure removing and being enriched with platinum palladium from silver electrolyte is as follows:
1. taking the coconut husk charcoal that grain diameter is 6 ~ 20 orders, add in above-mentioned electrolyte, vibrate 1 ~ 2h, filters out the coconut husk charcoal being loaded with platinum palladium, and coconut husk charcoal addition is 5 ~ 50g/L；
2. with nitric acid as strippant, being added by load coconut husk charcoal in strippant, react 1 ~ 2h at 35 ~ 50 DEG C, leach coconut husk charcoal, concentration of nitric acid is 3 ~ 6mol/L；
3. repeat the above steps is 1. 2., until coconut husk charcoal loses activity；The coconut husk charcoal that can not be continuing with is returned earth of positive pole smelting furnace as ANODE SLIME TREATMENT adjuvant, reclaims residual noble metal in coconut husk charcoal simultaneously。
2. the method removed from silver electrolyte as claimed in claim 1 and be enriched with platinum palladium, is characterized in that: described coconut husk charcoal is the commerical grade coconut husk charcoal not adding any functional group modifying agent and dressing agent。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610126617.7A CN105695750A (en) | 2016-03-07 | 2016-03-07 | Method for removing platinum and palladium out of silver electrolyte and concentrating platinum and palladium |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610126617.7A CN105695750A (en) | 2016-03-07 | 2016-03-07 | Method for removing platinum and palladium out of silver electrolyte and concentrating platinum and palladium |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113106252A (en) * | 2021-02-20 | 2021-07-13 | 苏州硒诺唯新新材料科技有限公司 | Method for removing palladium from silver electrolyte by using multifunctional silica gel adsorbent |
| CN114774700A (en) * | 2022-04-27 | 2022-07-22 | 长沙华时捷环保科技发展股份有限公司 | Method for efficiently extracting platinum and palladium resources in silver electrolysis system |
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| CN102676837A (en) * | 2012-05-25 | 2012-09-19 | 四会市鸿明贵金属有限公司 | Method for recycling palladium from silver electrolyte by using dimethylglyoxime |
| CN102808084A (en) * | 2012-08-14 | 2012-12-05 | 云南大学 | Method for enriching platinum and palladium from pressurized cyanating solution |
| CN105112670A (en) * | 2015-09-08 | 2015-12-02 | 云南锡业集团（控股）有限责任公司铅业分公司 | Comprehensive recovery method for platinum and palladium in silver electrolyte |
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2016
- 2016-03-07 CN CN201610126617.7A patent/CN105695750A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102329959A (en) * | 2011-09-05 | 2012-01-25 | 中南大学 | Separation method of palladium from silver electrolyte |
| CN102676837A (en) * | 2012-05-25 | 2012-09-19 | 四会市鸿明贵金属有限公司 | Method for recycling palladium from silver electrolyte by using dimethylglyoxime |
| CN102808084A (en) * | 2012-08-14 | 2012-12-05 | 云南大学 | Method for enriching platinum and palladium from pressurized cyanating solution |
| CN105112670A (en) * | 2015-09-08 | 2015-12-02 | 云南锡业集团（控股）有限责任公司铅业分公司 | Comprehensive recovery method for platinum and palladium in silver electrolyte |
Non-Patent Citations (1)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113106252A (en) * | 2021-02-20 | 2021-07-13 | 苏州硒诺唯新新材料科技有限公司 | Method for removing palladium from silver electrolyte by using multifunctional silica gel adsorbent |
| CN113106252B (en) * | 2021-02-20 | 2024-04-09 | 苏州硒诺唯新新材料科技有限公司 | Method for removing palladium from silver electrolyte by utilizing multifunctional silica gel adsorbent |
| CN114774700A (en) * | 2022-04-27 | 2022-07-22 | 长沙华时捷环保科技发展股份有限公司 | Method for efficiently extracting platinum and palladium resources in silver electrolysis system |
| CN114774700B (en) * | 2022-04-27 | 2024-05-24 | 长沙华时捷环保科技发展股份有限公司 | Method for efficiently extracting platinum-palladium resources in silver electrolysis system |
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Application publication date: 20160622 |