CN1048238A - The fragmentation dissolving methof of precious metal - Google Patents
The fragmentation dissolving methof of precious metal Download PDFInfo
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- CN1048238A CN1048238A CN90104468A CN90104468A CN1048238A CN 1048238 A CN1048238 A CN 1048238A CN 90104468 A CN90104468 A CN 90104468A CN 90104468 A CN90104468 A CN 90104468A CN 1048238 A CN1048238 A CN 1048238A
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- fragmentation
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- dissolving
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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
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Abstract
A kind of fragmentation dissolving methof of precious metal, be included in 700～1200 ℃ of mixing of materials fusion, fragmentations that contain precious metal with base metal fragmentation agent together, leach the fragmentation material with hydrochloric acid soln, leached mud is carried out operations such as aqueous solution chlorination dissolving, it is characterized in that, used fragmentation agent is the compound fragmentation agent of a kind of aluminium-zinc base alloy, its composition is Al10-90%, Zn10-90%, perhaps Al10-80%, Zn10-80%, Cu10-30%; Material is 1 with the weight ratio of fragmentation agent in the fragmentation process: 5-10.Present method can be used for containing the fragmentation dissolving of noble metal materials, fragmentation rate height, and it is simple and easy that fragmentation speed reaches processing soon.
Description
The present invention relates to the precious metal fragmentation dissolving methof that the material intermediate treatment is used in precious metals metallurgy and the analytic process.The fragmentation dissolving methof of some unmanageable precious metal and mineral and alloy particularly.
In precious metal hydrometallurgy and chemical analysis process, generally need earlier precious metal to be dissolved.Because precious metal has extremely strong erosion resistance and oxidation-resistance,, make it to become the solubility salt so classical traditional method is alkali-oxidation fusion.Yet alkali fusion is not only brought a large amount of basic metal into, and some native alloy (as osmiridium) can not fuse fully.Another kind method with chloroazotic acid or with the mixed-acid dissolution of hydrochloric acid and nitric acid, also is the method that is widely adopted promptly.But chloroazotic acid or mixed-acid dissolution be the flow process complexity not only, and human and material resources and energy consumption are big, and ambiance is poor, and working conditions is abominable, and environmental pollution is heavy, and the platinum metals can not be converted into fully only metallurgical state-chlorine title complex.
AnalChem, 1950,22(4), report in 590 pages.Propositions such as Deville in 1874: some native alloy (as the osirita native alloy) is not corroded by causticity reagent under the most violent condition, can go out the active noble metal powder of tool to obtain in small, broken bits in advance with zinc or lead fusion together subsequently with acidleach.After this, plumbous, zinc promptly is used as fragmentation agent (disaggregating reagent) at large.But the powder that obtains with the zinc fragmentation is thick; Lead can not same rhodium, ruthenium, osmium form alloy.Tin also is one of fragmentation agent of using always." precious metal ", 1981,2(1), reported with tin fragmentation iridium rhodium alloy situation for 18 pages.Its method is in advance with the crushing of alloy machinery.Pulverize, use the tin fragmentation again.This shows that the fragmentation rate of tin is low.Also useful copper, bismuth do the fragmentation agent report (" ANALYTICAL CHEMISTRY OF PLATINUM METALS, SIGmzbarg, NAEzerskaya work, N.KANER translates and (is translated from А н а
и т и-ч e с к а я Х и м и я П
а т и н о в ы х М e т а
о в), Edited by P.SHELNITZ, Keter Publishing House Jerusalem Ltd., 1975, P.15,17～20).But copper fragmentation temperature height, aftertreatment is cumbersome.Copper is difficult for removing, and can only use under special circumstances; Bismuth also is the aftertreatment trouble, easily forms mutualization thing with precious metal, and facile hydrolysis, is difficult to eliminate.
Over more than 100 year, the development of fragmentation agent is slowly.General report all invests in analysis and the metallurgical literature.Shang Weijian is the fragmentation dissolving methof of literary composition report precious metal specially.
Purpose of the present invention is to overcome the deficiency of prior art, selects a kind of fragmentation efficient height, fragmentation speed is fast, using method is simple and easy, aftertreatment is simpler new fragmentation agent, and precious metal is carried out the fragmentation dissolving.
The technology of the present invention solution is, research is by experiment selected easily with precious metal alloysization, and the base metal more than the binary that is not quite similar with precious metal alloys mechanism forms compound fragmentation agent, to reach purpose of the present invention.Compound fragmentation agent constituent element selection principle is: (1) is selected easily with precious metal alloysization and the different metallographic phase combination of alloying mechanism; (2) polynary combination, binary at least; (3) select low melting point metal combined.Or low melting point and refractory metal are combined, to reduce fragmentation (being alloying) temperature; (4) select metal with certain resistance of oxidation; (5) select the high metal of boiling point.To reduce volatilization; (6) contain the fragmentation agent again and answer processing characteristics good, be convenient to roll sheet or car bits; (7) the fragmentation temperature of compound fragmentation agent (with the alloying temperature of noble metal materials) can be at 700～1200 ℃.According to above-mentioned selection principle, technical characterictic of the present invention is: as compound fragmentation agent, the concrete composition of this compound fragmentation agent is (Wt%): Al 10～90 to (ⅰ) fragmentation operation with a kind of aluminum zn-based alloys, and Zn 10～90; (ⅱ) material for the treatment of fragmentation during fragmentation is 1: 5～10 with the weight ratio of said compound fragmentation agent.The also alternative Cu that adds in said compound fragmentation agent.The concrete composition that adds the compound fragmentation agent of Cu is (Wt%): Al 10～80, and Zn 10～80, and Cu 10～30.Preferably, the material for the treatment of fragmentation during fragmentation is 1: 6～8 with the weight ratio of said compound fragmentation agent.
Using method of the present invention carries out fragmentation dissolved operation and is containing noble metal materials: make in 700～1200 ℃ of temperature and treat that the fragmentation material is with compound fragmentation agent mixed melting, fragmentation; Leach the fragmentation material with hydrochloric acid soln; Leached mud (noble metal powder) is carried out the aqueous solution chlorination dissolving.The preparation method of fragmentation agent is identical with general alloy electric furnace casting method.
Though the used compound fragmentation agent aluminum zn-based alloys of the present invention is a kind of known alloy from forming, for example the Japanese Patent spy opens clear 56-33450, spy and opens clear 57-200537, spy and open clear 62-1860, Deutsches Reichs-Patent DE2838774 A1 and all disclose with the compound fragmentation agent of the used Al-Zn of the present invention composition and overlap mutually or cross one another aluminum zn-based alloys, but the purpose of above-mentioned documents is not identical with purpose of the present invention.For example, the spy to open clear 56-33450 be the big aluminium-zinc base alloy of a kind of damping capacity.It is the manufacture method of a kind of vibrationproof with zinc base alloy that the spy opens clear 57-200537, it is a kind of plating Al-Zn alloy steel plate that the spy opens clear 62-1860, its purpose is to be used for steel plate vacuum evaporation, increase surface aesthetic and solidity to corrosion, DE2838774A1 then is as the electrode materials in the metal magnetic defectoscope with Al-Zn base alloy.In addition, according to retrieval, yet and do not find and the close alloy of the compound fragmentation agent of Al-Zn-Cn used in the present invention composition more there is not report used as the fragmentation agent.
Single-element fragmentation agent with prior art is compared, compound fragmentation agent of the present invention is because of being multicomponent, and each constituent element is not quite similar with the alloying mechanism of precious metal, (general equal can reach whole fragmentations), fragmentation speed fast (most materials can be finished fragmentation in several minutes to tens of minutes after reaching selected alloying temperature) so its fragmentation rate height to precious metal, the noble metal powder of gained superfine (mean particle size 0.0061～0.0073 μ m), thereby the aqueous solution chlorination that is highly advantageous to dissolving, dissolution rate is fast, dissolution rate is high.Experiment showed, that purpose of the present invention reaches fully.
Embodiment 1
The fragmentation agent component of Al75Wt% and Zn25Wt% (is called for short Al
75Zn
25, below analogize) and add furnace melting, ingot casting by fusing point height order, roll sheet after the cooling and demolding.Then with platinoiridita, platinum rhodium, rhodium iridium alloy waste material and osmiridium sheet grain according to material: the ratio of fragmentation agent=1: 8 is mixed mutually with the fragmentation agent, carries out fragmentation respectively.Compound is placed in the plumbago crucible, adds topped dose of NaCl, at the retort furnace internal heating to selected temperature.Insulation for some time or be not incubated, come out of the stove.The fused alloy is fallen in iron pan.Before solidifying, stir broken with metal bar.Naturally cool to room temperature.Leach the fragmentation material with hydrochloric acid soln, use earlier the 10(volume) leaching of % hydrochloric acid, the process that leaches with backsight increases concentration.When leaching end, keep solution PH＜1.Filter, use earlier the 1(volume) % salt acid elution leached mud (alloy powder), wash with water again, in 110 ℃ of oven dry (to osmiridium fragmentation powder nature or vacuum decompression drying).The gained powder is separated with the residual alloys of not fragmentation.Reach the intact precious metal alloys residual volume of not fragmentation with soaking time and determine its fragmentation speed, it the results are shown in table 1.
By table 1 as seen, for the Pt of thick 0.24～0.34mm
75Ir
25Alloy slice is heated to selected temperature, and being incubated 0～5 minute is complete fragmentation.Pt for φ 0.5mm
90Rh
10The alloy silk is heated to selected temperature, comes out of the stove fragmentation fully immediately.The fragmentation speed of osmiridium is relevant with its composition, and in this example, being incubated 180 minutes is complete fragmentation.Ir
60Rh
40Alloy is with traditional more difficult fragmentation of fragmentation agent.When for example using the tin fragmentation, need machinery crushing in advance, pulverize, use the tin fragmentation again, and fragmentation speed is very slow.With method fragmentation of the present invention, do not need preprocessing, reaching the selected temperature insulation was complete fragmentation in 90～180 minutes.
Embodiment 2
Method by embodiment 1 prepares Al
65Zn
25Cu
10Compound fragmentation agent.Then by treating the fragmentation material: fragmentation agent=1: 8(W/W) the platinum iridium alloy material is mixed with the fragmentation agent.The method of pressing embodiment 1 insulation for some time, is come out of the stove at retort furnace internal heating to 850 ℃.Below operation is with embodiment 1.When the Lan Seshi of copper solutions appears in leach liquor, promptly reach the terminal point of leaching, and make PH＜1 of solution.Below operation is with embodiment 1.Gained the results are shown in Table 2.
Embodiment 3
Method prepared composition by embodiment 1 is respectively Al
50Zn
50, Al
75Zn
25And Al
90Zn
10Compound fragmentation agent, then to Pt
75Ir
25Alloyed scrap carries out fragmentation.In order to compare, simultaneously to material also with traditional method zinc fragmentation.Measure the rate of body weight gain (=gained powder anharmonic ratio material is heavy) and the specific surface area of powder after the fragmentation, calculate the mean particle size of powder, the results are shown in table 3.By table 3 as seen, be 2.27～19.9% with the rate of body weight gain of compound fragmentation agent gained powder, with the rate of body weight gain of zinc fragmentation gained powder then up to 40.1%.Powder mean particle sizes with compound fragmentation agent gained is 0.0061～0.0073 μ m.Reached the granularity of micropowders, with the zinc fragmentation then mean particle size be 0.14 μ m, be 21 times of the mean particle size of compound fragmentation agent fragmentation.
Embodiment 4
The purpose of fragmentation is in order to quicken the dissolving of noble metal materials.For this reason, elder generation is by the method Al of embodiment 1
75Zn
25Compound fragmentation agent is to Pt
75Ir
25Alloy slice carries out fragmentation.Then to the Pt of fragmentation gained
75Ir
25Powder carries out the dissolving of static state (not stirring) aqueous solution chlorination under normal temperature, normal pressure.After chlorinating dissolution stops, residue is all used the tube sealing chlorinating dissolution, analyze its platinum, iridium content, the results are shown in table 4.By table 4 as seen.The chlorinating dissolution rate all 〉=99.99%.
Table 2
| Inventory g | Shape and size mm | Fragmentation temperature ℃ | Soaking time min | Residual volume g |
| 1.000 | Sheet material | 850 | 40 | 0 |
| 1.003 | Thick 0.24～0.34 | ″ | 20 | 0 |
| 1.001 | ″ | 10 | 0 | |
Table 3
| Inventory g | The fragmentation agent | Powder rate of body weight gain % | Powder mean particle sizes μ m |
| 5.001 | Zn | 40.1 | 0.14 |
| 3.002 | Al 50Zn 50 | 2.27 | 0.0061 |
| 3.004 | Al 75Zn 25 | 10.9 | 0.0063 |
| 3.003 | Al 90Zn 10 | 19.9 | 0.0073 |
Claims (3)
1, a kind of fragmentation dissolving methof of precious metal is included in the mixing of materials fusion that contains precious metal for the treatment of fragmentation in 700～1200 ℃ of temperature with base metal fragmentation agent together.Fragmentation, leach the fragmentation material, leached mud (noble metal powder) carried out operations such as aqueous solution chlorination dissolving, it is characterized in that with hydrochloric acid soln:
(ⅰ) used base metal fragmentation agent is a kind of compound fragmentation agent aluminum zn-based alloys, and its composition is (Wt%) Al10～90, Zn10～90;
(ⅱ) material for the treatment of fragmentation during fragmentation is 1: 5～10 with the weight ratio of said compound fragmentation agent.
2, method as claimed in claim 1 is characterized in that also can adding Cu in said compound fragmentation agent, and its composition is (Wt%): Al 10～80, and Zn 10～80, and Cu 10～30.
3, require 1 and 2 method as the power thing, the material for the treatment of fragmentation when it is characterized in that fragmentation is 1: 6～8 with the weight ratio of said compound fragmentation agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90104468A CN1015268B (en) | 1990-06-14 | 1990-06-14 | Fragmentation dissolving methof of noble metal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90104468A CN1015268B (en) | 1990-06-14 | 1990-06-14 | Fragmentation dissolving methof of noble metal |
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| Publication Number | Publication Date |
|---|---|
| CN1048238A true CN1048238A (en) | 1991-01-02 |
| CN1015268B CN1015268B (en) | 1992-01-01 |
Family
ID=4878576
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN90104468A Expired CN1015268B (en) | 1990-06-14 | 1990-06-14 | Fragmentation dissolving methof of noble metal |
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| CN (1) | CN1015268B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1073463C (en) * | 1997-06-14 | 2001-10-24 | 路江鸿 | Quick dissolving method for pure platinum or platinum alloy and use |
| CN102549177A (en) * | 2009-07-01 | 2012-07-04 | 贵金属回收私人有限公司 | Smelting method |
| CN103215454A (en) * | 2013-04-09 | 2013-07-24 | 贵研资源（易门）有限公司 | Rhodium reduction activation dissolution method |
| CN107116230A (en) * | 2017-03-23 | 2017-09-01 | 贵研铂业股份有限公司 | A kind of preparation method of platinum black |
-
1990
- 1990-06-14 CN CN90104468A patent/CN1015268B/en not_active Expired
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1073463C (en) * | 1997-06-14 | 2001-10-24 | 路江鸿 | Quick dissolving method for pure platinum or platinum alloy and use |
| CN102549177A (en) * | 2009-07-01 | 2012-07-04 | 贵金属回收私人有限公司 | Smelting method |
| CN103215454A (en) * | 2013-04-09 | 2013-07-24 | 贵研资源（易门）有限公司 | Rhodium reduction activation dissolution method |
| CN103215454B (en) * | 2013-04-09 | 2014-07-02 | 贵研资源（易门）有限公司 | Rhodium reduction activation dissolution method |
| CN107116230A (en) * | 2017-03-23 | 2017-09-01 | 贵研铂业股份有限公司 | A kind of preparation method of platinum black |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1015268B (en) | 1992-01-01 |
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