CN101575674A - Method for recovering platinum metal from melting trapped material - Google Patents
Method for recovering platinum metal from melting trapped material Download PDFInfo
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- CN101575674A CN101575674A CNA011223391A CN01122339A CN101575674A CN 101575674 A CN101575674 A CN 101575674A CN A011223391 A CNA011223391 A CN A011223391A CN 01122339 A CN01122339 A CN 01122339A CN 101575674 A CN101575674 A CN 101575674A
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- palladium
- rhodium
- trapped material
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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
Abstract
The invention relates to a method for recovering platinum metal from plasma melting trapped material. The method comprises the following steps: firstly, digesting material in concentrated sulphuric acid; secondly, roasting the sulphuric acid digested slag; thirdly, mixing the roasted product with solid hydroxide and performing caustic fusion; fourthly, dissolving the alkaline digested slag in HCL; fifthly, substituting the dissolved solution with active metal such as iron; and sixthly, dissolving the substituted slag through HCL+H2O2 to obtain rich solution of platinum metal. The rich solution of noble metal includes a small amount of copper and zinc and a trace amount of lead, tin and iron, thus recovering the Pt by higher than 99.66 percent, the Pd by higher than 99.7 percent and Rh by higher than 98.1 percent. The method solves the problem that noble metal in plasma melting trapped material is not easy to be transferred into solution and is suitable for treating materials with high silicon content and strong corrosion resistance.
Description
The present invention relates to reclaim the method for platinum metals, especially from melting trapped material, reclaim the method for platinum metals.
Reclaiming the platinum metals with plasma melting from purifying vehicle exhaust spent catalyst and chemical catalyst is the new and high technology that the eighties just occurs mid-term.In August, 1989, press of Beijing University of Technology publishes " application of plasma technique in metallurgy " book of Jerome Fanman chief editor and has done the elaboration of this respect.This technology is to make trapping agent with iron the platinum metals in the catalyzer is enriched in the iron phase, and this device can separate and discharge slag continuously, interval type ground discharging metal." PlatinumMet Bull " 4 phases in 1985 had reported once that U.S. Texasgulf Mineral and Metals Inc. had built up the plasma arc smelting furnace of 3MW in September, 1984, and this equipment can year be produced ton surplus the plasma material 30 that contains 2126.25 kilograms of platinum metals.Present annual tens of tons of plasma body enriched substance that produce of the U.S., platinum group metal number ton, but owing to economical and technical reason, the U.S. also lacks the production technique of effectively handling plasma body enriched substance recovery platinum metals at present.Therefore, originate from several tons of plasma body enriched substance of the U.S., wherein platinum metals content is about 300 kilograms, is at present to be bought by my company to handle, and has from now on to enlarge and buys technical foundation and the economic base of handling.In enrichment in the iron powder of platinum metals, also claim trapping metals or trapped material, the grade of platinum metals can be up to percentum.Although the grade of platinum metals is very high in the trapped material, it is quite difficult technically therefrom to reclaim platinum, palladium, rhodium.Mainly be that this trapped material has very strong erosion resistance, handle (as HCl+Cl with hydrochloric acid oxidizer commonly used
2, HCl+NaClO
3Deng) can not be molten complete, even also very difficult molten intact with the chloroazotic acid processing, and in dissolution process, also produce a considerable amount of silica gel, solid-liquid separation can't be carried out.The article of the J.E.Hoffman that " Metals " 1988 the 6th periodicals carry is pointed out, under the plasma melting temperature, high temperature is above 2000 ℃, if carbon containing in the material, then catalyst matrix---the silicon in the trichroite will be reduced to Pure Silicon Metal, silicon forms alloy with the iron that has captured the platinum metals, and this alloy has extremely strong erosion resistance to acid, make continue after extremely difficult to the processing of platinum metals enriched substance.We find that in the acid treatment insoluble slag of this type of trapped material the platinum metals has formed new alloys such as Fe-PGM and Fe-Si-PGM with iron, silicon.Find also that simultaneously silicone content is high more in the trapped material, erosion resistance is strong more.C.G.Anderson has delivered one piece about extract the treatment process report of platinum metals from trapped material in nineteen ninety-five IPMI meeting.He uses the nitrous acid-sulfuric acid pressure oxidation leaching-out method of Sunshine company invention to handle the trapped material that contains 400 ounces/ton of 1260 ounces/ton of Pt, Pd, 70 ounces/ton of Rh, its main technique step is that trapped material and nitrous acid-sulfuric acid are mixed, under 50～155 ℃ of temperature, pressurization is leached in the autoclave of 90 pounds/in2 of pressure, obtains to contain the enrichment slag of 1375 ounces/ton of 7200 ounces/ton of Pt, Pd, 120 ounces/ton of Rh.Part Pd and Rh have changed leach liquor in the oxidation leaching process, he is reclaimed with suitable technology.The treatment process of Anderson makes the grade of platinum bring up to 22.3% from 3.9%.The weak point of this method is: the platinum metals in the enrichment slag still is contained in the Fe-Si-PGM alloy, and is still very difficult when further handling with ordinary method; The rate of recovery of the platinum of obtaining, palladium, rhodium is all lower, and the reaction conditions of technology is complicated.
The purpose of this invention is to provide a kind of from siliceous height, erosion resistance strong be the method that reclaims platinum, palladium, rhodium the melting trapped material of trapping metals with iron.
Realize the method for platinum, palladium, rhodium in the described recovery melting trapped material of the object of the invention, comprise following process steps successively:
1. with material in 700～1100 ℃ of following roastings 2～6 hours;
2. by identical weight unit than fired slags: solid alkali=1: 2～6, will 1. go on foot the gained fired slags and mix with solid alkali, heated 2～6 hours in 400～800 ℃ times, solid alkali is at least a of NaOH, KOH, BaO;
3. go out 2. to go on foot gained alkali fusion thing with a large amount of water loggings, clarification, solid-liquid separation;
4. use acidic solution HCl or HCl+H
2SO
4Any dissolving 3. go on foot gained water logging slag;
5. with at least a precious metal slag that from 4. go on foot the gained acidic solution, displaces of active metal zinc, magnesium, aluminium, iron;
6. use acidic solution HCl+H
2O
2, HCl+NaClO
3, HCl+Cl
2, HCl+HNO
3Any dissolving 5. go on foot gained precious metal slag, obtain being rich in the rich solution of precious metal, adopt tradition to reclaim technology afterwards and extract wherein platinum, palladium, rhodium.
For realizing the object of the invention better, can carry out step 1. before, in 160～250 ℃ down with vitriol oil digestion melting trapped materials 2～6 hours, dilute with big water gaging subsequently, solid-liquid separation afterwards, the gained solid materials with step 1., 2., 3., 4., 5., 6. subsequent treatment; Vitriol oil consumption in the vitriol oil digestion step can be defined as vitriol oil volume: weight of material=1 liter: 300～600 grams; Can determine that also vitriol oil digestion temperature is 160～220 ℃, the digestion time is 2～4 hours, and vitriol oil digestion consumption is a vitriol oil volume: weight of material=1 liter: 450～550 grams; The maturing temperature of step in 1. can also be defined as 800～1000 ℃, roasting time is defined as 2～4 hours; The correlation parameter of step in 2. can adopt fired slags: solid alkali=1: 3～5, and 450～750 ℃ of Heating temperatures, heat-up time 2～4, solid alkali is NaOH; This external carrying out adds an amount of H in the step process 4.
2O
2, HClO, NaClO
3Any better effects if; Step is 5. middle to adopt pulverous active metal can make reaction more complete rapidly.
The present invention is directed to iron is that the purifying vehicle exhaust spent catalyst melting trapped material of trapping agent--composition iron, nickel, silicon are main in the trapped material, precious metal is based on platinum, palladium, rhodium, by above-mentioned six processing steps, make precious metal grade utmost point low levels from melting trapped material rise to that Pt+Pd+Rh accounts for more than 90% in the replacement slag of platinum metals, the grade of metal platinum is enriched to 64.9% from 5.12%, palladium is enriched to 10.4% from 0.953%, and rhodium is enriched to 9.25% from 0.709%; Impurity only has a little copper zinc and trace lead, tin, iron in the last concentration of precious metal liquid, and the rate of recovery index that reaches is: Pt＞99.66%, Pd＞99.7%, Rh＞98.1%; Used main agents is common soda acid, and reagent consumption is few, and facility investment is low, and is simple to operate, and work atmosphere is good.Product of roasting in the processing method and solid hydroxide mixing alkali fusion, water logging have been discharged most silicon, have destroyed the alloy that platinum metals and iron form, and have solved the extremely difficult difficult problem that changes solution in platinum metals in the iron trapping agent melting trapped material.If make trapped material elder generation and strong sulfuric acid response, then can discharge most of base metal iron, save expensive solid alkali consumption.
The purity of agents useful for same of the present invention is chemical pure or technical pure, and described tradition reclaims technology and is: traditional precipitator method, cationic exchange-chemical reagent reduction method, conventional solvent extraction process.
One of applied trapped material of the present invention gray finely powdered has magnetic diffusivity, can be picked up by magnet.The chemical analysis results of sample quartering is listed in table 1 behind this trapped material mixing.
The chemical analysis results of table 1 material (%)
Embodiment 1
1. get 5000 gram powdery trapped materials and advance the electric furnace roasting, 1000 ℃ of temperature controls, 5 hours reaction times.2. the solid NaOH+BaO of 3 times of product of roasting and weight mixes, contain in the iron crucible, carry out alkali fusion, 700 ℃ of temperature, 4 hours time, cold slightly being transferred in the cardinal principle ponding of coming out of the stove, fully stir with complete dissolve silica, carry out solid-liquid separation, except that the Pt that contains trace, do not contain Pd and Rh in the alkaline waste liquor.3. alkaline leached mud HCl+NaClO
3+ H
2SO
4The dissolving, lysate filters once, 4. uses iron powder+zinc dust precipitation enrichment, in the displacement liquid concentration of Pt, Pd, Rh all＜2ppm.5. replacement slag is with HCl and feed Cl
2Lysate is filtered in dissolving, and noble metal recovery rate is respectively in the gained filtrate: Pt 98.5%, and Pd 98.5%, and Rh 97.0%.This kind concentration of precious metal liquid can separate purification with traditional precipitator method.
Embodiment 2
1. get 8000 gram powdery trapped materials and advance the electric furnace roasting, 700 ℃ of temperature controls, 4 hours reaction times.2. the solid NaOH+KOH of 4 times of product of roasting and weight mixes, contain in the iron crucible, carry out alkali fusion, 600 ℃ of temperature, 3 hours time, cold slightly being transferred in the cardinal principle ponding of coming out of the stove, fully stir with complete dissolve silica, carry out solid-liquid separation, except that the Pt that contains trace, do not contain Pd and Rh in the alkaline waste liquor.3. alkaline leached mud dissolves with HCl+HClO, and lysate filters once, 4. uses iron powder+zinc powder+magnesium powder substitution enrichment, in the displacement liquid concentration of Pt, Pd, Rh all＜2ppm.5. replacement slag HCl+HNO
3Lysate is filtered in the mixed solution dissolving, and noble metal recovery rate is respectively in the gained filtrate: Pt 98.5%, and Pd 98.5%, and Rh 97.0%.This kind concentration of precious metal liquid can be produced platinum, palladium, rhodium ternary hybrid metal with traditional cationic exchange-chemical reagent reduction method.
Embodiment 3
1. get 1.5 liters of the vitriol oils in a little iron pan, add 450 gram trapped materials, constantly stir with little spades, slowly be heated to 160 ℃ of top temperatures from the bottom of a pan with electric furnace, be incubated after 6 hours, dense thick reactant is changed in 10 premium on currency with the iron spoon, and a large amount of ferric sulfate that generated are dissolved, filter the rich and honour scraps of output black.2. the laggard electric furnace of the rich and honour scraps drying of gained sulfuric acid digestion was in 800 ℃ of roastings 2 hours.3. the solid NaOH with 2 times of this product of roasting and weight mixes, contain in the iron crucible, in 500 ℃ of following alkali fusions 2 hours, in the cold slightly transfer entry of coming out of the stove with complete dissolve silica, solid-liquid separation afterwards, iron crucible washes with water.4. the alkaline leached mud of water logging dissolves with HCl, and lysate filters once, 5. uses the precious metal in iron powder+aluminium powder+magnesium powder substitution enrichment solution subsequently.6. twice replaced rich and honour scraps HCl+H
2O
2Lysate is filtered in dissolving, and noble metal recovery rate is respectively in the gained filtrate: Pt 98.8%, Pd98.9%, Rh97.7%.Separate purification gained concentration of precious metal liquid with traditional precipitator method.
Embodiment 4
1. get 1.5 liters of the vitriol oils in a little iron pan, add 700 gram melting trapped materials, constantly stir with little spades, slowly be heated to 220 ℃ of top temperatures from the bottom of a pan with electric furnace, be incubated after 2 hours, dense thick reactant is changed in 10 premium on currency with the iron spoon, a large amount of ferric sulfate of generation are dissolved.Filter the rich and honour scraps of back output black.Detect precious metal concentration (representing) in the spent acid solution by ppm; Pt＜1, Pd＜1, Rh＜7.0, base metal concentration (g/L): Fe 10.65, and Ni 1.05, Cu＜0.0005.2. sulfuric acid digestion slag is dried laggard electric furnace roasting, and 800 ℃ of temperature controls are incubated 4 hours.3. product of roasting mixes with the solid NaOH+BaO of 4 times of weight, contains in the iron crucible, carries out alkali fusion, 600 ℃ of temperature, and 4 hours time, with complete dissolve silica, iron crucible washes with water in the cold slightly transfer entry of coming out of the stove.Alkali solution is colourless substantially, contains Pt:7.8ppm after the solid-liquid separation in the alkaline waste liquor, Pd, Rh＜2ppm, and this step has been discharged 89.3% of total silicon amount.4. alkaline leached mud HCl+NaClO
3Dissolving, lysate filters once, 5. replaces enrichment with iron plate, the concentration of replacing Pt, Pd, Rh in the waste liquid all＜2ppm.6. twice replaced slag HCl+H
2O
2Lysate is filtered in dissolving, and adjusting volume is one liter, and analyzing wherein main components and concentration is (g/L): Pt 35.0, and Pd 6.7, and Rh 4.9, and Cu 6.0, and Zn 1.9.This kind concentration of precious metal liquid can separate purification with the conventional solvent extraction process.Noble metal recovery rate is respectively: Pt 97.7%, Pd～100%, and Rh 98.8%.
Embodiment 5
1. get 2 liters of the vitriol oils in a little iron pan, add 1000 gram trapped materials, constantly stir with little spades, between slowly being heated to 250 ℃ of top temperatures with electric furnace from the bottom of a pan, be incubated after 2 hours, dense thick reactant is changed in 10 premium on currency with the iron spoon, a large amount of ferric sulfate of generation are dissolved.Filter the rich and honour scraps of back output black.Precious metal concentration (representing) in the spent acid solution of discharging by ppm: Pt＜1, Pd＜1, Rh 17.2. sulfuric acid digestion slag is dried laggard electric furnace roasting, and 1100 ℃ of temperature controls are incubated 2 hours.3. product of roasting mixes with the solid BaO of 6 times of weight, contains in the iron crucible, carries out alkali fusion, 800 ℃ of temperature, and 4 hours time, with complete dissolve silica, iron crucible washes with water in the cold slightly transfer entry of coming out of the stove.Alkali solution is colourless substantially, contains Pt:4.0ppm after the solid-liquid separation in the alkaline waste liquor, Pd＜1ppm, and Rh＜2ppm discharges 95.4% of total silicon amount in the raw material.4. alkaline leached mud HCl+H
2SO
4+ NaClO
3Dissolving, lysate filters once, 5. uses the zinc dust precipitation enrichment, the concentration of replacing Pt, Pd, Rh in the waste liquid all＜2ppm.6. twice replaced slag HCl+HNO
3Lysate is filtered in dissolving, and analyzing wherein main components and concentration is (g/L): Pt 51.2, and Pd 9.6, and Rh 7.4.Noble metal recovery rate is respectively: Pt～100%, Pd～100%, Rh～98%.
Embodiment 6
1. get 5000 gram powdery trapped materials and advance the electric furnace roasting, 1000 ℃ of temperature controls, 5 hours reaction times.2. the solid NaOH+BaO of 3 times of product of roasting and weight mixes, contain in the iron crucible, carry out alkali fusion, 700 ℃ of temperature, 4 hours time, cold slightly being transferred in the cardinal principle ponding of coming out of the stove, fully stir with complete dissolve silica, carry out solid-liquid separation, except that the Pt that contains trace, do not contain Pd and Rh in the alkaline waste liquor.3. alkaline leached mud HCl+H
2O
2+ H
2SO
4Dissolving, lysate filters once, 4. replaces enrichment with iron block+spelter, in the displacement liquid concentration of Pt, Pd, Rh all＜2ppm.5. replacement slag is with HCl and feed Cl
2Lysate is filtered in dissolving, and noble metal recovery rate is respectively in the gained filtrate: Pt98.5%, Pd98.5%, Rh97.0%.This kind concentration of precious metal liquid can separate purification with traditional precipitator method or solvent extration.
Embodiment 7
1. get 2 liters of the vitriol oils in a little iron pan, add 1200 gram trapped materials, constantly stir with little spades, slowly be heated to 200 ℃ of top temperatures from the bottom of a pan with electric furnace, be incubated after 5 hours, dense thick reactant is changed in 10 premium on currency with the iron spoon, a large amount of ferric sulfate of generation are dissolved.Filter the rich and honour scraps of back output black.Precious metal concentration (representing) in the spent acid solution of discharging: Pt＜1, Pd＜1, Rh＜7.0, base metal concentration (g/L) by ppm; Fe:10.65, Ni:1.05, Cu＜0.0005.2. sulfuric acid digestion slag is dried laggard electric furnace roasting, and 900 ℃ of temperature controls are incubated 3 hours.3. the solid NaOH+KOH+BaO of 3 times of product of roasting and weight mixes, and contains in the iron crucible, carries out alkali fusion, 750 ℃ of temperature, and 3 hours time, in the cold slightly transfer entry of coming out of the stove, fully stir with complete dissolve silica, iron crucible washes with water.Alkali solution is colourless substantially, contains Pt:7.8ppm after the solid-liquid separation in the alkaline waste liquor, Pd, Rh＜2ppm, and this step is discharged 89.5% of total silicon amount.4. alkaline leached mud dissolves with HCl+HClO, and lysate filters once, 5. uses aluminium powder+zinc dust precipitation enrichment, in the waste liquid of displacement back the concentration of Pt, Pd, Rh all＜2ppm.6. twice replaced slag HCl+NaClO
3Dissolving, the main components and concentration that filters in the lysate of back is (g/L): Pt:35.0, Pd:6.7, Rh:4.9, Cu:6.0, Zn:1.9.This kind concentration of precious metal liquid can adopt the conventional solvent extraction process to separate purification.Noble metal recovery rate is respectively: Pt 97.7%, Pd～100%, and Rh 98.8%.
Claims (9)
1. method that reclaims platinum, palladium, rhodium from melting trapped material comprises following process steps successively:
1. with material in 700～1100 ℃ of following roastings 2～6 hours;
2. by same units weight ratio fired slags: solid alkali=1: 2～6, will 1. go on foot the gained fired slags and mix with solid alkali, heated 2～6 hours down in 400～800 ℃, solid alkali is at least a of NaOH, KOH, BaO;
3. go out 2. to go on foot gained alkali fusion thing with a large amount of water loggings, clarification, solid-liquid separation:
4. use acidic solution HCl or HCl+H
2SO
4Any dissolving 3. go on foot gained water logging slag:
5. with at least a precious metal slag that from 4. go on foot the gained acidic solution, displaces of active metal zinc, magnesium, aluminium, iron;
6. use acidic solution HCl+H
2O
2, HCl+NaClO
3, HCl+Cl
2, HCl+HNO
3Any dissolving 5. go on foot gained precious metal slag, obtain being rich in the rich solution of precious metal, adopt tradition to reclaim technology afterwards and extract wherein platinum, palladium, rhodium.
2. the method that from melting trapped material, reclaims platinum, palladium, rhodium according to claim 1, it is characterized in that carry out described step 1. before, use vitriol oil digestion melting trapped material 2～6 hours down in 160～250 ℃, subsequently with big water gaging dilution, solid-liquid separation afterwards, the gained solid materials with described step 1., 2., 3., 4., 5., 6. subsequent treatment.
3. the method that reclaims platinum, palladium, rhodium from melting trapped material according to claim 2 is characterized in that the vitriol oil consumption in the described vitriol oil digestion step is a vitriol oil volume: weight of material=1 liter: 300～600 grams.
4. the method that from melting trapped material, reclaims platinum, palladium, rhodium according to claim 3, it is characterized in that described vitriol oil digestion temperature is 160～220 ℃, the digestion time is 2～4 hours, and vitriol oil digestion consumption is a vitriol oil volume: weight of material=1 liter: 450～550 grams.
5. the method that reclaims platinum, palladium, rhodium from melting trapped material according to claim 1 is characterized in that the 1. described maturing temperature of step is 800～1000 ℃, and roasting time is 2～4 hours.
6. the method that from melting trapped material, reclaims platinum, palladium, rhodium according to claim 1, it is characterized in that the 2. described fired slags of step: solid alkali=1: 3～5, Heating temperature are 450～750 ℃, 2～4 hours heat-up times, solid alkali is NaOH.
7. the method that reclaims platinum, palladium, rhodium from melting trapped material according to claim 1 is characterized in that in carrying out step process 4., adds H
2O
2, HClO, NaClO
3Any.
8. the method that reclaims platinum, palladium, rhodium from melting trapped material according to claim 1 is characterized in that the 5. described metathetical active metal that is used for of step is a powder.
9. the method that from melting trapped material, reclaims platinum, palladium, rhodium according to claim 1, it is characterized in that carry out described step 1. before, use vitriol oil digestion melting trapped material 2～4 hours down in 160～220 ℃, vitriol oil digestion consumption is the vitriol oil: material=1 liter: 450～550 grams, subsequently with big water gaging dilution, solid-liquid separation afterwards, the gained solid materials with described step 1., 2., 3., 4., 5., 6. subsequent treatment, described step 1. maturing temperature is 800～1000 ℃, roasting time is 2～4 hours, described step is fired slags 2.: solid alkali=1: 3～5, Heating temperature is 450～750 ℃, and 2～4 hours heat-up times, solid alkali is NaOH, carry out described step 4. the time, adding H
2O
2, HClO, NaClO
3Any, 5. described step is used for the metathetical active metal is powder or block.
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| CN102212699A (en) * | 2011-05-23 | 2011-10-12 | 重庆国际复合材料有限公司 | Method for recovering noble metal |
| CN102247841A (en) * | 2010-07-29 | 2011-11-23 | 张超 | Method for recovering catalyst rhodium from industrial waste liquid of carbonyl synthesis of acetic anhydride |
| CN102796878A (en) * | 2012-08-27 | 2012-11-28 | 昆明贵金属研究所 | Method for enriching rhodium from rhodium-containing organic waste liquid |
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| CN104073625A (en) * | 2014-07-14 | 2014-10-01 | 贵研资源（易门）有限公司 | Pretreatment method before enriching and recycling precious of metal in plasma smelting |
| CN105441680A (en) * | 2015-11-18 | 2016-03-30 | 金川集团股份有限公司 | Method for selectively separating precious metal |
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| CN107312931A (en) * | 2017-05-22 | 2017-11-03 | 昆明理工大学 | It is a kind of at the same reclaim noble metal and prepare HIGH-PURITY SILICON method |
| CN107312931B (en) * | 2017-05-22 | 2018-11-27 | 昆明理工大学 | Method that is a kind of while recycling noble metal and prepare HIGH-PURITY SILICON |
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