CN106282568A - A kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier - Google Patents
A kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier Download PDFInfo
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- CN106282568A CN106282568A CN201510285196.8A CN201510285196A CN106282568A CN 106282568 A CN106282568 A CN 106282568A CN 201510285196 A CN201510285196 A CN 201510285196A CN 106282568 A CN106282568 A CN 106282568A
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Abstract
The invention discloses a kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier.This technique is that inefficacy metallic carrier auto-exhaust catalyst is added directly into high-temperature melting furnace fusing, it is poured on water cooler quickly cooling or atomization is dusted, the former makes platinum group metal alloy be formed to enbrittle and be easy to be broken into the alloy that granule is tiny, and the latter forms tiny platinum group metal alloy；Obtain the tiny and golden acid adding Selectively leaching base metal of platinum group metal, through filtering and washing, it is thus achieved that platinum group metal concentrate, it is achieved platinum group metal efficiently concentrating.The method is when high melt, technology carrier itself is as platinum group metal trapping agent, need not add any trapping agent, after fusing, platinum group metal enters in alloy melt, and follow-up cooling or atomization are dusted, and the alloy forming granule tiny is easy to Selectively leaching base metal, therefore whole process is simple to operate, platinum yield height, concentration ratio height, environmental protection, low cost, industrial applications prospect is good.
Description
Technical field
The invention belongs to rare precious metal field of metallurgy, relate to a kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier.
Background technology
Spent automotive exhaust catalysts carrier has cordierite and metallic carrier etc., at present, as follows from the method for the enrichment of spent automotive exhaust catalysts carrier or extraction platinum group metal:
Peace peak et al. invention is a kind of siderophore spent automotive exhaust catalysts platinum group metal recovery method (application publication number: CN104294048A), it is characterised in that step: 1) spent catalyst is crushed, collect powder granule；2) powder granule is put into ultrasonic washing unit with fragment and is separated；By iron plate surface clean, the liquid after cleaning merges filtration with the liquid inside ultrasonic washing unit；3) by filter residue and drying, roasting, solid takes out；4) pulverize；5) powder body adds reactor, makes a gesture of measuring addition hydrochloric acid according to the weight of solid-to-liquid ratio 1:1-5, heating, being passed through chlorine under liquid level, reaction is filtered, with the deionized water filter wash cake of 0.5-5 times of solid weight after terminating, platinum group metal leach reaction temperature at 40-90 DEG C, response time 2-10h；Obtain leachate；6) leachate uses extract and separate Pd, Pt, Rh successively；Pd extractant is the one in isoamyl sulfide, DOSO, 2-hydroxyl-5-octyl group diphenyl-ketoxime, and Pt extractant is trialkylamine, and Rh extractant is tributyl phosphate.
Congratulating pulk et al. and disclose a kind of method (application publication number: CN104073641A) reclaiming noble metal from spent auto-catalysts, step is as follows: (1) material early stage processes；(2) dispensing, batch mixing, is mixed in proportion the material processed in step (1), and inefficacy cordierite is automobile catalyst 75-85 part of carrier, magnetic iron ore 2-4 part, smelter coke 1-3 part, Calx 10-13 part, fluorite ore 1-3 part；(3) use plasma heating furnace that gained material is processed.1. in plasma heating furnace, it is passed through the argon that purity is 99.99%, in making stove, keeps tiny structure power；2. when plasma in-furnace temperature is in the range of 1500-1600 DEG C, start to be fed in plasma heating furnace step (2) gained material；3., after melting 3-6 hour, slag phase floss hole starts slagging；4., after step (2) gained material adds, after 1600-1650 DEG C is incubated 30 minutes, opens metal phase floss hole, obtain the alloy rich in noble metal.Using this method, platinum, palladium, rhodium total recovery is more than 98%, and wherein the response rate of platinum is more than 98%；Palladium recovery rate is more than 98%；The response rate of rhodium is more than 97%.
Dong Haigang et al. has invented a kind of method (application publication number: CN104178634A) of high-efficiency cleaning recovery platinum group metal from spent auto-catalysts, its step includes that (1) is melting trapped: carry out high melt with trapping agent, reducing agent, slag former after spent automotive exhaust catalysts being mixed, it is thus achieved that trapping metal-platinum-group metal alloy；(2) alloy phase oxidation blowing: trapping metal-platinum-group metal alloy blows by blasting oxidizing gas；(3) high-grade platinum group metal enriched substance separated and dissolved: by the dissolving of oxidisability solvent, ionic energy transfer, it is thus achieved that platinum group metal solution, exchange tail washings adds alkali neutralization precipitation, and precipitate returns as melting operation trapping agent；(4) Refining of Platinum Metals: platinum group metal solution obtains platinum group metal product by Refining.Present invention achieves the high efficiente callback of platinum group metal, the platinum group metal response rate is more than 99%, and in smelting slag, platinum+palladium+rhodium content is less than 10g/t, and trapping agent recycles, cleanliness without any pollution, it is easy to industrializing implementation.
The good melting enrichment-wet separation technique that describes in dry side extracts the method (patent of invention number: 201210060308.6) of noble metal from spent auto-catalysts, relates to a kind of method extracting platinum group metal from automobile catalyst.Step of the present invention includes: after catalyst is mixed homogeneously with adjuvants such as flux through fusion process concentration of precious metal alloy mutually in；Through acid flux material Selectively leaching separation base metal and obtain noble metal concentrate after alloy phase efflorescence；Noble metal concentrate is carried out refine output noble metal products.The present invention has obvious advantage compared with single wet treatment flow process: unit product reagent consumption and pollutant are greatly decreased, and the noble metal response rate is greatly improved, shortens flow process, cost reduction, and economy and obvious environment benefit improve.
Li Yong et al. invents a kind of method (CN103334010A) of melting enriching noble metals from spent automotive exhaust catalysts.The method uses copper-sulphide ores to be trapping agent, and main flow is: (1) abrasive material: spent automotive exhaust catalysts is ground and obtains the powder that granularity is 30 ~ 200 mesh；(2) batch mixing: ground material is uniformly mixed with trapping agent, flux and other adjuvant；(3) melting: the material of mix homogeneously is loaded in graphite crucible, carries out melting in high-temperature electric resistance furnace；(4) it is separated: biphase after melting is separated, obtains being enriched the noble metal copper matte regulus phase of more than 98.5% and the slag phase of noble metal ＜ 3 g/t.The method using the present invention can effectively shorten operating process, reduces production cost, and to more environment-friendly.
Bi Xiangguang et al. discloses the dissolving method (application publication number: CN103526033A) of platinum group metal in a kind of automobile spent catalyst enriched substance.More particularly it relates to the dissolving method of platinum group metal in a kind of automobile spent catalyst enriched substance.The step of the present invention includes: automobile spent catalyst being enriched with the platinum group metal enrichment thing obtained, after pretreatment, adds oxidant and make abundant, the quick dissolving in platinum group metal proceed in solution in hydrochloric acid medium, insoluble matter is reprocessed after filtering.The method has platinum group metal response rate height, flow process is short, environmental protection pressure is little, low cost and other advantages.
Bi Xiangguang et al. discloses the method (application publication number: CN103526034A) reclaiming platinum group metal from automobile spent catalyst.More specifically, platinum group metal wet-process activation leaching method in a kind of automobile spent catalyst is related to.The present invention, by adding the platinum group metal in oxidant Strengthen education automobile spent catalyst after wet-process activation pretreatment, makes the leaching rate of platinum group metal particularly rhodium increase substantially, and the method is safe and reliable, metal recovery rate is high, production cost is relatively low.
Fan Xingxiang describes for dead catalyst in " rare metal " the 2nd phase in 2014, using ferrum as supplementary set agent, it is proposed that the noble metal that the process route of low-temperature reduction-mill choosing-acidleach is enriched with in dead catalyst.Primary study residue and trapping agent proportioning, reduction temperature, recovery time, additive formula, reducing agent proportioning, the mog impact on index.By experiment, it is determined that optimal processing parameter: residue and trapping agent proportioning are 1.0: 1.5, and reduction temperature is 1220 DEG C, and the recovery time is 6 h, and additive formula is the 10% of trapping agent weight ratio, and coal dust proportioning is the 9% of trapping agent weight ratio, Ball-milling Time 45 min.Use scanning electron microscope (SEM) and X-ray diffraction material phase analysis (XRD) that reduzate is analyzed, result shows, in reduction process, add additive to promote ferrum crystal grain agglomeration and can effectively trap platinum group metal, ferrum grain size range is 50 ~ 150 μm after carrying out reduction, and physics patchiness is presented mutually with slag, follow-up mill choosing separates.Selected by mill, obtain platinum group metal reduced iron powder, use X-ray diffraction material phase analysis (XRD) that iron powder is analyzed, analyze and show that its thing is mainly metallic iron mutually, achieve metallic iron to separate with stone-like pulse, lay the foundation for follow-up acid molten enrichment platinum group metal.Under the process conditions determined, obtain platinum group metal enriched substance, wherein: Pt 47495.3 g/t；Pd 12756.8 g/t；Rh 23145.5 g/t, molten to acid from raw material, platinum, palladium, rhodium concentration ratio is respectively 551.30, and 512.73,545.90, the response rate is respectively 98.16%, and 91.22%, 97.35%.By experiment, metallic iron can the effective platinum group metal in enriched catalytic agent, this technique have be simple to operate and friendly to environment, high accumulation rate and the advantage such as practical, can be the offer reference of platinum group metal secondary resource beneficiation technologies.
Wu Guoyuan describes from wet method, pyrogenic process and gas phase three angles of volatilization in " rare metal " the 3rd phase in 2002, review the enrichment method of noble metal in noble metal catalyst, and describe sub sulphide method of using, the method for volatile carrier material aluminium sesquioxide enriching noble metals.
A kind of method (application publication number: CN103649348A) using non-ferrous metal waste residue to be enriched with and reclaim noble metal from discarded mobile phone printed circuit board (PCB) and discarded automobile catalyst has been invented in the bright Zhu of Korea S's gold, and described non-ferrous metal waste residue is the industrial waste of discharge from the technical process of refining non-ferrous metals such as copper, lead and zinc etc..More specifically, the present invention relates at high temperature be included in ferrum oxide in non-ferrous metal waste residue by melted to non-ferrous metal waste residue, discarded mobile phone PCB and discarded automobile catalyst with reduction and separation by single process, and separate copper, ferrum, stannum and nickel contained in discarded mobile phone PCB by melted simultaneously, to use the alloy metal collector as noble metal of the ferrum, copper, stannum and the nickel that are generated, and from being included in the method being enriched with and reclaiming Au Ag Pt Pd and rhodium etc. discarded mobile phone PCB and discarded automobile catalyst.The method that the present invention uses non-ferrous metal waste residue to be enriched with and reclaim noble metal from discarded mobile phone PCB and discarded automobile catalyst comprises the following steps: mixing and melt non-ferrous metal waste residue and solvent, it controls thing for residue compositions；Discarded mobile phone PCB and discarded automobile catalyst are incorporated in obtained motlten metal, then melt；With motlten metal is kept the predetermined time to be classified as the alloy phase of concentration of precious metal and without the slag phase of noble metal.
Congratulate pulk et al. and invent a kind of method (application for a patent for invention number: 201310104285.9) being enriched with platinum group metal from alumina base dead catalyst.It is an object of the invention to overcome the deficiency of above-mentioned prior art, thering is provided a kind of method being enriched with platinum group metal from alumina base dead catalyst, the method adaptation material scope is wide, dissolving carrier effect is good, platinum group metal enrichment times high, be enriched with content height in platinum group metal in slag, height is reclaimed in platinum group metal, equipment corrosion is low.A kind of method being enriched with platinum group metal from alumina base dead catalyst, comprises the following steps: A, once burn；B, pulverizing；C, pressurization alkali are molten；D, filtration；E, secondary burning.It is wide that the present invention adapts to material scope；Dissolution ratio of aluminum oxide is more than 95%；Platinum group metal is enriched with 80～120 times, and concentration effect is good；In slag in the range of platinum group metal content 10～40%, beneficially postorder Refining of Platinum Metals；In process of enriching, the response rate of platinum group metal is more than 99%；Equipment corrosion is low.
Hillside plot is ploughed department et al. and is disclosed a kind of method (patent of invention number: 200710153756.X) reclaiming platinum family element, including by pending platinum group elemental substance and the copper source material containing copper oxide, load together with flux component and reducing agent in closed electric furnace, be allowed to melt；The mainly motlten metal of metallic copper is deposited in below the molten slag layer of mainly oxide；;Enrichment is deposited in the platinum family element in following motlten metal, it is characterized in that, from electric furnace, discharge copper content be reduced to the molten slag of 3.0 weight % or lower, and loading the copper source material in electric furnace is that particle diameter is not less than 0.1MM and the graininess copper source material less than 10MM.
To sum up, spent automotive exhaust catalysts metallic carrier uses high temperature melting, it is poured on water cooler quickly cooling or atomization is dusted, the former makes platinum group metal alloy be formed to enbrittle and be easy to be broken into the alloy that granule is tiny, the latter forms tiny platinum group metal alloy, acid adding Selectively leaching, it is achieved platinum group metal efficiently concentrating.At inspection information, the method shows that there is not been reported.
Summary of the invention
For problem above, it is an object of the invention to provide a kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier, the method: fusing, water-cooled or atomization are dusted, acid adding Selectively leaching enrichment platinum group metal.This method flow process is simple, platinum yield height, concentration ratio height, environmental protection, low cost, industrialization prospect is good.
The technical solution used in the present invention is: a kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier, a kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier, it is characterised in that sequentially include the following steps: (1) and inefficacy metallic carrier auto-exhaust catalyst is added directly into high-temperature melting furnace fusing；(2) being poured on water cooler quickly cooling or atomization is dusted, the former makes platinum group metal alloy be formed to enbrittle and be easy to be broken into the alloy that granule is tiny, and the latter forms tiny platinum group metal alloy；(3) the tiny and golden acid adding Selectively leaching base metal of platinum group metal is obtained, through filtering and washing, it is thus achieved that platinum group metal concentrate, it is achieved platinum group metal efficiently concentrating.From raw material to platinum group metal concentrate, platinum group metal yield is more than 98.50%, and concentration ratio is more than 20 times.The method is when high melt, and technology carrier itself is as platinum group metal trapping agent, and after fusing, platinum group metal enters in alloy melt, and follow-up cooling or atomization are dusted, and the alloy forming granule tiny is easy to Selectively leaching base metal.
Inefficacy metallic carrier auto-exhaust catalyst is added directly into high-temperature melting furnace fusing by step (1), and wherein high-temperature melting furnace is plasma heating furnace, intermediate frequency furnace, coreless induction furnace etc., and fusion temperature is at 1300 ~ 1650 DEG C, and the time is at 0.5-4.0h.Step (2) is poured on water cooler quickly cooling or atomization is dusted, the former makes platinum group metal alloy be formed to enbrittle and be easy to be broken into the alloy that granule is tiny, the latter forms tiny platinum group metal alloy, wherein water cooler is metal cabinet, logical cooling water cools down, and atomization is dusted and poured the atomization of nebulizer back warp gases at high pressure into for melt.Step (3) obtains the tiny and golden acid adding Selectively leaching base metal of platinum group metal, through filtering and washing, obtain platinum group metal concentrate, realize platinum group metal efficiently concentrating, wherein acid is sulphuric acid, hydrochloric acid, nitric acid etc., consumption is the 10-70% of alloy sulfonium phase weight ratio, temperature is 30-95 DEG C, and the time is 1-5h, and liquid-solid ratio is 3:1 ~ 5:1.
Advantages of the present invention essentially consists in:
(1) when high melt, technology carrier itself is as platinum group metal trapping agent, and high melt realizes platinum group metal and efficiently traps；
(2) after fusing, platinum group metal enters in alloy melt, and follow-up cooling or atomization are dusted, and the alloy that formation granule is tiny is easy to Selectively leaching base metal and is realized platinum group metal efficiently concentrating；
(3) this method is simple to operate, platinum yield height, concentration ratio height, environmental protection, low cost, industrialization prospect is good.
Accompanying drawing explanation
Fig. 1 is the process chart of a kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with instantiation, the present invention is described in further detail:
Embodiment 1
See accompanying drawing 1, condition: inefficacy metallic carrier auto-exhaust catalyst 1000g, use plasma heating furnace melting, dust through atomization, form tiny platinum group metal dust；Using sulfuric acid leaching base metal, consumption is the 60% of alloy sulfonium phase weight ratio, temperature is 55 DEG C, and the time is 4h, and liquid-solid ratio is 5:1, and platinum group metal enrichment reaches 25 times, and yield is 98.67%.
Embodiment 2
See accompanying drawing 1, condition: inefficacy metallic carrier auto-exhaust catalyst 3000g, use high-frequency melting furnace, water cooled after, broken, form tiny platinum group metal dust；Using sulfuric acid leaching base metal, consumption is the 80% of alloy sulfonium phase weight ratio, temperature is 85 DEG C, and the time is 4h, and liquid-solid ratio is 5:1, and platinum group metal enrichment reaches 30 times, and yield is 99.10%.
Embodiment 3
See accompanying drawing 1, condition: inefficacy metallic carrier auto-exhaust catalyst 5000g, use high-frequency melting furnace, dust through atomization, form tiny platinum group metal dust；Using salt Ore Leaching, consumption is the 50% of alloy sulfonium phase weight ratio, temperature is 65 DEG C, and the time is 5h, and liquid-solid ratio is 3:1, and platinum group metal enrichment reaches 24 times, and yield is 98.67%.
Embodiment 4
See accompanying drawing 1, condition: inefficacy metallic carrier auto-exhaust catalyst 8000g, use high-frequency melting furnace, water cooled after, broken, form tiny platinum group metal dust；Using sulphuric acid, consumption is the 60% of alloy sulfonium phase weight ratio, temperature is 55 DEG C, and the time is 4h, and liquid-solid ratio is 5:1, and platinum group metal enrichment reaches 28 times, and yield is 98.43%.
Embodiment 5
See accompanying drawing 1, condition: inefficacy metallic carrier auto-exhaust catalyst 4000g, use plasma heating furnace melting, dust through atomization, form tiny platinum group metal dust；Using nitric acid to leach base metal, consumption is the 90% of alloy sulfonium phase weight ratio, temperature is 95 DEG C, and the time is 4h, and liquid-solid ratio is 5:1, and platinum group metal enrichment reaches 30 times, and yield is 98.81%.
Claims (4)
1. the method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier, it is characterised in that sequentially include the following steps: (1) and inefficacy metallic carrier auto-exhaust catalyst is added directly into high-temperature melting furnace fusing；(2) being poured on water cooler quickly cooling or atomization is dusted, the former makes platinum group metal alloy be formed to enbrittle and be easy to be broken into the alloy that granule is tiny, and the latter forms tiny platinum group metal alloy；(3) obtaining the tiny and golden acid adding Selectively leaching base metal of platinum group metal, through filtering and washing, it is thus achieved that platinum group metal concentrate, it is achieved platinum group metal efficiently concentrating, from raw material to platinum group metal concentrate, platinum group metal yield is more than 98.50%, and concentration ratio is more than 20 times.
A kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier the most according to claim 1, it is characterized in that inefficacy metallic carrier auto-exhaust catalyst is added directly into high-temperature melting furnace fusing by step (1), wherein high-temperature melting furnace is plasma heating furnace, intermediate frequency furnace, coreless induction furnace etc., fusion temperature is at 1300 ~ 1650 DEG C, and the time is at 0.5-4.0h.
A kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier the most according to claim 1, it is characterized in that step (2) is poured on water cooler quickly cooling or atomization is dusted, the former makes platinum group metal alloy be formed to enbrittle and be easy to be broken into the alloy that granule is tiny, the latter forms tiny platinum group metal alloy, wherein water cooler is metal cabinet, logical cooling water cools down, and atomization is dusted and poured the atomization of nebulizer back warp gases at high pressure into for melt.
A kind of method being enriched with platinum group metal from spent automotive exhaust catalysts metallic carrier the most according to claim 1, it is characterized in that step obtains the tiny and golden acid adding Selectively leaching base metal of platinum group metal, through filtering and washing, obtain platinum group metal concentrate, realizing platinum group metal efficiently concentrating, wherein acid is sulphuric acid, hydrochloric acid, nitric acid etc., and consumption is the 10-70% of alloy sulfonium phase weight ratio, temperature is 30-95 DEG C, time is 1-5h, and liquid-solid ratio is 3:1 ~ 5:1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110184467A (en) * | 2019-07-02 | 2019-08-30 | 上海贺利氏工业技术材料有限公司 | A kind of processing method of automobile exhaust purifier |
| CN110735042A (en) * | 2019-11-08 | 2020-01-31 | 北京科技大学 | Crushing method of Fe-PGMs (Fe-PGMs) alloy |
| CN110983028A (en) * | 2019-11-21 | 2020-04-10 | 云龙县铂翠贵金属科技有限公司 | Method for recovering platinum group metal from automobile exhaust purification waste catalyst |
| CN113403484A (en) * | 2021-05-31 | 2021-09-17 | 苏州市富荣环保科技有限公司 | Method for dissolving and purifying precious metal from electronic waste |
| CN113564364A (en) * | 2021-07-30 | 2021-10-29 | 安徽元琛环保科技股份有限公司 | Method for recovering valuable metal from retired automobile three-way catalyst |
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| CN101509077A (en) * | 2009-02-19 | 2009-08-19 | 昆明贵金属研究所 | Method for extracting platinum, palladium, rhodium from automotive catalyst of ore phase reconstruction |
| 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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| CN101509077A (en) * | 2009-02-19 | 2009-08-19 | 昆明贵金属研究所 | Method for extracting platinum, palladium, rhodium from automotive catalyst of ore phase reconstruction |
| 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110184467A (en) * | 2019-07-02 | 2019-08-30 | 上海贺利氏工业技术材料有限公司 | A kind of processing method of automobile exhaust purifier |
| CN110735042A (en) * | 2019-11-08 | 2020-01-31 | 北京科技大学 | Crushing method of Fe-PGMs (Fe-PGMs) alloy |
| CN110983028A (en) * | 2019-11-21 | 2020-04-10 | 云龙县铂翠贵金属科技有限公司 | Method for recovering platinum group metal from automobile exhaust purification waste catalyst |
| CN113403484A (en) * | 2021-05-31 | 2021-09-17 | 苏州市富荣环保科技有限公司 | Method for dissolving and purifying precious metal from electronic waste |
| CN113564364A (en) * | 2021-07-30 | 2021-10-29 | 安徽元琛环保科技股份有限公司 | Method for recovering valuable metal from retired automobile three-way catalyst |
| CN113564364B (en) * | 2021-07-30 | 2022-12-16 | 安徽元琛环保科技股份有限公司 | Method for recovering valuable metal from retired automobile three-way catalyst |
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