CN102251098B - Method for extracting rare noble metals - Google Patents
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Abstract
The invention relates to a method for extracting rare noble metals, which comprises the following steps: mixing the raw material containing rare noble metals with metal chloride; treating the mixture with a chlorine/carbon monoxide gas mixture at about 450-800 DEG C; cooling the mixture, and extracting with hydrochloric acid; and filtering and washing. The method has the advantages of high extraction rate, good reproducibility and low time consumption, can be used for basically recycling rare noble metals in the raw material, and can also be used for accurate quantitative analysis on the metals in the raw material. The method provided by the invention is especially used for treating waste automobile catalysts.
Description
Technical field
The present invention relates to extract the method for rare precious metal, relate more specifically to extract for example platinum metals, rare earth metal lanthanum cerium and the rare metal method of vanadium gallium for example for example of precious metal, especially extract the method for platinum metals and Rare Earth Lanthanum cerium in the junked-auto catalyzer.
Background technology
Rare precious metal comprises this three class of precious metal, rare earth metal and rare metal.Wherein precious metal has 8 kinds, and they are gold and silver, platinum, ruthenium, palladium, rhodium, iridium, osmium, and wherein platinum, ruthenium, palladium, rhodium, iridium, osmium are called again the platinum metals.Rare earth metal has 17 kinds, and they are lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium.Rare metal has 17 kinds, and content is rare in the earth's crust, extracts difficulty larger, and they are lithium, beryllium, titanium, rubidium, caesium, tungsten, molybdenum, vanadium, rhenium, tantalum, niobium, zirconium, hafnium, gallium, indium, thallium, germanium.
There is a serious shortage in the supply for China's platinum metals natural mineral resource reserves, and the Platinum metals resources reserves of finding out in 2008 are 324.13 tons, account for 0.46% of world's total reserves.China's platinum metals year output is approximately 200 kilograms at present, can not satisfy the needs of national defence and industry far away, 90% above dependence on import of annual requirement.Therefore, how from raw material such as natural mineral matter, waste material etc., to extract efficiently precious metal very important economic and social benefit is arranged.
In recent years, along with the high speed development of Domestic Automotive Industry, formed a large amount of inefficacy cleaning catalyst for tail gases of automobiles (abbreviation automobile catalyst), wherein very large some is external manufacturer production, and raw material sources are in abroad.Platinum metals simple substance content summation is 0.1-0.3wt.% in external most automobile catalysts of producing; The rare earth oxide content summation is generally 5.0wt.%, and this two metalloid all is important strategic goods and materials in the world.Pt content is generally 300-1000ppm in the automobile catalyst, and Pd content is 200-800ppm, and Rh content is 50-100ppm.At present China produced about 500 tons spent auto-catalysts in 1 year, approximately 600 kilograms of platiniferous, palladium, rhodiums, expect 2014 after, the spent auto-catalysts of generation will reach 5000 tons, platiniferous, palladium, rhodium are above 6 tons.Whole world 85%Rh, 50%Pd, 43%Pt in 2004 are used for the manufacturing of cleaning catalyst for tail gases of automobiles.The abandoned car catalyzer is primary platinum metals secondary resources in many countries at present.
In addition, in the industrial production such as petrochemical complex, also can produce inefficacy rare precious metal catalyzer, also have the problem that how to reclaim rare precious metal wherein.
Overwhelming majority automobile catalyst carrier is to be made by the stupalith of good thermal shock, such as trichroite or aluminium sesquioxide, wherein trichroite is the most frequently used stupalith, and the platinum metals platinum rhodium palladium and the catalyst aid Rare Earth Lanthanum cerium that play katalysis just load on such carrier.Platinum metals platinum rhodium palladium exists with metal simple-substance or metal oxide form in the abandoned car catalyzer, and the Rare Earth Lanthanum cerium exists with oxide form.The so-called extraction transferred to these elements in the catalyzer in the solution from solid exactly.In addition, platinum metals platinum rhodium palladium content is low in the abandoned car catalyzer, and (XRF) can not all record with XRF; Rare Earth Lanthanum cerium XRF analysis result is semiquantitative.Except XRF, the at present quantitative analysis of these elements all is by extracting and this two step of concentration analysis.The platinum metals that automobile catalyst is contained and rare earth metal Quantitative Study are difficult point and and the focuses of research always.Therefore, efficiently, almost from raw material, extract up hill and dale precious metal and rare earth metal and not only can almost reclaim up hill and dale precious metal and rare earth metal, and the content of precious metal and rare earth metal lays the first stone in the raw material in order to analyze exactly.
Routinely, with chloroazotic acid high temperature (95 ℃) wet processing automobile catalyst, the extraction yield of platinum and rhodium is respectively less than 60% and 45%.Main fiery ensaying and molten these two kinds of methods of acid of adopting are extracted in the platinum metals at present.
Fire assaying is alloy phase and the slag phase that generates the platinum group metal after automobile catalyst is mixed with reductive agent, fusing assistant in high-temperature fusion more than 1000 ℃.Isolate alloy phase, with acid dissolving alloy phase the platinum metals is transferred in the acid solution.But fire assaying is not high to rhodium extraction yield in the automobile catalyst, generally is lower than 90%.The second, this method step is many, length consuming time (generally taking 4 days).The 3rd, fire assaying needs experience to come per sample regulation experiment condition, poor reproducibility.
Acid pasting mainly is to adopt the molten sample technology of sealing pressing, carries out in polytetrafluoroethylcontainer container.But this method sampling amount only has about 0.1 gram, and sample representation is low, easily causes large error.The second, metal rhodium is difficult to dissolving in the catalyzer in acid, causes the rhodium extraction yield low, and analytical error is large.The 3rd, usually because the polytetrafluoroethylcontainer container poor sealing causes the sample high pressure steam to leak, thereby cause analytical error.
A kind of extraction yield is high in order to seek, favorable reproducibility, few rare precious metal extracting method of time spent, the spy proposes a kind of chlorination extracting method in the present invention, this method can not only the high efficiency extraction raw material for example platinum metals platinum rhodium palladium and rare metal of the precious metal in the spent auto-catalysts for example, and rare earth metal wherein for example the lanthanum cerium also can be simultaneously by high efficiency extraction, thereby reach the purpose of extracting simultaneously multiple rare precious metal.The method also for quantitative analysis raw material exactly for example in the spent auto-catalysts content of rare precious metal provide the foundation.
Summary of the invention
The extraction raw material that the present invention proposes that a kind of extraction yield is high, favorable reproducibility, time spent is few is rare precious metal platinum metals platinum rhodium palladium and/or the rare earth metal method of lanthanum cerium for example for example in the spent auto-catalysts for example.The method can be used for the efficient recovery rare precious metal, and is used for the preprocessing process before the quantitative analysis raw material rare precious metal.
The principle of the inventive method be with raw material for example in the automobile catalyst precious metal for example the metal simple-substance of platinum metals platinum rhodium palladium or oxide compound and rare earth metal for example the oxide compound of lanthanum cerium be transformed into complex chlorides or the single muriate of metal by the chlorination of middle temperature pyrogenic process, these muriates are dissolved in the hydrochloric acid soln, so just they are all transferred in the solution by solid, then reclaim or be used for analyzing.
Particularly, rare precious metal precious metal platinum metals platinum rhodium palladium and/or the rare earth metal method of lanthanum cerium for example for example in the automobile catalyst for example in the extraction raw material that the invention provides that a kind of extraction yield is high, favorable reproducibility, time spent is few, it may further comprise the steps:
With raw material for example automobile catalyst mix with metal chloride;
2. under about 450-850 ℃ temperature, use the mixture gas treatment mixture of chlorine and carbon monoxide;
3. will use hydrochloric acid leaching after the mixture cooling; With
4. filtration washing;
Extract thus rare precious metal contained in the raw material for example platinum rhodium palladium and lanthanum cerium.
Wherein, metal chloride can be selected from muriate or iron(ic) chloride or aluminum chloride and their any mixture of basic metal or alkaline-earth metal.
The treatment temp of the mixed gas of chlorine and carbon monoxide can be preferably 650-800 ℃.
The mass rate ratio of chlorine and carbon monoxide can be Cl
2/ CO=1/10 to 2 is preferably 1/5 to 8/5.
The hydrochloric acid that is used for leaching can be dilute hydrochloric acid, and its concentration can be 3-15% (w/w); Its volume can be 3-40 times of raw material weight.
Rare precious metal extracting method of the present invention compared with prior art has the following advantages and beneficial effect:
1) this method can make rare precious metal in the raw material for example in the spent auto-catalysts precious metal for example the extraction yield of platinum rhodium palladium and rare earth metal such as lanthanum cerium all more than 90%, even more than 99%;
2) this method is simple, as a result favorable reproducibility;
3) this method only makes for example a small amount of chlorination of cat ceramic base carrier (trichroite or aluminium sesquioxide) of carrier of rare precious metal, and keep carrier not melt, and the muriate such as the aluminum chloride that generate are dissolved in the extracting solution in aftertreatment, therefore the loss amount of raw material solid is usually lower, for example less than 12%; Because carrier is less to be chlorinated, the chlorine consumption is lower;
4) pressure that uses of this method is very near normal pressure (normal atmosphere), and is not high to the equipment sealing requirements;
Therefore 5) muriate in the reaction end gas and chlorine are easy to remove by absorption, and whole process is to environment, thereby the method is environmental protection;
6) this method maximum temperature can be 850 ℃, be lower than the temperature of fire assaying, thereby energy consumption is lower, and because temperature is low, not high to equipment requirements, long service life, equipment is simple, less investment;
7) starting material of the method use are less, and the cost of material is low;
8) this method step is few, and the time spent generally is less than 5 hours, and the time spent is well below fire assaying;
9) this method can be extracted multiple rare precious metal simultaneously.This method can not only the high efficiency extraction raw material in precious metal, rare metal, precious metal platinum metals platinum rhodium palladium for example in the spent auto-catalysts for example, and rare earth metal wherein for example the lanthanum cerium also can be simultaneously by high efficiency extraction, thereby reach the purpose of extracting simultaneously these metals.The method also for rare precious metal in the quantitative analysis raw material exactly for example in the spent auto-catalysts content of precious metal and rare earth metal provide the foundation.
Embodiment
Method of the present invention will at length be illustrated in this part, wherein take contain precious metal for example the junked-auto catalyzer of platinum rhodium palladium and rare earth metal such as lanthanum cerium as example, yet, those skilled in the art are to be understood that, method of the present invention is not limited in and is applied to automobile catalyst, also can be applied to the raw material that other contain rare precious metal, the similar catalyzer that for example uses in the petrochemical industry, natural mineral etc.Precious metal can be ruthenium, rhodium, palladium, osmium, iridium, platinum, gold and silver etc.Rare metal can be vanadium, gallium, rhenium, niobium, tantalum, molybdenum, tungsten, indium, thallium, germanium etc.Rare earth metal can be the lanthanide series metal that comprises scandium.
In the method for the invention, add the metal chloride for example muriate of basic metal or alkaline-earth metal or iron(ic) chloride or aluminum chloride and their any mixture such as NaCl, KCl, MgCl
2Deng purpose be that the precious metal that raw material contains is converted into water-soluble various complex chlorides such as NaPdCl
3, PdFeCl
5, PdAlCl
5Or single muriate such as PdCl
2This type of complex chlorides is usually than the easily molten and difficult decomposition of single muriate, volatilization.The add-on of metal chloride can be for example 2-30wt.% of catalyst fines weight of raw material.Raw material and metal chloride can be Powdered.Particle diameter to raw material powder and metal chloride powder does not have special requirement, but preferably the particle diameter of raw material powder is less than 0.1 millimeter, and the particle diameter of metal chloride is less than 0.3 millimeter.
The effect of chlorine and carbon monoxide is further chloridized raw material in the method for the invention, and the mass rate ratio of the two can be Cl
2/ CO=1/10 to 2 is preferably 1/5 to 8/5.The total mass rate of chlorine and carbon monoxide can be 200-1000mL/min according to raw material weight.The treatment time of chlorine and carbon monoxide can be determined preferably 1-2 hour as required.
Use in the method for the invention chlorine and carbon monoxide chlorination rare precious metal, every kind of metal has an optimal chlorination range of reaction temperature, and for example metal species, this bottom material of raw material the Nomenclature Composition and Structure of Complexes are relevant with chlorine flowrate with many factors for it.
The hydrochloric acid that is used in the method for the invention leaching can be dilute hydrochloric acid, and its concentration can be 3-15% (w/w); Its volume can be 3-40 times of raw material weight; Its effect is that complex chlorides and the single muriate that will generate in the raw material extract in the solution, to reclaim or sampling analysis.During leaching, can this solidliquid mixture is for example several to dozens of minutes 80-100 ℃ of heating, to accelerate leaching.Then carry out filtration washing after the cooling and reclaim, perhaps sampling analysis.
In the method for the invention, before processing with chlorine and carbon monoxide, also mixture can be carried out oxidation pre-treatment with oxygen or air, for example 0.5-2 hour under about 400-600 ℃ temperature; Its objective is and remove raw material such as the impurity such as carbon distribution in the spent catalyst, although it has been generally acknowledged that the impurity such as carbon distribution is on not impact of chloridized.Can cool to room temperature after the oxidation pre-treatment, be kept in the hermetically drying container, in order to next step chloridized; Also can directly be warming up to above-mentioned chlorination temperature and carry out next step chloridized.Temperature-rise period of the present invention can for example carry out under the condition of argon gas passing into rare gas element such as the process that is warming up to oxidation pre-treatment temperature and chloridized temperature, then switches to the processing gas that will use.
The muriatic analytical procedure of rare precious metal can be the concentration with precious metal such as platinum rhodium palladium in plasma mass (ICP-MS) or other methods analyst filtrate in the filtrate, concentration with rare metal and rare earth metal such as lanthanum cerium in ICP-AES (ICP-AES) or other methods analyst filtrate is designated as C
i(ppm).The volume of filtrate is B (mL) after measured.
Then weight is the extracted amount x of certain metal i in the raw material of W
iFor:
In this article, metal fall refers to raw material powder after above-mentioned pyrogenic process chlorination and wet method aftertreatment, transfers to the ratio percentage of this kind metal quality that contains in this kind of the solubility metal quality and the raw material powder that drops into reaction in the extracting solution of aftertreatment.The extraction yield η of metal i is expressed as:
μ is for to use other International Standards Method, and such as the precious metal fire assaying analysis that the specialty analysis personnel carry out, the weight percentage of certain metal i in the raw material that draws can be regarded standard value.
Analyzing relative error RE is:
Extracted amount standard deviation (STDEV) is:
Embodiment 1
Particle diameter 0.1-0.05 millimeter 5.00g spent auto-catalysts dried powder and particle diameter 0.1-0.05 millimeter 0.50g NaCl dried powder are mixed, and packing into is arranged in the up and down reaction tubes of the flat-temperature zone of open tubular furnace.Then tube furnace is warming up to 400 ℃ under logical argon gas condition, again argon gas is switched to oxygen, reacted 1 hour, with the oxidation pre-treatment mixture.Oxygen is switched to argon gas, again tube furnace is warming up to 680 ℃ under logical argon gas condition.Again argon gas is switched to chlorine and carbon mono oxide mixture, reacted 2 hours, with platinum metals platinum rhodium palladium and the Rare Earth Lanthanum cerium in the chlorinated mixture material.The mass rate ratio of the chlorine that passes into and carbon monoxide is controlled at Cl
2/ CO=1, both mass rate sums are 500mL/min.After the chlorination, furnace temperature is cooled to 400 ℃, opens tube furnace upper part, furnace temperature is cooled to rapidly below 100 ℃, reaction tubes is taken out.With the muriate that the mixture in the dilute hydrochloric acid solution washing reaction pipe and its inwall adhere to, the solid that washes out is put into a cone-shaped glass bottle with grinding port plug together with washing lotion.Dilute hydrochloric acid concentration is 10% (w/w), and used dilute hydrochloric acid volume is 150mL during leaching.Solution in the cone-shaped glass bottle was heated filtration washing when being cooled to low-grade fever (40 ℃) 5 minutes at 90 ℃.
Analyze the concentration (ppm) of platinum metals platinum rhodium palladium in the filtrate with plasma mass (ICP-MS), analyze the concentration (ppm) of filtrate middle-weight rare earths lanthanum cerium with ICP-AES (ICP-AES), be designated as C
i(ppm); Adopt the Rh of ICP-MS during analysis
103Line, Pd
106Line, Pt
195Line.The volume of filtrate is designated as V after measured.。Above operation repeats three times.Use above-mentioned formula, calculate extracted amount, average extracted amount, extraction yield, extracted amount standard deviation, the results are shown in the table 1.After measured, catalyst solid loss mean value is 11.8%.
As seen, three times five kinds of metals in the same catalyzer are extracted, measured to repeated experiments, and every kind of metal carrying taken amount standard deviation (STDEV) therefore extracts favorable reproducibility all less than 0.02%; The extraction yield η of platinum rhodium palladium lanthanum cerium can reach more than 99% basically.Analyze relative error RE all less than 2%, satisfy the quantitative analysis requirement.
The extraction of precious metal and rare earth metal in table 1 spent catalyst
Embodiment 2
Except without the dioxygen oxidation pretreatment catalyst, all the other are with embodiment 1, and the result lists in the table 2.As shown in Table 2, without the dioxygen oxidation pretreatment catalyst, platinum palladium chlorination extraction yield η still reaches 93%, and the extraction yield η of rhodium lanthanum cerium reaches about 95%, also has the good extraction effect, but does not satisfy the requirement of quantitative analysis.
The extraction of precious metal and rare earth metal in table 2 spent catalyst (non-oxidation pre-treatment)
| Pd 106 | Pt 195 | Rh 103 | CeO 2 | La 2O 3 | |
| Extracted amount x i | 0.036％ | 0.0465％ | 0.0201％ | 0.63％ | 0.962％ |
| Standard value (μ) | 0.0401％ | 0.0502％ | 0.0211％ | 0.676％ | 0.998％ |
| Extraction yield η | 89.8％ | 92.6％ | 95.3％ | 93.2％ | 96.4％ |
Embodiment 3
Except not adding NaCl, all the other are with embodiment 1, and the result lists in the table 3.As shown in Table 3, when not adding NaCl, the extraction yield η of platinum rhodium palladium lanthanum cerium illustrates and adds metal chloride importance in the present invention less than 80%.
The extraction of precious metal and rare earth metal (without NaCl) in table 3 spent catalyst
| Pd 106 | Pt 195 | Rh 103 | CeO 2 | La 2O 3 | |
| Extracted amount x i | 0.0288％ | 0.039％ | 0.0156％ | 0.46％ | 0.74％ |
| Standard value (μ) | 0.0401％ | 0.0502％ | 0.0211％ | 0.676％ | 0.998％ |
| Extraction yield η | 71.8％ | 77.7％ | 73.9％ | 68.0％ | 74.1％ |
Claims (8)
1. method of extracting simultaneously precious metal in the raw material, rare metal and rare earth metal, it may further comprise the steps:
1) described raw material is mixed with metal chloride;
2) the described mixture of pre-treatment under 400-600 ℃ temperature with oxygen or air;
3) this mixture of mixture gas treatment of usefulness chlorine and carbon monoxide under 450-850 ℃ temperature;
4) will leach under 80-100 ℃ temperature with hydrochloric acid after the described mixture cooling; With
5) filtration washing.
2. method according to claim 1, wherein said metal chloride is selected from muriate or iron(ic) chloride or aluminum chloride and their any mixture of basic metal or alkaline-earth metal.
3. method according to claim 1, wherein the mass rate ratio of chlorine and carbon monoxide is Cl
2/ CO=1/10 to 2.
4. method according to claim 1, wherein said hydrochloric acid is dilute hydrochloric acid, its concentration is 3-15% (w/w).
5. method according to claim 4, the volume of wherein said dilute hydrochloric acid be described raw material weight 3-40 doubly.
6. method according to claim 1 and 2, the add-on of wherein said metal chloride is the 2-30wt.% of the weight of described raw material.
7. method according to claim 1, the treatment time of the mixed gas of wherein said chlorine and carbon monoxide is 1-2 hour.
8. method according to claim 1, wherein said raw material is the junked-auto catalyzer.
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| CN103361485B (en) * | 2012-04-09 | 2015-01-21 | 深圳市格林美高新技术股份有限公司 | Technology for comprehensively recycling rare noble metals in waste LED (light-emitting diode) |
| CN102978401A (en) * | 2012-11-26 | 2013-03-20 | 沈少波 | Method for recovering rare earth and other metals from neodymium iron boron and samarium cobalt magnetic material waste |
| CN103205563A (en) * | 2013-05-06 | 2013-07-17 | 沈少波 | Method for extracting rare noble metals by wet method |
| CN103398865B (en) * | 2013-07-24 | 2015-11-18 | 贵研资源（易门）有限公司 | The sampling of platinum group metal high-area carbon spent catalyst and method for making sample |
| CN111455192A (en) * | 2020-04-29 | 2020-07-28 | 江苏北矿金属循环利用科技有限公司 | Method for recovering palladium from low-grade palladium-containing indissolvable waste catalyst |
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