CN107326183A - The method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst carries palladium - Google Patents
The method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst carries palladium Download PDFInfo
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- CN107326183A CN107326183A CN201710467171.9A CN201710467171A CN107326183A CN 107326183 A CN107326183 A CN 107326183A CN 201710467171 A CN201710467171 A CN 201710467171A CN 107326183 A CN107326183 A CN 107326183A
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- catalyst
- gas clean
- abandoned car
- palladium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/048—Recovery of noble metals from waste materials from spent catalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
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Abstract
The present invention discloses a kind of method that efficient impurity elimination of abandoned car tai-gas clean-up catalyst carries palladium.This method at least comprises the following steps：1) powder of abandoned car tai-gas clean-up catalyst is subjected to dissolving leaching, filtration treatment using leachate, takes filtrate；2) by step 1) obtained filtrate progress anion exchange resin process is handled, remove impurity cationic present in the filtrate；3) using many sulfur organics to step 2) obtained mixed liquor carries out heavy rhodium processing；4) soluble ammonium salt is added in the residual solution obtained to the heavy rhodium processing, carries out heavy palladium processing.This method is handled abandoned car tai-gas clean-up catalyst, and the leaching rate of palladium is high, final DNA purity be up to 98% and more than, and this method flow is simple, and cost is low, environmentally friendly, suitable for popularization and application.
Description
Technical field
Technical field, more particularly to a kind of abandoned car tai-gas clean-up catalyst are recycled the present invention relates to platinum group metal
The method that efficient impurity elimination carries palladium.
Background technology
Cleaning catalyst for tail gases of automobiles contains substantial amounts of platinum-group noble metals, such as platinum, palladium, rhodium, these platinum-group noble metals tool
There is catalysis characteristics.As the improvement of people's living standards, automobile consumption product, which are obtained, tells development, the annual a large amount of vapour of the thing followed
Car is scrapped.And in abandoned car, comprising tai-gas clean-up catalyst turned into the maximum consumption field in platinum group metal, and platinum
Race's metal price is expensive and storage capacity is few, increasingly rare, so carrying out recovery to platinum group metal in abandoned car catalyst has
Great commercial value.
At present, the recovery method of the abandoned car tai-gas clean-up catalyst by carrier of cordierite ceramic mainly has melting rich
Collect pyrogenic process and hydrochloric acid and sodium hypochlorite Selective dissolution wet method.Wherein, melting concentration method high energy consumption, investment is big；Hydrochloric acid and hypochlorous acid
Chlorine is easily generated in sodium Selective dissolution removal process, it is harmful, environment may be polluted.Meanwhile, aluminium, magnesium etc. are miscellaneous
When the presence of matter is for separation and Extraction platinum group metal palladium, aluminium ion and magnesium ion can form flocculent deposit and be mixed into the precipitation of palladium
In so that palladium precipitation contains impurity.
Automobile typically has 8~15 years service life, by the car ownership and growth rate of current China, in the coming years
China will welcome the peak of abandoned car.It is living and domestic abandoned car tai-gas clean-up catalyst is more using cordierite ceramic as carrier
Property component platinum group metal in palladium content it is higher, realize palladium high efficiente callback have higher economic benefit.
Therefore, for palladium content is higher, abandoned car tai-gas clean-up catalyst by carrier of cordierite ceramic seeks one
The efficient impurity elimination of kind carries palladium, environment-friendly and lower-cost new method is particularly important.
The content of the invention
Reclaim net with dissolving hydrometallurgic recovery method recycling abandoned car tail gas to solve above-mentioned existing melting enrichment pyrogenic process
Change in catalyst and there is high energy consumption, investment is big or produces in pernicious gas and catalyst the impurity such as aluminium, magnesium to separation and Extraction
It is the problems such as adverse effect that platinum group metal palladium is present, high the embodiments of the invention provide a kind of abandoned car tai-gas clean-up catalyst
The method that effect impurity elimination carries palladium.
In order to reach foregoing invention purpose, the embodiment of the present invention employs following technical scheme：
A kind of method that efficient impurity elimination of abandoned car tai-gas clean-up catalyst carries palladium, at least comprises the following steps：
1) abandoned car tai-gas clean-up catalyst powder is subjected to dissolving leaching, filtration treatment using leachate, takes filtrate；
2) by step 1) obtained filtrate progress anion exchange resin process is handled, remove miscellaneous present in the filtrate
Matter cation；
3) using many sulfur organics to step 2) obtained mixed liquor carries out heavy rhodium processing；
4) soluble ammonium salt is added in the residual solution obtained to the heavy rhodium processing, carries out heavy palladium processing.
The method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst that the above embodiment of the present invention is provided carries palladium, is first passed through
Leachate carries out leaching palladium metal to catalyst, then carries out removal of impurities processing using anion exchange resin so that the leaching of palladium
Rate is high, final DNA purity be up to 98% and more than, and this method flow is simple, and cost is low, environmentally friendly, suitable for promoting
Using.
Brief description of the drawings
Fig. 1 is the technique for the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst provided in an embodiment of the present invention carries palladium
Schematic flow sheet.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
As shown in figure 1, the embodiment of the present invention provides the side that a kind of efficient impurity elimination of abandoned car tai-gas clean-up catalyst carries palladium
Method, at least comprises the following steps：
1) powder of abandoned car tai-gas clean-up catalyst is subjected to dissolving leaching, filtration treatment using leachate, takes filter
Liquid；
2) by step 1) obtained filtrate progress anion exchange resin process is handled, remove miscellaneous present in the filtrate
Matter cation；
3) using many sulfur organics to step 2) obtained mixed liquor carries out heavy rhodium processing；
4) soluble ammonium salt is added in the residual solution obtained to the heavy rhodium processing, carries out heavy palladium processing.
Above-mentioned preparation method is further described in detail below.
In above-mentioned steps 1) before, abandoned car tai-gas clean-up catalyst is crushed, ground, is washed and filtration treatment,
So that catalyst powder is broken into powder, and it is clean, can be by 200~250 mesh mesh screens, to facilitate leaching.
Preferably, the liquid of leachate and abandoned car tail-gas catalyst powder feeds intake mass ratio for (8~15) admittedly:1, when solid
When body inventory is more than or less than the ratio, the leaching rate rapid decrease of palladium is unfavorable for leaching.
Preferably, leachate is the mixed solution of hydrochloric acid and hydrogen peroxide.In the leachate, it is ensured that hydrochloric acid it is final concentration of
4~7mol/L；Final concentration of 1.0~1.8mol/L of hydrogen peroxide in the leachate.In order to ensure the hydrochloric acid final concentration of addition
In 4~7mol/L, concentrated hydrochloric acid should be added thereto.
Preferably, the time of dissolving leaching process is 1~3h.
During the feeding intake of leachate, first water and concentrated hydrochloric acid are added, it is ensured that fluid temperature is 60~98 DEG C, and
Hydrogen peroxide is added dropwise under stirring condition again, to avoid hydrogen peroxide from directly being volatilized in liquid is added to, and the condition of stirring
Control speed with being added dropwise, can cause hydrogen peroxide to incorporate in hydrochloric acid solution rapidly, and hydrogen peroxide improves salt as oxidant
Leaching effect of the acid to palladium.
It is further preferred that the final concentration of hydrochloric acid and hydrogen peroxide is respectively 5~6mol/L, 1.2~1.5mol/L, preferably
Extraction time is 2~3h.Under the dissolving leaching condition, the leaching rate highest of palladium, beyond this concentration range, the leaching rate of palladium
Decline, and the concentration of oxidant hydrogen peroxide can also influence leaching rate, under conditions of hydrochloric acid is as leaching acid solution, add oxidant
Hydrogen peroxide can effectively improve leaching effect.
In a preferred embodiment, abandoned car catalyst fines is after leachate dissolving is leached, using vacuum filtration
Mode will be separated by filtration containing palladium, the leachate of rhodium and filter residue, take filtrate, filter residue is uniformly processed.
Impurity cationic in the filtrate obtained, such as Al are removed using anion exchange resin3+、Mg2+, so that obtain compared with
For pure platinum group metal mixed liquor, disturbed so as to avoid impurity cationic from extracting generation to follow-up palladium metal.
It is further preferred that using acidity to be carried out again for 5~10mol/L hydrochloric acid to the anion exchange resin after removal of impurities
It is raw；Regenerated liquid uses zinc dust precipitation, and obtained replacement slag is uniformly processed.
Preferably, many sulfur organics are at least one of thioether, disulphide, polysulfide.
In a preferred embodiment, soluble ammonium salt is solid ammonium chloride, is advantageous in that using solid ammonium chloride, solid
Ammonium chloride, being capable of fast Acquisition palladium when gradually dissolving so that the purity of palladium is high in precipitation.
It is further preferred that adding solid ammonium chloride after after palladium completely precipitation, also solution is filtered, to obtain pure palladium
Salt ammonium chloropalladate.
Preferably, in addition to rhodium precipitation refining treatment is carried out, the step of extracting rhodium product.
The method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst that the above embodiment of the present invention is provided carries palladium, is first passed through
Leachate carries out leaching palladium metal to catalyst, then carries out removal of impurities processing using anion exchange resin so that the leaching of palladium
Rate is high, final DNA purity be up to 98% and more than, and this method flow is simple, and cost is low, environmentally friendly, suitable for promoting
Using.
Palladium is carried in order to preferably embody the efficient impurity elimination of abandoned car tai-gas clean-up catalyst provided in an embodiment of the present invention
Method, is further illustrated below by multiple embodiments.
Embodiment 1
A kind of method that efficient impurity elimination of abandoned car tai-gas clean-up catalyst carries palladium, comprises the following steps：
1) abandoned car tai-gas clean-up catalyst crushed, ground, being washed and drying process, and passing through 200 mesh nets
Sieve, obtains the powder of abandoned car tai-gas clean-up catalyst；
2) mass ratio fed intake according to the powder of leachate and abandoned car tai-gas clean-up catalyst is 10：1 ratio is entered
Row feeds intake；Specifically, 12mol/L hydrochloric acid and suitable quantity of water are first added into reaction system, then puts into abandoned car tail gas clean-up
The powder of catalyst, under agitation, 85 DEG C is warming up to by reaction system, 35% hydrogen peroxide is then added dropwise, constantly
Stirring, reacts 2h, after reaction terminates, is filtered by vacuum 3 times, takes each thing in filtrate (also referred to as adsorption liquid), detection filtrate (adsorption liquid)
The content of matter, it is specific as shown in table 1；
3) by step 2) obtained filtrate, by anion exchange resin, collects the liquid by anion exchange resin
(also referred to as desorbed solution), and detect each content of material contained in the liquid (desorbed solution)；
4) appropriate many sulfur organics are put into above-mentioned desorbed solution, are stirred, are stood, filtering takes filtrate, and precipitation carries out essence
Refining is handled；
5) to step 4) obtained filtrate adds solid ammonium chloride, and stir, stand, filtering takes precipitation.
Each material composition detection and analysis result before and after the anion exchange resin of table 1
| Sample number into spectrum | Pd(mg/L) | Al(g/L) | Mg(mg/L) | Fe(mg/L) | Si(mg/L) |
| Adsorption liquid | 3.1 | 1.88 | 618.5 | 43.2 | 11.7 |
| Stripping liquid | 41.4 | 1.3mg/L | -- | 0.01 | 7.0 |
As known from Table 1, Rh, Al, Mg, Fe, Si concentration are extremely low in stripping liquid after resin adsorption, or even inspection is not measured
Come, impurity is seldom in stripping liquid, and Pd content is higher, illustrate by anion exchange resin, can be by sun such as aluminium, iron, magnesium
Pd content is greatly increased in ion remaval, desorbed solution, can obtain purer Pb, is conducive to subsequently sinking Pb, is obtained in heavy Pb
Ammonium chloropalladate in, purity is 98.2%.
Embodiment 2
A kind of method that efficient impurity elimination of abandoned car tai-gas clean-up catalyst carries palladium, comprises the following steps：
1) abandoned car tai-gas clean-up catalyst crushed, ground, being washed and drying process, and passing through 250 mesh nets
Sieve, obtains the powder of abandoned car tai-gas clean-up catalyst；
2) it is 8 according to the powder of the leachate and abandoned car tai-gas clean-up catalyst mass ratio that feeds intake：1 ratio is thrown
Material；Specifically, 12mol/L hydrochloric acid and suitable quantity of water are first added into reaction system, then puts into abandoned car exhaust purification catalytic
The powder of agent, under agitation, 90 DEG C is warming up to by reaction system, 35% hydrogen peroxide is then added dropwise, is stirred continuously,
3h is reacted, after reaction terminates, is filtered by vacuum 3 times, containing for each material in filtrate (also referred to as adsorption liquid), detection filtrate (adsorption liquid) is taken
Amount, it is specific as shown in table 2；
3) by step 2) obtained filtrate, by anion exchange resin, collects the liquid by anion exchange resin
(also referred to as desorbed solution), and detect each content of material contained in the liquid (desorbed solution)；
4) appropriate many sulfur organics are put into above-mentioned desorbed solution, are stirred, are stood, filtering takes filtrate, and precipitation carries out essence
Refining is handled；
5) to step 4) obtained filtrate adds solid ammonium chloride, and stir, stand, filtering takes precipitation.
Each material composition detection and analysis result before and after the anion exchange resin of table 2
| Sample number into spectrum | Pd(mg/L) | Al(g/L) | Mg(mg/L) | Fe(mg/L) | Si(mg/L) |
| Adsorption liquid | 3.0 | 1.76 | 622.5 | 40.8 | 11.0 |
| Stripping liquid | 42.3 | 1.1mg/L | -- | 0.01 | 7.2 |
As known from Table 2, Rh, Al, Mg, Fe, Si concentration are extremely low in stripping liquid after resin adsorption, or even inspection is not measured
Come, impurity is seldom in stripping liquid, and Pd content is higher, illustrate by anion exchange resin, can be by sun such as aluminium, iron, magnesium
Pd content is greatly increased in ion remaval, desorbed solution, can obtain purer Pb, is conducive to subsequently sinking Pb, is obtained in heavy Pb
Ammonium chloropalladate in, purity is 99.36%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent substitution or improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (10)
1. a kind of method that efficient impurity elimination of abandoned car tai-gas clean-up catalyst carries palladium, at least comprises the following steps：
1) powder of abandoned car tai-gas clean-up catalyst is subjected to dissolving leaching, filtration treatment using leachate, takes filtrate；
2) by step 1) obtained filtrate progress anion exchange resin process is handled, remove the sun of impurity present in the filtrate
Ion；
3) using many sulfur organics to step 2) obtained mixed liquor carries out heavy rhodium processing；
4) soluble ammonium salt is added in the residual solution obtained to the heavy rhodium processing, carries out heavy palladium processing.
2. the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst as claimed in claim 1 carries palladium, it is characterised in that：Institute
It is hydrochloric acid and the mixed liquor of hydrogen peroxide to state leachate；Final concentration of 4~7mol/L of hydrochloric acid in the leachate；The leachate
Final concentration of 1.0~1.8mol/L of middle hydrogen peroxide.
3. the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst as claimed in claim 1 carries palladium, it is characterised in that：Institute
The liquid for stating leachate and the abandoned car tai-gas clean-up catalyst powder feeds intake mass ratio for (8~15) admittedly:1.
4. the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst as claimed in claim 2 carries palladium, it is characterised in that：Institute
State the addition sequence of leachate first to add hydrochloric acid, then hydrogen peroxide is added dropwise.
5. the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst as claimed in claim 2 carries palladium, it is characterised in that：Institute
Soluble ammonium salt is stated for solid ammonium chloride.
6. the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst as claimed in claim 1 carries palladium, it is characterised in that：Institute
The temperature for stating dissolving leaching process is 60~98 DEG C, and the time that the dissolving is leached is 1~3h.
7. the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst as claimed in claim 1 carries palladium, it is characterised in that：Institute
State step 1) in be filtered into vacuum filtration.
8. the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst as claimed in claim 1 carries palladium, it is characterised in that：Also
Pretreatment including powder is made to abandoned car tai-gas clean-up catalyst and the powder is carried out into washing and drying processing is walked
Suddenly.
9. the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst as claimed in claim 2 carries palladium, it is characterised in that：Institute
State final concentration of 5~6mol/L of hydrochloric acid in leachate；Final concentration of 1.2~1.5mol/L of hydrogen peroxide.
10. the method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst as claimed in claim 1 carries palladium, it is characterised in that：
The powder of the abandoned car tai-gas clean-up catalyst crosses the sieve of 200~250 mesh before dissolving is leached using leachate.
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| CN201710467171.9A CN107326183A (en) | 2017-06-19 | 2017-06-19 | The method that the efficient impurity elimination of abandoned car tai-gas clean-up catalyst carries palladium |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1448522A (en) * | 2002-04-04 | 2003-10-15 | 中国石油化工股份有限公司 | Method of recovering noble metal from spent catalyst containing noble metal |
| CN103526033A (en) * | 2013-10-21 | 2014-01-22 | 昆明贵研催化剂有限责任公司 | Method for dissolving platinum group metals in automobile spent catalyst enrichment |
| CN104831073A (en) * | 2015-05-04 | 2015-08-12 | 昆明正江工贸有限责任公司 | Technology for recovering platinum, palladium and rhodium from spent auto-catalyst |
-
2017
- 2017-06-19 CN CN201710467171.9A patent/CN107326183A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1448522A (en) * | 2002-04-04 | 2003-10-15 | 中国石油化工股份有限公司 | Method of recovering noble metal from spent catalyst containing noble metal |
| CN103526033A (en) * | 2013-10-21 | 2014-01-22 | 昆明贵研催化剂有限责任公司 | Method for dissolving platinum group metals in automobile spent catalyst enrichment |
| CN104831073A (en) * | 2015-05-04 | 2015-08-12 | 昆明正江工贸有限责任公司 | Technology for recovering platinum, palladium and rhodium from spent auto-catalyst |
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Application publication date: 20171107 |