CN105907975A - Method for comprehensively utilizing carbon-containing waste Pd/Al2O3 catalyst of petroleum chemical industry - Google Patents
Method for comprehensively utilizing carbon-containing waste Pd/Al2O3 catalyst of petroleum chemical industry Download PDFInfo
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- CN105907975A CN105907975A CN201610452103.0A CN201610452103A CN105907975A CN 105907975 A CN105907975 A CN 105907975A CN 201610452103 A CN201610452103 A CN 201610452103A CN 105907975 A CN105907975 A CN 105907975A
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- catalyst
- weak base
- roasting
- al2o3
- 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
- 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
- C22B7/008—Wet processes by an alkaline or ammoniacal 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
-
- 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
-
- 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
- C22B21/00—Obtaining aluminium
- C22B21/0007—Preliminary treatment of ores or scrap or any other metal source
-
- 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
- C22B21/00—Obtaining aluminium
- C22B21/0015—Obtaining aluminium by wet processes
- C22B21/0023—Obtaining aluminium by wet processes from waste materials
- C22B21/003—Obtaining aluminium by wet processes 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
Abstract
The invention provides a method for comprehensively utilizing a carbon-containing waste Pd/Al2O3 catalyst of the petroleum chemical industry. The method mainly includes the steps of excitation and pre-grinding through a planetary ball mill, sodium salt roasting, weak base leaching and the like. The waste catalyst is subjected to mechanical excitation through the planetary ball mill firstly, so that the chemical activity of a material is enhanced; the effects of decarbonization and sodium treatment are achieved after the waste catalyst is roasted for a period of time, so that Al2O3 in the raw material is converted into water-soluble Na2O.Al2O3, and the Na2O.Al2O is subjected to weak base leaching, so that effective separation of Pd from Al2O3 is achieved, the aluminum dissolution rate is over 99%, the Pd concentration ratio is over 43 times, and the recovery rate is larger than 99.9%. The method has the advantages that the process is short, operation is easy and convenient, the leaching time is short, and the method is suitable for large-scale application.
Description
Technical field
The invention belongs to secondary resource and recycle field, relate to a kind of comprehensive reutilization carbon containing oil
Industrial and commercial bank's industry is given up Pd/Al2O3The method of catalyst, it is achieved palladium and the comprehensive reutilization of aluminum, thus for alleviating
Platinum metals resources scarcity creates favorable conditions.
Background technology
Platinum group metal possesses many unique, superior physicochemical properties, its modern industry, military project and
High technology industry technology has special applications that is important and that can not be replaced by other metals or material, has " modern work
Industry vitamin " and the good reputation of " the first high-technology metal ".China is the consumption state of the platinum group metal of whole world maximum,
But mineral resources critical shortage, along with a large amount of exploitation of Platinum metals resources, platinum group metal secondary provides
Source has been increasingly becoming the primary raw material extracting platinum group metal.Platinum group metal dead catalyst because its kind is many,
Valuable metal content is high and becomes the main secondary resource reclaiming platinum group metal, reclaims platinum from dead catalyst
Race's metal production cost compared with primary metal production is low a lot of times, can reduce the same of energy resource consumption in a large number
Time can also reduce the harm to environment, therefore, it is achieved the high efficiente callback of Catalyst in Platinum Group Metal utilizes
Seem most important.
At present, the method for domestic process platinum group metal dead catalyst mainly has CL method, platinum group metal
Dissolution method and carrier dissolution method three kinds.CL method needs to control stronger leaching condition and oxidizing atmosphere,
The carrier and the active component that make spent catalyst are dissolved the most simultaneously and are proceeded to solution, extract from solution the most again
Platinum group metal.Carrier and noble metal dissolve simultaneously, can improve the noble metal response rate.Shortcoming is reagent consumption
Amount is big, and carrier metal separates difficulty with platinum group metal, produces substantial amounts of waste liquid and brings environmental pollution.Platinum family
What dissolving metal method was conventional has pressure cyanide method and chloridising, and cyanide belongs to violent in toxicity, controls strict, pipe
Reason difficulty, equipment investment is big, and chloridising is usually with the hydrochloric acid solution containing one or more oxidants,
Such as HCl+Cl2、HCl+H2O2、HCl+NaClO3, HCl+NaClO and HCl+HNO3Urge Deng dissolving to give up
Platinum group metal in agent, the method working condition is severe, high to equipment requirements, easily causes environmental pollution,
Be not suitable for large-scale production.What carrier dissolution method was conventional has molten (melting) method of acid and alkali molten (melting) method, this
Method can make platinum group metal be effectively enriched with because of it, carrier can also be carried out reasonable efficient recovery simultaneously,
Thus increasingly paid attention to by everybody.
Patent CN 101036889A discloses the recovery method of a kind of catalyst made from platonic, and described platiniferous gives up
Catalyst uses the method for sulphuric acid pressure leaching to dissolve carrier, then leached mud carries out roasting and takes off
Carbon processes.The shortcoming of the method is also to dissolve part platinum group metal while sulphuric acid pressure leaching aluminum, needs
Additional reducing agent is wanted to enter the loss of leachate to reduce platinum group metal.On the other hand in leachate, impurity is many,
Aluminum is not effectively reclaimed.
Patent CN 1143682A discloses a kind of recovery noble metal and side of aluminum from useless aluminium-based catalyst
Method, obtains rich and honour regulus by the method for digestion-water logging dealuminzation.The method uses highly basic hydroxide
Sodium adds water-wet after mixing with dead catalyst, sintering reaction occurs under the conditions of high-temperature roasting, but uses hydrogen
Sodium oxide easily lumps as product during sodium agent roasting, and bond furnace wall, causes discharge especially difficult, separately
Outward, highly basic melted under high temperature can react with platinum group metal, causes the solution loss of platinum group metal.Central-South
University Wang Ming et al. is for its carbonaceous waste Pt/Al2O3Catalyst have employed after raw material roasting decarburization with hydroxide
Sodium mixing adds roasting after water-wet, and the technique that calcining is dissolved in water reclaims the platinum in dead catalyst and aluminum, should
Method uses two-stage roasting, in addition to there is identical problem with patent CN 1143682A, two sections of roastings
Burn not only long flow path, and have to be through the process of a cooling in process of the test, for continuous print stream
Ability of swimming commercial production, cooling procedure is difficult to realize, and easily brings technological process to extend capital expenditure increasing etc.
Problem.
The series of problems existed for current above-mentioned technological process, the special proposition present invention.
Summary of the invention
It is an object of the invention to provide a kind of efficiently comprehensive reutilization petroleum chemical industry carbonaceous waste Pd/
Al2O3The method of catalyst.The method can make palladium be effectively enriched with and can realize returning of alumina catalyst support
Receive and utilize, beneficially resource recycling and sustainable development.The method technique is simple, flow process is short, easy
In enforcement, it is suitable for use of large-scale production.
A kind of comprehensive reutilization carbon containing petroleum chemical industry gives up Pd/Al2O3The method of catalyst, step bag
Including: mechanical activation pre-grinding-sodium roasting-weak base leaches, reclaim aluminum in leachate, palladium is enriched with in slag,
Sodium roasting additive therefor is Disodium oxalate..
Above-mentioned method: useless Pd/Al2O3Catalyst slightly breaks to-3mm, is milled to mog in advance and is
-200 mesh account for 70%～80%.
Above-mentioned method: the consumption of Disodium oxalate. is useless Pd/Al2O31.5～2.5 of aluminum content in catalyst
Times.
Above-mentioned method: sodium roasting temperature is 650 DEG C～850 DEG C, and roasting time is 60min～100min.
Above-mentioned method: use NaOH solution to leach when weak base leaches.
Above-mentioned method: the dilute NaOH solution using mass fraction to be 0.5%～3% when weak base leaches leaches.
Above-mentioned method: when weak base leaches, the liquid-solid ratio of calcining after weak caustic solution and sodium roasting is
3～8, temperature 60 C～100 DEG C, mixing speed: 250～400r/min, extraction time 30～60min.
Advantages of the present invention essentially consists in: catalyst is after mechanical activation, and reactivity strengthens so that roasting
Burn temperature reduction, the response time shortens；, while there is natridization reaction in raw ore and one section of roasting of sodium agent
Reach the effect of de-carbon, shorten technological process, reduce energy consumption, the combustion heat release of carbon, be also beneficial to fall
Low outside heating load；The sodium agent used is the Disodium oxalate. with reproducibility, is possible not only to anti-with aluminium oxide
Sodium metaaluminate (Na soluble in water should be generated2O.Al2O3), can protect simultaneously platinum group metal palladium not with sodium
Agent reaction generates compound soluble in water, and leaching process need not additional reducing agent to reduce noble metal
The loss of palladium, carrier is dissolved as NaAl (OH) under alkaline solution4, it is simple to reclaim aluminum, ensure that palladium simultaneously
High concentration ratio, it is achieved that palladium and the synthetical recovery of aluminum.The dissolution rate of aluminum reaches more than 99%, the richness of Pd
Collection ratio is more than 43 times, and the response rate is more than 99.9%.The method reclaims field at aluminum base Used palladium catalyst to be had
The most wide application prospect.
Detailed description of the invention:
It is intended to further illustrate the present invention below in conjunction with embodiment, and the unrestricted present invention.
Material condition: in dead catalyst used, C content is 9.2%, Al2O3Content is 76.76%, and Pd contains
Amount is 2120g/t.
Embodiment 1: useless Pd/Al2O3Catalyst slightly breaks to-3mm, and planetary ball mill is milled to ore grinding in advance
Fineness accounts for 70%～80% for-200 mesh, takes the raw material after mechanical activation pre-grinding, adds theoretical amount 1.5 times
Na2C2O4Stir and add water-wet and be placed in Muffle furnace roasting 100min under the conditions of 650 DEG C,
The calcining obtained is fluffy, without caking phenomenon；Calcining mass fraction is the sodium hydroxide solution of 0.5%
Leaching 30min, leaching condition is liquid-solid ratio 3:1,95 DEG C of water-baths, mixing speeds 300r/min.Taking off of aluminum
Except rate 84.14%, the removal efficiency 98.79% of carbon, palladium is all enriched in slag.
Embodiment 2: useless Pd/Al2O3Catalyst slightly breaks to-3mm, and planetary ball mill is milled to ore grinding in advance
Fineness accounts for 70%～80% for-200 mesh, takes the raw material after mechanical activation pre-grinding, adds theoretical amount 2.0 times
Na2C2O4Stir and add water-wet and be placed in Muffle furnace roasting 100min under the conditions of 750 DEG C,
The calcining obtained is fluffy, without caking phenomenon；Calcining mass fraction is the sodium hydroxide solution leaching of 3%
Going out 30min, leaching condition is liquid-solid ratio 3:1,95 DEG C of water-baths, mixing speeds 300r/min.The removing of aluminum
Rate 91.86%, carbon removal efficiency 99.12%, palladium is all enriched in slag.
Embodiment 3: useless Pd/Al2O3Catalyst slightly breaks to-3mm, and planetary ball mill is milled to ore grinding in advance
Fineness accounts for 70%～80% for-200 mesh, takes the raw material after mechanical activation pre-grinding, adds theoretical amount 2.5 times
Na2C2O4Stir and add water-wet and be placed in Muffle furnace roasting 100min under the conditions of 800 DEG C,
The calcining obtained is fluffy, without caking phenomenon；Calcining mass fraction is the sodium hydroxide solution leaching of 3%
Going out 60min, leaching condition is liquid-solid ratio 3:1,95 DEG C of water-baths, mixing speeds 300r/min.The removing of aluminum
Rate 95.91%, carbon removal efficiency 99.34%, palladium is all enriched in slag.
Embodiment 4: useless Pd/Al2O3Catalyst slightly breaks to-3mm, and planetary ball mill is milled to ore grinding in advance
Fineness accounts for 70%～80% for-200 mesh, takes the raw material after mechanical activation pre-grinding, adds theoretical amount 2.5 times
Na2C2O4Stir and add water-wet and be placed in Muffle furnace roasting 80min under the conditions of 850 DEG C,
The calcining arrived is fluffy, without caking phenomenon；Calcining mass fraction is the sodium hydroxide solution leaching of 3%
30min, leaching condition is liquid-solid ratio 3:1,95 DEG C of water-baths, mixing speeds 300r/min.The removal efficiency of aluminum
98.57%, carbon removal efficiency 99.35%, palladium is all enriched in slag.
Embodiment 5: useless Pd/Al2O3Catalyst slightly breaks to-3mm, and planetary ball mill is milled to ore grinding in advance
Fineness accounts for 70%～80% for-200 mesh, takes the raw material after mechanical activation pre-grinding, adds theoretical amount 2.5 times
Na2C2O4Stir and add water-wet and be placed in Muffle furnace roasting 100min under the conditions of 850 DEG C,
The calcining obtained is fluffy, without caking phenomenon；Calcining mass fraction is the sodium hydroxide solution leaching of 3%
Going out 60min, leaching condition is liquid-solid ratio 3:1,95 DEG C of water-baths, mixing speeds 300r/min.The removing of aluminum
Rate 99.63%, carbon removal efficiency 99.51%, palladium is all enriched in slag.
Reference examples 1: take the raw material after mechanical activation pre-grinding, adds the NaOH stirring of theoretical amount 2.0 times
Uniformly adding water-wet and be placed in Muffle furnace roasting 100min under the conditions of 850 DEG C, calcining is tied in container
Block is serious, and hardness is big；Calcining ultra-pure water leaches 60min, leaching condition be liquid-solid ratio 3:1,95 DEG C
Water-bath, mixing speed 300r/min.The removal efficiency 93.73% of aluminum, carbon removal efficiency 98.74%, in leachate
Palladium content 31.08mg/L, the loss of palladium is serious.
Reference examples 2: take the raw material after mechanical activation pre-grinding, roasting 1h decarburization under the conditions of 600 DEG C, after cooling
Add the Na of theoretical amount 2.5 times2C2O4Stir and add water-wet and be placed in Muffle furnace at 850 DEG C of bars
Roasting 100min under part, the calcining obtained is fluffy, without caking phenomenon；Calcining mass fraction is 3%
Sodium hydroxide solution leach 60min, leaching condition is liquid-solid ratio 3:1,95 DEG C of water-baths, mixing speeds
300r/min.The removal efficiency 95.28% of aluminum, carbon removal efficiency 99.58%, double diffusion is the most complicated.
Reference examples 3: the most activated, takes raw material and adds the Na of theoretical amount 2.5 times2C2O4Stir and add
Water-wet is placed in Muffle furnace roasting 150min under the conditions of 850 DEG C, and the calcining obtained is fluffy,
Without caking phenomenon；Calcining mass fraction is the sodium hydroxide solution leaching 60min of 3%, and leaching condition is
Liquid-solid ratio 3:1,95 DEG C of water-baths, mixing speeds 300r/min.The removal efficiency 87.48% of aluminum, carbon removal efficiency
99.27%.Not having mechanical activation, the sodium of aluminum is incomplete, and removal efficiency is low, the level of the present invention to be reached,
Roasting time have to be extended.
Reference examples 4: take the raw material after mechanical activation pre-grinding, adds the Na of theoretical amount 2.5 times2C2O4Stir
Mix and uniformly add water-wet and be placed in Muffle furnace roasting 100min under the conditions of 850 DEG C, the calcining obtained in
Fluffy, without caking phenomenon；Calcining ultra-pure water leaches 60min, leaching condition be liquid-solid ratio 3:1,95
DEG C water-bath, mixing speed 300r/min.The removal efficiency 75.26% of aluminum, carbon removal efficiency 99.45%.
Claims (7)
1. a comprehensive reutilization carbon containing petroleum chemical industry gives up Pd/Al2O3The method of catalyst, it is special
Levy and be: step includes: mechanical activation pre-grinding-sodium roasting-weak base leaches, leachate reclaims aluminum, palladium
Being enriched with in slag, sodium roasting additive therefor is Disodium oxalate..
Method the most according to claim 1, it is characterised in that: useless Pd/Al2O3Catalyst slightly break to
Below-3mm, is milled to mog in advance and accounts for 70%～80% for-200 mesh.
Method the most according to claim 1, it is characterised in that: the consumption of Disodium oxalate. is useless Pd/Al2O3
1.5～2.5 times of aluminum content in catalyst.
4. according to the method described in claim 1 or 3, it is characterised in that: sodium roasting temperature is
650 DEG C～850 DEG C, roasting time is 60min～100min.
Method the most according to claim 1, it is characterised in that: use NaOH molten when weak base leaches
Immersion goes out.
Method the most according to claim 5, it is characterised in that: use mass fraction when weak base leaches
It it is the dilute NaOH solution leaching of 0.5%～3%.
7. according to the method described in claim 1 or 5 or 6, it is characterised in that: weak base when weak base leaches
The liquid-solid ratio of the calcining after solution and sodium roasting is 3～8, temperature 60 C～100 DEG C, stirring speed
Degree: 250～400r/min, extraction time 30～60min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521140A (en) * | 2016-11-06 | 2017-03-22 | 陈礼华 | Oil-carbon-sulfur removing high-alkali sodium roasting process |
| CN107841628A (en) * | 2017-10-31 | 2018-03-27 | 昆明理工大学 | A kind of microwave treatment platinum dead catalyst separation aluminium and the method for being enriched with platinum |
| CN108187764A (en) * | 2018-01-17 | 2018-06-22 | 河南能源化工集团研究院有限公司 | Classified utilization method after dimethyl oxalate synthesis palladium Al catalysts failure |
| CN108950603A (en) * | 2018-08-31 | 2018-12-07 | 营口忠旺铝业有限公司 | A kind of method for electrolyzing aluminum improving electrolyte dissolution degree |
| CN111647751A (en) * | 2020-06-18 | 2020-09-11 | 安徽工业大学 | Method for enriching platinum group metals from automobile waste catalyst |
| CN115003830A (en) * | 2020-01-30 | 2022-09-02 | 国立大学法人福井大学 | Method for recovering platinum group metal, composition containing platinum group metal, and ceramic material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106521140A (en) * | 2016-11-06 | 2017-03-22 | 陈礼华 | Oil-carbon-sulfur removing high-alkali sodium roasting process |
| CN107841628A (en) * | 2017-10-31 | 2018-03-27 | 昆明理工大学 | A kind of microwave treatment platinum dead catalyst separation aluminium and the method for being enriched with platinum |
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| CN111647751A (en) * | 2020-06-18 | 2020-09-11 | 安徽工业大学 | Method for enriching platinum group metals from automobile waste catalyst |
| CN111647751B (en) * | 2020-06-18 | 2022-04-05 | 安徽工业大学 | Method for enriching platinum group metals from automobile waste catalyst |
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