CN105907975B - A kind of carbon containing petroleum chemical industry of comprehensive reutilization gives up Pd/Al2O3The method of catalyst - Google Patents

A kind of carbon containing petroleum chemical industry of comprehensive reutilization gives up Pd/Al2O3The method of catalyst Download PDF

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CN105907975B
CN105907975B CN201610452103.0A CN201610452103A CN105907975B CN 105907975 B CN105907975 B CN 105907975B CN 201610452103 A CN201610452103 A CN 201610452103A CN 105907975 B CN105907975 B CN 105907975B
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catalyst
sodium
roasting
aluminium
weak base
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CN105907975A (en
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李骞
姜涛
郭宇峰
董海刚
杨永斌
徐斌
饶雪飞
胡龙
邹强
张雁
李光辉
范晓慧
陈许玲
张元波
彭志伟
甘敏
杨凌志
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Central South University
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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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a kind of useless Pd/Al of the carbon containing petroleum chemical industry of comprehensive reutilization2O3The method of catalyst.This method mainly includes the steps such as planetary ball mill activation pre-grinding, sodium roasting, weak base leaching.Dead catalyst carries out mechanical activation by planetary ball mill first, strengthens material chemism, then reaches the effect of decarburization and sodium by one section of roasting, by the Al in raw material2O3It is converted into Na soluble in water2O.Al2O3, weak base, which leaches, dissolves Na2O.Al2O3To realize Pd and Al2O3Efficiently separate, the dissolution rate of aluminium reaches more than 99%, Pd concentration ratio more than 43 times, and the rate of recovery is more than 99.9%.The present invention has the advantages that flow is short, simple to operate, extraction time is short, is adapted to large-scale application.

Description

A kind of carbon containing petroleum chemical industry of comprehensive reutilization gives up Pd/Al2O3Catalyst Method
Technical field
The invention belongs to secondary resource recycling field, is related to a kind of carbon containing petroleum chemical industry of comprehensive reutilization and gives up Pd/Al2O3The method of catalyst, the comprehensive reutilization of palladium and aluminium is realized, so as to have to alleviate deficient create of Platinum metals resources Sharp condition.
Background technology
Platinum group metal possesses many unique, superior physicochemical properties, and it is in modern industry, military project and high technology industry skill There are special applications that are important and can not being substituted by other metals or material in art, there is " modern industry vitamin " and " the first high skill The good reputation of art metal ".China is the consumption state of global maximum platinum group metal, but mineral resources critical shortage, with platinum family gold Belong to a large amount of utilization of resource, platinum group metal secondary resource has been increasingly becoming the primary raw material of extraction platinum group metal.Platinum group Metal dead catalyst turns into the secondary resource of main recovery platinum group metal because its species is more, valuable metal content is high, is urged from useless Platinum group metal production cost compared with primary metal produces is reclaimed in agent and wants low a lot of times, can largely reduce the same of energy resource consumption When can also reduce harm to environment, therefore, realize the high efficiente callback of Catalyst in Platinum Group Metal using seeming most important.
At present, the method for domestic processing platinum group metal dead catalyst mainly have fully dissolved method, platinum group metal dissolution method and Three kinds of carrier dissolution method.Fully dissolved method needs to control stronger leaching condition and oxidizing atmosphere, make spent catalyst carrier and All dissolving is transferred to solution to active component simultaneously, then extracts platinum group metal from solution again.Carrier and noble metal dissolve simultaneously, can Improve the noble metal rate of recovery.Shortcoming is that reagent consumption amount is big, and carrier metal and platinum group metal separation are difficult, produce substantial amounts of waste liquid Bring environmental pollution.What platinum group metal dissolution method was commonly used has pressure cyanide method and chloridising, and cyanide category violent in toxicity, control is sternly Lattice, difficult management, equipment investment is big, and chloridising is usually with the hydrochloric acid solution containing one or more of oxidants, such as HCl+ Cl2、HCl+H2O2、HCl+NaClO3, HCl+NaClO and HCl+HNO3Deng the platinum group metal in dissolving dead catalyst, the method life Inclement condition is produced, it is high to equipment requirement, environmental pollution is easily caused, is not suitable for large-scale production.What carrier dissolution method was commonly used has acid Molten (molten) method and alkali soluble (molten) method, the method can also be carried out because it can be such that platinum group metal is effectively enriched with to carrier Rationally effectively recovery, so as to increasingly be paid attention to by everybody.
Patent CN 101036889A disclose a kind of recovery method of catalyst made from platonic, and described platinum-containing waste catalyst is adopted Carrier is dissolved with the method for sulfuric acid pressure leaching, roasting carbonization treatment then is carried out to leached mud.The shortcomings that this method Also part platinum group metal can be dissolved while being sulfuric acid pressure leaching aluminium, it is necessary to which additional reducing agent enters leaching to reduce platinum group metal Go out the loss of liquid.Impurity is more in another aspect leachate, and aluminium is not reclaimed effectively.
Patent CN 1143682A disclose a kind of method that noble metal and aluminium are reclaimed from useless aluminium-based catalyst, by disappearing The method of change-water logging dealuminzation obtains rich and honour regulus.This method uses highly basic sodium hydroxide to add after being mixed with dead catalyst Water is soaked, and product is easily tied when sintering reaction occurring under the conditions of high-temperature roasting, but being calcined using sodium hydroxide as sodium agent Block, furnace wall is bonded, causes discharge especially difficult, in addition, the highly basic melted under high temperature can react with platinum group metal, cause platinum family golden The solution loss of category.Central South University Wang Ming et al. is directed to its carbonaceous waste Pt/Al2O3Catalyst employ raw material roasting decarburization after with Sodium hydroxide, which mixes, adds water to be calcined after soaking, and platinum and aluminium in the technique recovery dead catalyst that calcining is dissolved in water, this method are adopted With two-stage roasting, in addition to it the problem of identical be present with patent CN 1143682A, two-stage roasting not only long flow path, Er Qieshi The process by a cooling is had to during testing, for continuous continuous-flow type industrial production, cooling procedure is not easy to realize, holds Technological process is easily brought to extend the problems such as capital expenditure increases.
The present invention is proposed for a series of problems, spy existing for current above-mentioned technological process.
The content of the invention
It is an object of the invention to provide a kind of efficiently comprehensive reutilization petroleum chemical industry carbonaceous waste Pd/Al2O3Catalyst Method.This method can make palladium obtain the recycling that effectively enrichment and can realizes alumina catalyst support, be advantageous to resource repetition Using and sustainable development.This method technique is simple, flow is short, easy to implement, is adapted to use of large-scale production.
A kind of carbon containing petroleum chemical industry of comprehensive reutilization gives up Pd/Al2O3The method of catalyst, step include：Machinery is living Change pre-grinding-sodium roasting-weak base to leach, reclaim aluminium in leachate, palladium is enriched with slag, and sodium roasting additive therefor is Sodium oxalate.
Above-mentioned method：Useless Pd/Al2O3Catalyst is slightly broken to -3mm, is milled to mog in advance and is accounted for 70% for -200 mesh ~80%.
Above-mentioned method：The dosage of sodium oxalate is useless Pd/Al2O31.5~2.5 times of aluminium content in catalyst.
Above-mentioned method：Sodium roasting temperature is 650 DEG C~850 DEG C, and roasting time is 60min~100min.
Above-mentioned method：Leached when weak base leaches using NaOH solution.
Above-mentioned method：Weak base uses mass fraction to be leached for 0.5%~3% dilute NaOH solution when leaching.
Above-mentioned method：The liquid-solid ratio of weak caustic solution and the calcining after sodium roasting is 3~8 when weak base leaches, temperature 60 DEG C~100 DEG C, mixing speed:250~400r/min, 30~60min of extraction time.
Advantages of the present invention essentially consists in：Catalyst is after mechanical activation, reactivity enhancing so that sintering temperature drops The low, reaction time shortens；The one section of roasting of raw ore and sodium agent, occurs to reach the effect except carbon while natridization reaction, shortens Technological process, energy consumption is reduced, the combustion heat release of carbon, is also beneficial to reduce outside heating load；The sodium agent used is with reduction Property sodium oxalate, not only can generate sodium metaaluminate (Na soluble in water with oxidation reactive aluminum2O.Al2O3), while can protect Platinum group metal palladium does not generate compound soluble in water with sodium agent reaction, and leaching process does not need additional reducing agent expensive to reduce The loss of Metal Palladium, carrier are dissolved as NaAl (OH) under alkaline solution4, it is easy to reclaim aluminium, while ensure that the high enrichment of palladium Than realizing the synthetical recovery of palladium and aluminium.The dissolution rate of aluminium reaches more than 99%, Pd concentration ratio more than 43 times, and the rate of recovery is big In 99.9%.This method has very wide application prospect in aluminium base Used palladium catalyst recycling field.
Embodiment：
The present invention is intended to further illustrate with reference to embodiment, is not intended to limit the present invention.
Material condition：C content is 9.2%, Al in dead catalyst used2O3Content is that 76.76%, Pd contents are 2120g/ t。
Embodiment 1：Useless Pd/Al2O3Catalyst is slightly broken to -3mm, and planetary ball mill is milled to mog as -200 in advance Mesh accounts for 70%~80%, takes the raw material after mechanical activation pre-grinding, adds the Na of 1.5 times of theoretical amount2C2O4Stir Jia Shuirun It is placed in after wet in Muffle furnace and is calcined 100min under the conditions of 650 DEG C, obtained calcining is in fluffy, no caking phenomenon；Calcining is used The sodium hydroxide solution that mass fraction is 0.5% leaches 30min, and leaching condition is liquid-solid ratio 3:1st, 95 DEG C of water-baths, mixing speeds 300r/min.The removal efficiency 84.14% of aluminium, the removal efficiency 98.79% of carbon, palladium is all enriched in slag.
Embodiment 2：Useless Pd/Al2O3Catalyst is slightly broken to -3mm, and planetary ball mill is milled to mog as -200 in advance Mesh accounts for 70%~80%, takes the raw material after mechanical activation pre-grinding, adds the Na of 2.0 times of theoretical amount2C2O4Stir and add water It is placed in after wetting in Muffle furnace and is calcined 100min under the conditions of 750 DEG C, obtained calcining is in fluffy, no caking phenomenon；Calcining 30min is leached with the sodium hydroxide solution that mass fraction is 3%, leaching condition is liquid-solid ratio 3:1st, 95 DEG C of water-baths, mixing speeds 300r/min.The removal efficiency 91.86% of aluminium, carbon removal efficiency 99.12%, palladium is all enriched in slag.
Embodiment 3：Useless Pd/Al2O3Catalyst is slightly broken to -3mm, and planetary ball mill is milled to mog as -200 in advance Mesh accounts for 70%~80%, takes the raw material after mechanical activation pre-grinding, adds the Na of 2.5 times of theoretical amount2C2O4Stir Jia Shuirun It is placed in after wet in Muffle furnace and is calcined 100min under the conditions of 800 DEG C, obtained calcining is in fluffy, no caking phenomenon；Calcining is used The sodium hydroxide solution that mass fraction is 3% leaches 60min, and leaching condition is liquid-solid ratio 3:1st, 95 DEG C of water-baths, mixing speeds 300r/min.The removal efficiency 95.91% of aluminium, carbon removal efficiency 99.34%, palladium is all enriched in slag.
Embodiment 4：Useless Pd/Al2O3Catalyst is slightly broken to -3mm, and planetary ball mill is milled to mog as -200 in advance Mesh accounts for 70%~80%, takes the raw material after mechanical activation pre-grinding, adds the Na of 2.5 times of theoretical amount2C2O4Stir Jia Shuirun It is placed in after wet in Muffle furnace and is calcined 80min under the conditions of 850 DEG C, obtained calcining is in fluffy, no caking phenomenon；Calcining matter Measure the sodium hydroxide solution that fraction is 3% and leach 30min, leaching condition is liquid-solid ratio 3:1st, 95 DEG C of water-baths, mixing speed 300r/ min.The removal efficiency 98.57% of aluminium, carbon removal efficiency 99.35%, palladium is all enriched in slag.
Embodiment 5：Useless Pd/Al2O3Catalyst is slightly broken to -3mm, and planetary ball mill is milled to mog as -200 in advance Mesh accounts for 70%~80%, takes the raw material after mechanical activation pre-grinding, adds the Na of 2.5 times of theoretical amount2C2O4Stir Jia Shuirun It is placed in after wet in Muffle furnace and is calcined 100min under the conditions of 850 DEG C, obtained calcining is in fluffy, no caking phenomenon；Calcining is used The sodium hydroxide solution that mass fraction is 3% leaches 60min, and leaching condition is liquid-solid ratio 3:1st, 95 DEG C of water-baths, mixing speeds 300r/min.The removal efficiency 99.63% of aluminium, carbon removal efficiency 99.51%, palladium is all enriched in slag.
Reference examples 1：Take the raw material after mechanical activation pre-grinding, the NaOH for adding 2.0 times of theoretical amount stirs Jia Shuirun It is placed in after wet in Muffle furnace and 100min is calcined under the conditions of 850 DEG C, calcining lumps seriously in container, and hardness is big；Calcining is used Ultra-pure water leaches 60min, and leaching condition is liquid-solid ratio 3:1st, 95 DEG C of water-baths, mixing speed 300r/min.The removal efficiency of aluminium 93.73%, carbon removal efficiency 98.74%, palladium content 31.08mg/L in leachate, the loss of palladium is serious.
Reference examples 2：The raw material after mechanical activation pre-grinding is taken, 1h decarburizations are calcined under the conditions of 600 DEG C, theoretical use is added after cooling The Na of 2.5 times of amount2C2O4Stir plus water wetting after be placed in Muffle furnace and be calcined 100min under the conditions of 850 DEG C, obtained roasting Sand is in fluffy, no caking phenomenon；The sodium hydroxide solution that calcining mass fraction is 3% leaches 60min, and leaching condition is liquid Admittedly than 3:1st, 95 DEG C of water-baths, mixing speed 300r/min.The removal efficiency 95.28% of aluminium, carbon removal efficiency 99.58%, double diffusion It is too complicated.
Reference examples 3：It is not activated, take raw material to add the Na of 2.5 times of theoretical amount2C2O4Stir plus water wetting is rearmounted 150min is calcined under the conditions of 850 DEG C in Muffle furnace, obtained calcining is in fluffy, no caking phenomenon；Calcining quality point Number leaches 60min for 3% sodium hydroxide solution, and leaching condition is liquid-solid ratio 3:1st, 95 DEG C of water-baths, mixing speed 300r/min. The removal efficiency 87.48% of aluminium, carbon removal efficiency 99.27%.There is no mechanical activation, the sodium of aluminium is incomplete, and removal efficiency is low, to reach The level of the present invention, it is necessary to extend roasting time.
Reference examples 4：The raw material after mechanical activation pre-grinding is taken, adds the Na of 2.5 times of theoretical amount2C2O4Stir and add water It is placed in after wetting in Muffle furnace and is calcined 100min under the conditions of 850 DEG C, obtained calcining is in fluffy, no caking phenomenon；Calcining 60min is leached with ultra-pure water, leaching condition is liquid-solid ratio 3:1st, 95 DEG C of water-baths, mixing speed 300r/min.The removal efficiency of aluminium 75.26%, carbon removal efficiency 99.45%.

Claims (4)

  1. The Pd/Al 1. a kind of carbon containing petroleum chemical industry of comprehensive reutilization gives up2O3The method of catalyst, it is characterised in that：Step bag Include：Mechanical activation pre-grinding-sodium roasting-weak base leaches, and reclaims aluminium in leachate, palladium is enriched with slag, sodium roasting institute It is sodium oxalate with additive；
    The dosage of sodium oxalate is useless Pd/Al2O31.5~2.5 times of aluminium content in catalyst；
    Sodium roasting temperature is 650 DEG C~850 DEG C,
    Weak base uses mass fraction to be leached for 0.5%~3% dilute NaOH solution when leaching.
  2. 2. according to the method for claim 1, it is characterised in that：Useless Pd/Al2O3Catalyst is slightly broken to -3mm, is milled in advance Mog is that -200 mesh account for 70%~80%.
  3. 3. according to the method for claim 1, it is characterised in that：The sodium roasting time is 60min~100min.
  4. 4. according to the method for claim 1, it is characterised in that：Weak caustic solution and the roasting after sodium roasting when weak base leaches The liquid-solid ratio of sand is 3~8, temperature 60 C~100 DEG C, mixing speed:250~400r/min, 30~60min of extraction time.
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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
CN108187764B (en) * 2018-01-17 2020-11-06 河南能源化工集团研究总院有限公司 Grading utilization method for invalid palladium-aluminum catalyst synthesized by dimethyl oxalate
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
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
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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