CN103194606B - Method for concentrating platinum group metals from alumina-based waste catalyst - Google Patents
Method for concentrating platinum group metals from alumina-based waste catalyst Download PDFInfo
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- CN103194606B CN103194606B CN201310104285.9A CN201310104285A CN103194606B CN 103194606 B CN103194606 B CN 103194606B CN 201310104285 A CN201310104285 A CN 201310104285A CN 103194606 B CN103194606 B CN 103194606B
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- spent catalyst
- platinum group
- alumina base
- filter residue
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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 relates to the field of extraction of platinum group metals, particularly relates to a method for concentrating platinum group metals from an alumina-based waste catalyst, and the method overcomes the defects of the prior art. The method is suitable for a wide range of materials; and based on the method, the carrier dissolution effect is good, the platinum group metal concentration rate is high, the content of platinum group metals in concentrated slag is high, the recovery rate of platinum group metals is high, and the equipment corrosion degree is low. The method for concentrating platinum group metals from an alumina-based waste catalyst comprises the steps of: (A) primary incineration; (B) crushing; (C) pressure alkali dissolution; (D) filtering; and (E) secondary incineration. The method is suitable for a wide range of materials; the dissolution ratio of aluminum oxide is more than 95 percent; the concentration degree of platinum group metals is 80-120, and the concentration effect is good; the content of platinum group metals in slag is in the range of 10-14 percent, thereby being beneficial for the post procedure of refining platinum group metals; and the recovery rate of platinum group metals in concentration technology is more than 99 percent; and the equipment corrosion degree is low.
Description
Technical field
The present invention relates to the refinement field of platinum metals, be specifically related to the method for enrichment platinum metals from alumina base spent catalyst.
Background technology
Platinum metals comprises platinum (Pt), palladium (Pd), ruthenium (Ru), rhodium (Rh), osmium (Os), 6 kinds of metals of iridium (Ir), and their content in the earth's crust is low, reserves are few, expensive.
Platinum metals has been widely used in the catalyzer of hydrogenation, dehydrogenation, reformation, oxidation, isomerization, disproportionation, cracking and desamination reaction.Because the factors such as poisoning, carbon deposit, carrier structure variation, metal grain gathering or loss cause catalyzer to lose activity, catalyzer needs periodic replacement.In the time that catalyzer finishes work-ing life, platinum metals loss is very little, and these spent catalysts have huge value equally.Platinum metals is recycled and is significant.
The recovery method of spent catalyst can be divided into pyrogenic process and wet method by the difference of technique.Wherein pyrogenic process has melting concentration method, pyrogenic process chlorination process and burning method, and wet method comprises carrier dissolution method, solubilization of active ingredient method and CL method.
General hydrometallurgic recovery platinum metals and the valuable metal of adopting from alumina base spent catalyst.Wet method is mainly divided acid-soluble method and the molten support methods of alkali.Acid-soluble method has selects to dissolve support methods, selection dissolving precious metal method, CL method, and acid-soluble method only adapts to solubility γ-Al
2o
3carried catalyst, is not suitable for processing soluble crystal formation θ-Al
2o
3, δ-Al
2o
3and α-Al
2o
3base is the spent catalyst of carrier.
The molten support methods of alkali is to select to dissolve Al
2o
3base carrier, does not dissolve noble metal component, reclaims precious metal from insoluble slag.The molten support methods energy of alkali processing soluble γ-Al
2o
3carrier spent catalyst, also can dissolve insoluble θ-Al
2o
3, δ-Al
2o
3and α-Al
2o
3carrier spent catalyst, the molten support methods of alkali can be processed various crystal form A l
2o
3base is the spent catalyst of carrier, wide accommodation.
Under normal pressure, alkaline solution can dissolve Al in spent catalyst
2o
3carrier, but dissolved efficiency is low, dissolution rate only has 50～70%, and quantity of alkali consumption is large, and production cost is high; High temperature alkali fuse Al
2o
3it is high that carrier melts energy consumption, and equipment corrosion is serious.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned prior art, provide a kind of from alumina base spent catalyst the method for enrichment platinum metals, the method adapt to material scope wide, dissolve that carrier is effective, platinum metals enrichment times is high, in enrichment slag high, the platinum metals of platinum metals content reclaim high, equipment corrosion is low.
To achieve these goals, technical scheme of the present invention is:
A method for enrichment platinum metals from alumina base spent catalyst, comprises the following steps:
A, once burning: the alumina base spent catalyst of platinum group metal is burned, contain charcoal to catalyzer and be less than 1%;
B, pulverizing: the spent catalyst after steps A gained is made charcoal is milled to 70～90 orders;
C, pressurization alkali molten: the alumina base spent catalyst that step B gained is crushed, add the NaOH solution of 28-32%, NaOH solution and alumina base spent catalyst weight ratio are 2～3: 1, the reductive agent that adds again alumina base spent catalyst weight 5-10 ‰ was warming up to 120～140 DEG C, pressure 0.3～0.5MPa in 2 hours, constant temperature, constant voltage 1.5～2.5 hours, be warmed up to 190～200 DEG C at 0.5-1.5 hour, pressure is 1.2～1.6MPa, constant temperature 2～4 hours;
D, filtration: by step C gained solution, 130～140 DEG C of filtrations, filter residue is used 80 DEG C of hot washes of 5～10 times of amounts of filter residue weight at every turn, wash 3～4 times, in washing lotion without NaAlO
2, obtain platinum group metal filter residue;
E, secondary burning: step D gained platinum group metal filter residue is carried out to secondary burning, be less than 1% to platinum group metal filter residue containing charcoal and obtain platinum metals enrichment slag.
Incineration temperature in steps A is 600～700 DEG C.
Reductive agent in step C is hydration callosity, sodium formiate or ferrous sulfate, preferably uses sodium formiate.
Incineration temperature in step e is 600～700 DEG C
.
The present invention pressurize alkaline solution dissolve Al
2o
3carrier, in airtight autoclave, charging capacity is the capacity of 50% reactor, adopts periodical operation, heating, along with the rising of temperature, the pressure in still can increase, alkali dissolution Al
2o
3the speed of carrier can be accelerated.Alkali dissolved under pressure carrier A l
2o
3reaction see (1) formula.Al
2o
3+ 2NaOH → 2NaAlO
2,owing to can carrying a small amount of SiO at spent catalyst secretly during in collection process
2impurity, alkali can dissolve SiO
2generate the Na of solubility
2siO
3, obtain platinum metals enrichment slag content high.
Alkali is larger to the corrodibility of platinum, palladium, because platinum is distributed in Al active ingredient with fines
2o
3carrier surface, active good, more easily by alkali dissolution, so in the molten process of pressurization alkali, the sodium formiate of interpolation 5～10 ‰, as reductive agent, suppresses platinum metals and enters dissolving, improves the rate of recovery of platinum metals.
beneficial effect of the present invention:
1, to adapt to material scope wide in the present invention: the molten support methods of pressurization alkali adapts to various crystal formation alumina supporter spent catalyst, can process solvable crystal formation γ-Al
2o
3the spent catalyst of carrier, also can process soluble crystal formation θ-Al
2o
3, δ-Al
2o
3and α-Al
2o
3the spent catalyst of carrier.
2, to dissolve carrier effective in the present invention: alumina dissolution rate is greater than 95%.
3, platinum metals of the present invention enrichment is doubly high: 80～120 times of platinum metals enrichments, concentration effect is good.
4, in enrichment slag of the present invention, platinum metals content is high: in slag, in platinum metals content 10～40% scopes, be conducive to postorder Refining of Platinum Metals.
5, platinum metals of the present invention is reclaimed high: in process of enriching, the rate of recovery of platinum metals is greater than 99%.
6, present device corrosion is low: alkali is little to equipment corrosion, and equipment material requires low, is easy to realize industrialization.
Brief description of the drawings
Fig. 1 is process flow diagram of the present invention.
Specific embodiment
embodiment 1
As shown in Figure 1, a kind of from alumina base spent catalyst the method for enrichment platinum metals, comprise the following steps:
A, once burning: platiniferous alumina base spent catalyst is burned at 600 DEG C, contain charcoal to catalyzer and be less than 1%;
B, pulverizing: the spent catalyst after steps A gained is made charcoal is milled to 70 orders;
C, pressurization alkali molten: the alumina base spent catalyst 500g that step B gained is crushed, platinum content is 2059g/T, add 28% NaOH solution 1000g, then add the hydration callosity of 2.5g, put into stainless steel autoclave, in 2 hours, be warming up to 140 DEG C, pressure 0.3MPa, constant temperature, constant voltage, after 2.5 hours, were warmed up to 190 DEG C at 1.5 hours, pressure is 1.2MPa, constant temperature 2 hours;
D, filtration: by step C gained solution, 130 DEG C of filtrations, filter residue 9.55g uses 80 DEG C of hot washes of 47.75g at every turn, wash 3～4 times, with hydrochloric acid check in washing lotion without NaAlO
2, in filtrate, platinum content is 0.0001g/L, in dissolution process, platinum scatter coefficient 0.12%, obtains filter residue;
E, secondary burning: step D gained filter residue is carried out to secondary burning at 600 DEG C, be less than 1% to filter residue containing charcoal and obtain platinum metals slag, platinum enrichment slag 4.53g, platinum content is 22.61%, 110.3 times of enrichments, in enrichment process, the platinum rate of recovery is 99.49%.
embodiment 2
A method for enrichment platinum metals from alumina base spent catalyst, comprises the following steps:
A, once burning: platiniferous alumina base spent catalyst is burned at 620 DEG C, contain charcoal to catalyzer and be less than 1%;
B, pulverizing: the spent catalyst after steps A gained is made charcoal is milled to 75 orders;
C, pressurization alkali molten: the alumina base spent catalyst 500g that step B gained is crushed, platinum content is 2172g/T, add 30% NaOH solution 1000g, then add 3g sodium formiate, put into stainless steel autoclave, in 2 hours, be warming up to 135 DEG C, pressure 0.3MPa, constant temperature, constant voltage 2.5 hours, be warmed up to 190 DEG C at 1 hour, pressure is 1.3MPa, constant temperature 2.5 hours;
D, filtration: by step C gained solution, 130 DEG C of filtrations, filter residue 10.85g uses 80 DEG C of hot washes of 65.1g at every turn, wash 3～4 times, with hydrochloric acid check in washing lotion without NaAlO
2, in filtrate, platinum content is less than 0.0001g/L, and in dissolution process, platinum scatter coefficient 0.13%, obtains filter residue;
E, secondary burning: step D gained filter residue is carried out to secondary burning at 620 DEG C, be less than 1% to filter residue containing charcoal and obtain platinum metals slag, platinum enrichment slag 5.83g, platinum content is 18.52%, 85.8 times of enrichments, in enrichment process, the platinum rate of recovery is 99.42%.
embodiment 3
A method for enrichment platinum metals from alumina base spent catalyst, comprises the following steps:
A, once burning: will burn at 650 DEG C containing palladium alumina base spent catalyst, and contain charcoal to catalyzer and be less than 1%;
B, pulverizing: the spent catalyst after steps A gained is made charcoal is milled to 80 orders;
C, pressurization alkali molten: the alumina base spent catalyst 500g that step B gained is crushed, palladium content is 2979g/T, add 30% NaOH solution 1250g, then add 4g sodium formiate, put into stainless steel autoclave, in 2 hours, be warming up to 130 DEG C, pressure 0.4MPa, constant temperature, constant voltage 2 hours, be warmed up to 195 DEG C at 1 hour, pressure is 1.4MPa, constant temperature 3 hours;
D, filtration: by step C gained solution, 135 DEG C of filtrations, filter residue 10.9g uses 85 DEG C of hot washes of 87.2g at every turn, wash 3～4 times, with hydrochloric acid check in washing lotion without NaAlO
2, in filtrate, palladium content is 0.0005g/L, in dissolution process, palladium scatter coefficient 0.16%, obtains filter residue;
E, secondary burning: step D gained filter residue is carried out to secondary burning at 650 DEG C, be less than 1% to filter residue containing charcoal and obtain platinum metals slag, palladium enrichment slag 5.86g, palladium content is 25.29%, 85.3 times of enrichments, in enrichment process, palladium recovery rate is 99.50%.
embodiment 4
A method for enrichment platinum metals from alumina base spent catalyst, comprises the following steps:
A, once burning: will burn at 680 DEG C containing palladium alumina base spent catalyst, and contain charcoal to catalyzer and be less than 1%;
B, pulverizing: the spent catalyst after steps A gained is made charcoal is milled to 85 orders;
C, pressurization alkali molten: the alumina base spent catalyst 500g that step B gained is crushed, palladium content is 1536g/T, add 32% NaOH solution 1500g, then add 4.5g sodium formiate, put into stainless steel autoclave, in 2 hours, be warming up to 125 DEG C, pressure 0.4MPa, constant temperature, constant voltage 1.5 hours, be warmed up to 200 DEG C at 1 hour, pressure is 1.6 MPa, constant temperature 3.5 hours;
D, filtration: by step C gained solution, 140 DEG C of filtrations, filter residue 9.3g uses 80 DEG C of hot washes of 83.7g at every turn, wash 3～4 times, with hydrochloric acid check in washing lotion without NaAlO
2, in filtrate, palladium content is 0.0005g/L, in dissolution process, palladium scatter coefficient 0.18%, obtains filter residue;
E, secondary burning: step D gained filter residue is carried out to secondary burning at 680 DEG C, be less than 1% to filter residue containing charcoal and obtain platinum metals slag, palladium enrichment slag 4.26g, palladium content is 17.9%, 117.4 times of enrichments, in enrichment process, palladium recovery rate is 99.29%.
embodiment 5
A method for enrichment platinum metals from alumina base spent catalyst, comprises the following steps:
A, once burning: will burn at 7000 DEG C containing palladium alumina base spent catalyst, and contain charcoal to catalyzer and be less than 1%;
B, pulverizing: the spent catalyst after steps A gained is made charcoal is milled to 90 orders;
C, pressurization alkali molten: the alumina base spent catalyst 500g that step B gained is crushed, palladium content is 2566g/T, add 32% NaOH solution 1500g, then add 5g ferrous sulfate, put into stainless steel autoclave, in 2 hours, be warming up to 120 DEG C, pressure 0.5MPa, constant temperature, constant voltage 1.5 hours, be warmed up to 200 DEG C at 0.5 hour, pressure is 1.6 MPa, constant temperature 4 hours;
D, filtration: by step C gained solution, 140 DEG C of filtrations, filter residue 11g uses 80 DEG C of hot washes of 110g at every turn, wash 3～4 times, with hydrochloric acid check in washing lotion without NaAlO
2, in filtrate, palladium content is 0.0005g/L, in dissolution process, palladium scatter coefficient 0.15%, obtains filter residue;
E, secondary burning: step D gained filter residue is carried out to secondary burning at 680 DEG C, be less than 1% to filter residue containing charcoal and obtain platinum metals slag, palladium enrichment slag 5.98g, palladium content is 21.30%, 83.6 times of enrichments, in enrichment process, palladium recovery rate is 99.28%.
Claims (5)
1. a method for enrichment platinum metals from alumina base spent catalyst, is characterized in that, comprises the following steps:
A, once burning: the alumina base spent catalyst of platinum group metal is burned, contain charcoal to catalyzer and be less than 1%;
B, pulverizing: the spent catalyst after steps A gained is made charcoal is milled to 70～90 orders;
C, pressurization alkali molten: the alumina base spent catalyst that step B gained is crushed, add the NaOH solution of 28-32%, NaOH solution and alumina base spent catalyst weight ratio are 2～3: 1, the reductive agent that adds again alumina base spent catalyst weight 5-10 ‰ was warming up to 120～140 DEG C, pressure 0.3～0.5MPa in 2 hours, constant temperature, constant voltage 1.5～2.5 hours, be warmed up to 190～200 DEG C at 0.5-1.5 hour, pressure is 1.2～1.6MPa, constant temperature 2～4 hours; Described reductive agent is a kind of in hydration callosity, sodium formiate or ferrous sulfate;
D, filtration: by step C gained solution, 130～140 DEG C of filtrations, filter residue is used 80 DEG C of hot washes of 5～10 times of amounts of filter residue weight at every turn, wash 3～4 times, in washing lotion without NaAlO
2, obtain platinum group metal filter residue;
E, secondary burning: step D gained platinum group metal filter residue is carried out to secondary burning, be less than 1% to platinum group metal filter residue containing charcoal and obtain platinum metals enrichment slag.
According to claim 1 a kind of from alumina base spent catalyst the method for enrichment platinum metals, it is characterized in that, comprise the following steps:
A, once burning: the alumina base spent catalyst of platinum group metal is burned, contain charcoal to catalyzer and be less than 1%;
B, pulverizing: the spent catalyst after steps A gained is made charcoal is milled to 80 orders;
C, pressurization alkali molten: the alumina base spent catalyst that step B gained is crushed, add 30% NaOH solution, NaOH solution and alumina base spent catalyst weight ratio are 2.5: 1, add again the reductive agent of alumina base spent catalyst weight 8 ‰, in 2 hours, be warming up to 130 DEG C, pressure 0.4MPa, constant temperature, constant voltage 2 hours, be warmed up to 195 DEG C at 1 hour, pressure is 1.4MPa, constant temperature 3 hours;
D, filtration: by step C gained solution, 135 DEG C of filtrations, filter residue is used 80 DEG C of hot washes of 8 times of amounts of filter residue weight at every turn, wash 3～4 times, in washing lotion without NaAlO
2, obtain platinum group metal filter residue;
E, secondary burning: step D gained platinum group metal filter residue is carried out to secondary burning, be less than 1% to platinum group metal filter residue containing charcoal and obtain platinum metals enrichment slag.
According to claim 1 and 2 a kind of from alumina base spent catalyst the method for enrichment platinum metals, it is characterized in that, the incineration temperature in described steps A is 600～700 DEG C.
According to claim 1 and 2 a kind of from alumina base spent catalyst the method for enrichment platinum metals, it is characterized in that, the incineration temperature in described step e is 600～700 DEG C
.
According to claim 3 a kind of from alumina base spent catalyst the method for enrichment platinum metals, it is characterized in that, the incineration temperature in described step e is 600～700 DEG C
.
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| CN104342557A (en) * | 2013-10-22 | 2015-02-11 | 上海派特贵金属环保科技有限公司 | Method for recovering platinum from waste catalyst |
| CN106153602A (en) * | 2016-02-29 | 2016-11-23 | 永兴贵研资源有限公司 | A kind of gathering and measuring method of platinum, palladium, rhodium in auto-exhaust catalyst and process slag |
| CN108707751A (en) * | 2018-06-20 | 2018-10-26 | 贵研资源（易门）有限公司 | A kind of restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid |
| CN110627099B (en) * | 2019-11-06 | 2021-09-17 | 山东聚杰环保科技有限公司 | Method for preparing high-purity aluminum sulfate and co-producing poly-silicon ferric aluminum sulfate by using waste catalyst |
| CN111411240A (en) * | 2020-04-23 | 2020-07-14 | 贺利氏贵金属技术(中国)有限公司 | Method for recovering noble metal from waste catalyst containing noble metal |
| CN113234931A (en) * | 2021-05-14 | 2021-08-10 | 昆明理工大学 | Failure Pt/Al2O3Method for comprehensively recovering platinum and aluminum from catalyst |
| CN113293301B (en) * | 2021-05-21 | 2022-05-03 | 北京科技大学 | Method for recovering platinum group metals from metal carrier waste automobile exhaust catalyst |
| CN114574708B (en) * | 2022-02-18 | 2024-01-26 | 武汉理工大学 | Method for recovering metal platinum from waste automobile tail gas three-way catalyst |
| CN114892015A (en) * | 2022-05-05 | 2022-08-12 | 昆明贵研新材料科技有限公司 | From useless Al 2 O 3 Method for enriching and recovering precious metals in base precious metal catalyst |
| CN114836629A (en) * | 2022-05-05 | 2022-08-02 | 昆明贵研新材料科技有限公司 | Enrichment method of waste silicon dioxide carrier noble metal catalyst |
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| JPS5415530B2 (en) * | 1973-12-08 | 1979-06-15 | ||
| CN1043250C (en) * | 1995-08-23 | 1999-05-05 | 中国有色金属工业总公司昆明贵金属研究所 | Method and digesting surface for recovering noble metals and aluminium from waste aluminium base catalyst |
| CN101036889B (en) * | 2006-03-14 | 2010-08-04 | 上海耀华铂制品有限公司 | Recycling method of catalyzer having platinum |
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