CN107190147B - A method of selective dissolution recycles platinum from platinum-containing waste catalyst - Google Patents
A method of selective dissolution recycles platinum from platinum-containing waste catalyst Download PDFInfo
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- CN107190147B CN107190147B CN201710383466.8A CN201710383466A CN107190147B CN 107190147 B CN107190147 B CN 107190147B CN 201710383466 A CN201710383466 A CN 201710383466A CN 107190147 B CN107190147 B CN 107190147B
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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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Abstract
The method of the present invention relates to a kind of from aluminium base platinum catalyst selective dissolution recycling platinum.Suitable for recycling platinum from the platinum-containing waste catalyst that carrier is aluminium oxide.Process route is as follows: roasting decarburization → aluminium oxide makes the transition → crushes levigate → inorganic acid oxidation dissolution platinum → Pro-concentration with ion exchange process purifying platinum → platinum precipitating and reduction → spongy platinum product.This method technique is brief, and cost recovery is low, metal high income, and the platinum rate of recovery is greater than 98.5%, spongy platinum purity >=99.95%.
Description
Technical field
The invention belongs to technical field of wet metallurgy, and in particular to one kind selective dissolution from platinum-containing waste catalyst recycles
The method of platinum.
Background technique
Platinum group metal, resource scarcity, the content in the earth's crust only have 0.001-0.01g/t (Pt 0.005g/t), price
Valuableness also has and its important use in addition to extremely important economic value in modern science and technology and industrial development process
On the way.Platinum group metal has excellent catalytic performance.In chemical industry, especially in petro chemical industry, oil-refinery industry, doctor
In medicine and energy industry, the catalyst of platinum group metal such as platinum, palladium is widely used.For platinum, petrochemical industry (reform and
Catalytic pyrolysis), chemical fertilizer industry (synthetic ammonia catalyst) and eliminate the fields such as automobile exhaust pollution and be widely used.In addition, electronics,
The fields such as glass ceramics and military project also have highly important purposes.China platinum group metal lacks, and foreign exchange need to be spent from state every year
Outer import platinum group metal meets the needs of the development of the national economy.Thus, platinum group metal is recycled in continuous improvement from dead catalyst
Engineering and industrialization level, be particularly important.
Platinum is recycled from dead catalyst, there are two kinds of process routes of pyrogenic process and wet process, practical application is based on wet process.It separates pure
Change platinum group metal, the classical precipitation method still account for critical role, and shortcoming is that process is many and diverse tediously long, and metal recovery rate is low；It is molten
Also there are many researchs and report in agent extraction and Strong acid ion-exchanger purifying platinum group metal, but in industrial application, really effectively and
Excellent extractant and ion exchange resin is few.Domestic current solvent extraction technology, operational effect are not sufficiently stable, product quality
Also unstable, higher cost, operating environment is poor.
The technique that the complete molten-R410 resin adsorption of the carrier of the inventions such as Zhang Fangyu, Li Yonghua recycles platinum from dead catalyst
(patent No. ZL94118736.5), the leaching rate and the rate of recovery of platinum are higher, but the complete molten rear solid-liquor separation of carrier is difficult, and leachate needs
With multistage clarify, cause total liquid-solid ratio (> 20V/W) bigger than normal, This reduces both leaching equipment processing capacities, and increase absorption and
The burden of bunkerage, while also adding the pressure of wastewater treatment.The study found that alumina support transition denaturation after, no
Easily by sulfuric acid dissolution, the technique for taking insoluble selective dissolution platinum of carrier leaches liquid-solid ratio and is no more than 6V/W, avoids carrier
The shortcomings that complete molten technique liquid-solid ratio filtration difficulty bigger than normal, the processing capacity of equipment is improved, cost recovery is reduced.
Therefore, a kind of method for needing to research and develop, design the recycling of the selective dissolution from platinum-containing waste catalyst platinum, has solved
State problem.
Summary of the invention
The side of the technical problem to be solved in the present invention is to provide a kind of from platinum-containing waste catalyst selective dissolution recycling platinum
Method reduces cost recovery to improve the processing capacity of equipment.
In order to realize the purpose, the technical solution adopted by the present invention is that:
A method of selective dissolution recycles platinum from platinum-containing waste catalyst comprising the steps of:
1. platinum-containing waste catalyst is roasted first；
Above-mentioned platinum-containing waste catalyst is the Pt-Al containing Pt0.05~0.30wt.%2O3Dead catalyst, Al therein2O3For
γ-Al2O3；
After being fired processing, organic matter and carbon distribution are removed, while by catalyst carrier γ-Al2O3It is transformed into α-Al2O3；
2. the alumina support after roasting transition is carried out pulverizing and jevigating；
3. levigate alumina support is carried out inorganic acid oxidation dissolution platinum, platiniferous lysate is obtained, adjusts acidity with alkali
To 0.1~3.0mol/L；
4. being adsorbed platiniferous lysate by R410 resin column to be carried out to platinum with the 20~80ml/h of flow velocity set
Enrichment and purifying, obtain the R410 resin column of adsorption saturation；
5. the R410 resin column of adsorption saturation to be carried out to the elution of platinum, platinum leacheate is obtained；
6. Production of Ammonium Chloride ammonium chloroplatinate precipitate is added in the high-concentration platinum leacheate of Pt concentration > 8g/L；
The return of Pt concentration≤8g/L high-concentration platinum leacheate continues as eluent return step 5., to elute next
It is saturated R410 resin column；
7. 6. ammonium chloroplatinate precipitate that step obtains is sized mixing with 60 DEG C or more hot water, reducing agent reduction is added, obtains sea
Continuous platinum product.
Further, the method for a kind of recycling of the selective dissolution from platinum-containing waste catalyst platinum as described above, step is 1.
In, maturing temperature is 300 DEG C~1200 DEG C, and calcining time is 2~8h.
Further, the method for a kind of recycling of the selective dissolution from platinum-containing waste catalyst platinum as described above, step is 2.
In, alumina support carry out pulverizing and jevigating, it is levigate after granularity be 60~300 mesh.
Further, the method for a kind of recycling of the selective dissolution from platinum-containing waste catalyst platinum as described above, step is 3.
In, the inorganic acid that selective dissolution platinum uses is one or both of hydrochloric acid, sulfuric acid, and solid NaCl and liquid is added
NaClO3Selective dissolution platinum, initial acidity are 0.5~4mol/L, and liquid-solid ratio is that 2/1~10/1, NaCl additional amount is useless for platiniferous
2~20%, NaClO of catalyst raw material weight3Dosage is 1~10%, NaClO of platinum-containing waste catalyst raw material weight3It is made into 50
~100g/L solution, is slowly continuously added to, adds in 3h.
Further, the method for a kind of recycling of the selective dissolution from platinum-containing waste catalyst platinum as described above, step is 3.
In, solution temperature is 40 DEG C~100 DEG C, and the reaction time is 2~8h.
Further, the method for a kind of recycling of the selective dissolution from platinum-containing waste catalyst platinum as described above, step is 4.
In, the time of contact for adsorbing platinum is 5~50min, adsorb the acidity of stoste by add sulfuric acid or sodium hydroxide be adjusted to 0.1~
3mol/L, adsorption temp are 10~50 DEG C.
Further, the method for a kind of recycling of the selective dissolution from platinum-containing waste catalyst platinum as described above, step is 5.
In, the platinum on resin is eluted as eluent using perchloric acid, eluent mass concentration is 5~30%, elutes time of contact
For 10~100min, temperature is 20 DEG C~60 DEG C；
After the completion of absorption, 10 bed volumes are washed with distilled water, the perchloric acid elution 10 for being then 10% with mass concentration
A bed volume.
Further, the method for a kind of recycling of the selective dissolution from platinum-containing waste catalyst platinum as described above, step is 6.
In, analytically pure ammonium chloride is used, ammonium chloride dosage is 1~5 times that determining theoretical amount is calculated according to reaction equation,
Precipitation temperature is 10~50 DEG C, and the sedimentation time is 2~20h.
Further, the method for a kind of recycling of the selective dissolution from platinum-containing waste catalyst platinum as described above, step is 7.
In, used reducing agent is to analyze pure hydrazine hydrate, and dosage is 1~5 times that determining theoretical amount is calculated according to reaction equation,
Reduction temperature is 50~100 DEG C, and the time is 1~5h.
Compared with the conventional method, process flow is short, equipment is simple, the amount of solution of dead catalyst output for technical solution of the present invention
Less, adsorption tail liquid can return to leaching.Specific beneficial effect is:
1, it takes high-temperature roasting to make the transition, not only eliminates carbon distribution and organic matter, but also realize the transition of aluminium oxide, so that aluminium is not
It is leached and achievees the purpose that selective dissolution platinum.
2, adsorb platinum after tail washings, after adding number acid and oxidant, return as leaching agent use, realize waste water recycling without
Outlet.
3, using selective dissolution-R410 resin absorption technique, short flow, equipment is simple, and the rate of recovery is high, and product is pure
Degree is high.
Specific embodiment
Technical solution of the present invention is described in detail combined with specific embodiments below.
A kind of method of the recycling of the selective dissolution from platinum-containing waste catalyst platinum of the present invention comprising the steps of:
1. platinum-containing waste catalyst is roasted first；Maturing temperature is 300 DEG C~1200 DEG C, and calcining time is 2~8h.
Above-mentioned platinum-containing waste catalyst is the Pt-Al containing Pt0.05~0.30wt.%2O3Dead catalyst, Al therein2O3For
γ-Al2O3；
After being fired processing, organic matter and carbon distribution are removed, while by catalyst carrier γ-Al2O3It is transformed into α-Al2O3；
2. will roasting transition after alumina support carry out pulverizing and jevigating, it is levigate after granularity be 60~300 mesh.
3. levigate alumina support is carried out inorganic acid oxidation dissolution platinum, platiniferous lysate is obtained, adjusts acidity with alkali
To 0.1~3.0mol/L；
The inorganic acid that selective dissolution platinum uses is one or both of hydrochloric acid, sulfuric acid, and solid NaCl and liquid is added
Body NaClO3Selective dissolution platinum, initial acidity are 0.5~4mol/L, and liquid-solid ratio is that 2/1~10/1, NaCl additional amount is platiniferous
2~20%, NaClO of dead catalyst raw material weight3Dosage is 1~10%, NaClO of platinum-containing waste catalyst raw material weight3It is made into
50~100g/L solution, is slowly continuously added to, and adds in 3h.Solution temperature is 40 DEG C~100 DEG C, and the reaction time is 2~8h.
4. being adsorbed platiniferous lysate by R410 resin column to be carried out to platinum with the 20~80ml/h of flow velocity set
Enrichment and purifying, obtain the R410 resin column of adsorption saturation；
The time of contact for adsorbing platinum is 5~50min, adsorbs the acidity of stoste by adding sulfuric acid or sodium hydroxide to be adjusted to
0.1~3mol/L, adsorption temp are 10~50 DEG C.
5. the R410 resin column of adsorption saturation to be carried out to the elution of platinum, platinum leacheate is obtained；
In the present embodiment, the platinum on resin is eluted as eluent using perchloric acid, eluent mass concentration is 5~
30%, elution time of contact is 10~100min, and temperature is 20 DEG C~60 DEG C；After the completion of absorption, it is washed with distilled water 10 beds
Then volume elutes 10 bed volumes with the perchloric acid that mass concentration is 10%.
6. Production of Ammonium Chloride ammonium chloroplatinate precipitate is added in the high-concentration platinum leacheate of Pt concentration > 8g/L；
The return of Pt concentration≤8g/L high-concentration platinum leacheate continues as eluent return step 5., to elute next
It is saturated R410 resin column；
In the present embodiment, analytically pure ammonium chloride is used, ammonium chloride dosage is to calculate really according to reaction equation
1~5 times of fixed theoretical amount, precipitation temperature are 10~50 DEG C, and the sedimentation time is 2~20h.
7. 6. ammonium chloroplatinate precipitate that step obtains is sized mixing with 60 DEG C or more hot water, reducing agent reduction is added, obtains sea
Continuous platinum product.
In the present embodiment, used reducing agent is to analyze pure hydrazine hydrate, and dosage is to be calculated really according to reaction equation
1~5 times of fixed theoretical amount, reduction temperature are 50~100 DEG C, and the time is 1~5h.
According to operating procedure disclosed by the invention and related parameter, those skilled in the art can be according to the operation of this method
Principle achieves the object of the present invention, and is not limited to using equipment used in specific embodiment itself and its usage mode.
Specific embodiment is as follows:
Embodiment one
Pt-Al containing Pt0.28%2O3Dead catalyst 100g, roasts 4h at 1200 DEG C, and pulverizing and jevigating to 300 mesh will be ground
50ml hydrochloric acid, 100ml sulfuric acid, 10gNaCl, 10gNaClO is added in thin alumina powder3, water 800ml, stirred at 70 DEG C anti-
6h is answered, 1000ml leachate is obtained by filtration, contains Pt277.2mg/L, Pt leaching rate is 99.0%.
After leachate adjusts acidity to 0.2mol/L with alkali, with the flow of 60ml/h, by the R410 resin that 50ml is housed
Column is adsorbed, and adsorption tail liquid contains Pt0.2mg/L, and Pt adsorption rate is 99.9%.
After the completion of absorption, 10 bed volumes are washed with distilled water, then 10 bed volumes is eluted with 10% H acid, obtains
500ml leacheate, contains Pt552.6mg/L, and Pt washout rate is 99.4%.
In terms of platinum content in leacheate, the platinum rate of recovery is 98.7%.
Embodiment two
Pt-Al containing Pt0.28%2O3Dead catalyst 10kg, roasts 6h at 700 DEG C, and pulverizing and jevigating to 200 mesh will be ground
10L hydrochloric acid, 5L sulfuric acid, 1kgNaCl, 1kgNaClO is added in thin alumina powder3, water 65L, 60 in 100L enamel reaction still
It is stirred to react 6h at DEG C, 85L leachate is obtained by filtration, contains Pt327.1mg/L, Pt leaching rate is 99.3%.
After leachate adjusts acidity to 1.8mol/L with alkali, with the flow of 900ml/h, by the R410 tree that 500ml is housed
Rouge column is adsorbed, and adsorption tail liquid contains Pt0.2mg/L, and Pt adsorption rate is 99.9%.
After the completion of absorption, 15 bed volumes are washed with distilled water, then 15 bed volumes is eluted with 15% H acid, obtains
The low concentration leacheate of high concentration leacheate and 5000ml of the 2500ml containing Pt8.2g/L containing Pt1.42g/L, Pt washout rate are
99.3%.
Eluent is used as in the return of low concentration leacheate.High concentration leacheate is precipitated and is restored down carry out spongy platinum
Preparation, obtain spongy platinum product 20.55g, purity is greater than 99.95%, and impurity meets national standard and middle petrochemical industry standard.
20.55g platinum product adds the 7.1g amount of metal in low concentration leacheate, and the platinum rate of recovery is 98.7%.
Claims (1)
1. a kind of method of the recycling of the selective dissolution from platinum-containing waste catalyst platinum, which is characterized in that comprise the steps of:
1. platinum-containing waste catalyst is roasted first；
Above-mentioned platinum-containing waste catalyst is the Pt-Al containing Pt0.05~0.30wt.%2O3Dead catalyst, Al therein2O3For γ-
Al2O3；
After being fired processing, organic matter and carbon distribution are removed, while by catalyst carrier γ-Al2O3It is transformed into α-Al2O3；
2. the alumina support after roasting transition is carried out pulverizing and jevigating；
3. levigate alumina support is carried out inorganic acid oxidation dissolution platinum, platiniferous lysate is obtained, adjusts acidity to 0.1 with alkali
~3.0mol/L；
4. being adsorbed platiniferous lysate by R410 resin column to be enriched with to platinum with the 20~80ml/h of flow velocity set
With purifying, the R410 resin column of adsorption saturation is obtained；
5. the R410 resin column of adsorption saturation to be carried out to the elution of platinum, platinum leacheate is obtained；
6. Production of Ammonium Chloride ammonium chloroplatinate precipitate is added in the high-concentration platinum leacheate of Pt concentration > 8g/L；
The return of Pt concentration≤8g/L low concentration platinum leacheate continues as eluent return step 5., to elute next saturation
R410 resin column；
7. 6. ammonium chloroplatinate precipitate that step obtains is sized mixing with 60 DEG C or more hot water, reducing agent reduction is added, obtains spongy platinum
Product；
Step 1. in, maturing temperature be 300 DEG C~1200 DEG C, calcining time be 2~8h；
Step 2. in, alumina support carry out pulverizing and jevigating, it is levigate after granularity be 60~300 mesh；
Step 3. in, inorganic acid that selective dissolution platinum uses is one or both of hydrochloric acid, sulfuric acid, and solid NaCl is added
And liquid NaClO3Selective dissolution platinum, initial acidity are 0.5~4mol/L, and liquid-solid ratio is that 2/1~10/1, NaCl additional amount is
2~20%, NaClO of platinum-containing waste catalyst raw material weight3Dosage is 1~10%, NaClO of platinum-containing waste catalyst raw material weight3
It is made into 50~100g/L solution, is slowly continuously added to, is added in 3h；Step 3. in, solution temperature be 40 DEG C~100 DEG C, instead
It is 2~8h between seasonable；
Step 4. in, adsorb platinum time of contact be 5~50min, adsorb the acidity of stoste by adding sulfuric acid or sodium hydroxide tune
Whole is 0.1~3mol/L, and adsorption temp is 10~50 DEG C；
Step 5. in, elute the platinum on resin as eluent using perchloric acid, eluent mass concentration is 5~30%, leaching
Washing time of contact is 10~100min, and temperature is 20 DEG C~60 DEG C；
After the completion of absorption, 10 bed volumes are washed with distilled water, then elute 10 beds with the perchloric acid that mass concentration is 10%
Volume；
Step 6. in, use analytically pure ammonium chloride, ammonium chloride dosage is that determining theory is calculated according to reaction equation
1~5 times of amount, precipitation temperature are 10~50 DEG C, and the sedimentation time is 2~20h；
Step 7. in, used reducing agent is to analyze pure hydrazine hydrate, and dosage is that determining theory is calculated according to reaction equation
1~5 times of amount, reduction temperature are 50~100 DEG C, and the time is 1~5h.
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| CN108315564A (en) * | 2017-12-28 | 2018-07-24 | 核工业北京化工冶金研究院 | The method that a kind of molten carrier recycles platinum from aluminium-based catalyst |
| CN112322900B (en) * | 2020-10-30 | 2023-01-24 | 格林美股份有限公司 | Method for extracting platinum, palladium and rhodium from automobile exhaust waste catalyst |
| CN115275241A (en) * | 2022-08-03 | 2022-11-01 | 湖南理工学院 | Method for recycling waste platinum catalyst |
| CN117587246B (en) * | 2023-11-30 | 2024-05-14 | 横峰县凯怡实业有限公司 | Method for recovering platinum from waste platinum tin alumina catalyst |
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| CN1067926A (en) * | 1991-06-24 | 1993-01-13 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovering platinum from waste catalyst |
| CN1123843A (en) * | 1994-11-30 | 1996-06-05 | 核工业北京化工冶金研究院 | Recovery of platinum family elements from waste catalysts |
| CN103131857A (en) * | 2011-11-29 | 2013-06-05 | 沈阳有色金属研究院 | Method for purifying platinum group metal from waste three-way catalyst |
| 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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- 2017-05-26 CN CN201710383466.8A patent/CN107190147B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1067926A (en) * | 1991-06-24 | 1993-01-13 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovering platinum from waste catalyst |
| CN1123843A (en) * | 1994-11-30 | 1996-06-05 | 核工业北京化工冶金研究院 | Recovery of platinum family elements from waste catalysts |
| CN103131857A (en) * | 2011-11-29 | 2013-06-05 | 沈阳有色金属研究院 | Method for purifying platinum group metal from waste three-way catalyst |
| 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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