CN111549226A - Method for recovering nickel, platinum and ruthenium from failed Raney nickel catalyst - Google Patents
Method for recovering nickel, platinum and ruthenium from failed Raney nickel catalyst Download PDFInfo
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- CN111549226A CN111549226A CN202010333718.8A CN202010333718A CN111549226A CN 111549226 A CN111549226 A CN 111549226A CN 202010333718 A CN202010333718 A CN 202010333718A CN 111549226 A CN111549226 A CN 111549226A
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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
- C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
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- 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
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
- C22B11/026—Recovery of noble metals from waste materials from spent catalysts
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention provides a method for recovering nickel, platinum and ruthenium from a failed Raney nickel catalyst, which comprises the following steps: adding sodium carbonate powder into the failed Raney nickel catalyst and then roasting; leaching and filtering to obtain a leaching material and a leaching solution, and discharging the leaching solution to a wastewater treatment system; adding dilute sulfuric acid into the leaching material, heating for leaching, and then carrying out hot filtration to obtain a nickel-removed leaching solution and a precious metal-rich aggregate; adding oxalic acid into the nickel-removing leaching solution to obtain nickel oxalate, and calcining the nickel oxalate at high temperature and reducing the nickel oxalate with hydrogen to obtain nickel powder; the noble metal enrichment material adopts chlorination and refining processes to obtain sponge platinum and sponge ruthenium. The method has simple operation process, all valuable metals are recovered, and the yield of nickel, platinum and ruthenium is over 98 percent.
Description
Technical Field
The invention belongs to the field of metallurgical technology, and relates to a method for recovering nickel, platinum and ruthenium from a failed Raney nickel catalyst.
Background
The raney nickel catalyst mainly comprises nickel-aluminum alloy, and precious metal is loaded on the surface of the raney nickel catalyst, so that the raney nickel catalyst is widely applied to a plurality of industrial processes and organic synthesis reactions due to strong adsorption, high catalytic performance and high thermal stability to hydrogen. The catalyst used for a certain period often loses the catalytic action, and a large petrochemical enterprise can produce dozens of tons of the catalyst every year. Because of high nickel content and single type of other main impurity elements, if the nickel is not recycled, the method not only pollutes the environment, but also wastes precious resources.
The common treatment of spent raney nickel catalysts is to leach the aluminum with a strong base under certain conditions and then extract the nickel or nickel salt product.
Such as: chinese patent CN106834702A discloses a method for producing nickel salt by using waste Raney nickel catalyst, which comprises the steps of magnetic separation of waste Raney catalyst, washing of waste catalyst by using trisodium phosphate and sodium dodecyl benzene sulfonate aqueous solution, alkali liquor soaking to remove aluminum and silicon, aqua regia dissolution, hydrogen peroxide oxidation and pH adjustment to remove impurities, sodium carbonate nickel precipitation and acid dissolution, etc. to obtain nickel salt product. The method has a complex process flow, and the precious metals in the catalyst are not recycled, so that the waste of resources is caused.
Such as: chinese patent CN87101713B is a method for recovering nickel carbonyl from waste raney nickel catalyst, which comprises washing, drying, reducing and extracting nickel carbonyl from waste catalyst. The method only recovers nickel in the Raney nickel catalyst, and the produced hydroxyl nickel has higher impurity element content.
Disclosure of Invention
Aiming at the defects and shortcomings of the existing invalid Raney nickel catalyst treatment technology, the invention provides a method for recovering nickel, platinum and ruthenium from the invalid Raney nickel catalyst, which has high extraction efficiency and simple flow and can completely recover valuable metals.
The technical scheme adopted by the invention for solving the problems is as follows:
a method for recovering nickel, platinum and ruthenium from a spent raney nickel catalyst, comprising the steps of:
step (1): adding sodium carbonate powder into the failed Raney nickel catalyst, uniformly mixing to obtain a mixed material, and roasting the mixed material in a resistance furnace;
step (2): adding pure water into the mixture roasted in the step (1), heating and soaking the mixture added with the pure water, filtering and washing to obtain a leachate and a leaching material, and discharging the leachate to a wastewater treatment system;
and (3): adding dilute sulfuric acid into the leaching material obtained in the step (2), heating and leaching the leaching material added with the dilute sulfuric acid, and then carrying out hot filtration to obtain a nickel-removing leaching solution and a precious metal-rich aggregate;
and (4): adding oxalic acid into the nickel-removing leaching solution obtained in the step (3) to obtain nickel oxalate, and calcining the nickel oxalate at high temperature and reducing the nickel oxalate with hydrogen to obtain nickel powder;
and (5): and (4) performing chlorination and refining processes on the noble metal enriched material obtained in the step (3) to obtain sponge platinum and sponge ruthenium.
The method for recovering nickel, platinum and ruthenium from the failed Raney nickel catalyst is characterized in that the mass of the sodium carbonate powder added in the step (1) is 4-5 times of the aluminum content in the failed Raney nickel catalyst; the technological conditions for placing the mixed material into a resistance furnace for roasting are as follows: the roasting temperature is 800-900 ℃, and the roasting time is 1-2 h.
The method for recovering nickel, platinum and ruthenium from the failed Raney nickel catalyst is characterized in that the process conditions of heating and water leaching of the mixed material added with pure water in the step (2) are as follows: the water immersion temperature is 50-60 ℃, and the water immersion time is 2-3 h.
The method for recovering nickel, platinum and ruthenium from the failed Raney nickel catalyst is characterized in that 4-5 mol of dilute sulfuric acid is added into the leaching material in the step (3); the process conditions for heating and leaching the leaching material added with the dilute sulfuric acid are as follows: the leaching temperature is 85-95 ℃, and the leaching time is 4-6 h.
According to the method for recovering nickel, platinum and ruthenium from the failed Raney nickel catalyst, the method is characterized in that when oxalic acid is added into the nickel-removing leaching solution in the step (4), the mass of the oxalic acid added is 1.2-1.5 times of the nickel content in the nickel-removing leaching solution; the technological conditions of nickel oxalate through high-temperature calcination and hydrogen reduction to produce nickel powder are as follows: the calcining temperature is 1200-1500 ℃, the hydrogen reduction temperature is 350-450 ℃, and the hydrogen flow is 20-30L/h.
Compared with the prior art, the invention has the following beneficial technical effects: the method can comprehensively recover valuable metals in the failed Raney nickel catalyst, thereby effectively reducing the treatment cost of the catalyst; the yield of nickel, platinum and ruthenium can reach more than 95 percent; the method adopts oxalic acid to precipitate nickel, so that the nickel extraction process can be shortened, and the grade of the produced nickel powder reaches more than 98 percent; the whole process is simple to operate, small in occupied area of equipment, low in energy consumption and good in environment.
Drawings
FIG. 1 is a process flow diagram of the method of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and specific examples.
Referring to fig. 1, a method for recovering nickel, platinum and ruthenium from a spent raney nickel catalyst according to the present invention comprises the steps of: step (1): adding sodium carbonate powder into the failed Raney nickel catalyst, uniformly mixing to obtain a mixed material, and roasting the mixed material in a resistance furnace; the mass of the added sodium carbonate powder is 4-5 times of the aluminum content in the failed Raney nickel catalyst; the technological conditions for placing the mixed material into a resistance furnace for roasting are as follows: the roasting temperature is 800-900 ℃, and the roasting time is 1-2 h. Step (2): adding pure water into the mixture roasted in the step (1), heating and soaking the mixture added with the pure water, filtering and washing to obtain a leachate and a leaching material, discharging the leachate to a wastewater treatment system, and reserving the leaching material for later use; the process conditions for heating and water leaching the mixed material added with the pure water are as follows: the water immersion temperature is 50-60 ℃, and the water immersion time is 2-3 h. And (3): adding dilute sulfuric acid into the leaching material obtained in the step (2), heating and leaching the leaching material added with the dilute sulfuric acid, and then carrying out hot filtration to obtain a nickel-removing leaching solution and precious metal-rich aggregate, wherein nickel is leached into the solution to form the nickel-removing leaching solution, and precious metals are enriched to form the precious metal-rich aggregate. 4-5 mol of dilute sulfuric acid is added into the leaching material; the process conditions for heating and leaching the leaching material added with the dilute sulfuric acid are as follows: the leaching temperature is 85-95 ℃, and the leaching time is 4-6 h. And (4): adding oxalic acid into the nickel-removing leaching solution obtained in the step (3), precipitating to produce nickel oxalate, and calcining the nickel oxalate at high temperature and reducing the nickel oxalate with hydrogen to produce nickel powder; when oxalic acid is added into the nickel-removing leaching solution, the mass of the added oxalic acid is 1.2-1.5 times of the nickel content in the nickel-removing leaching solution; the technological conditions of nickel oxalate through high-temperature calcination and hydrogen reduction to produce nickel powder are as follows: the calcining temperature is 1200-1500 ℃, the hydrogen reduction temperature is 350-450 ℃, and the hydrogen flow is 20-30L/h. And (5): and (4) obtaining sponge platinum and sponge ruthenium from the noble metal enriched material obtained in the step (3) by adopting the existing chlorination and refining processes. By the method, valuable metals in the failed Raney nickel catalyst are all recovered, and the yield of nickel, platinum and ruthenium is over 98 percent.
Example 1
100g of spent Raney nickel catalyst containing 48.58g of nickel, 33mg of platinum, 0.14g of ruthenium and 32.89g of aluminum was taken. Adding 135g of sodium carbonate powder into 100g of failed Raney nickel catalyst, uniformly mixing to obtain a mixed material, adding the mixed material into a clay crucible, and then placing the clay crucible into a resistance furnace for roasting, wherein the roasting process conditions are as follows: roasting at 800 deg.c for 1 hr, and naturally cooling. Transferring the cooled mixed material into a beaker, and adding pure water, wherein the liquid-solid mass ratio of the pure water to the cooled mixed material is 5: 1, heating the mixed material added with pure water to 50 ℃, soaking in water for 2h, sequentially filtering and washing to obtain leachate and 62.1g of leaching material, and discharging the leachate to a wastewater treatment system. Adding 350mL of 4mol dilute sulfuric acid into the leaching material, heating the leaching material added with the dilute sulfuric acid to 85 ℃, continuously stirring and replenishing water, leaching for 4 hours, and then filtering and washing to obtain 520mL of nickel-removing leaching solution and 14.7g of precious metal-rich aggregate, wherein the nickel content in the nickel-removing leaching solution is 92.23g/L, the platinum content in the leaching residue is 2245g/t, and the ruthenium content in the leaching residue is 0.952%. Adding 57g of oxalic acid into the nickel-removing leaching solution for nickel precipitation to obtain 118.56g of nickel oxalate, calcining the nickel oxalate at 1200 ℃, transferring the calcined nickel oxalate into a quartz boat, and performing hydrogen reduction at 350 ℃ to obtain 47.44g of nickel powder, wherein the grade of the nickel powder is 98.45%. The noble metal-rich aggregate adopts the traditional method to produce 32.09mg of sponge platinum and 0.135g of sponge ruthenium. The direct yield of nickel was 97.65%, the direct yield of platinum was 97.24%, and the direct yield of ruthenium was 96.36%.
Example 2
1kg of spent Raney nickel catalyst was taken, containing 521.6g of nickel, 346mg of platinum, 182g of ruthenium and 305.4g of aluminum. Adding 1.53kg of sodium carbonate powder into 1kg of failed Raney nickel catalyst, uniformly mixing to obtain a mixed material, adding the mixed material into a clay crucible, and then placing the clay crucible into a resistance furnace for roasting, wherein the roasting process conditions are as follows: roasting at 900 deg.c for 2 hr, and naturally cooling. Transferring the cooled mixed material into a beaker, and adding pure water, wherein the liquid-solid mass ratio of the pure water to the cooled mixed material is 5: 1, heating the mixed material added with pure water to 60 ℃, soaking in water for 3h, sequentially filtering and washing to obtain leachate and 0.684kg of leaching material, and discharging the leachate to a wastewater treatment system. Adding 3.5L of 5mol of dilute sulfuric acid into the leaching material, heating the leaching material added with the dilute sulfuric acid to 95 ℃, continuously stirring and replenishing water, leaching for 6 hours, filtering and washing to obtain 4.126L of nickel-removing leaching solution and 0.128kg of precious metal-rich aggregate, wherein the nickel content in the nickel-removing leaching solution is 120.54g/L, the platinum content in the leaching residue is 2617g/t, and the ruthenium content in the leaching residue is 1.367%. Adding 0.597kg of oxalic acid into the nickel-removing leaching solution for nickel precipitation to obtain 1.24kg of nickel oxalate, calcining the nickel oxalate at 1500 ℃, transferring the calcined nickel oxalate into a quartz boat, and performing hydrogen reduction at 450 ℃ to obtain 0.496kg of nickel powder, wherein the grade of the nickel powder is 99.2%. The noble metal-rich aggregate adopts the traditional method to produce 332.9mg of sponge platinum and 0.173kg of sponge ruthenium. The direct yield of nickel was 95.21%, the direct yield of platinum was 96.21%, and the direct yield of ruthenium was 95.05%.
Claims (5)
1. A method for recovering nickel, platinum and ruthenium from a spent raney nickel catalyst, comprising the steps of:
step (1): adding sodium carbonate powder into the failed Raney nickel catalyst, uniformly mixing to obtain a mixed material, and roasting the mixed material in a resistance furnace;
step (2): adding pure water into the mixture roasted in the step (1), heating and soaking the mixture added with the pure water, filtering and washing to obtain a leachate and a leaching material, and discharging the leachate to a wastewater treatment system;
and (3): adding dilute sulfuric acid into the leaching material obtained in the step (2), heating and leaching the leaching material added with the dilute sulfuric acid, and then carrying out hot filtration to obtain a nickel-removing leaching solution and a precious metal-rich aggregate;
and (4): adding oxalic acid into the nickel-removing leaching solution obtained in the step (3) to obtain nickel oxalate, and calcining the nickel oxalate at high temperature and reducing the nickel oxalate with hydrogen to obtain nickel powder;
and (5): and (4) performing chlorination and refining processes on the noble metal enriched material obtained in the step (3) to obtain sponge platinum and sponge ruthenium.
2. The method for recovering nickel, platinum and ruthenium from the spent raney nickel catalyst as claimed in claim 1, wherein the mass of the sodium carbonate powder added in step (1) is 4-5 times of the aluminum content in the spent raney nickel catalyst; the technological conditions for placing the mixed material into a resistance furnace for roasting are as follows: the roasting temperature is 800-900 ℃, and the roasting time is 1-2 h.
3. The method for recovering nickel, platinum and ruthenium from the spent Raney nickel catalyst as claimed in claim 1, wherein the process conditions of heating and water immersion of the mixed material added with pure water in the step (2) are as follows: the water immersion temperature is 50-60 ℃, and the water immersion time is 2-3 h.
4. The method for recovering nickel, platinum and ruthenium from the spent raney nickel catalyst according to claim 1, characterized in that in step (3) 4mol-5mol of dilute sulfuric acid is added to the leaching material; the process conditions for heating and leaching the leaching material added with the dilute sulfuric acid are as follows: the leaching temperature is 85-95 ℃, and the leaching time is 4-6 h.
5. The method for recovering nickel, platinum and ruthenium from a spent raney nickel catalyst according to claim 1, wherein when oxalic acid is added to the nickel-removing leach solution in the step (4), the mass of the oxalic acid added is 1.2 to 1.5 times of the nickel content in the nickel-removing leach solution; the technological conditions of nickel oxalate through high-temperature calcination and hydrogen reduction to produce nickel powder are as follows: the calcining temperature is 1200-1500 ℃, the hydrogen reduction temperature is 350-450 ℃, and the hydrogen flow is 20-30L/h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1769504A (en) * | 2004-11-04 | 2006-05-10 | 日矿金属株式会社 | Method of recovering platinum and rhenium from waste catalyst |
| CN101824540A (en) * | 2009-12-10 | 2010-09-08 | 佛山市邦普镍钴技术有限公司 | Method for separating and reclaiming metal nickel and tin from waste materials containing nickel and tin |
| CN106011477A (en) * | 2016-06-28 | 2016-10-12 | 昆明贵金属研究所 | Method for recycling platinum group metal from ineffective automobile catalysts |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1769504A (en) * | 2004-11-04 | 2006-05-10 | 日矿金属株式会社 | Method of recovering platinum and rhenium from waste catalyst |
| CN101824540A (en) * | 2009-12-10 | 2010-09-08 | 佛山市邦普镍钴技术有限公司 | Method for separating and reclaiming metal nickel and tin from waste materials containing nickel and tin |
| CN106011477A (en) * | 2016-06-28 | 2016-10-12 | 昆明贵金属研究所 | Method for recycling platinum group metal from ineffective automobile catalysts |
Non-Patent Citations (1)
| Title |
|---|
| 费多尔钦科: "《粉末冶金》", 31 May 1974 * |
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