CN103173619A - Method for recovering nickel and tungsten by waste nickel and tungsten catalyst - Google Patents
Method for recovering nickel and tungsten by waste nickel and tungsten catalyst Download PDFInfo
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Abstract
The invention provides a method for recovering nickel and tungsten by a waste nickel and tungsten catalyst. The method comprises the following steps of: first, reducing roasting the waste nickel and tungsten catalyst at a high temperature to reduce nickel and ferric ions in the waste nickel and tungsten catalyst to metals nickel and iron, wherein other oxidants are not reduced; then, adding a copper liquid to the roasted material, replacing metals nickel and iron with copper ions, wherein nickel and iron are in ionic states to enter into the liquid; then, filtering and extracting the replaced and leached liquid; separating nickel from copper and iron, wherein the raffinate obtained by extraction is a pure nickel liquid which can be directly concentrated and crystallized to obtain nickel crystals; mixing the filter residue replaced and leached with sodium carbonate, roasting at a high temperature and washing with hot water to obtain a liquid containing sodium tungstate, wherein the filter residue is used for recovering aluminum and copper; performing acidification to the liquid containing sodium tungstate; and washing and drying the filtered filter residue with hot water to obtain tungstic acid with purity over 98.5%.
Description
Technical field
The present patent application relates to the method that reclaims tungsten and nickel from waste and old nickel tungsten series catalysts, belongs to metal recovery and environmental technology field.
Background technology
Nickel tungsten series catalysts is widely used in hydrofining and hydrocracking, and its main component is the materials such as the silicon-dioxide of aluminum oxide, 5% left and right of nickel oxide, 50% left and right of tungstic oxide, 2% left and right of 25% left and right and a small amount of iron, vanadium.Waste and old nickel tungsten series catalysts contains the metals such as tungsten, nickel, if can recycle, will produce huge economic benefit, has also avoided discarded pollution on the environment and the destruction of nickel tungsten series catalysts simultaneously.
But at present in the open document that discloses, the less report that reclaims metallic nickel and tungsten relevant for nickel tungsten series catalysts, most patent documentations also only relate to metallic nickel in single recovery nickel-containing catalyst or tungsten-containing catalyst or the method and apparatus of tungsten.Also exist the defective that processing step complexity, reaction conditions requirement are high, be unfavorable for cost control in these methods, restricted the development of this art, also be unfavorable for recovery and the utilization of resource, do not meet the megatrend of present energy-conserving and environment-protective.
Summary of the invention
The present patent application is namely for the problems referred to above that exist in present waste and old nickel tungsten series catalysts recycling field, proposes a kind of method of comprehensive reutilization metallic nickel and tungsten, and the method is with low cost, and the rate of recovery is high, is fit to apply.
Specifically, the described waste and old nickel tungsten series catalysts of the present patent application reclaims the method for tungsten nickel, comprises following processing step:
1) reducing roasting: at the temperature of 600～800 ℃, use reductive agent waste and old nickel tungsten series catalysts is carried out roasting, 1～4 hour reaction times, the metal simple-substance that makes nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into nickel and iron, and aluminum oxide, Tungsten oxide 99.999 and silicon-dioxide can not be reduced;
2) displacement is leached: add copper solutions in the product after roasting, metallic nickel and iron and cupric ion generation replacement(metathesis)reaction, becoming nickel ion and iron ion enters in solution, wherein, copper ion concentration is 0.5～3mol/L, the pH value of regulator solution is 1.0～2.0, and temperature of reaction is 60～80 ℃, and extraction time is 2～6 hours;
3) extracting and separating: the solution that will replace after leaching filters, and filtrate being contained the solution of nickel ion and a small amount of iron ion and cupric ion, and the pH value of solution is adjusted to 3.0～4.5, then extracts, and nickel is separated from copper and iron;
4) condensing crystal: in upper step, the raffinate that obtains after extraction is pure nickel solution, and directly condensing crystal obtains the nickel crystal, and strip liquor is the solution that contains cupric ion and iron ion, can return in step 2, is used for obtaining nickel ion and iron ion;
5) high-temperature roasting: with the filter residue mixture of sodium carbonate roasting of displacement leaching in step 2, the roasting temperatures of 500～800 ℃ 2～6 hours, sodium carbonate is 1.2～2.0: 1 with the ratio of the mole number of tungsten, material after roasting is with the hot wash of 60～99 ℃, the solid-liquid mass ratio is 1: 4～12, washing time is 1～3 hour, obtains containing the solution of sodium wolframate, and filter residue is in order to reclaim aluminium and copper;
6) reclaim tungsten: the solution that contains sodium wolframate that step 5 is obtained goes back to adjust pH to 0.5～2.0 with acid, reacted at the temperature of 75～99 ℃ 2～4 hours, the filter residue that obtains after filtration is with the hot wash of 80～99 ℃, the solid-liquid mass ratio is 1: 8～12, filter residue after washing was dried under 80～120 ℃ 2～8 hours, obtained purity and be the wolframic acid more than 98.5%.
Further, in step 1, described reductive agent comprises the common reductive agents such as charcoal or hydrogen, and reductive agent is 1: 0.05～0.2 with the ratio of the total moles of nickel and iron, and take charcoal as example, concrete reaction equation is as follows:
2NiO+C-2Ni+CO
2
2FeO+C-2Fe+CO
2
In step 2, cupric ion (Cu in the copper solutions that adds
2+) the ratio of mole number and the total moles of nickel and iron be 1.2～1.5: 1, copper solutions comprises copper sulfate, cupric chloride or copper nitrate solution, the concrete chemical equation that occurs is as follows:
Ni+Cu
2+-Ni
2++Cu
Fe+Cu
2+-Fe
2++Cu
In step 3, with the pH regulator to 3.0 of solution～4.5, alkaline solution used comprises ammoniacal liquor, sodium hydroxide or potassium hydroxide solution with alkaline solution, and the concentration of alkaline solution is 1～10mol/L.
In addition, in step 3, extraction agent used comprises P204 or P507.
Take P204 as example, mass ratio is that 20～30% P204 mixes 70～80% sulfonated kerosene, saponification degree is 50～75%, and the volume ratio of organic phase and water is 1: 0.5～2, through obtaining raffinate and extraction liquid after 8～10 grades of extractions, 4～6 grades of washings and 4～6 grades of back extractions; Wherein, washings and strip liquor are respectively the acid solution that H+ concentration is 0.5～1.2mol/L and 3～4.5mol/L.
In step 4, the concrete grammar that condensing crystal obtains the nickel crystal is that the degree Beaume that solution containing nickel is evaporated to solution is between 50～55, then through 10～15 hours, makes the nickel solution temperature be reduced between 20～40 ℃, through the separation of 12～24 hours, the solid particulate that obtains was the nickel crystal again.
In step 5, reaction equation is as follows:
WO
3+Na
2CO
3-Na
2WO
4+CO
2
In step 6, the acid that is used for back adjust pH comprises the common acid such as sulfuric acid, hydrochloric acid, and reaction equation is as follows:
WO
4 2-+2H
+-H
2WO
4。
The described method of the present patent application has advantages of following:
1, the rate of recovery is high: through aforesaid method, can obtain purity and reach wolframic acid more than 98.5%;
2, simple process, with low cost: the processing condition of present method and reagent used is easy being easy to get all, is conducive to cost control;
3, the comprehensive reutilization degree is high, and present method can be carried out comprehensive reutilization to metals such as tungsten, nickel and aluminium and copper.
Description of drawings
Accompanying drawing is the process flow diagram of the described method of the present patent application.
Embodiment
Below in conjunction with accompanying drawing and concrete example; the method that the described waste and old nickel tungsten series catalysts of the present patent application is reclaimed tungsten nickel is described and illustrates; purpose is better to understand technology contents of the present invention for the public; rather than to the restriction of described technology contents; under identical or approximate principle, to the improvement that described processing step carries out, comprise that reaction conditions, agents useful for same improve and replace; reach identical purpose, all within the present patent application technical scheme required for protection.
Embodiment one
Described waste and old nickel tungsten series catalysts reclaims the method for tungsten nickel, comprises following processing step:
1. reducing roasting: at the temperature of 600 ℃, use charcoal waste and old nickel tungsten series catalysts is carried out roasting, 4 hours reaction times, the metal simple-substance that makes nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into nickel and iron, and aluminum oxide, Tungsten oxide 99.999, silicon-dioxide can not be reduced, and reacts as follows:
2NiO+C-2Ni+CO
2
2FeO+C-2Fe+CO
2
2. displacement is leached: adding concentration in the product after roasting is the copper-bath of 0.5mol/L, the pH value of solution is adjusted to 1.0～2.0, at the temperature of 80 ℃, extraction time is 2 hours, metallic nickel and iron and cupric ion generation replacement(metathesis)reaction, become nickel ion and iron ion and enter in solution, displacement obtains Ni
2+And Fe
2+The chemical equation that ion occurs is as follows:
Ni+Cu
2+-Ni
2++Cu
Fe+Cu
2+-Fe
2++Cu
3. extracting and separating: the solution that will replace after leaching filters, and filtrate being contained the solution of nickel ion and a small amount of iron ion and cupric ion, and the pH value of solution is adjusted to 3.0, then uses the P204 extracting and separating, and nickel is separated from copper and iron;
4. condensing crystal: in upper step, the raffinate that obtains after extraction is pure nickel solution, the degree Beaume that solution containing nickel is evaporated to solution is 50, through 10 hours, the nickel solution temperature is reduced between 20 ℃ again, through separation in 12 hours, the solid particulate that obtains was the nickel crystal, and strip liquor is the solution that contains cupric ion and iron ion, can return in step 2, be used for obtaining nickel ion and iron ion;
5. high-temperature roasting: with the filter residue mixture of sodium carbonate roasting of displacement leaching in step 2, the roasting temperatures of 500 ℃ 6 hours, sodium carbonate is 1.2: 1 with the ratio of the mole number of tungsten, material after roasting is with the hot wash of 60 ℃, the solid-liquid mass ratio is 1: 4, washing time is 3 hours, obtains containing the solution of sodium wolframate, reacts as follows:
WO
3+Na
2CO
3-Na
2WO
4+CO
2
6. recovery tungsten: the solution that contains sodium wolframate that step 5 is obtained returns adjust pH to 0.5 with sulphuric acid soln, reaction is 4 hours at the temperature of 75 ℃, the filter residue that obtains after filtration is with the hot wash of 80 ℃, the solid-liquid mass ratio is 1: 8, filter residue after washing was dried 8 hours under 80 ℃, obtain wolframic acid, reaction equation is: WO
4 2-+ 2H
+-H
2WO
4
Embodiment two
Described waste and old nickel tungsten series catalysts reclaims the method for tungsten nickel, comprises following processing step:
1. reducing roasting: at the temperature of 800 ℃, use hydrogen waste and old nickel tungsten series catalysts is carried out roasting, 1 hour reaction times, the metal simple-substance that makes nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into nickel and iron, and aluminum oxide, Tungsten oxide 99.999, silicon-dioxide can not be reduced;
2. displacement is leached: adding concentration in the product after roasting is the Cupric Chloride Solution of 3mol/L, wherein, copper ion concentration is 0.5～3mol/L, the pH value of regulator solution is 2.0, temperature of reaction is 60 ℃, and extraction time is 6 hours, metallic nickel and iron and cupric ion generation replacement(metathesis)reaction, become nickel ion and iron ion and enter in solution, displacement obtains Ni
2+And Fe
2+The chemical equation that ion occurs is as follows:
Ni+Cu
2+-Ni
2++Cu
Fe+Cu
2+-Fe
2++Cu
3. extracting and separating: the solution that will replace after leaching filters, filtrate being contained the solution of nickel ion and a small amount of iron ion and cupric ion, with concentration be the 1mol/L sodium hydroxide solution with the pH regulator to 4.5 of solution, then extract with extraction agent P507, nickel is separated from copper and iron;
4. condensing crystal: in upper step, the raffinate that obtains after extraction is pure nickel solution, then the degree Beaume that solution containing nickel is evaporated to solution is 55, through 15 hours, make the nickel solution temperature be reduced to 40 ℃, then through the separation of 24 hours, the solid particulate that obtains is the nickel crystal, strip liquor is the solution that contains cupric ion and iron ion, can return in step 2, is used for obtaining nickel ion and iron ion;
5. high-temperature roasting: with the filter residue mixture of sodium carbonate roasting of displacement leaching in step 2, the roasting temperatures of 800 ℃ 2 hours, sodium carbonate is 2.0: 1 with the ratio of the mole number of tungsten, material after roasting is with the hot wash of 99 ℃, the solid-liquid mass ratio is 1: 12, washing time is 3 hours, obtains containing the solution of sodium wolframate, reacts as follows:
WO
3+Na
2CO
3-Na
2WO
4+CO
2
6. recovery tungsten: the solution that contains sodium wolframate that step 5 is obtained returns adjust pH to 2.0 with hydrochloric acid, reaction is 2 hours at the temperature of 99 ℃, the filter residue that obtains after filtration is with the hot wash of 99 ℃, the solid-liquid mass ratio is 1: 12, filter residue after washing was dried 2 hours under 120 ℃, obtain highly purified wolframic acid, reaction equation is: WO
4 2-+ 2H
+-H
2WO
4
Embodiment three
Described waste and old nickel tungsten series catalysts reclaims the method for tungsten nickel, comprises following processing step:
1, reducing roasting: at the temperature of 700 ℃, use the reductive agent charcoal waste and old nickel tungsten series catalysts is carried out roasting, 3 hours reaction times, the metal simple-substance that makes nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into nickel and iron, and aluminum oxide, Tungsten oxide 99.999, silicon-dioxide can not be reduced, and reacts as follows:
2NiO+C-2Ni+CO
2
2FeO+C-2Fe+CO
2
2, displacement is leached: adding concentration in the product after roasting is the 2mol/L copper nitrate solution, and the pH value of regulator solution is 1.5, and temperature of reaction is 70 ℃, extraction time is 4 hours, metallic nickel and iron and cupric ion generation replacement(metathesis)reaction become nickel ion and iron ion and enter in solution, and displacement obtains Ni
2+And Fe
2+The chemical equation that ion occurs is as follows:
Ni+Cu
2+-Ni
2++Cu
Fe+Cu
2+-Fe
2++Cu；
3, extracting and separating: the solution that will replace after leaching filters, and filtrate being contained the solution of nickel ion and a small amount of iron ion and cupric ion, and the pH value of solution is adjusted to 3.5, then extracts with extraction agent P204, and nickel is separated from copper and iron;
4, condensing crystal: in upper step, the raffinate that obtains after extraction is pure nickel solution, be that 5mol/L ammoniacal liquor is with the pH regulator to 3.5 of solution with concentration, directly condensing crystal obtains the nickel crystal, strip liquor is the solution that contains cupric ion and iron ion, can return in step 2, be used for obtaining nickel ion and iron ion;
5, high-temperature roasting: with the filter residue mixture of sodium carbonate roasting of displacement leaching in step 2, the roasting temperatures of 600 ℃ 4 hours, sodium carbonate is 1.6: 1 with the ratio of the mole number of tungsten, material after roasting is with the hot wash of 75 ℃, the solid-liquid mass ratio is 1: 8, and washing time is 2 hours, obtains containing the solution of sodium wolframate, filter residue reacts as follows in order to reclaim aluminium and copper:
WO
3+Na
2CO
3-Na
2WO
4+CO
2
6, reclaim tungsten: the solution that contains sodium wolframate that step 5 is obtained returns adjust pH to 1.0 with nitric acid, reaction is 3 hours at the temperature of 85 ℃, the filter residue that obtains after filtration is with the hot wash of 90 ℃, the solid-liquid mass ratio is 1: 10, filter residue after washing was dried 6 hours under 100 ℃, obtain highly purified wolframic acid, react as follows: WO
4 2-+ 2H
+-H
2WO
4
Embodiment four
Described waste and old nickel tungsten series catalysts reclaims the method for tungsten nickel, comprises following processing step:
1. reducing roasting: at the temperature of 650 ℃, use hydrogen waste and old nickel tungsten series catalysts is carried out reducing roasting, 2 hours reaction times, the metal simple-substance that makes nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into nickel and iron, and aluminum oxide, Tungsten oxide 99.999, silicon-dioxide can not be reduced;
2. displacement is leached: adding concentration in the product after roasting is the 1.5mol/L Cupric Chloride Solution, the pH value that displacement is leached is 1.5, temperature of reaction is 65 ℃, extraction time is 3 hours, metallic nickel and iron and cupric ion generation replacement(metathesis)reaction, become nickel ion and iron ion and enter in solution, displacement is leached and is obtained Ni2+ and Fe
2+The chemical equation that ion occurs is as follows:
Ni+Cu
2+-Ni
2++Cu
Fe+Cu
2+-Fe
2++Cu；
3. extracting and separating: the solution that will replace after leaching filters, and filtrate being contained the solution of nickel ion and a small amount of iron ion and cupric ion, and the pH value of solution is adjusted to 4.0, then extracts with extraction agent P507, and nickel is separated from copper and iron;
4. condensing crystal: in upper step, the raffinate that obtains after extraction is pure nickel solution, and directly condensing crystal obtains the nickel crystal, and strip liquor is the solution that contains cupric ion and iron ion, can return in step 2, for obtaining nickel ion and iron ion;
5. high-temperature roasting: with the filter residue mixture of sodium carbonate roasting of displacement leaching in step 2, the roasting temperatures of 650 ℃ 5 hours, sodium carbonate is 1.6: 1 with the ratio of the mole number of tungsten, material after roasting is with the hot wash of 85 ℃, the solid-liquid mass ratio is 1: 6, and washing time is 1.5 hours, obtains containing the solution of sodium wolframate, filter residue reacts as follows in order to reclaim aluminium and copper:
WO
3+Na
2CO
3-Na
2WO
4+CO
2；
6. recovery tungsten: the solution that contains sodium wolframate that step 5 is obtained returns adjust pH to 1.0 with hydrochloric acid, reaction is 2.5 hours at the temperature of 82 ℃, the filter residue that obtains after filtration is with the hot wash of 92 ℃, the solid-liquid mass ratio is 1: 10, filter residue after washing was dried 5 hours under 100 ℃, obtain highly purified wolframic acid, react as follows: WO
4 2-+ 2H
+-H
2WO
4
Claims (9)
1. a waste and old nickel tungsten series catalysts reclaims the method for tungsten nickel, and it is characterized in that: described method comprises following processing step:
1) reducing roasting: at the temperature of 600～800 ℃, use reductive agent waste and old nickel tungsten series catalysts is carried out roasting, 1～4 hour reaction times, the metal simple-substance that makes nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into nickel and iron, and aluminum oxide, Tungsten oxide 99.999, silicon-dioxide can not be reduced;
2) displacement is leached: add copper solutions in the product after roasting, metallic nickel and iron and cupric ion generation replacement(metathesis)reaction, becoming nickel ion and iron ion enters in solution, wherein, copper ion concentration is 0.5～3mol/L, the pH value of regulator solution is 1.0～2.0, and temperature of reaction is 60～80 ℃, and extraction time is 2～6 hours;
3) extracting and separating: the solution that will replace after leaching filters, and filtrate being contained the solution of nickel ion and a small amount of iron ion and cupric ion, and the pH value of solution is adjusted to 3.0～4.5, then extracts, and nickel is separated from copper and iron;
4) condensing crystal: in upper step, the raffinate that obtains after extraction is pure nickel solution, and directly condensing crystal obtains the nickel crystal, and strip liquor is the solution that contains cupric ion and iron ion, can return in step 2, is used for obtaining nickel ion and iron ion;
5) the filter residue mixture of sodium carbonate roasting that high-temperature roasting: with step 2), displacement is leached, the roasting temperatures of 500～800 ℃ 2～6 hours, sodium carbonate is 1.2～2.0: 1 with the ratio of the mole number of tungsten, material after roasting is with the hot wash of 60～99 ℃, the solid-liquid mass ratio is 1: 4～12, washing time is 1～3 hour, obtains containing the solution of sodium wolframate, and filter residue is in order to reclaim aluminium and copper;
6) solution that contains sodium wolframate that recovery tungsten: with step 5) obtains goes back to adjust pH to 0.5～2.0 with acid, reacted at the temperature of 75～99 ℃ 2～4 hours, the filter residue that obtains after filtration is with the hot wash of 80～99 ℃, the solid-liquid mass ratio is 1: 8～12, filter residue after washing was dried under 80～120 ℃ 2～8 hours, obtained purity and be the wolframic acid more than 98.5%.
2. method according to claim 1, is characterized in that: in step 1) in, described reductive agent comprises charcoal or hydrogen, reductive agent is 1: 0.05～0.2 with the ratio of the total moles of nickel and iron.
3. method according to claim 1, is characterized in that: in step 2) in, Cu in the copper solutions that adds
2+The mole number of ion is 1.2～1.5: 1 with the ratio of the total moles of nickel and iron, and copper solutions comprises copper sulfate, cupric chloride or copper nitrate solution.
4. method according to claim 1, is characterized in that: in step 3) in, the solution that is used for regulator solution pH value comprises that concentration is ammoniacal liquor, sodium hydroxide or the potassium hydroxide solution of 1～10mol/L.
5. method according to claim 1, is characterized in that: in step 3) in, extraction agent used comprises P204 or P507.
6. method according to claim 5 is characterized in that: the mass ratio that consists of of described extraction agent P204 is that 20～30% P204 mixes 70～80% sulfonated kerosene, and its saponification degree is 50～75%, and the volume ratio of organic phase and water is 1: 0.5～2.
7. method according to claim 5, is characterized in that: in step 3) in extraction process in, through 8～10 grades of extractions, 4～6 grades the washing and 4～6 grades of back extractions after obtain raffinate and extraction liquid, wherein, washings and strip liquor are respectively H
+Concentration is the acid solution of 0.5～1.2mol/L and 3～4.5mol/L.
8. method according to claim 1, it is characterized in that: in step 4) in, the degree Beaume that solution containing nickel is evaporated to solution is between 50～55, again through 10～15 hours, make the nickel solution temperature be reduced between 20～40 ℃, through the separation of 12～24 hours, the solid particulate that obtains was the nickel crystal again.
9. method according to claim 1, is characterized in that: in step 6) in, the acid that is used for back adjust pH comprises sulfuric acid or hydrochloric acid.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106435189A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for metalized pellets |
| CN106435187A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for thermal state metallized pellets |
| CN106435190A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for metallized pellets |
| CN106435188A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for hot metallized pellets |
| CN106834702A (en) * | 2017-02-20 | 2017-06-13 | 山东科技大学 | The method that nickel salt is produced using waste nickel catalyst |
| CN110841647A (en) * | 2019-12-04 | 2020-02-28 | 大连理工大学 | Method for recycling waste skeleton nickel catalyst |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106435189A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for metalized pellets |
| CN106435187A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for thermal state metallized pellets |
| CN106435190A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for metallized pellets |
| CN106435188A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for hot metallized pellets |
| CN106435190B (en) * | 2016-08-30 | 2018-08-28 | 江苏省冶金设计院有限公司 | A kind of processing method and system of metallized pellet |
| CN106834702A (en) * | 2017-02-20 | 2017-06-13 | 山东科技大学 | The method that nickel salt is produced using waste nickel catalyst |
| CN110841647A (en) * | 2019-12-04 | 2020-02-28 | 大连理工大学 | Method for recycling waste skeleton nickel catalyst |
| CN110841647B (en) * | 2019-12-04 | 2021-05-14 | 大连理工大学 | Method for recycling waste skeleton nickel catalyst |
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| CN103173619B (en) | 2014-06-11 |
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