CN103173619B - 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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- CN103173619B CN103173619B CN201110432230.1A CN201110432230A CN103173619B CN 103173619 B CN103173619 B CN 103173619B CN 201110432230 A CN201110432230 A CN 201110432230A CN 103173619 B CN103173619 B CN 103173619B
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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 tungstic oxide of 25% left and right, the nickel oxide of 2% left and right, the aluminum oxide of 50% left and right, the silicon-dioxide of 5% left and right and a small amount of material such as iron, vanadium.Waste and old nickel tungsten series catalysts contains the metal 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 disclosing, less have a report that reclaims metallic nickel and tungsten about nickel tungsten series catalysts, most patent documentations also only relates to metallic nickel in single recovery nickel-containing catalyst or tungsten-containing catalyst or the method and apparatus of tungsten.In these methods, also exist the defect that processing step complexity, reaction conditions requirement are high, be unfavorable for cost control, restricted the development of this art, be also unfavorable for recovery and the utilization of resource, do not meet the megatrend of current energy-conserving and environment-protective.
Summary of the invention
The present patent application is the problems referred to above that exist in current 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 applicable to applying.
Specifically, the waste and old nickel tungsten series catalysts described in the present patent application reclaims the method for tungsten nickel, comprises following processing step:
1) reducing roasting: at the temperature of 600～800 ℃, application reductive agent carries out roasting to waste and old nickel tungsten series catalysts, 1～4 hour reaction times, make nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into the metal simple-substance of nickel and iron, and aluminum oxide, Tungsten oxide 99.999 and silicon-dioxide can not be reduced;
2) displacement is leached: in the product after roasting, add copper solutions, 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 after displacement is leached filters, and the solution that filtrate being contained nickel ion and a small amount of iron ion and cupric ion, is adjusted to 3.0～4.5 by the pH value of solution, then extracts, and nickel is separated from copper and iron;
4) condensing crystal: in upper step, the raffinate obtaining after extraction is pure nickel solution, and directly condensing crystal obtains 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: by the filter residue mixture of sodium carbonate roasting that in 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, the hot wash of 60～99 ℃ for material after roasting, solid-liquid mass ratio is 1: 4～12, washing time is 1～3 hour, obtains the solution that contains sodium wolframate, and filter residue is in order to reclaim aluminium and copper;
6) reclaim tungsten: adjust pH to 0.5～2.0 are gone back in the solution that contains sodium wolframate that step 5 is obtained acid, at the temperature of 75～99 ℃, react 2～4 hours, the hot wash of 80～99 ℃ for the filter residue obtaining after filtration, solid-liquid mass ratio is 1: 8～12, filter residue after washing is dried 2～8 hours at 80～120 ℃, and obtaining purity is more than 98.5% wolframic acid.
Further, in step 1, described reductive agent comprises the reductive agent that charcoal or hydrogen etc. are common, 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 adding
2+) mole number be 1.2～1.5: 1 with the ratio of the total moles of nickel and iron, copper solutions comprises copper sulfate, cupric chloride or copper nitrate solution, the concrete chemical equation occurring is as follows:
Ni+Cu
2+-Ni
2++Cu
Fe+Cu
2+-Fe
2++Cu
In step 3, with alkaline solution, by the pH regulator to 3.0 of solution～4.5, alkaline solution used comprises ammoniacal liquor, sodium hydroxide or potassium hydroxide 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, after 8～10 grades of extractions, 4～6 grades of washings and 4～6 grades of back extractions, obtains raffinate and extraction liquid; 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 nickel crystal is that the degree Beaume that solution containing nickel is evaporated to solution is between 50～55, then through 10～15 hours, nickel solution temperature is reduced between 20～40 ℃, through the separation of 12～24 hours, the solid particulate obtaining was nickel crystal again.
In step 5, reaction equation is as follows:
WO
3+Na
2CO
3-Na
2WO
4+CO
2
In step 6, comprise for the acid of returning adjust pH the acid that sulfuric acid, hydrochloric acid etc. are common, reaction equation is as follows:
WO
4 2-+2H
+-H
2WO
4。
Method described in the present patent application, has advantages of following:
1, the rate of recovery is high: through aforesaid method, can obtain purity and reach more than 98.5% wolframic acid;
2, simple process, with low cost: all easy being easy to get of the processing condition of present method and reagent used, are conducive to cost control;
3, comprehensive reutilization degree is high, and present method can be carried out comprehensive reutilization to metals such as tungsten, nickel and aluminium and copper.
Accompanying drawing explanation
Accompanying drawing is the process flow diagram of method described in the present patent application.
Embodiment
Below in conjunction with accompanying drawing and concrete example; the method that waste and old nickel tungsten series catalysts described in the present patent application is reclaimed to tungsten nickel is described and illustrates; object is better to understand technology contents of the present invention for the public; rather than restriction to described technology contents; under identical or approximate principle, the improvement that described processing step is carried out, comprises that reaction conditions, agents useful for same improve and replace; reach identical object, all within the present patent application technical scheme required for protection.
Embodiment mono-
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 ℃, application charcoal carries out roasting to waste and old nickel tungsten series catalysts, 4 hours reaction times, make nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into the metal simple-substance of 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: in the product after roasting, adding concentration 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 after displacement is leached filters, and the solution that filtrate being contained nickel ion and a small amount of iron ion and cupric ion, is adjusted to 3.0 by the pH value of solution, then uses P204 extracting and separating, and nickel is separated from copper and iron;
4. condensing crystal: in upper step, the raffinate obtaining after extraction is pure nickel solution, the degree Beaume that solution containing nickel is evaporated to solution is 50, through 10 hours, nickel solution temperature is reduced between 20 ℃ again, through separation in 12 hours, the solid particulate obtaining was 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: by the filter residue mixture of sodium carbonate roasting that in step 2, displacement is leached, the roasting temperatures of 500 ℃ 6 hours, sodium carbonate is 1.2: 1 with the ratio of the mole number of tungsten, the hot wash of 60 ℃ for material after roasting, solid-liquid mass ratio is 1: 4, washing time is 3 hours, obtains the solution that contains sodium wolframate, reacts as follows:
WO
3+Na
2CO
3-Na
2WO
4+CO
2
6. reclaim tungsten: the solution that the contains sodium wolframate sulphuric acid soln that step 5 is obtained returns adjust pH to 0.5, at the temperature of 75 ℃, react 4 hours, the hot wash of 80 ℃ for the filter residue obtaining after filtration, solid-liquid mass ratio is 1: 8, filter residue after washing is dried 8 hours at 80 ℃, obtain wolframic acid, reaction equation is: WO
4 2-+ 2H
+-H
2wO
4.
Embodiment bis-
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 ℃, application hydrogen carries out roasting to waste and old nickel tungsten series catalysts, in 1 hour reaction times, makes nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into the metal simple-substance of nickel and iron, and aluminum oxide, Tungsten oxide 99.999, silicon-dioxide can not be reduced;
2. displacement is leached: in the product after roasting, adding concentration 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 after displacement is leached filters, the solution that filtrate being contained nickel ion and a small amount of iron ion and cupric ion, with concentration be 1mol/L sodium hydroxide solution by 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 obtaining after extraction is pure nickel solution, then the degree Beaume that solution containing nickel is evaporated to solution is 55, through 15 hours, make nickel solution temperature be reduced to 40 ℃, then through the separation of 24 hours, the solid particulate obtaining is nickel crystal, 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: by the filter residue mixture of sodium carbonate roasting that in step 2, displacement is leached, the roasting temperatures of 800 ℃ 2 hours, sodium carbonate is 2.0: 1 with the ratio of the mole number of tungsten, the hot wash of 99 ℃ for material after roasting, solid-liquid mass ratio is 1: 12, washing time is 3 hours, obtains the solution that contains sodium wolframate, reacts as follows:
WO
3+Na
2CO
3-Na
2WO
4+CO
2
6. reclaim tungsten: the solution that the contains sodium wolframate hydrochloric acid that step 5 is obtained returns adjust pH to 2.0, at the temperature of 99 ℃, react 2 hours, the hot wash of 99 ℃ for the filter residue obtaining after filtration, solid-liquid mass ratio is 1: 12, filter residue after washing is dried 2 hours at 120 ℃, obtain highly purified wolframic acid, reaction equation is: WO
4 2-+ 2H
+-H
2wO
4.
Embodiment tri-
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 ℃, application reductive agent charcoal carries out roasting to waste and old nickel tungsten series catalysts, 3 hours reaction times, make nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into the metal simple-substance of 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: in the product after roasting, adding concentration is 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 after displacement is leached filters, and the solution that filtrate being contained nickel ion and a small amount of iron ion and cupric ion, is adjusted to 3.5 by the pH value of solution, then extracts with extraction agent P204, and nickel is separated from copper and iron;
4, condensing crystal: in upper step, the raffinate obtaining after extraction is pure nickel solution, be that 5mol/L ammoniacal liquor is by the pH regulator to 3.5 of solution by concentration, directly condensing crystal obtains nickel crystal, 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: by the filter residue mixture of sodium carbonate roasting that in step 2, displacement is leached, the roasting temperatures of 600 ℃ 4 hours, sodium carbonate is 1.6: 1 with the ratio of the mole number of tungsten, the hot wash of 75 ℃ for material after roasting, solid-liquid mass ratio is 1: 8, and washing time is 2 hours, obtains the solution that contains sodium wolframate, filter residue, in order to reclaim aluminium and copper, reacts as follows:
WO
3+Na
2CO
3-Na
2WO
4+CO
2
6, reclaim tungsten: the solution that the contains sodium wolframate nitric acid that step 5 is obtained returns adjust pH to 1.0, at the temperature of 85 ℃, react 3 hours, the hot wash of 90 ℃ for the filter residue obtaining after filtration, solid-liquid mass ratio is 1: 10, filter residue after washing is dried 6 hours at 100 ℃, obtain highly purified wolframic acid, react as follows: WO
4 2-+ 2H
+-H
2wO
4.
Embodiment tetra-
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 ℃, application hydrogen carries out reducing roasting to waste and old nickel tungsten series catalysts, in 2 hours reaction times, makes nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into the metal simple-substance of nickel and iron, and aluminum oxide, Tungsten oxide 99.999, silicon-dioxide can not be reduced;
2. displacement is leached: in the product after roasting, adding concentration is 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 after displacement is leached filters, and the solution that filtrate being contained nickel ion and a small amount of iron ion and cupric ion, is adjusted to 4.0 by the pH value of solution, then extracts with extraction agent P507, and nickel is separated from copper and iron;
4. condensing crystal: in upper step, the raffinate obtaining after extraction is pure nickel solution, and directly condensing crystal obtains 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: by the filter residue mixture of sodium carbonate roasting that in step 2, displacement is leached, the roasting temperatures of 650 ℃ 5 hours, sodium carbonate is 1.6: 1 with the ratio of the mole number of tungsten, the hot wash of 85 ℃ for material after roasting, solid-liquid mass ratio is 1: 6, and washing time is 1.5 hours, obtains the solution that contains sodium wolframate, filter residue, in order to reclaim aluminium and copper, reacts as follows:
WO
3+Na
2CO
3-Na
2WO
4+CO
2；
6. reclaim tungsten: the solution that the contains sodium wolframate hydrochloric acid that step 5 is obtained returns adjust pH to 1.0, at the temperature of 82 ℃, react 2.5 hours, the hot wash of 92 ℃ for the filter residue obtaining after filtration, solid-liquid mass ratio is 1: 10, filter residue after washing is dried 5 hours at 100 ℃, obtain highly purified wolframic acid, react as follows: WO
4 2-+ 2H
+-H
2wO
4.
Claims (3)
1. waste and old nickel tungsten series catalysts reclaims a method for tungsten nickel, it is characterized in that: described method comprises following processing step:
1) reducing roasting: at the temperature of 600～800 ℃, application reductive agent carries out roasting to waste and old nickel tungsten series catalysts, 1～4 hour reaction times, make nickel oxide in waste and old nickel tungsten series catalysts and ferric oxide be converted into the metal simple-substance of nickel and iron, and aluminum oxide, Tungsten oxide 99.999, silicon-dioxide can not be reduced, described reductive agent is charcoal or hydrogen, and reductive agent is 1:0.05～0.2 with the ratio of the total moles of nickel and iron;
2) displacement is leached: in the product after roasting, add copper solutions, 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, and the pH value of regulator solution is 1.0～2.0, and temperature of reaction is 60～80 ℃, extraction time is 2～6 hours, Cu in the copper solutions adding
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;
3) extracting and separating: the solution after displacement is leached filters, the solution that filtrate being contained nickel ion and a small amount of iron ion and cupric ion, the pH value of solution is adjusted to 3.0～4.5, then extract, nickel is separated from copper and iron, solution for regulator solution pH value comprises that concentration is ammoniacal liquor, sodium hydroxide or the potassium hydroxide solution of 1～10mol/L, and extraction agent used comprises P204 or P507;
4) condensing crystal: in upper step, the raffinate obtaining after extraction is pure nickel solution, directly condensing crystal obtains 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, the degree Beaume that solution containing nickel is evaporated to solution is between 50～55, then through 10～15 hours, nickel solution temperature is reduced between 20～40 ℃, through the separation of 12～24 hours, the solid particulate obtaining was nickel crystal again;
5) high-temperature roasting: by step 2) middle filter residue mixture of sodium carbonate roasting of replacing leaching, 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, the hot wash of 60～99 ℃ for material after roasting, solid-liquid mass ratio is 1:4～12, washing time is 1～3 hour, obtains the solution that contains sodium wolframate, and filter residue is in order to reclaim aluminium and copper;
6) reclaim tungsten: adjust pH to 0.5～2.0 are gone back in the solution that contains sodium wolframate that step 5) is obtained acid, at the temperature of 75～99 ℃, react 2～4 hours, the hot wash of 80～99 ℃ for the filter residue obtaining after filtration, solid-liquid mass ratio is 1:8～12, filter residue after washing is dried 2～8 hours at 80～120 ℃, obtaining purity is more than 98.5% wolframic acid, is sulfuric acid or hydrochloric acid for the acid of returning adjust pH.
2. method according to claim 1, 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.
3. method according to claim 1, it is characterized in that: in the extraction process in step 3), after 8～10 grades of extractions, 4～6 grades of washings and 4～6 grades of back extractions, obtain raffinate and extraction liquid, wherein, washings and strip liquor are respectively the acid solution that H+ concentration is 0.5～1.2mol/L and 3～4.5mol/L.
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|---|---|---|---|
| CN201110432230.1A CN103173619B (en) | 2011-12-21 | 2011-12-21 | Method for recovering nickel and tungsten by waste nickel and tungsten catalyst |
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| CN106435187B (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 thermal state metal pellet |
| 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 |
| 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 |
| 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 |
| 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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