CN114075625A - Method for recovering valuable metals in carbon black - Google Patents
Method for recovering valuable metals in carbon black Download PDFInfo
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- CN114075625A CN114075625A CN202010832761.9A CN202010832761A CN114075625A CN 114075625 A CN114075625 A CN 114075625A CN 202010832761 A CN202010832761 A CN 202010832761A CN 114075625 A CN114075625 A CN 114075625A
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- carbon black
- molybdenum
- nickel
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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
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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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
- 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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- 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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
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- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering valuable metals in carbon black, which recovers valuable nickel, vanadium and molybdenum metals in the byproduct carbon black of devices such as an oil-gas gasification furnace, a flexible coking device and the like through the treatment procedures such as drying, roasting, leaching, precipitating and the like, thereby avoiding the environmental pollution caused by burning the carbon black as solid waste; the recovery rate of the valuable metals molybdenum, nickel and vanadium in the carbon black is 92-98.5%, and the method has the advantages of wide raw material source, high recovery rate of the valuable metals, environmental friendliness and the like.
Description
Technical Field
The invention relates to the field of metal recovery, in particular to a method for recovering valuable metals in carbon black.
Background
With the increasing deterioration of crude oil, the efficient clean conversion and optimized utilization of heavy oil are important problems for ensuring energy safety and sustainable development of national economy and society, and the utilization of heavy oil residues is one of the key problems. The gasification of heavy oil residue to produce hydrogen is increasingly paid attention by various large refineries due to the characteristics of good economic benefit, flexible raw materials, clean products and the like. A large amount of carbon black can be produced as a byproduct in the gasification process of heavy oil, at present, the carbon black is mainly used as solid waste for incineration treatment, and a large amount of valuable metals such as nickel, vanadium and molybdenum in the carbon black cannot be recycled. If the metal nickel, vanadium and molybdenum in the carbon black can be recovered, the pollution of carbon black incineration to the environment can be reduced, valuable metals can be recovered, and the secondary utilization of resources is realized.
At present, the metal recovery application of a refinery plant is that one or two of metals such as molybdenum, vanadium, cobalt, platinum, tungsten and the like are recovered from a hydrogenation supported waste catalyst, the main component of the supported catalyst is a carrier, the carrier is made of materials such as inert silica, alumina, clay or a mixture of the inert silica, the alumina, the clay and the like, and active components such as nickel, molybdenum, tungsten and the like are attached to the carrier.
Chinese patent CN 101435027B discloses a method for recovering high-purity molybdenum from molybdenum-containing spent catalyst, which comprises the steps of crushing the molybdenum-containing spent catalyst, fully mixing the crushed molybdenum-containing spent catalyst with alkaline substances and magnesium oxide, roasting at high temperature, leaching molybdenum into a solution, purifying the solution and recovering the molybdenum; chinese patent CN 1453379A discloses a process for extracting vanadium and/or molybdenum from waste catalyst of aluminum oxide carrier by wet method, firstly removing oil from waste catalyst at high temperature, then adding alkali and high-temperature sodium oxide for roasting, leaching roasted clinker with water to obtain sodium vanadate and sodium molybdate, adding ammonium salt into clarified solution for precipitating vanadium to obtain ammonium metavanadate, and extracting to obtain ammonium molybdate; chinese patent CN 111321296A discloses a method for recovering vanadium and nickel from waste petroleum catalyst, which comprises removing carbon and sulfur organic matters contained in the waste catalyst by roasting process, crushing the residue, heating and volatilizing in vacuum to obtain high-vanadium and high-nickel intermediate products, dissolving by weak acid dissolution method, removing aluminum and other impurity elements by adjusting pH value, finally obtaining high-purity vanadium and nickel metal, and realizing selective and high-efficiency recovery of vanadium and nickel.
The method can only recover one or two metals, the recovery variety is single, and the temperature in the roasting process is higher, so that a large amount of metal loss is caused. Different from a supported catalyst, the carbon black has high water content and high dehydration energy consumption, the main component after drying is carbon which is extremely easy to burn, the temperature is difficult to control during roasting, the particle size of the carbon black is small, and the carbon black is extremely easy to scatter in the roasting process, so that a large amount of metal loss is caused.
Disclosure of Invention
Aiming at the technical defects, the invention aims to provide a method for recovering valuable metals in carbon black, which can solve the problems of high difficulty and high cost in recovering a large amount of metals in the existing carbon black and can also solve the problems of single metal recovery variety and low metal recovery rate in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for recovering valuable metals from carbon black, comprising the steps of:
the method comprises the following steps: the carbon black is dehydrated by filter pressing, and is further dried by heating, and the water content of the carbon black is removed to be below 15 percent;
step two: roasting the carbon black at high temperature (or roasting by a sodium method), and removing combustible components such as carbon, sulfur and the like in the carbon black to obtain ash rich in metallic nickel, vanadium and molybdenum; roasting at 500-800 ℃ for 2-6 h, controlling air quantity in the roasting process, and recovering ash content carried in flue gas by adopting a cyclone separator and a cloth bag;
step three: if the blank in the second step is roasted, leaching the obtained ash with alkaline liquor; and if the sodium roasting is adopted in the second step, leaching with water. Filtering and washing the leached solution to obtain a molybdenum-vanadium solution and nickel-containing residue;
step four: acid washing is carried out on the nickel-containing residue, nickel is dissolved and leached, the leaching temperature is 70-100 ℃, and the leaching time is 1.5-5.5 h; adjusting the pH value to 8-12 by adding sodium hydroxide or potassium hydroxide, precipitating nickel in a nickel hydroxide form at the precipitation temperature of 30-70 ℃ for 1-5 h;
step five: adding ammonium salt into the molybdenum-vanadium solution obtained in the step three to enable vanadium to be precipitated in the form of ammonium vanadate, wherein the precipitation temperature is 60-90 ℃, the precipitation time is 0.5-3.5 hours, molybdenum is remained in the solution, and ammonium metavanadate can be further processed to obtain vanadium flakes or vanadium powder;
step six: gradually adding one or more of hydrochloric acid, sulfuric acid, carbonic acid, phosphoric acid and nitric acid into the molybdenum-containing solution to adjust the pH value to 1-3 h, and precipitating molybdenum in the form of ammonium polymolybdate under strong stirring at the precipitation temperature of 30-70 ℃ for 0.5-2 h.
The invention has the beneficial effects that: the problem that metal in the carbon black can not be recovered or the recovery cost is too high at present can be solved, the pollution to the environment caused by direct burning of the carbon black is avoided, and waste is changed into valuable; can recover three metals of nickel, vanadium and molybdenum, solves the problems of single recovery variety and low recovery rate in the prior art, and has the total recovery rate of more than 92 percent.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of a method for recovering valuable metals from carbon black according to an embodiment of the present invention.
Detailed Description
For better illustrating the objects, aspects and advantages of the present invention, the following detailed description of the embodiments of the present invention is only a part of the embodiments of the present invention, and other embodiments obtained by those skilled in the art without inventive efforts shall fall within the scope of the present invention.
Example 1
As shown in fig. 1, a method for recovering valuable metals from carbon black includes the steps of:
1) carrying out filter pressing and heating dehydration on the water-containing carbon black until the water content is 5%;
2) roasting the carbon black for 4 hours at the temperature of 600 ℃, removing combustible impurities such as carbon, sulfur and the like in the carbon black, and obtaining ash rich in metallic nickel, vanadium and molybdenum;
3) adding sodium hydroxide solution, stirring and leaching at the leaching temperature of 80 ℃ for 3h, washing, and filtering to obtain a molybdenum-vanadium-containing solution and a nickel-containing residue;
4) adding sulfuric acid into the nickel-containing residue to dissolve and leach the nickel, wherein the leaching temperature is 85 ℃, and the leaching time is 2.5 hours; leaching, filtering, adding sodium hydroxide into the filtrate to adjust the pH value to 9.0, precipitating nickel in the form of nickel hydroxide at the precipitation temperature of 50 ℃ for 2 hours;
5) adding ammonium chloride into the molybdenum and vanadium solution obtained in the third step to precipitate vanadium in the form of ammonium vanadate, wherein the precipitation temperature is 75 ℃, the precipitation time is 1h, washing is carried out to obtain ammonium metavanadate, and molybdenum is reserved in the solution;
6) gradually adding acid into the molybdenum-containing solution to adjust the pH value to 2.0, precipitating molybdenum in the form of ammonium polymolybdate under strong stirring, wherein the precipitation temperature is 50 ℃, and the precipitation time is 1 h;
through calculation and analysis, the recovery rate of nickel is 95.1%, the recovery rate of vanadium is 93.3%, and the recovery rate of molybdenum is 93.6%.
Example 2
As shown in fig. 1, a method for recovering valuable metals from carbon black includes the steps of:
1) carrying out filter pressing and heating dehydration on the water-containing carbon black until the water content is 1.5%;
2) uniformly mixing the dehydrated carbon black with sodium carbonate according to the ratio of 1:1, roasting for 4h at 550 ℃, and removing combustible carbon, sulfur and other impurities in the carbon black to obtain ash rich in metallic nickel, vanadium and molybdenum;
3) adding water, stirring and leaching, wherein the leaching temperature is 85 ℃, the leaching time is 3 hours, and washing and filtering are carried out to obtain a molybdenum-vanadium-containing solution and a nickel-containing residue;
4) adding sulfuric acid into the nickel-containing residue to dissolve and leach nickel, wherein the leaching temperature is 80 ℃, and the leaching time is 3 hours; leaching, filtering, adding sodium hydroxide into the filtrate to adjust the pH value to 10.0, precipitating nickel in the form of nickel hydroxide at the precipitation temperature of 50 ℃ for 2.5 h;
5) adding ammonium chloride into the molybdenum and vanadium solution obtained in the third step to precipitate vanadium in the form of ammonium vanadate, wherein the precipitation temperature is 75 ℃, the precipitation time is 1h, washing is carried out to obtain ammonium metavanadate, and molybdenum is reserved in the solution;
6) gradually adding acid into the molybdenum-containing solution to adjust the pH value to 2.0, precipitating molybdenum in the form of ammonium polymolybdate under strong stirring, wherein the precipitation temperature is 50 ℃, and the precipitation time is 1 h;
through calculation and analysis, the recovery rate of nickel is 94.7%, the recovery rate of vanadium is 94.2%, and the recovery rate of molybdenum is 94.1%.
Example 3
As shown in fig. 1, a method for recovering valuable metals from carbon black includes the steps of:
1) carrying out filter pressing and heating dehydration on the water-containing carbon black until the water content is 2.0%;
2) uniformly mixing the dehydrated carbon black with sodium carbonate according to the ratio of 1:0.5, roasting for 3h at 700 ℃, and removing combustible carbon, sulfur and other impurities in the carbon black to obtain ash rich in metallic nickel, vanadium and molybdenum;
3) adding water, stirring and leaching, wherein the leaching temperature is 85 ℃, the leaching time is 3 hours, and washing and filtering are carried out to obtain a molybdenum-vanadium-containing solution and a nickel-containing residue;
4) adding sulfuric acid into the nickel-containing residue to dissolve and leach nickel, wherein the leaching temperature is 80 ℃, and the leaching time is 3 hours; leaching, filtering, adding sodium hydroxide into the filtrate to adjust the pH value to 10.0, precipitating nickel in the form of nickel hydroxide at the precipitation temperature of 50 ℃ for 2.5 h;
5) adding ammonium sulfate into the molybdenum and vanadium solution obtained in the third step to precipitate vanadium in the form of ammonium vanadate, wherein the precipitation temperature is 75 ℃, the precipitation time is 1h, washing is carried out to obtain ammonium metavanadate, and molybdenum is reserved in the solution;
6) gradually adding acid into the molybdenum-containing solution to adjust the pH value to 1.0, precipitating molybdenum in the form of ammonium polymolybdate under strong stirring, wherein the precipitation temperature is 50 ℃, and the precipitation time is 1 h;
through calculation and analysis, the recovery rate of nickel is 94.6%, the recovery rate of vanadium is 93.8%, and the recovery rate of molybdenum is 93.4%.
The present invention is capable of other embodiments, and any changes and modifications made within the spirit and scope of the present invention are intended to be included therein.
Claims (7)
1. A method for recovering valuable metals from carbon black, comprising the steps of:
the method comprises the following steps: the carbon black is dehydrated by filter pressing, and is further dried by heating, and the water content of the carbon black is removed to be below 15 percent;
step two: roasting the dehydrated carbon black at high temperature (or roasting by an alkali sodium method), and removing combustible carbon, sulfur and other components in the carbon black to obtain ash rich in metallic nickel, vanadium and molybdenum;
step three: if the blank in the second step is roasted, leaching the obtained ash with alkaline liquor; and if the sodium method is adopted for roasting in the second step, leaching with water. Filtering and washing the leached solution to obtain a molybdenum-vanadium solution and nickel-containing residue;
step four: washing the nickel-containing residue with acid, and dissolving and leaching nickel; precipitating nickel in the form of nickel hydroxide by adjusting the pH value by adding alkali;
step five: adding ammonium salt into the molybdenum-vanadium solution obtained in the third step to precipitate vanadium in the form of ammonium vanadate, retaining molybdenum in the solution, and further processing ammonium metavanadate to obtain vanadium flakes or vanadium powder;
step six: gradually adding an acid solution into the molybdenum-containing solution to adjust the pH value to acidity, precipitating molybdenum in the form of ammonium polymolybdate under strong stirring, and heating to obtain molybdic acid or molybdenum trioxide.
2. The method for recovering valuable metals from carbon black according to claim 1, wherein in the first step, the carbon black dehydration is performed by a combination of various methods such as filter pressing, heating evaporation and the like, and the heat generated by calcination is fully utilized to perform dehydration, so that the energy consumption for dehydration is minimized.
3. The method for recovering valuable metals from carbon black according to claim 1, wherein in the second step, the roasting temperature is 500-800 ℃, the roasting time is 2-6 h, the air volume is controlled in the roasting process, and a cyclone separator and a cloth bag are adopted to recover ash content carried in flue gas.
4. The method for recovering valuable metals from carbon black according to claim 1, wherein in the third step, the leaching temperature is 70-100 ℃, and the leaching time is 1.5-5.5 h.
5. The method for recovering valuable metals from carbon black according to claim 1, wherein the strong acid used in the fourth step is one or more of sulfuric acid, nitric acid and phosphoric acid, the leaching temperature is 70-100 ℃, and the leaching time is 1.5-5.5 h. The alkali used in the precipitation is sodium hydroxide or potassium hydroxide, the precipitation temperature is 30-70 ℃, the pH value is 8-10, and the precipitation time is 1-5 h.
6. The method for recovering valuable metals from carbon black according to claim 1, wherein the ammonium salt used in the fifth step is ammonium chloride or ammonium sulfate, and the precipitation temperature is 60-90 ℃ and the precipitation time is 0.5-3.5 hours.
7. The method for recovering valuable metals from carbon black according to claim 1, wherein in the sixth step, the acid solution is one or more of hydrochloric acid, sulfuric acid, carbonic acid, phosphoric acid and nitric acid, the precipitation temperature is 30-70 ℃, and the precipitation time is 0.5-2 h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6193941B1 (en) * | 1996-06-01 | 2001-02-27 | Krupp Uhde Gmbh | Process for producing a metallurgical raw material from oil containing heavy metals |
| US20100111787A1 (en) * | 2007-03-13 | 2010-05-06 | Man Joo Kim | Method of recovering valuable metals from the vrds spent catalyst |
| CN102134643A (en) * | 2010-01-21 | 2011-07-27 | 英特卫普公司 | Metal recovery from hydroconverted heavy effluent |
| CN102971439A (en) * | 2010-03-04 | 2013-03-13 | 英特卫普公司 | Method of metals recovery from refinery residues |
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2020
- 2020-08-18 CN CN202010832761.9A patent/CN114075625A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6193941B1 (en) * | 1996-06-01 | 2001-02-27 | Krupp Uhde Gmbh | Process for producing a metallurgical raw material from oil containing heavy metals |
| US20100111787A1 (en) * | 2007-03-13 | 2010-05-06 | Man Joo Kim | Method of recovering valuable metals from the vrds spent catalyst |
| CN102134643A (en) * | 2010-01-21 | 2011-07-27 | 英特卫普公司 | Metal recovery from hydroconverted heavy effluent |
| CN102971439A (en) * | 2010-03-04 | 2013-03-13 | 英特卫普公司 | Method of metals recovery from refinery residues |
Non-Patent Citations (1)
| Title |
|---|
| 沈浚: "《合成氨》", 31 January 2001 * |
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