CN114574700A - Method for extracting tungsten oxide from tungsten waste - Google Patents
Method for extracting tungsten oxide from tungsten waste Download PDFInfo
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- CN114574700A CN114574700A CN202011402065.0A CN202011402065A CN114574700A CN 114574700 A CN114574700 A CN 114574700A CN 202011402065 A CN202011402065 A CN 202011402065A CN 114574700 A CN114574700 A CN 114574700A
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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
- C01G41/00—Compounds of tungsten
- C01G41/02—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
- C22B1/005—Preliminary treatment of scrap
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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
- C22B34/36—Obtaining tungsten
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/106—Other heavy metals refractory metals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention mainly discloses a method for extracting tungsten oxide from tungsten waste, which comprises the following main steps: removing deposited metal and impurities on the surface of the tungsten waste by using an acidic solution, removing aluminum metal on the surface of the tungsten waste by using a strong oxidant, performing oxidation leaching treatment on the tungsten waste by using the acidic solution, and filtering at least one tungsten oxide from the acidic solution. As can be seen from the foregoing description, the method of the present invention has the advantage of simple process steps, and can effectively extract high-purity and high-quality tungsten oxide from tungsten waste, thereby effectively reducing the environmental pollution caused by tungsten waste. Finally, the method of the invention is applied to related industries, and can achieve the significant contribution of tungsten resource recycling.
Description
Technical Field
The invention relates to the technical field of waste recycling, in particular to a method for refining tungsten oxide from tungsten waste.
Background
With the rapid development of technology, solid-state Light-emitting elements have been widely used in the manufacture of lighting devices and display devices, wherein the known solid-state Light-emitting elements include Organic Light-emitting diodes (LEDs) and Organic Light-emitting diodes (OLEDs). Engineers involved in the design and fabrication of OLED and/or LED devices for a long time should know that tungsten boats are indispensable consumables for fabricating cathode metal layers by using vapor deposition equipment. After the evaporation process is finished, the surface of the used tungsten boat is covered with metal residues and tungsten oxides, so that the used tungsten boat cannot be reused in the next evaporation process. It should be understood that as the number of times the evaporation process is performed increases, the amount of tungsten boat waste also increases.
Engineers involved in the design and fabrication of solid state light emitting devices have long known that tungsten is a metal that is not easily recycled and is polluting. At present, the commonly used tungsten waste recycling technology includes: mechanical crushing, saltpeter method, zinc melting method, electrolytic method, roasting-ammonia leaching method, etc.; among them, these conventional recycling methods have the disadvantages of large environmental pollution, low recovery rate, complicated process steps, etc., so that there is still no technology for effectively recovering tungsten oxide from tungsten waste. Therefore, how to extract (recover) tungsten metal from tungsten waste is an issue and a technical development goal that are regarded by manufacturers.
Disclosure of Invention
The invention mainly aims to provide a method for extracting tungsten oxide from tungsten waste, which comprises the following main steps: removing deposited metal and impurities on the surface of the tungsten waste by using an acidic solution, removing aluminum metal on the surface of the tungsten waste by using a strong oxidant, performing oxidation leaching treatment on the tungsten waste by using the acidic solution, and filtering at least one tungsten oxide from the acidic solution. As can be seen from the foregoing description, the method of the present invention has the advantage of simple process steps, and can effectively extract high-purity and high-quality tungsten oxide from tungsten waste, thereby effectively reducing the environmental pollution caused by tungsten waste. Finally, the method of the invention is applied to related industries, and can achieve the significant contribution of tungsten resource recycling.
To achieve the above object, an embodiment of the method for extracting tungsten oxide from tungsten waste according to the present invention comprises the following steps:
(1) placing at least one tungsten waste into a first solution such that the tungsten waste and the first solution have a first weight/volume ratio (w/v) ranging from 0.5:2.5 to 1.5: 3.5; wherein the first solution is formed by mixing an organic solvent and a first acidic solution according to a first volume/volume ratio (v/v), and the first volume/volume ratio is between 0.5:1 and 1.5: 2;
(2) continuously adding a cleaning agent into the first solution, and adding a low carbon alcohol into the first solution after waiting for at least 1 hour of reaction time; wherein, in the first solution, the lower alcohol, the organic solvent and the first acidic solution have a second volume/volume ratio ranging from 0.5:0.5:1 to 1.5:1.5: 2;
(3) taking out the tungsten waste from the first solution, and then sequentially putting the tungsten waste and a second solution into a second acidic solution to obtain a third solution; wherein the volume of the second acidic solution is twice of the volume of the organic solvent, and the second solution is formed by mixing an oxidant and a third acidic solution according to a third volume/volume ratio, wherein the third volume/volume ratio is between 0.5:2.5 and 1.5: 3.5;
(4) adding an aqueous solution into the third solution, wherein the volume of the aqueous solution is the same as that of the organic solvent;
(5) taking out the tungsten waste from the third solution, and then putting the tungsten waste into a fourth solution; wherein the fourth solution is formed by mixing a fourth acidic solution and a fifth acidic solution according to a fourth volume/volume ratio, and the fourth volume/volume ratio is 1: 1; and
(6) and performing a filtering treatment on the fourth solution, thereby filtering at least one tungsten oxide from the fourth solution.
In one embodiment, the organic solvent is any one of the following: tetrahydrofuran (THF), acetone, isopropanol, nitrogen methyl pyrrolidone, methylene chloride, toluene, benzene, a mixture of any two of the foregoing, or a mixture of any two or more of the foregoing.
In one embodiment, the first acidic solution, the third acidic solution and the fifth acidic solution are all hydrochloric acid with a mass percentage concentration of 37%, and the second acidic solution is hydrochloric acid with a mass percentage concentration of 18.5%.
In one embodiment, the cleaning agent is ethylene glycol or a glycol ether.
In one embodiment, the oxidizing agent is 30% by weight of hydrogen peroxide, and the fourth acidic solution is 60% by weight of nitric acid.
In one embodiment, the tungsten oxide comprises tungsten trioxide (WO)3) With tungsten blue (WO)2.9)。
The invention is described in detail below with reference to the drawings and specific examples, but the invention is not limited thereto.
Drawings
FIG. 1 is a flow chart of a method of extracting tungsten oxide from tungsten waste in accordance with the present invention;
FIG. 2 is an actual image of the first solution and the waste tungsten boat after completion of steps S1-S2;
FIG. 3 is an actual image of the third solution and the waste tungsten boat after completion of steps S3-S4;
FIG. 4 is an actual image of the fourth solution and the waste tungsten boat after completion of the step S5;
fig. 5 is an actual image diagram showing the tungsten oxide obtained by completing step S6;
FIG. 6 is an XRD spectrum of tungsten oxide;
FIG. 7 is an SEM image of tungsten oxide; and
figure 8 is an EDX spectrum of tungsten oxide.
Detailed Description
In order to more clearly describe the method for extracting tungsten oxide from tungsten waste, a preferred embodiment of the present invention will be described in detail below with reference to the accompanying drawings.
Referring to fig. 1, a flow chart of a method for extracting tungsten oxide from tungsten waste according to the present invention is shown. The invention provides a process for extracting tungsten oxide from tungsten waste, which comprises the following steps of S1: placing at least one tungsten waste into a first solution such that the tungsten waste and the first solution have a first weight/volume ratio (w/v) ranging from 0.5:2.5 to 1.5: 3.5. Engineers involved in the design and fabrication of OLED and/or LED devices for a long time should know that tungsten boats are indispensable consumables for fabricating cathode metal layers by using vapor deposition equipment. After the evaporation process is finished, the surface of the used tungsten boat is covered with metal residues and tungsten oxides, so that the used tungsten boat cannot be reused in the next evaporation process. Therefore, in one embodiment, the tungsten waste in step S1 may be, but is not limited to, tungsten boats that have already been used.
In one embodiment, the first solution is formed by mixing an organic solvent and a first acidic solution according to a first volume/volume ratio (v/v), and the first volume/volume ratio is between 0.5:1 and 1.5: 2. Wherein the organic solvent may be any one of the following: tetrahydrofuran (THF), acetone, isopropanol, nitrogen methyl pyrrolidone, methylene chloride, toluene, benzene, a mixture of any two of the foregoing, or a mixture of any two or more of the foregoing, for example, is Tetrahydrofuran (THF). On the other hand, the first acidic solutions are all hydrochloric acid with a mass percentage concentration of 37%. Explained in more detail, an exemplary embodiment of step S1 is as follows: 500 g of the waste tungsten boat was placed in a beaker containing 1 l of tetrahydrofuran (i.e., 99% by volume) and 0.5 l of hydrochloric acid (37% by mass).
The method flow then proceeds to step S2: continuously adding a cleaning agent into the first solution, and after waiting for at least 1 hour of reaction time to elapse, adding a lower alcohol into the first solution such that the lower alcohol, the organic solvent, and the first acidic solution have a second volume/volume ratio in the first solution ranging from 0.5:0.5:1 to 1.5:1.5: 2. In one possible embodiment, the cleaning agent may be ethylene glycol or a glycol ether, and the second volume/volume ratio is 1:1:1.5 (v/v). In more detail, an exemplary embodiment of step S2 is as follows: 1 liter of ethylene glycol (99 vol.%) was added to the first solution, which was allowed to react for one hour, followed by 1 liter of methanol (99.5 vol.%) to the first solution.
It should be noted that the present invention contemplates steps S1-S2 for removing deposited metal and impurities from the surface of the tungsten waste (waste tungsten boat) by using an acidic solution. FIG. 2 is an actual image showing the first solution and the waste tungsten boat after the steps S1-S2 are completed.
Continuously, the method flow executes step S3: taking out the tungsten waste from the first solution, and then sequentially putting the tungsten waste and a second solution into a second acidic solution to obtain a third solution. Then, the method flow proceeds to step S4: adding an aqueous solution to the third solution. In a practical embodiment, the second acidic solution is hydrochloric acid with a concentration of 18.5% by mass and has a volume twice that of the organic solvent. In another aspect, the second solution is formed by mixing an oxidant and a third acidic solution at a third volume/volume ratio (v/v), and the third volume/volume ratio is between 0.5:2.5 and 1.5: 3.5. In a practical embodiment, the third acidic solution is hydrochloric acid with a mass percentage concentration of 37%, and the oxidant is hydrogen peroxide with a mass percentage concentration of 30%. More specifically, exemplary embodiments of steps S3-S4 are as follows: the waste tungsten boat processed in steps S1 to S2 is first put into 2 liters of hydrochloric acid (mass percentage concentration is 18.5%), and then a second solution containing 0.5 liters of hydrogen peroxide (mass percentage concentration is 30%) and 1.5 liters of hydrochloric acid (mass percentage concentration is 37%) is added, and finally 1 liter of water is added.
It should be noted that, the present invention contemplates steps S3-S4 for removing aluminum metal from the surface of tungsten waste by using a strong oxidizing agent, as shown in the following chemical formula I: 2Al +6HClO4→2Al(ClO4)3+3H2. FIG. 3 is an actual image showing the third solution and the waste tungsten boat after the steps S3-S4 are completed.
Continuously, the method flow executes step S5: taking out the tungsten waste from the third solution, and then putting the tungsten waste into a fourth solution. In one embodiment, the fourth solution is formed by mixing a fourth acidic solution and a fifth acidic solution according to a fourth volume/volume ratio (v/v), and the fourth volume/volume ratio is 1:1. For example, the fourth acidic solution is nitric acid, and the fifth acidic solutions are hydrochloric acids. In more detail, an exemplary embodiment of step S5 is as follows: the waste tungsten boat processed in steps S3 to S4 is put into a fourth solution containing 1 liter of nitric acid (60% by mass) and 1 liter of hydrochloric acid (37% by mass), and the waste tungsten boat is subjected to an oxidation leaching process using an acidic solution, as shown in the following chemical formulas two and three:
the chemical formula II: w +6HNO3+6HCl→WCl6+6NO2(g)+6H2O;
The chemical formula III: WCl6+5H2O→WO3+6HCl+2H2O。
Briefly, the present invention contemplates step S5 for performing an oxidative leaching process on the tungsten waste using an acidic solution. Fig. 4 is an actual image showing the fourth solution and the waste tungsten boat after the completion of step S5.
As shown in fig. 1, the method flow finally performs step S6: and performing a filtering treatment on the fourth solution, thereby filtering at least one tungsten oxide from the fourth solution. According to practical experimental data, the tungsten oxide comprises tungsten trioxide (WO)3) With tungsten blue (WO)2.9). Fig. 5 shows an actual image of the tungsten oxide obtained by completing step S6.
In order to confirm that the obtained tungsten oxide did contain tungsten trioxide (WO)3) The inventors completed XRD, SEM and EDX analysis of the tungsten oxide obtained in step S6. Wherein, XRD is english abbreviation of X-ray diffraction (X-ray diffraction), SEM is Scanning electron microscope (Scanning electron microscope), and Energy-scattering X-ray spectrum (Energy-dispersive X-ray spectroscopy) is english abbreviation of X-ray diffraction (SEM). Fig. 6 shows an XRD spectrum of tungsten oxide, fig. 7 shows an SEM image of tungsten oxide, and fig. 8 shows an EDX spectrum of tungsten oxide. Obviously, the experimental data of fig. 6, 7 and 8 confirm that the tungsten oxide does contain tungsten trioxide (WO)3)。
Thus, all embodiments of the method for extracting tungsten oxide from tungsten waste disclosed herein have been fully and clearly illustrated. Moreover, it is clear from the above description that the present invention has the following features and advantages:
(1) the invention mainly discloses a method for extracting tungsten oxide from tungsten waste, which comprises the following main steps: removing deposited metal and impurities on the surface of the tungsten waste by using an acidic solution, removing aluminum metal on the surface of the tungsten waste by using a strong oxidant, performing oxidation leaching treatment on the tungsten waste by using the acidic solution, and filtering at least one tungsten oxide from the acidic solution.
(2) As can be seen from the foregoing description, the method of the present invention has the advantage of simple process steps, and can effectively extract high-purity and high-quality tungsten oxide from tungsten waste, thereby effectively reducing the environmental pollution caused by tungsten waste. Finally, the method of the invention is applied to related industries, and can achieve the significant contribution of tungsten resource recycling.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it should be understood that various changes and modifications can be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A method for refining tungsten oxide from tungsten waste is characterized by comprising the following steps:
(1) placing at least one tungsten waste into a first solution such that the tungsten waste and the first solution have a first weight/volume ratio (w/v) ranging from 0.5:2.5 to 1.5: 3.5; wherein the first solution is formed by mixing an organic solvent THF) and a first acidic solution (HCl) according to a first volume/volume ratio (v/v), and the first volume/volume ratio is between 0.5:1 and 1.5: 2;
(2) continuously adding a cleaning agent (EG) into the first solution, and after waiting for at least 1 hour of reaction time to elapse, adding a lower alcohol (MeOH) into the first solution; wherein, in the first solution, the lower alcohol, the organic solvent and the first acidic solution have a second volume/volume ratio ranging from 0.5:0.5:1 to 1.5:1.5: 2;
(3) taking out the tungsten waste from the first solution, and then sequentially putting the tungsten waste and a second solution into a second acidic solution (HCl) to obtain a third solution; wherein the volume of the second acidic solution (HCl) is twice of the volume of the organic solvent, and the second solution is formed by mixing an oxidant and a third acidic solution (HCl) according to a third volume/volume ratio, and the third volume/volume ratio is between 0.5:2.5 and 1.5: 3.5;
(4) adding an aqueous solution into the third solution, wherein the volume of the aqueous solution is the same as that of the organic solvent;
(5) taking out the tungsten waste from the third solution, and then putting the tungsten waste into a fourth solution; wherein the fourth solution is a fourth acidic solution (HNO)3) And a fifth acidic solution (HCl) in a fourth volume/volume ratio of 1: 1; and
(6) and performing a filtering treatment on the fourth solution, thereby filtering at least one tungsten oxide from the fourth solution.
2. The method as claimed in claim 1, wherein the organic solvent is any one of the following: tetrahydrofuran, acetone, isopropanol, azomethylpyrrolidone, methylene chloride, toluene, benzene, a mixture of any two of the foregoing, or a mixture of any two or more of the foregoing.
3. The method as claimed in claim 1, wherein the first acidic solution, the third acidic solution and the fifth acidic solution are all hydrochloric acid with a concentration of 37% by mass, and the second acidic solution is hydrochloric acid with a concentration of 18.5% by mass.
4. The method for extracting tungsten oxide from tungsten waste as claimed in claim 1, wherein the cleaning agent is ethylene glycol or glycol ether.
5. The method of claim 1, wherein the oxidizing agent is an oxidant.
6. The method as claimed in claim 1, wherein the fourth acidic solution is nitric acid with a concentration of 60% by mass.
7. The method of extracting tungsten oxide from tungsten waste as claimed in claim 1, wherein the tungsten oxide comprises tungsten trioxide (WO)3With tungsten blue WO2.9。
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