CN111960389A - Method for recycling metal tellurium from tellurium-containing waste through vacuum fractional condensation - Google Patents
Method for recycling metal tellurium from tellurium-containing waste through vacuum fractional condensation Download PDFInfo
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- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 113
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 55
- 239000002184 metal Substances 0.000 title claims abstract description 55
- 239000002699 waste material Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000009833 condensation Methods 0.000 title claims abstract description 34
- 230000005494 condensation Effects 0.000 title claims abstract description 34
- 238000004064 recycling Methods 0.000 title claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 150000002739 metals Chemical class 0.000 claims abstract description 12
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 17
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 17
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 claims description 11
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052793 cadmium Inorganic materials 0.000 claims description 8
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- MOAOBEKGMNGXJG-UHFFFAOYSA-N [Te].[Te].[Te].[Au].[Au] Chemical compound [Te].[Te].[Te].[Au].[Au] MOAOBEKGMNGXJG-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000002351 wastewater Substances 0.000 abstract description 4
- 239000002912 waste gas Substances 0.000 abstract description 3
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract 1
- 238000009853 pyrometallurgy Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 15
- 238000002386 leaching Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 239000008151 electrolyte solution Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- 239000011133 lead Substances 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- VOADVZVYWFSHSM-UHFFFAOYSA-L sodium tellurite Chemical compound [Na+].[Na+].[O-][Te]([O-])=O VOADVZVYWFSHSM-UHFFFAOYSA-L 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- 229910002899 Bi2Te3 Inorganic materials 0.000 description 1
- 229910004613 CdTe Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001245 Sb alloy Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910001215 Te alloy Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 239000002140 antimony alloy Substances 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- QWUZMTJBRUASOW-UHFFFAOYSA-N cadmium tellanylidenezinc Chemical compound [Zn].[Cd].[Te] QWUZMTJBRUASOW-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005363 electrowinning Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 ferrous metals Chemical class 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
-
- 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
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
-
- 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
- C22B17/00—Obtaining cadmium
- C22B17/02—Obtaining cadmium by dry processes
-
- 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
-
- 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
- C22B7/001—Dry 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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for recycling metal tellurium from tellurium-containing waste through vacuum fractional condensation, which belongs to the technical field of non-ferrous metal pyrometallurgy and resource regeneration, and the method comprises the steps of firstly placing the tellurium-containing waste into a vacuum fractional condensation furnace, vacuumizing, heating to a certain temperature, then carrying out vacuum thermal decomposition, then adjusting the temperature for fractional condensation, preserving the temperature for a period of time, and stopping the operation to respectively obtain metal tellurium and other valuable metals; the method has the advantages of simple process, convenient operation, simple required equipment, no waste water and gas, low cost, high universality of raw materials, capability of treating the tellurium-containing waste with any component, and safe and controllable process.
Description
Technical Field
The invention relates to a method for recycling metal tellurium from tellurium-containing waste materials through vacuum fractional condensation, and belongs to the technical field of pyrometallurgical smelting of non-ferrous metals and resource regeneration.
Background
Tellurium is a rare dispersion element, and the abundance of the continental crust is only 5 multiplied by 10-7The vitamin is known as vitamin of modern industry, national defense and advanced technology, and is one of indispensable elements in the modern high-tech field. In 2019, the global tellurium yield is about 470 tons, but the consumption demand is more than 1000 tons, and the supply and demand gap is large. Due to the uniqueness of tellurium resources, sources and routes of tellurium mainly include associated metal ores such as copper, lead and zinc, independent tellurium ores (mainly comprising tellurium and bismuth) and waste tellurium-based materials. In recent years, with the large-scale application of tellurium-based compounds in the fields of new materials such as photo-thermal materials, photo-electrical materials and the like, the recovery of tellurium from waste tellurium-based materials has become one of important sources of tellurium. According to statistics, CdTe and Bi2Te3The utilization rate of tellurium in the production and processing process of the telluride is about 60% -70%, a large amount of leftover materials, cutting scraps and other waste tellurium-containing materials are generated, and the tellurium-based materials end the service cycle, so that the tellurium content in the waste materials produced in the industry every year is about 200 tons, and severe waste of tellurium resources is caused if comprehensive recycling is not performed.
In the research of the extraction method of the metal tellurium, the raw material components are complex, and the research is mainly carried out at home and abroad around the extraction process of a chemical wet method (oxidation leaching-reduction-replacement, chlorination method, oxygen pressure leaching method, acid leaching and the like). However, the wet extraction process has long flow, high production cost, high requirement on equipment, and the problems of waste water, waste residue and the like.
In recent years, with the excessive development of mineral resources, mineral resources with high grade and relatively simple mineral components are increasingly lacking, and low-grade mineral resources of lean ores, complex ores and multi-metal paragenic ores gradually become main raw materials for smelting, so that the extraction difficulty of tellurium is increased more and more. Compared with the shortage of tellurium mineral resources, the development and utilization of tellurium resources in urban mines can be the main stream in the futureThe development direction is. Studies and applications of Zhang Weiqi (tellurium-antimony-bismuth-tellurium alloy powder extraction of tellurium) [ J]2017(2) the tellurium-bismuth-antimony alloy compound powder is sulfated and roasted at the low temperature of 450 ℃, so that tellurium in the roasted sand is transformed into tellurium dioxide, and the tellurium recovery rate of 92.58 percent is obtained. Dissolving tellurium dioxide in alkali to generate sodium tellurite, adding dilute sulfuric acid into the tellurium-containing solution to adjust the pH value step by step for neutralization, purification and impurity removal to obtain high-tellurium-containing purified liquid, and continuously adding dilute sulfuric acid for neutralization to obtain high-grade tellurium dioxide for extracting fine tellurium intermediate materials. Han scholar (Bi)2Te3Recovery of waste powder from base refrigeration crystal bar processing and optimization of thermoelectric performance [ J]2017(1) removing impurities in waste powder from bismuth telluride crystal bar waste through vacuum calcination and 1-time and 2-time smelting to obtain bismuth telluride powder, adding a proper amount of tellurium and antimony raw materials, and performing pressure sintering to prepare a P-type material with better performance, wherein the recovery rate of the waste powder is over 85.73 percent, but the preparation of the P-type alloy material has high requirement on the mixing uniformity of the recovered powder, high energy consumption for repeated smelting and impurity removal, high cost of pressure sintering equipment and immature industrialization technology for preparing the P-type material through powder metallurgy, and the technology stays in a laboratory stage mostly, and the applicability of the technology to the N-type material is not reported. Li Qixu (research on recovery of tellurium from cadmium Zinc telluride Process [ J)]2015, 33(2): 193-196) of Zhejiang university of science and technology, and the tellurium in the tellurium-zinc-cadmium is recovered by a hydrothermal oxidation-acid leaching-reduction method, and the recovery rate of the tellurium is examined by changing the hydrothermal temperature, the sulfuric acid concentration, the liquid-solid ratio and the addition amount of sodium sulfite. In the previous researches, the extraction process method of the metal tellurium mainly adopts a wet method as a main method and adopts a fire method or a physical method as an auxiliary method, the process links are more, and the production cost and the environmental protection have higher pressure.
In the patent of publication No. CN 107849783, the separation and recovery of tellurium and bismuth are realized by taking bismuth telluride as a raw material and adopting hydrometallurgical methods such as oxidation leaching, reduction, replacement, filtration and the like. In patent publication No. CN 102953080B, electrowinning of tellurium from cadmium telluride was studied.
In the patent publication US 7731920, a system and method for separating tellurium from cadmium waste by using an acid leaching method to effect ion exchange by changing conditions of ph, temperature, time, etc. of the leachate is described. In the patent publication CN 1994869A, the crushed and ground material is added to molten alkali metal hydroxide or a mixture thereof with alkali metal carbonate, and alkali dissolution is carried out at 640-720 ℃; adding an oxidant; leaching the melt with water once or twice; neutralizing the leaching solution with acid, wherein the reaction end point pH is 5-6, and obtaining tellurium dioxide; dissolving tellurium dioxide with alkali to prepare a solution, preparing a sodium tellurite solution, and electrodepositing to finally obtain the metal tellurium. In the patent publication No. CN 103849783a, a bismuth telluride raw material with a certain particle size is provided, and crude bismuth and crude tellurium can be obtained after the steps of heating, oxidizing leaching, filtering, washing, reducing, secondary oxidizing leaching and the like. Patent application No. 20111025011.5 proposes contacting a cadmium telluride containing component with a first electrolyte solution, contacting an opposing electrode with a second electrolyte solution spaced from the first electrolyte solution by anions, and applying a voltage differential between the cadmium telluride containing component and the opposing electrode to cause tellurium to migrate out of the cadmium telluride containing component and deposit on the opposing electrode. Patent application No. 201010162679.6 proposes contacting the cadmium telluride component with an electrolyte solution having a pH above about 9, contacting the opposing electrode with the electrolyte solution, and adding a voltage difference between the cadmium telluride component and the opposing electrode to cause tellurium to migrate out of the cadmium telluride component and deposit on the opposing electrode. Patent application No. CN201810716395.3 proposes a vacuum distillation method for recovering tellurium and bismuth from bismuth telluride materials. Patent application No. CN201810716395.3 proposes that sulfur is added to react with cadmium in cadmium telluride waste, and then tellurium is obtained through vacuum distillation. The above patents have certain effect in processing tellurium-containing materials, but have the problems of waste liquid and waste residue generation, low purity of extracted tellurium, incapability of thorough separation and the like.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides a method for recycling metal tellurium by vacuum fractional condensation of tellurium-containing waste. The method has the advantages of simple process, convenient operation, simple required equipment, no waste water and gas, low cost, high universality of raw materials, capability of treating the tellurium-containing waste with any component, and safe and controllable process.
The invention is realized by the following technical scheme: the method comprises the steps of firstly placing tellurium-containing waste in a vacuum fractional condensation furnace, vacuumizing, raising the temperature to a certain temperature, then carrying out vacuum thermal decomposition, then adjusting the temperature for fractional condensation, preserving the temperature for a period of time, and stopping operation to respectively obtain metal tellurium and other valuable metals.
The method comprises the following specific steps:
placing tellurium-containing waste into a vacuum fractional condensation furnace, vacuumizing to 1-500 Pa, heating to 400-650 ℃, and preserving heat for 30-120 min;
and (2) continuing heating to 700-1000 ℃, enabling tellurium and other volatile metals to enter a gas phase to form mixed metal steam, controlling the temperature of a condensation zone of tellurium to be 200-400 ℃, keeping the temperature for 30-90 min, stopping the operation, and cooling to room temperature to obtain metal tellurium and other valuable metals respectively.
And (2) the tellurium-containing waste materials in the step (1) are lead telluride, bismuth telluride, cadmium telluride and gold telluride waste materials.
The vacuum fractional condensation furnace in the step (1) is a vacuum tube furnace, a certain temperature gradient is formed in the furnace, and the temperature of each section is controllable.
And (3) the vacuum degree of the system is 1-500 Pa during fractional condensation in the step (2).
And (3) mixing metal vapor components in the step (2) into tellurium, lead, bismuth, cadmium and the like.
The content of the tellurium obtained in the step (2) is more than 99%, and the purity of other valuable metals such as lead, bismuth, cadmium and the like is more than 90%.
The invention has the beneficial effects that:
(1) the method has the advantages of simple process, convenient operation, simple required equipment, no waste water and gas, low cost, high universality of raw materials, capability of treating the tellurium-containing waste with any component, and safe and controllable process.
(2) Because the tellurium-containing waste materials are complex in components and the occurrence state of elements is not easy to master, the telluride is easy to thermally decompose through thermodynamic calculation, the decomposition reaction temperature is further reduced under the vacuum condition, but more intermediate reactions and reverse reactions are associated.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1:
as shown in fig. 1, the method for recovering tellurium metal from tellurium-containing waste comprises the following specific steps:
firstly, 100kg of tellurium-containing waste (the main component is bismuth telluride) is placed in a vacuum fractional condensation furnace, the vacuum fractional condensation furnace is vacuumized to 1 Pa, the temperature is raised to 400 ℃, and the heat preservation time is 30 min;
and (2) continuing heating to 700 ℃, enabling tellurium and other volatile metals to enter a gas phase to form mixed metal steam, controlling the temperature of a condensation zone of tellurium to be between 200 and 400 ℃, keeping the temperature for 30min, stopping the operation, and cooling to 23 ℃ to respectively obtain metal tellurium and bismuth.
The purity of the obtained tellurium metal reaches 99%, and the purity of the bismuth reaches 95%.
Example 2:
as shown in fig. 1, the method for recovering tellurium metal from tellurium-containing waste comprises the following specific steps:
step 1, firstly, placing 100kg of tellurium-containing waste (the main component is lead telluride) in a vacuum fractional condensation furnace, vacuumizing to 500Pa, heating to 650 ℃ and preserving heat for 120 min;
and 2, continuously heating to 1000 ℃, enabling tellurium and other volatile metals to enter a gas phase to form mixed metal steam, controlling the temperature of a condensation zone of tellurium to be 200-400 ℃, keeping the temperature for 90min, stopping the operation, and cooling to 25 ℃ to obtain metal tellurium and lead respectively.
The purity of the obtained tellurium metal reaches 99.5 percent, and the purity of lead reaches 98 percent.
Example 3
Step 1, firstly, placing 100kg of tellurium-containing waste (mainly containing gold telluride) in a vacuum fractional condensation furnace, vacuumizing to 100Pa, heating to 500 ℃ and preserving heat for 90 min;
and 2, continuously heating to 800 ℃, enabling tellurium and other volatile metals to enter a gas phase to form mixed metal steam, controlling the temperature of a condensation area of tellurium to be 200-400 ℃, keeping the temperature for 60min, stopping the operation, and cooling to room temperature to obtain metal tellurium and metal gold respectively.
The purity of the obtained tellurium metal reaches 99.9 percent, and the purity of the gold reaches 99 percent.
Example 4
As shown in fig. 1, the method for recovering tellurium metal from tellurium-containing waste comprises the following specific steps:
step 1, firstly, placing 100kg of tellurium-containing waste (mainly containing cadmium telluride) in a vacuum fractional condensation furnace, vacuumizing to 100Pa, heating to 500 ℃ and preserving heat for 90 min;
and 2, continuously heating to 800 ℃, enabling tellurium and other volatile metals to enter a gas phase to form mixed metal steam, controlling the temperature of a condensation zone of tellurium to be 200-400 ℃, keeping the temperature for 60min, stopping the operation, and cooling to room temperature to obtain metal tellurium and metal cadmium respectively.
The purity of the obtained tellurium metal reaches 99.5 percent, and the purity of cadmium reaches 98 percent.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (6)
1. A method for recycling metal tellurium from tellurium-containing waste through vacuum fractional condensation is characterized in that the tellurium-containing waste is placed in a vacuum fractional condensation furnace, then vacuum pumping is carried out, vacuum thermal decomposition is carried out after temperature rising, then fractional condensation is carried out through temperature adjustment, operation is stopped after heat preservation, and metal tellurium and other valuable metals are obtained respectively.
2. The method for recovering tellurium metal by vacuum fractional condensation of tellurium-containing waste as claimed in claim 1, wherein: the method comprises the following specific steps:
placing tellurium-containing waste into a vacuum fractional condensation furnace, vacuumizing to 1-500 Pa, heating to 400-650 ℃, and preserving heat for 30-120 min;
and (2) continuing heating to 700-1000 ℃, enabling tellurium and other volatile metals to enter a gas phase to form mixed metal steam, controlling the temperature of a condensation zone of tellurium to be 200-400 ℃, keeping the temperature for 30-90 min, stopping the operation, and cooling to room temperature to obtain metal tellurium and other valuable metals respectively.
3. The method for recovering tellurium metal by vacuum fractional condensation of tellurium-containing waste as claimed in claim 2, wherein: and (2) the tellurium-containing waste materials in the step (1) are lead telluride, bismuth telluride, cadmium telluride and gold telluride waste materials.
4. The method for recovering tellurium metal by vacuum fractional condensation of tellurium-containing waste as claimed in claim 2, wherein: the vacuum fractional condensation furnace in the step (1) is a vacuum tube furnace, the temperature gradient is formed in the furnace, and the temperature of each section is controllable.
5. The method for recovering the metallic tellurium by the vacuum fractional condensation of the tellurium-containing waste as claimed in claim 2, wherein: the vacuum degree of the system is 1-500 Pa during fractional condensation.
6. The method for recovering tellurium metal by vacuum fractional condensation of tellurium-containing waste as claimed in claim 2, wherein: and (3) mixing the components of the metal steam in the step (2) into tellurium, lead, bismuth and cadmium.
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