CN105624404A - Environmental-friendly comprehensive utilization method for waste residues - Google Patents
Environmental-friendly comprehensive utilization method for waste residues Download PDFInfo
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- CN105624404A CN105624404A CN201610011499.5A CN201610011499A CN105624404A CN 105624404 A CN105624404 A CN 105624404A CN 201610011499 A CN201610011499 A CN 201610011499A CN 105624404 A CN105624404 A CN 105624404A
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- waste residue
- comprehensive utilization
- ionic liquid
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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
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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
- C22B61/00—Obtaining metals not elsewhere provided for in this subclass
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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)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Processing Of Solid Wastes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses an environmental-friendly comprehensive utilization method for waste residues, and belongs to the field of comprehensive utilization of resources. The environmental-friendly comprehensive utilization method for the waste residues is characterized by comprising the following steps: (1) waste residue selection; (2) waste residue treatment; (3) extractive additive addition; (4) ionic liquid addition; (5) roasting reaction; and (6) leaching. Compared with the prior art, the environmental-friendly comprehensive utilization method disclosed by the invention is capable of obviously lowering temperature of extractive reaction, therefore a large amount of energy is saved, and emission of carbon dioxide and particulate matter is reduced; the comprehensive utilization method is environmental friendly; while vanadium is extracted efficiently, effective extraction and comprehensive utilization can also be performed on tellurium in the waste residues; and the environmental-friendly comprehensive utilization method for the waste residues is a double-purpose method.
Description
Technical field
The invention discloses a kind of eco-friendly waste residue method of comprehensive utilization, belong to the field of comprehensive utilization of resources.
Background technology
Climb the special zone that the only one that western strategic resource pilot development zone is domestic at present is set up for the purpose of mineral resources comprehensive utilization. To Flos Bombacis Malabarici, the domestic vanadium titanium of western, Goats in Liangshan Prefecture and Ya'an, rare earth and tellurium bismuth resource carry out comprehensive process and utilization. Vanadium, tellurium belong to yttrium, are a kind of important strategic materials. Because it has excellent alloy and catalytic action, it is widely used in the national defence such as metallurgy, chemical industry, machinery, electronic instrument, automobile boats and ships, light industry sophisticated technology department. Vanadium, tellurium is currently without the rich ore that can individually develop, always low-grade with other mineral intergrowth. Particularly at Panxi Diqu, vanadium, tellurium content in mine tailing or waste residue is not low. If able to research and develop a kind of novel, eco-friendly extracting method, not only there is important economic implications, also there is highly important strategic importance.
Ionic liquid, as the term suggests, it is simply that it is made up of zwitterion completely, the salt compounds being at room temperature in a liquid state. Different from traditional solid salt, with the fuse salt molecule that liquid condition exists, there is designability, different zwitterions can be combined into miscellaneous ionic liquid. By selecting different zwitterions, or it is introduced directly into specific functional group and modifies, the character to ionic liquid, as fusing point, viscosity, hydrophobicity are adjusted, meet different needs. Ionic liquid is because of the saturated vapor pressure substantially not recorded, thus the chemical solvent using ionic liquid more traditional than use more conforms to eco-friendly Green Development theory. Ionic liquid has designability, and by adjusting different zwitterions pair, it is possible to design kind difference, the special ionic liquid meeting different needs comes.
We find by studying, the ionic liquid of the functionalization through particular design is combined with nano-calcium carbonate or calcium oxide, it is applied to waste residue comprehensive utilization, the temperature of extracting reaction can be greatly lowered, simultaneously can also reclaim, with significantly high yield, the rare scattered strategy element that vanadium, tellurium two kinds are important.
Summary of the invention
The invention discloses a kind of eco-friendly waste residue method of comprehensive utilization, climb the current distinctive waste residue in western strategic resource pilot development zone according to China, therefrom extract the strategic materials that rare bulk weight such as vanadium, tellurium is wanted.
The concrete technical scheme that the present invention specifically adopts is:
A kind of eco-friendly waste residue method of comprehensive utilization, comprises the following steps:
(1) selected waste residue: detect via ICP-MS, the selected waste residue containing vanadium, two kinds of metals of tellurium.
Preferred waste residue be contain by weight percentage the amount of vanadium metal be 0.1%-2%, amount containing metallic tellurium be 0.01%-0.6%; And with the amount containing vanadium metal for 0.5%-1.5%, the waste residue that amount is 0.05%-0.5% containing metallic tellurium is best.
(2) waste residue is processed: waste residue selected in step (1) is carried out ball milling and process of sieving, the waste residue after being processed.
The powder body of the waste residue after process is preferably 20 order-250 orders, and with 80-200 order for the best.
(3) extraction auxiliary agent is added: in the waste residue after process, add nano-calcium carbonate or nano calcium oxide, or by both mixture with arbitrary proportion mixing, mix homogeneously.
The particle size distribution of nano-calcium carbonate or nano calcium oxide is preferably 20-250 nanometer, and with 50-100 nanometer for best. The consumption of nano-calcium carbonate or nano calcium oxide by the 1%-10% of extraction slag quality, and with 2%-8% for the best.
(4) ionic liquid is added: in the waste residue of step (3), add ionic liquid; The chemical formula of described ionic liquid is:
(5) reaction: step (4) adding the waste residue mix homogeneously of ionic liquid, joins in multisection type numeral temperature control Muffle furnace and react, reaction temperature is 500 DEG C-850 DEG C, and the response time is 1-10 hour.
Wherein, reaction temperature 550 DEG C-700 DEG C is best; 1.5-5 hour response time was best.
(6) leach: the powder body after above-mentioned steps (5) being sintered leaches with described ionic liquid, filters insoluble matter, the calcium salt of the ionic liquid i.e. calcium salt of Vanadium Concentrationin and tellurium mutually. By simply regulate pH value can by vanadium, tellurium calcium salt from ionic liquid mutually in release, subsequently through conventional method (such as literature method " steel vanadium titanium ", 2012,33,30-34.) prepared vanadium metal, tellurium. Ionic liquid obtains reuse.
Compared with prior art, the beneficial effects of the present invention is:
1) present invention adds described ionic liquid and introduces the reaction of congruent melting, forms liquid phase, makes sintering temperature step-down, carry out liquid phase reactive sintering, it is achieved low-temperature sintering, reduce the temperature of sintering. In follow-up leaching extraction process, introduce custom-designed ionic liquid, to reaching following purpose: a. is by adjusting the radius size of cation middle cavity, reach containing vanadium, one best absorption (chelation) ability of tellurium sintered product, namely only with the just energy enrichment as much as possible of a small amount of ionic liquid; B. by regulating, pH value is energy-conservation reaches absorption, the effect resolved, so that ionic liquid can be reused.
2) present invention can significantly reduce the temperature extracting reaction, thus saving mass energy and the discharge reducing carbon dioxide and particulate matter; Emit no waste water simultaneously, save valuable freshwater resources, environmental friendliness.
3) while high efficiency extracts vanadium, moreover it is possible to the tellurium in waste residue carrying out effective extraction and comprehensive utilization, is a kind of method killed two birds with one stone, ionic liquid can repeat to apply mechanically simultaneously, reduces cost.
Detailed description of the invention
It is further detailed below in conjunction with specific embodiment.
Embodiment 1
Weigh the described waste residue of 1000 grams, separate through ICP-MS before extracting, it is determined that wherein contain vanadium 1.0 grams, tellurium 0.6 gram. Ball milling, sieves, particle size distribution 100 order. Being subsequently added calcium carbonate and each 3 grams of the calcium oxide of 80 nanometer particle sizes, continuously add ionic liquid 20 grams, add in multisection type numeral temperature control Muffle furnace, design temperature is 600 DEG C, 2.5 hours response time. After leaching, investigating vanadium, the response rate of tellurium, result: to vanadium 85%, to tellurium 90%.
Claims (8)
1. an eco-friendly waste residue method of comprehensive utilization, it is characterised in that in turn include the following steps:
(1) selected waste residue: after testing, the selected waste residue containing vanadium, two kinds of metals of tellurium;
(2) waste residue is processed: selected waste residue is carried out ball milling and process of sieving, the waste residue after being processed;
(3) extraction auxiliary agent is added: in the waste residue after process, add nano-calcium carbonate, nano calcium oxide or the mixture mixed by both, mix homogeneously with arbitrary proportion;
(4) ionic liquid is added: in the waste residue of step (3), add ionic liquid; The chemical formula of described ionic liquid is:
(5) reaction: step (4) adding the waste residue mix homogeneously of ionic liquid, joins in multisection type numeral temperature control Muffle furnace and react, reaction temperature is 500 DEG C-850 DEG C, and the response time is 1-10 hour;
(6) leach: the powder body after above-mentioned steps (5) being sintered leaches with described ionic liquid, filters insoluble matter, the calcium salt of the ionic liquid i.e. calcium salt of Vanadium Concentrationin and tellurium mutually.
2. eco-friendly waste residue method of comprehensive utilization according to claim 1, it is characterised in that contain vanadium metal in the waste residue described in step (1) by weight percentage and be 0.1%-2%, be 0.01%-0.6% containing metallic tellurium.
3. eco-friendly waste residue method of comprehensive utilization according to claim 1, it is characterised in that the powder body of the waste residue after the process described in step (2) is 20 order-250 orders.
4. eco-friendly waste residue method of comprehensive utilization according to claim 1, it is characterised in that the particle size distribution of the nano-calcium carbonate described in step (3) or nano calcium oxide is 20-250 nanometer.
5. eco-friendly waste residue method of comprehensive utilization according to claim 1, it is characterised in that the reaction temperature described in step (5) is 550 DEG C-700 DEG C.
6. eco-friendly waste residue method of comprehensive utilization according to claim 1, it is characterised in that the response time described in step (5) is 1.5-5 hour.
7. the eco-friendly waste residue method of comprehensive utilization according to claim 1 or claim 4, it is characterised in that the consumption of the nano-calcium carbonate described in step (3) or nano calcium oxide by the 1%-10% of extraction waste residue weight.
8. the eco-friendly waste residue method of comprehensive utilization according to claim 1 or claim 5, it is characterised in that the 10%-25% that consumption is waste residue weight of the ionic liquid described in step (4).
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Citations (5)
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| JP2006080488A (en) * | 2004-08-12 | 2006-03-23 | Bridgestone Corp | Non-aqueous electrolytic solution for electric double layer capacitor and non-aqueous electrolytic solution electric double layer capacitor |
| WO2008152452A2 (en) * | 2007-06-11 | 2008-12-18 | Mehlin Matthews | System and method for isotope separation |
| CN101597776A (en) * | 2009-07-07 | 2009-12-09 | 武汉大学 | A kind of metal sulfide M 1The metallurgical method of S |
| CN103031571A (en) * | 2012-12-13 | 2013-04-10 | 彩虹集团公司 | Method for electrodepositing gallium at low temperature by using ionic liquid |
| CN103924084A (en) * | 2014-03-21 | 2014-07-16 | 南通大学 | Method for recovering valuable metal element in waste phosphor by using phosphonium ionic liquid |
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2016
- 2016-01-08 CN CN201610011499.5A patent/CN105624404B/en active Active
Patent Citations (5)
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| JP2006080488A (en) * | 2004-08-12 | 2006-03-23 | Bridgestone Corp | Non-aqueous electrolytic solution for electric double layer capacitor and non-aqueous electrolytic solution electric double layer capacitor |
| WO2008152452A2 (en) * | 2007-06-11 | 2008-12-18 | Mehlin Matthews | System and method for isotope separation |
| CN101597776A (en) * | 2009-07-07 | 2009-12-09 | 武汉大学 | A kind of metal sulfide M 1The metallurgical method of S |
| CN103031571A (en) * | 2012-12-13 | 2013-04-10 | 彩虹集团公司 | Method for electrodepositing gallium at low temperature by using ionic liquid |
| CN103924084A (en) * | 2014-03-21 | 2014-07-16 | 南通大学 | Method for recovering valuable metal element in waste phosphor by using phosphonium ionic liquid |
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| 姚佳良等: ""两种咪唑类室温离子液体对Te纳米棒状结构生长的影响"", 《化学研究与应用》 * |
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| 赵秋凝等: ""离子液体在稀散金属及其合金电沉积中的应用"", 《稀有金属》 * |
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