CN108285981A - A kind of burned-coal fly ash puies forward uranium method - Google Patents
A kind of burned-coal fly ash puies forward uranium method Download PDFInfo
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/18—Extraction of metal compounds from ores or concentrates by wet processes with the aid of microorganisms or enzymes, e.g. bacteria or algae
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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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0221—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching
- C22B60/0226—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors
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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
- C22B7/02—Working-up flue dust
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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
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Abstract
The invention discloses a kind of burned-coal fly ash to put forward uranium method, by [Hbet]+[CF3COO]‑Ionic liquid and fermentation of Aspergillus niger liquid together leach burned-coal fly ash.It utilizes environmentally protective [Hbet]+[CF3COO]‑Ionic liquid and cheap fermentation of Aspergillus niger liquid leach the uranium in burned-coal fly ash, this puies forward uranium method difficult, the big problem of environmental pollution that solves Uranium extraction in current burned-coal fly ash.
Description
Technical field
The present invention relates to one kind putting forward uranium method, more particularly to provides a kind of utilization [Hbet]+[CF3COO]-Ionic liquid
The method for leaching uranium in burned-coal fly ash is cooperateed with fermentation of Aspergillus niger liquid.
Background technology
Burned-coal fly ash be from the flue gas of coal-burning boiler catching to fine ash, be that the inorganic mineral in coal is (main
To contain the elements such as silicon, aluminium, calcium, iron) by decomposition, sintering, melting and it is cooling after the grain size that is formed be 0.1 μm~100 μm
Between solid particle, content accounts for about the 5%~20% of coal-fired total amount.Its chemical composition is similar to clay, predominantly SiO2、
A12O3、Fe2O3, CaO and uncombusted charcoal, a small amount of Na2O, MgO and K2O etc., also micro U, Se, Sn, W, Cu, Ag, Pb,
The elements such as Ba, Cr, Mn.For a long time, China is production and the consumption big country of fossil energy coal, the discharge of burned-coal fly ash
Measure huge, only China's flying dust total release in 2010 is just up to 300,000,000 tons, it is contemplated that the annual emissions of the year two thousand twenty will also increase by 3 times.Coal passes through
Natural radioactive element uranium is largely enriched in flying dust after burning, and radioactive activity improves nearly 10 times.According to detection, China
Flying dust uranium grade is such as calculated with 200 μ g/g between 10~400 μ g/g, if China year fly ash emission amount is 300,000,000 tons, I
The content of uranium is up to 60,000 tons in the flying dust that state is discharged every year.Burned-coal fly ash is a kind of very important unconventional low-grade
Uranium resource.At the same time, the uranium in the burned-coal fly ash of storeyard is constantly leached under physics, chemical weathering, and with
Surface water and groundwater migrates, and radioactive pollution is caused to environment.Therefore, research and development burned-coal fly ash puies forward uranium method and is conducive to ensure
National strategy type natural uranium mineral resources are supplied, and uranium resource range can be utilized by expanding China, improve uranium resource deposit, be improved natural
Uranium production technology level, while can effectively solve the radioactive pollution of uranium-bearing burned-coal fly ash.
H is mostly used greatly at present2SO4、 NH4HSO4、(NH4)2CO3Equal leachants leach the uranium in burned-coal fly ash, or first
The uranium in burned-coal fly ash is enriched with using preconditioning techniques such as high-temperature roasting, magnetic separation, then uses H2SO4、 NH4HSO4、
(NH4)2CO3Equal leachants are leached.Although the above method can leach in burned-coal fly ash 30 ~ 80% uranium, actually answering
There are many deficiencies in, such as sour consumption is big, high energy consumption, of high cost, environmental pollution is serious, complicated for operation.It is therefore desirable to
Exploitation burned-coal fly ash puies forward uranium new method.
Invention content
Present invention solves the technical problem that being low-grade uranium-containing materials such as burned-coal fly ash, the acid consumption during uranium is put forward
Amount is big, high energy consumption, of high cost, environmental pollution is serious, complicated for operation etc..
The technical scheme is that providing one kind putting forward uranium method, by [Hbet]+[CF3COO]-Ionic liquid and aspergillus niger
Zymotic fluid together leaches uranium-containing materials.
The present invention is more particularly directed to by [Hbet]+[CF3COO]-Ionic liquid and fermentation of Aspergillus niger liquid together to burned-coal fly ash into
Row leaches.Wherein, the H in Hbet indicates that hydrogen, bet indicate glycine betaine.
Preferably, the preparation method of the fermentation of Aspergillus niger liquid is：Black-koji mould live body is cultivated with culture medium, is trained
Mycelia is removed after supporting, obtains fermentation of Aspergillus niger liquid.
Preferably, condition of culture is：It is cultivated in shaking table, the temperature setting of shaking table is 28-32 DEG C, and rotating speed is set as
100-200 rpm are filtered to remove mycelia after expanding culture 50-80 h.
Preferably, black-koji mould live body is cultivated with potato dextrose agar fluid nutrient medium.
Preferably, described [Hbet]+[CF3COO]-The preparation method of ionic liquid is：By beet alkali hydrochlorate (HbetCl)
Solution is added dropwise in trifluoroacetic acid sodium solution, obtains sediment, and sediment is filtered, washed, and is obtained [Hbet]+[CF3COO]-
Ionic liquid.
Preferably, the beet alkali hydrochlorate solution of 1 mol/L of 250mL is added dropwise to the trifluoro second of 250mL 1.2mol/L
In acid sodium solution, 1h is stirred, filtering obtains white depositions, is washed with deionized 3 times, is then dried in vacuo at room temperature
48 h are obtained [Hbet]+[CF3COO]-Ionic liquid.
Preferably, 0.1 ~ 5 g [Hbet] is added in every 5 g uranium-containing materials+[CF3COO]-Ionic liquid and 10 ~ 200mL are black
Aspergillus fermentation broth.
Preferably, 0.5 ~ 2 g [Hbet] is added in every 5 g uranium-containing materials+[CF3COO]-Ionic liquid and 30 ~ 120mL are black
Aspergillus fermentation broth.
It is highly preferred that 0.8 ~ 1.5 g [Hbet] is added in every 5 g uranium-containing materials+[CF3COO]-Ionic liquid and 40 ~
60mL fermentation of Aspergillus niger liquid.
Preferably, the temperature of leaching is 20-60 DEG C.
Preferably, extraction time 1-12h.
Preferably, the leaching on the magnetic stirrer that rotating speed is 10 ~ 200 rpm.
Preferably, the uranium-containing materials be burned-coal fly ash, uranium ore, uranium-bearing phosphate ore, radioactivity uranium-bearing incineration of waste fly
One or more of ash, uranium tailings.The uranium-containing materials are more preferably the low-grade uranium-bearings such as burned-coal fly ash, uranium ore, uranium tailings
Material, be particularly suitable for burned-coal fly ash carries uranium.
The present invention utilizes [Hbet]+[CF3COO]-Uranium in burned-coal fly ash is leached in ionic liquid and the collaboration of fermentation of Aspergillus niger liquid
Method includes the following steps：
（1）It prepares [Hbet]+[CF3COO]-Ionic liquid.Specially the beet alkali hydrochlorate solution of 1 mol/L of 250mL is dripped
It is added in the trifluoroacetic acid sodium solution of 250mL 1.2mol/L, stirs 1h, filtering obtains white depositions, is washed with deionized water
It washs 3 times, is then dried in vacuo 48 h at room temperature, obtain [Hbet]+[CF3COO]-。
（2）Prepare fermentation of Aspergillus niger liquid.Specially by black-koji mould live body potato dextrose agar fluid nutrient medium
（PDA）It is cultivated in shaking table, the temperature setting of shaking table is 30 DEG C, and rotating speed is set as 150 rpm, after expanding 60 h of culture, filtering
Mycelia is removed, fermentation of Aspergillus niger liquid is obtained.
（3）Leach the uranium in burned-coal fly ash.Using step（1）With（2）Obtained [Hbet]+[CF3COO]-Ionic liquid and
Fermentation of Aspergillus niger liquid leaches the burned-coal fly ash in the small dragon's pool power plant in Yunnan, and 0 ~ 5 is added specially into 5 g flying dust samples
g [Hbet]+[CF3COO]-Ionic liquid and 10 ~ 200mL fermentation of Aspergillus niger liquid in rotating speed are 10 ~ 200 rpm at 25 ~ 60 DEG C
Magnetic stirrer on leaching 1 ~ 12 h, then utilize uranium in spectrophotometer or ICP-MS analysis leachates and slag specimen
Content, and calculate separately liquid meter leaching rate and slag meter leaching rate.
（4）Recycle the uranium in leachate.Leachate is specially collected, after being tested by uranium concentration, pH value and Eh values, selection
Ion-exchange process recycles the uranium in leachate.
The present invention utilizes environmentally protective [Hbet] using burned-coal fly ash as research object+[CF3COO]-Ionic liquid and honest and clean
The fermentation of Aspergillus niger liquid of valence leaches the uranium in burned-coal fly ash, and the Uranium extraction solved in current burned-coal fly ash is difficult, ring
The heavy-polluted problem in border.
[Hbet] of the present invention+[CF3COO]-The side of uranium in burned-coal fly ash is leached in ionic liquid and the collaboration of fermentation of Aspergillus niger liquid
Method, method, has following technical advantage compared to existing technology：
（1）The environmentally protective environmental pollution of method that this patent provides is few.
（2）The method that this patent provides is high to the leaching rate of uranium in burned-coal fly ash.
（3）[Hbet] needed for method that this patent provides+[CF3COO]-Ionic liquid synthesis is simple.
（4）The fermentation of Aspergillus niger liquid needed for method that this patent provides can be cultivated continuously, and culture speed is fast, of low cost.
（5）The method that this patent provides is applicable not only to the leaching of uranium in burned-coal fly ash, and is also applied for containing mud or more
The low-grade uranium ore such as metal symbiosis, uranium-bearing phosphate ore, radioactivity uranium-bearing refuse incinerating flyash and low-grade uranium tailings are opened
Hair utilizes, and expands utilization of resources range, improves the rate of recovery of resource.
Specific implementation mode
With reference to embodiment, the invention will be further described.
I material
The small dragon's pool power plant burned-coal fly ash sample in Yunnan, aspergillus niger strain, beet alkali hydrochlorate, sodium trifluoroacetate
II principle
The principle of the present invention is：It utilizes [Hbet]+[CF3COO]-The acid effect of ionic liquid makes uranium be dissociated from burned-coal fly ash,
Exposure, then [Hbet]+[CF3COO]-The CF contained in ionic liquid3COO-Group and citric acid, grass in fermentation of Aspergillus niger liquid
The organic acids such as acid, malic acid, lactic acid and the uranium of exposure are complexed, and are leached from burned-coal fly ash to further strengthen uranium.
III method and step
A kind of utilization [Hbet]+[CF3COO]-The method that uranium in burned-coal fly ash is leached in ionic liquid and the collaboration of fermentation of Aspergillus niger liquid,
Its specific steps are：
（1）Using chemical synthesis, prepare [Hbet]+[CF3COO]-Ionic liquid.
（2）Using PDA culture medium culture aspergillus niger, fermentation of Aspergillus niger liquid is obtained.
（3）Using step（1）With（2）Obtained [Hbet]+[CF3COO]-Ionic liquid and fermentation of Aspergillus niger liquid are to Yunnan
The burned-coal fly ash in small dragon's pool power plant is leached.
（4）Concentration, pH value and the Eh values of uranium in leachate are measured, liquid meter leaching rate is calculated.
（5）The uranium content in slag specimen is measured, slag meter leaching rate is calculated.
（6）Recycle the uranium in leachate.
IV embodiment
Embodiment 1：[Hbet]+[CF3COO]-The preparation of ionic liquid：
It weighs 0.2 mol beet alkali hydrochlorates and is dissolved in 250mL distilled water and obtain solution A, weigh 0.3 mol sodium trifluoroacetates
It is dissolved in 250mL distilled water and obtains solution B, be then added dropwise to solution A in solution B in 30 min, stir 1h, filtering obtains
To white depositions, it is washed with deionized 3 times, is then dried in vacuo 48 h at room temperature, obtain [Hbet]+[CF3COO]-。
Embodiment 2：The preparation of fermentation of Aspergillus niger liquid：
0.1 good mL aspergillus niger bacterium solutions of conservation are added to activation in potato dextrose agar fluid nutrient medium (PDA), so
It takes the bacterium solution of partial activation to prepare the bacteria suspension that 10 mL OD values are 0.1 again afterwards, the training of PDA liquid is inoculated by 2 ‰ inoculum concentration
It supports in base, in shaking table（30 ℃、150 rpm）60 h of culture are enlarged, waits for that culture medium grows a large amount of mycelia, is filtered to remove
Mycelia obtains fermentation of Aspergillus niger liquid.
Embodiment 3：
It takes the small dragon's pool power plant burned-coal fly ash 5g in Yunnan to be placed in 150mL ground conical flasks, is separately added into 0.5 g [Hbet]+
[CF3COO]-Ionic liquid and 50 mL fermentation of Aspergillus niger liquid are stirred on the magnetic stirrer that rotating speed is 100 rpm at 25 DEG C
3h is leached, filtering obtains filtrate and slag specimen, slag specimen drying.The 5 mL filtrates and 0.1 g slag sample analysis uranium contents are taken to be respectively
5.62 mg/L and 0.1175 mg/L, while calculating separately liquid meter leaching rate and slag meter leaching rate.As a result liquid meter leaching rate is shown
It is 70.25%, slag meter leaching rate is 73.45%.
Embodiment 4：
It takes the small dragon's pool power plant burned-coal fly ash 5g in Yunnan to be placed in 150mL ground conical flasks, is separately added into 1 g [Hbet]+
[CF3COO]-Ionic liquid and 50 mL fermentation of Aspergillus niger liquid are stirred on the magnetic stirrer that rotating speed is 100 rpm at 25 DEG C
3h is leached, filtering obtains filtrate and slag specimen, slag specimen drying.The 5mL filtrates and 0.1 g slag sample analysis uranium contents is taken to be respectively
6.5064 mg/L and 0.1365mg/L, while calculating separately liquid meter leaching rate and slag meter leaching rate.As a result liquid meter leaching rate is shown
It is 81.33%, slag meter leaching rate is 85.34%.
Embodiment 5：
It takes the small dragon's pool power plant burned-coal fly ash 5g in Yunnan to be placed in 150mL ground conical flasks, is separately added into 1 g [Hbet]+
[CF3COO]-Ionic liquid and 50 mL fermentation of Aspergillus niger liquid, in stirring leaching on the magnetic stirrer that rotating speed is 100 rpm at 40 DEG C
Go out 3h, filter, obtains filtrate and slag specimen, slag specimen drying.The 5 mL filtrates and 0.1 g slag sample analysis uranium contents are taken to be respectively
7.0032 mg/L and 0.1418mg/L, while calculating separately liquid meter leaching rate and slag meter leaching rate.As a result liquid meter leaching rate is shown
It is 87.54%, slag meter leaching rate is 88.64%.
Embodiment 6：
It takes the small dragon's pool power plant burned-coal fly ash 5g in Yunnan to be placed in 150mL ground conical flasks, is separately added into 1 g [Hbet]+
[CF3COO]-Ionic liquid and 50 mL fermentation of Aspergillus niger liquid, in stirring leaching on the magnetic stirrer that rotating speed is 100 rpm at 40 DEG C
Go out 5 h, filter, obtains filtrate and slag specimen, slag specimen drying.The 5 mL filtrates and 0.1 g slag sample analysis uranium contents are taken to be respectively
7.2112mg/L and 0.1473mg/L, while calculating separately liquid meter leaching rate and slag meter leaching rate.Liquid meter leaching rate is 90.14%,
Slag meter leaching rate is 92.07%.
Embodiment 7：
It takes the small dragon's pool power plant burned-coal fly ash 5g in Yunnan to be placed in 150mL ground conical flasks, is separately added into 1 g [Hbet]+
[CF3COO]-Ionic liquid and 100 mL fermentation of Aspergillus niger liquid are stirred on the magnetic stirrer that rotating speed is 100 rpm at 40 DEG C
3h is leached, filtering obtains filtrate and slag specimen, slag specimen drying.The 5 mL filtrates and 0.1 g slag sample analysis uranium contents are taken to be respectively
3.6008mg/L and 0.1462mg/L, while calculating separately liquid meter leaching rate and slag meter leaching rate.Liquid meter leaching rate is 90.02%,
Slag meter leaching rate is 91.36%.
The technical scope of the present invention is not only restricted to the above embodiment, under the premise of not changing its main points, can do various
Change is implemented.Such as change [Hbet]+[CF3COO]-Ionic liquid quality, the volume of fermentation of Aspergillus niger liquid, extraction temperature,
Extraction time, and contained containing the low-grade uranium ore such as mud or more metal symbiosis, uranium-bearing phosphate ore, radioactivity using the method processing
Uranium refuse incinerating flyash and low-grade uranium tailings etc..It is similar to change and change the essence for belonging to the present invention.
Claims (10)
1. one kind putting forward uranium method, which is characterized in that by [Hbet]+[CF3COO]-Ionic liquid and fermentation of Aspergillus niger liquid are together to containing
Uranium material is leached.
2. putting forward uranium method as described in claim 1, which is characterized in that the preparation method of the fermentation of Aspergillus niger liquid is：With training
It supports base to cultivate black-koji mould live body, mycelia is removed after culture, obtains fermentation of Aspergillus niger liquid.
3. putting forward uranium method as claimed in claim 2, which is characterized in that condition of culture is：It is cultivated in shaking table, the temperature of shaking table
Degree is set as 28-32 DEG C, and rotating speed is set as 100-200 rpm, after expanding culture 50-80 h, is filtered to remove mycelia.
4. putting forward uranium method as claimed in claim 2, which is characterized in that with potato dextrose agar fluid nutrient medium to black song
Mould live body is cultivated.
5. putting forward uranium method as described in claim 1, which is characterized in that [Hbet]+[CF3COO]-The preparation of ionic liquid
Method is：Beet alkali hydrochlorate solution is added dropwise in trifluoroacetic acid sodium solution, sediment is obtained, sediment is filtered, washed, and is obtained
To [Hbet]+[CF3COO]-Ionic liquid.
6. putting forward uranium method as claimed in claim 5, which is characterized in that by the beet alkali hydrochlorate solution of 1 mol/L of 250mL
It is added dropwise in the trifluoroacetic acid sodium solution of 250mL 1.2mol/L, stirs 1h, filtering obtains white depositions, uses deionized water
Washing 3 times, is then dried in vacuo 48 h, obtains [Hbet] at room temperature+[CF3COO]-Ionic liquid.
7. putting forward uranium method as described in claim 1, which is characterized in that 0.1 ~ 5 g [Hbet] is added in every 5 g uranium-containing materials+
[CF3COO]-Ionic liquid and 10 ~ 200mL fermentation of Aspergillus niger liquid.
8. putting forward uranium method as described in claim 1, which is characterized in that the temperature of leaching is 20-60 DEG C, extraction time 1-
12h。
9. putting forward uranium method as described in claim 1, which is characterized in that the uranium-containing materials are burned-coal fly ash, uranium ore, uranium-bearing phosphorus
One or more of hydrochlorate mine, radioactivity uranium-bearing refuse incinerating flyash, uranium tailings.
10. putting forward uranium method as described in claim 1, which is characterized in that on the magnetic stirrer that rotating speed is 10 ~ 200 rpm
Leaching.
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| CN201810132670.7A CN108285981B (en) | 2018-02-09 | 2018-02-09 | Method for extracting uranium from fly ash of fire coal |
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| CN201810132670.7A CN108285981B (en) | 2018-02-09 | 2018-02-09 | Method for extracting uranium from fly ash of fire coal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111471859A (en) * | 2020-03-25 | 2020-07-31 | 南华大学 | Method for leaching uranium from low-grade uranium ore by macro-particle reinforced aspergillus niger |
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| CN111471859B (en) * | 2020-03-25 | 2021-08-20 | 南华大学 | Method for leaching uranium from low-grade uranium ore by macro-particle reinforced aspergillus niger |
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