CN109913671A - Microwave sulfating roasting-nanofiltration membrane enrichment recovery method for uranium niobium-titanium ore - Google Patents
Microwave sulfating roasting-nanofiltration membrane enrichment recovery method for uranium niobium-titanium ore Download PDFInfo
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- CN109913671A CN109913671A CN201910203825.6A CN201910203825A CN109913671A CN 109913671 A CN109913671 A CN 109913671A CN 201910203825 A CN201910203825 A CN 201910203825A CN 109913671 A CN109913671 A CN 109913671A
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Abstract
The invention provides a microwave sulfating roasting-nanofiltration membrane enrichment recovery method of uranium-niobium-titanium ore, which comprises the steps of mixing niobium-titanium-uranium ore powder with acid, roasting under the microwave condition to obtain roasted slag, leaching the roasted slag by using a leaching agent to obtain a leaching solution, and finally applying pressure to the leaching solution to filter redundant water through a nanofiltration membrane to obtain a uranium-containing concentrated solution. The leaching solution containing relevant metal salts is obtained by carrying out microwave roasting and acid leaching on the uranium-titanium-niobium ore powder, then a nanofiltration membrane is used for treating the leaching solution containing a large amount of metal salts and water molecules, the water molecules with smaller molecular mass pass through the nanofiltration membrane under certain pressure, and the uranium-containing metal salts are intercepted due to larger molecular mass, so that the uranium-containing concentrated solution with higher concentration is obtained.
Description
Technical field
The invention belongs to a kind of microwave of metal smelt technical field more particularly to betafite sulfating roasting-nanofiltrations
Film enriching and recovering method.
Background technique
Uranium is particularly important in the world energy minerals and strategic mineral resources, especially obtains wideling popularize in terms of nuclear power and answer
With, and the current nuclear power occupation rate in China is less than 4%, for this purpose, country proposes the planning of positive Nuclear Power Development.Currently, from uranium ore
Middle enriching and recovering uranium method specifically includes that ground-dipping uranium extraction, heap extraction uranium, concentrated acid curing high-speed rail leaching heap Leaching, serial heap leaching
Technology, bacterial oxidation heap Leaching etc..Conventional hydrometallurgy need by broken, ore grinding, leaching, separation of solid and liquid, ion exchange or/
It is complicated for operation with the methods of extraction, precipitating, dehydration, drying, it is suitable only for the leaching of high-grade uranium ore, if being used for low-grade uranium
Then cost is too high for ore.Dump leaching method is by the way that chemical solvent to be sprayed on the ore storage for the coarse crushing banked up in advance, selectively
The uranium in ore is dissolved, ion or complex ion is formed it into and is allowed to be transferred to solution, then further extracted.Dump leaching method
It is suitble to the leaching of low-grade ore, but that there are acid consumptions is big, period of heap leaching is long, hardened, blocking and causes to environment biggish in heap
The problems such as pollution, the effect is unsatisfactory.Although avoiding, the leaching mine period is long, acid consumption is big, broken for diafiltration lixiviation process (Chemical Leaching method)
Broken ore the problems such as energy consumption is high, hardened, but its is at high cost, economic benefit is not satisfactory.
Niobium titanium uranium contains 26.6% orange oxide, 34.80% niobium pentaoxide, 18.30% titanium dioxide and other impurities,
Its uranium grade is low, and density strength is all larger, extracts uranium, concentrated acid curing high-speed rail leaching dump leaching using traditional ground-dipping uranium extraction, heap
The technologies such as technology, serial heap leaching technology, bacterial oxidation dump leaching are extremely low to the rate of recovery degree of uranium, cause huge waste.
Summary of the invention
Based on this, the present invention provides a kind of microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite, passes through
This method can obtain the high uranium enrichment liquid of the uranium rate of recovery, high efficiency from betafite, and method is simple, environmentally protective.
Microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite of the present invention the following steps are included:
S1: betafite powder and acid-mixed conjunction are placed on and are roasted to obtain fired slags under microwave；
S2: fired slags are leached using leaching agent to obtain leachate；
S3: nanofiltration membrane is made it through to leachate application pressure and filters out excessive moisture, obtains uranium-bearing concentrate.
Compared with prior art, the present invention by microwave calcining and leaching agent by leaching to obtain betafite powder
Leachate containing uranium metal salt reuses the nanofiltration membrane that aperture is 1nm or so and handles the leachate, in certain pressure
Under, the small molecules such as lesser hydrone of molecular mass pass through nanofiltration membrane, and uranium metal salt is trapped since molecular mass is larger, from
And obtain the higher uranium-bearing concentrate of concentration.
Further, the pressure size is 0.1~2MPa.
Further, the microwave power is 300~1600W, and the microwave frequency is 2400~2500MHz.Pass through microwave
Roasting, can make betafite structure become loose, and particle surface generates a large amount of holes, be conducive to it is subsequent contacted with leaching agent,
Improve leaching rate.
Further, the pressure in step S3 is 0.5~1.5MPa.If leachate is excessively high by the pressure of nanofiltration membrane, it is easy
Generate bubble；It was discharged if bubble is too low slow；By pressure control within the scope of 0.5~1.5MPa then it is possible to prevente effectively from these
Problem.
Further, the acid and leaching agent are 98% concentrated sulfuric acid.
Further, the mass ratio of the concentrated sulfuric acid and betafite powder is (0.2~0.6) in step S1: 1.
Further, the quality of the concentrated sulfuric acid is the 5%~10% of mine weight in step S2.
Further, the treatment temperature of step S2 is 0~60 DEG C, and the leaching time is 0.5~2h, and leaching liquid-solid ratio is 3:
1~6:1.
Detailed description of the invention
Fig. 1 is flow chart of the method for the present invention.
Specific embodiment
As shown in Fig. 1 method flow diagram, the present invention pass through first microwave calcining make betafite generate loose hole so as to
In subsequent Ore Leaching, processing finally is carried out to leachate using nanofiltration membrane and filters off hydrone, obtains the very high concentration of uranium content
Liquid.Carry out the technical solution that the present invention will be described in detail below by way of specific embodiment.
Embodiment 1
Microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite of the present invention the following steps are included:
S1: betafite powder and acid-mixed conjunction are placed on and are roasted to obtain fired slags under microwave；
Specifically, the fine grinding after the betafite weight magnetic of uranium-bearing 0.24% is first obtained into betafite concentrate powder, so
The water that mine weighs 20% is added afterwards, wetting stirs evenly, adds the concentrated sulfuric acid, be stirred for, is uniformly mixed and obtains mixture slurry；Wherein
The mass ratio of the concentrated sulfuric acid and betafite concentrate powder is 0.25:1.
By mixture slurry be placed in self-control microwave tube type oven in, microwave power be 500W, microwave frequency 2450MHz, temperature
Degree carries out microwave calcining 20min under the conditions of being 210 DEG C and obtains fired slags.
S2: fired slags are leached using leaching agent to obtain leachate；
The sulfuric acid that mine weighs 5% is added in fired slags, is stirred under conditions of temperature is 20 DEG C with the speed of 150r/min
1h is then separated by solid-liquid separation, and supernatant liquid is taken to obtain leachate, wherein leaching liquid-solid ratio is 3:1.
S3: nanofiltration membrane is made it through to leachate application pressure and filters out excessive moisture, obtains uranium-bearing concentrate.
Will above-mentioned leachate be added nanofiltration membrane enriching machine in, setting nano-filtration membrane equipment pressure be 0.6MPa, flow velocity 30ml/
Min respectively obtains uranium-bearing concentrate and penetrating fluid in nanofiltration membrane two sides.
The rate of recovery by detecting and being calculated uranium in the present embodiment is 97.16%.
In the microwave sulfating roasting-nanofiltration membrane enriching and recovering method, contain orange oxide, niobium pentaoxide and dioxy
The betafite powder for changing titanium generates loose hole after microwave calcining, and sulfuric acid enters inside ore along hole by three oxidations
Uranium, niobium pentaoxide and titanium dioxide dissolution generate corresponding metal salt and enter in solution；It the use of aperture is finally 1nm's or so
When nanofiltration membrane handles leachate, the small molecules such as lesser hydrone of molecular mass pass through nanofiltration membrane, and uranium metal salt by
It is trapped in molecular mass is larger, to obtain the higher uranium-bearing concentrate of concentration.
Embodiment 2
Microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite of the present invention the following steps are included:
S1: betafite powder and acid-mixed conjunction are placed on and are roasted to obtain fired slags under microwave condition；
Specifically, the fine grinding after the betafite weight magnetic of uranium-bearing 0.288% is first obtained into betafite concentrate powder, so
The water that mine weighs 20% is added afterwards, wetting stirs evenly, adds the concentrated sulfuric acid, be stirred for, is uniformly mixed and obtains mixture slurry；Wherein
The mass ratio of the concentrated sulfuric acid and betafite concentrate powder is 0.3:1.
By mixture slurry be placed in self-control microwave tube type oven in, microwave power be 600W, microwave frequency 2400MHz, temperature
Degree carries out microwave calcining 30min under the conditions of being 240 DEG C and obtains fired slags.
S2: fired slags are leached using leaching agent to obtain leachate；
The sulfuric acid that mine weighs 7.5% is added in fired slags, is stirred under conditions of temperature is 40 DEG C with the speed of 200r/min
1.2h is mixed, is then separated by solid-liquid separation, supernatant liquid is taken to obtain leachate, wherein leaching liquid-solid ratio is 4:1.
S3: nanofiltration membrane is made it through to leachate application pressure and filters out excessive moisture, obtains uranium-bearing concentrate.
Above-mentioned leachate is added in nanofiltration membrane enriching machine, setting nano-filtration membrane equipment pressure is 0.75MPa, flow velocity is
50ml/min respectively obtains uranium-bearing concentrate and penetrating fluid in nanofiltration membrane two sides.
The rate of recovery by detecting and being calculated uranium in the present embodiment is 97.48%.
Embodiment 3
Microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite of the present invention the following steps are included:
S1: betafite powder and acid-mixed conjunction are placed on and are roasted to obtain fired slags under microwave condition；
Specifically, the fine grinding after the betafite weight magnetic of uranium-bearing 0.408% is first obtained into betafite concentrate powder, so
The water that mine weighs 20% is added afterwards, wetting stirs evenly, adds the concentrated sulfuric acid, be stirred for, is uniformly mixed and obtains mixture slurry；Wherein
The mass ratio of the concentrated sulfuric acid and betafite concentrate powder is 0.4:1.
By mixture slurry be placed in self-control microwave tube type oven in, microwave power be 750W, microwave frequency 2500MHz, temperature
Degree carries out microwave calcining 40min under the conditions of being 270 DEG C and obtains fired slags.
S2: fired slags are leached using leaching agent to obtain leachate；
The sulfuric acid that mine weighs 9% is added in fired slags, is stirred under conditions of temperature is 60 DEG C with the speed of 300r/min
1.5h is then separated by solid-liquid separation, and supernatant liquid is taken to obtain leachate, wherein leaching liquid-solid ratio is 5:1.
S3: nanofiltration membrane is made it through to leachate application pressure and filters out excessive moisture, obtains uranium-bearing concentrate.
Above-mentioned leachate is added in nanofiltration membrane enriching machine, nano-filtration membrane equipment pressure 1.0MPa, flow velocity 60ml/ are set
Min respectively obtains uranium-bearing concentrate and penetrating fluid in nanofiltration membrane two sides.
The rate of recovery by detecting and being calculated uranium in the present embodiment is 98.05%, and uranium enrichment liquid is dried
Uranium metal purity salt is 30% in solid afterwards.
Compared with the existing technology, the present invention is by passing through microwave calcining and acid for the very low betafite powder of uranium content
Leaching obtains the leachate containing uranium metal salt, reuses nanofiltration membrane and handles leachate, in 0.5~1.5MPa pressure
Under, the lesser hydrone of molecular mass passes through nanofiltration membrane, and uranium metal salt is trapped since molecular mass is larger, to obtain dense
Higher uranium-bearing concentrate is spent, the rate of recovery of uranium may be up to 98% or more.The method of the present invention is simple, environmentally protective, has very high
Benefit.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.
Claims (8)
1. a kind of microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite, it is characterised in that the following steps are included:
S1: betafite powder and acid-mixed conjunction are placed on and are roasted to obtain fired slags under microwave；
S2: fired slags are leached using leaching agent to obtain leachate；
S3: nanofiltration membrane is made it through to leachate application pressure and filters out excessive moisture, obtains uranium-bearing concentrate.
2. microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite, feature exist according to claim 1
In: the pressure size is 0.1~2MPa.
3. microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite, feature exist according to claim 2
In: the microwave power is 300~1600W, and the microwave frequency is 2400~2500MHz.
4. microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite, feature exist according to claim 3
In: the pressure in step S3 is 0.5~1.5MPa.
5. microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite, feature exist according to claim 4
In: the acid and leaching agent are 98% concentrated sulfuric acid.
6. microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite, feature exist according to claim 5
In: the mass ratio of the concentrated sulfuric acid and betafite powder is (0.2~0.6) in step S1: 1.
7. microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite, feature exist according to claim 6
In: the quality of the concentrated sulfuric acid is the 5%~10% of mine weight in step S2.
8. microwave sulfating roasting-nanofiltration membrane enriching and recovering method of betafite, feature exist according to claim 7
In: the treatment temperature of step S2 is 0~60 DEG C, and the leaching time is 0.5~2h, and leaching liquid-solid ratio is 3:1~6:1.
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Cited By (2)
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| CN112505264A (en) * | 2021-02-08 | 2021-03-16 | 中国工程物理研究院核物理与化学研究所 | A sea trial test device for uranium is carried to sea water |
| CN113265540A (en) * | 2021-04-14 | 2021-08-17 | 东华理工大学 | Method for strengthening extraction of uranium in low-grade uranium ore through microwave activation roasting |
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Application publication date: 20190621 |