CN106098130B - A kind of method that electroreduction processing low concentration uranium-bearing wastewater produces uranium oxide - Google Patents
A kind of method that electroreduction processing low concentration uranium-bearing wastewater produces uranium oxide Download PDFInfo
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- CN106098130B CN106098130B CN201610440841.3A CN201610440841A CN106098130B CN 106098130 B CN106098130 B CN 106098130B CN 201610440841 A CN201610440841 A CN 201610440841A CN 106098130 B CN106098130 B CN 106098130B
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/14—Processing by incineration; by calcination, e.g. desiccation
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Abstract
The invention discloses the method that a kind of electroreduction processing low concentration uranium-bearing wastewater produces uranium oxide.Appropriate short chain organic matter is first added in low concentration uranium-bearing wastewater, negative electrode is built based on combustible conductive material, anode is built based on stable conductive material；Uranium-containing waste water is handled using dc source or direct current pulse power source, high price uranium ion in water is set to be reduced to low price uranium ion on negative electrode, short chain organic matter is oxidized on anode containing carbon-based and hydroxyl reaction intermediate in water, by control voltage, reduction time, uranium-containing waste water mixing speed, promote low price uranium ion and the uranium-bearing material to form solid-state is complexed in cathode surface containing carbon-based and hydroxyl reaction intermediate；Finally by high temperature burning handling, cathode electrode material is removed, the purpose of high purity uranium oxide is reached.
Description
Technical field
The present invention relates to uranium-containing waste water processing, more particularly to low concentration uranium-bearing wastewater processing and high-purity uranium oxide is produced
Method.
Background technology
A certain amount of contain can be inevitably generated in the activities such as Uranium Mining smelting, uranium fuel refining and nuclear power station operation
Uranium waste water, not only toxicity is big for this kind of waste water, and also certain radioactivity, has great prestige to health and ecological environment
Coerce, therefore carry out uranium-containing waste water treatment research and have important practical significance.On the other hand, as China's Nuclear Power Industry is quickly sent out
Exhibition, the limited uranium fuel production capacity in the country, it is difficult to meet the demand that following Nuclear Power Industry develops, therefore extract recovery uranium-bearing and give up
Uranium resource in water, with major economic value.From the presence rule of uranium ion and its compound in water, typically contain
Uranium waste water is U (VI) aqueous solution of slant acidity mostly.
In recent decades, to eliminate the ambient influnence of low concentration uranium-bearing wastewater and reclaiming uranium resource therein, grind both at home and abroad
Study carefully and developed various wastewater processing method and technology, mainly there is ion-exchange, chemical precipitation method, absorption method, extraction, film skill
Art method, oxidation-reduction method etc..It is worth noting that, most of uranium-containing waste water processing methods and technology are because of application characteristic institute at present
Limit is more difficult while reaching ideal effect in uranium clearance and the aspect of the uranium rate of recovery two.For example, ion-exchange has removing coefficient
The advantages of height, good comprehensive removal effect, but ion exchange resin performance is easily done by Organic substance in water and coexisting ion
Influence is disturbed, thus it is limited to the uranium-containing waste water treatment effect of complicated component to this method；The technique of chemical precipitation method is simple, cost
It is relatively low, but the more difficult recovery of uranium-bearing sediment produced during large-scale application, it is retained in nature and easily causes secondary pollution.
In view of this, the present invention proposes a kind of low-voltage reduction treatment low concentration uranium-bearing wastewater high purity uranium oxide
Method.The high price uranium ion reduction complexing of low concentration in water can be finally translated into by high-purity solid-state uranium oxygen by this method
Compound, so as to reach the purpose of uranium pollutant and recovery high purity uranium oxide in water removal.
The content of the invention
The problem of existing for the above method and technology, the present invention is based on different valence state uranium ion and its compound water-soluble
Existing forms feature and electrochemical properties in liquid, propose a kind of low-voltage reduction treatment low concentration uranium-bearing wastewater high purity uranium
The method of oxide, to realize the purpose for removing uranium pollutant and recovery high purity uranium oxide in water removal.
The present invention cardinal principle be：In an acidic solution, U (VI) is reducible under certain potential is converted into U (IV), right
The electrode reaction answered is：UO2 2++ 4H+2e-=U4++ 2H2O E Q =0.327V vs.RHE.High toxicity compared to U (VI) and
Ease of solubility, U (IV) toxicity is relatively low, and easily with other ions in water and group (e.g., CO3 2-、OH-, dissolved oxygen etc.) complexing is heavy
Form sediment, facilitate centralized recovery.In addition, U (VI) electroreduction needs to occur under certain potential for U (IV) reaction, therefore
By controlling electric power output voltage size, it is ensured that the reaction that U (VI) is reduced to U (IV) preferentially occurs, and purposefully suppresses uranium-bearing
The reduction process of the coexisting ion of other in waste water and group, obtains the uranium-bearing material of high-purity.Therefore, the present invention is first in low concentration
Appropriate short chain organic matter is added in uranium-containing waste water, by applying the voltage of suitable size on yin, yang electrode, is promoted in water
U (VI) is reduced on negative electrode (reducing electrode) and is converted into U (IV), promotes the organic matter of addition to be aoxidized on anode (oxidizing electrode)
Containing carbon-based and hydroxyl reaction intermediate, further by stirring waste water solution and control voltage action time etc., to promote water
The U (IV) of middle generation is deposited on cathode surface with being gradually complexed containing carbon-based and hydroxyl reaction intermediate；At burning
Reason, removes cathode electrode material, obtains high-purity uranium oxide, reaches the purpose removed with uranium in recycle-water.
The technical scheme is that：A kind of method that electroreduction processing low concentration uranium-bearing wastewater produces uranium oxide, it is main
To be able to by pre-processing 3 key steps such as-uranium-containing waste water electroreduction-solid product heat treatment to low concentration uranium-bearing wastewater
Realize, it is specific as follows：
A, low concentration uranium-bearing wastewater pretreatment：The uranium-containing waste water that 100 mL uranium ions concentration are less than 0.05 mg/L is measured, profit
Filtration treatment is carried out to it with filtration gauze, the insoluble matter impurity in water is filtered off；Then, toward 0.1-2.0 mol/L of addition in water
Short chain organic matter, it is ensured that low concentration uranium-bearing wastewater pH value after pretreatment be less than 7.0.
B, uranium-containing waste water electroreduction：It is combustible with Carbon fibe paper etc. using pretreated uranium-containing waste water as electrolyte
Negative electrode (reducing electrode) is built based on conductive material, anode (oxidation electricity is built based on the stable conductive material such as graphite
Pole), build wastewater treatment electrolytic cell.Reduction treatment is carried out to uranium-containing waste water using dc source or direct current pulse power source, made
Electricity consumption is pressed in the range of 0.33-2.5 V, and total reduction treatment time, waste water mixing speed was at 5-100 revolutions per seconds in 1-10 h.
By fully processing, promote in water high price uranium ion to be converted into short chain organic matter in low price uranium ion, water in reducing electrode and exist
It is converted on oxidizing electrode containing carbon-based and hydroxyl reaction intermediate, most latter two reaction product is in reducing electrode surface complexation shape
Into the uranium-bearing material of solid-state.
C, solid product heat treatment：In atmosphere, the reducing electrode for having solid-state uranium-bearing material to deposition is carried out at high warm
Reason, according to electrode material material, heat treatment temperature is maintained between 300-1800 DEG C, and heat treatment time promotes electricity in 1-10 h
Pole material fully burns, and leaves solid-state uranium oxide of the purity more than 99%.
Brief description of the drawings
The present invention will be further described with embodiment below in conjunction with the accompanying drawings：Fig. 1 contains for the processing that the present invention is built
Uranium wastewater electrolytic pool device schematic diagram；Fig. 2 is uranium-bearing material deposition in different disposal period reducing electrode in embodiment 2
Situation of change；
Fig. 3 is the scanning electron microscope (SEM) photograph of the uranium-bearing material finally deposited in reducing electrode in embodiment 1；Fig. 4 is real to implement
The X-ray energy spectrogram for the uranium oxide produced in example 3.
Embodiment
Embodiments of the present invention are further illustrated below by specific example：
A, low concentration uranium-bearing wastewater pretreatment：The uranium-containing waste water that 100 mL uranium ions concentration are less than 0.05 mg/L is measured, profit
Filtration treatment is carried out to it with filtration gauze, the insoluble matter impurity in water is filtered off；Then, toward 0.1-2.0 mol/L of addition in water
Short chain organic matter, it is ensured that low concentration uranium-bearing wastewater pH value after pretreatment be less than 7.0.
B, uranium-containing waste water pulse electroreduction：It is flammable with Carbon fibe paper etc. using pretreated uranium-containing waste water as electrolyte
Negative electrode (reducing electrode) is built based on the conductive material of burning, anode (oxygen is built based on the stable conductive material such as graphite
Polarizing electrode), build wastewater treatment electrolytic cell（Shown in accompanying drawing 1）.Reduction treatment is carried out to uranium-containing waste water using direct current pulse power source,
Applied voltage in the range of 0.33-2.5 V, total reduction treatment time in 1-10 h, waste water mixing speed 5-100 turns/
Second.By fully processing, high price uranium ion in water is promoted to be converted into short chain organic matter in low price uranium ion, water in reducing electrode
It is converted on oxidizing electrode containing carbon-based and hydroxyl reaction intermediate, most latter two reaction product is in reducing electrode surface complexation
Form the uranium-bearing material of solid-state（Shown in accompanying drawing 2）.
C, solid product heat treatment：In atmosphere, the reducing electrode for having solid-state uranium-bearing material to deposition is carried out at high warm
Reason, according to electrode material material, heat treatment temperature is maintained between 300-1800 DEG C, and heat treatment time promotes electricity in 1-10 h
Pole material fully burns, and leaves solid-state uranium oxide of the purity more than 99%（Shown in accompanying drawing 3 and Fig. 4）.
Embodiment 1：Measure the fluorination tail gas elution that the Co., Ltd's uranium fuel refinery plants of 100 mL centers, four O tetra- are produced
Liquid, carries out filtration treatment to the waste water using the filtration gauze of 100 mesh, filters off the insoluble matter impurity in water；Again toward adding 5 in water
G acetic acid（Acetic acid, CH3COOH）, pretreated uranium-containing waste water pH value is 1.5 after testing, and U (VI), Na are mainly contained in waste water+、
F-、Cl-、CO3 2-、CH3COO-、H+It is 0.03 mg/L Deng, wherein U (VI) concentration.Then, using pretreated uranium-containing waste water as
Electrolyte, using carbon fiber paper as negative electrode (reducing electrode), using graphite as anode (oxidizing electrode), builds wastewater treatment electrolytic cell.
Uranium-containing waste water is handled using direct current pulse power source, electric power output voltage is 2.0 V, voltage is acted in each pulse period
Time is 20 ms, and the turn-off time is 100 ms, and waste water mixing speed maintains 5 revolutions per seconds, and processing total time is 5 h, in carbon
Fibrous paper electrode surface obtains the uranium-bearing material of one layer of solid-state.Finally, in atmosphere, there is the carbon of solid-state uranium-bearing material fine deposition
Tie up paper electrode and carry out high-temperature heat treatment, heat treatment temperature is 600 DEG C, and heat treatment time is 5 h, carbon fiber is fully burnt, most
Uranium oxide of the present invention is obtained eventually, and uranium oxide purity is higher than 99% after testing.
Embodiment 2 measures the mL of uranium-containing waste water 100 of Area, Zoige, Sichuan Uranium Mining smelting uranium generation, utilizes the mistake of 100 mesh
Filter gauze and filtration treatment is carried out to the waste water, filter off the insoluble matter impurity in water.Again toward adding 8 g ethanol in water（CH3CH2OH）,
Pretreated uranium-containing waste water pH value is 6.0 after testing, and U (VI), Na are mainly contained in waste water+、Cl-、NO3 -、Fe3+、Cu2+、Ca2+
It is 0.05 mg/L Deng, wherein U (VI) concentration.Then, using pretreated uranium-containing waste water as electrolyte, using conductive plastics as
Negative electrode (reducing electrode), using platinized platinum as anode (oxidizing electrode), builds wastewater treatment electrolytic cell.Using direct current pulse power source to containing
Uranium waste water is handled, and electric power output voltage is 1.2 V, and voltage action time is 20 ms in each pulse period, during shut-off
Between be 100 ms, waste water mixing speed maintains 50 revolutions per seconds, and processing total time is 3 h, is obtained in conductive plastics electrode surface
The uranium-bearing material of one layer of solid-state.Finally, in atmosphere, the conductive plastics electrode for having solid-state uranium-bearing material to deposition carries out high warm
Processing, heat treatment temperature is 800 DEG C, and heat treatment time is 10 h, makes conductive plastics divided combustion, finally gives of the present invention
Uranium oxide, uranium oxide purity is higher than 99% after testing.
Embodiment 3：The low concentration uranium-bearing wastewater that the operation of 100 mL uranium reactors is produced is measured, the filtering of 100 mesh is utilized
Gauze carries out filtration treatment to the waste water, filters off the insoluble matter impurity in water；Again toward adding 5 g acetaldehyde in water（CH3CHO）, warp
It is 4.5 to detect pretreated uranium-containing waste water pH value, and U (VI), Na are mainly contained in waste water+、F-、Cl-、CO3 2-、CH3CHO、H+Deng,
Wherein U (VI) concentration is 0.01 mg/L.Then, using pretreated uranium-containing waste water as electrolyte, using conductive rubber as negative electrode
(reducing electrode), using graphite as anode (oxidizing electrode), builds wastewater treatment electrolytic cell.Uranium-containing waste water is entered using dc source
Row processing, electric power output voltage is 0.5 V, and waste water mixing speed maintains 30 revolutions per seconds, and processing total time is 1 h, in conduction
Rubber electrode surface obtains the uranium-bearing material of one layer of solid-state.Finally, in atmosphere, there is the conductive rubber of solid-state uranium-bearing material to deposition
Gel electrode carries out high-temperature heat treatment, and heat treatment temperature is 500 DEG C, and heat treatment time is 5 h, conductive rubber is fully burnt, most
Uranium oxide of the present invention is obtained eventually, and uranium oxide purity is higher than 99% after testing.
It is that can be achieved to remove uranium in low concentration uranium-bearing wastewater to pollute by above-mentioned each embodiment and according to aforementioned processing methods
Thing and the purpose for reclaiming high purity uranium oxide.Uranium-containing waste water radioactivity after being handled by this method is substantially eliminated, simultaneously
Obtained high-purity uranium oxide is reclaimed, the object of the invention can be effectively reached.The embodiment of the present invention can be implemented, this hair
It is bright to be not limited to these embodiments.
Claims (6)
1. a kind of method that electroreduction processing low concentration uranium-bearing wastewater produces uranium oxide, it is characterised in that：It is in low concentration
Appropriate short chain organic matter is added in uranium-containing waste water, negative electrode is built based on combustible conductive material, with stable conduction
Anode is built based on material；Then, reduction treatment is carried out to uranium-containing waste water using dc source or direct current pulse power source, makes water
Middle high price uranium ion is reduced to short chain organic matter in low price uranium ion, water on negative electrode and is oxidized on anode containing carbon-based and hydroxyl
Reaction intermediate, by control voltage, reduction time, uranium-containing waste water mixing speed, promote low price uranium ion with it is carbon containing
The reaction intermediate of base and hydroxyl is complexed the uranium-bearing material to form solid-state in cathode surface；Finally, by high temperature burning handling, go
Except cathode electrode material, high-purity uranium oxide is made；Described low concentration uranium-bearing wastewater refers to that uranium ion concentration is less than 0.05
Mg/L uranium-containing waste water, species includes low concentration wastewater, uranium refinement and the uranium fuel production generation that uranium mining and hydrometallurgy are produced
Low concentration wastewater, uranium reactor operation produce low concentration wastewater；Described obtained high-purity uranium oxide, refers to finally produce
Uranium oxide purity more than 99%.
2. the method that electroreduction processing low concentration uranium-bearing wastewater according to claim 1 produces uranium oxide, its feature exists
In：The appropriate short chain organic matter of described addition refers to organic matter of the carbon number less than or equal to 10, species bag in organic molecule
Short chain Organic Alcohol is included including methanol, ethanol, ethylene glycol, short chain organic acid includes formic acid, acetic acid, short chain organic aldehyde include formaldehyde,
Acetaldehyde, short chain organic ether includes ether, dimethyl ether；The addition of organic matter is controlled in 0.1 mol/L to 2.0 in uranium-containing waste water
In the range of mol/L.
3. the method that electroreduction processing low concentration uranium-bearing wastewater according to claim 1 produces uranium oxide, its feature exists
In：Described builds negative electrode based on combustible conductive material, and its conductive material includes carbon fiber paper, conductive plastics, led
Electric rubber, conducting polymer.
4. the method that electroreduction processing low concentration uranium-bearing wastewater according to claim 1 produces uranium oxide, its feature exists
In：Described builds anode based on stable conductive material, and its conductive material includes conductive carbon material graphite, carbon black, leads
Electric diamond, FTO electro-conductive glass, ITO electro-conductive glass, conductive corrosion-resistant sheet metal and metallic plate, conductivity ceramics, conductive carbonized
Thing, Conducting boride, conductive nitride, the stable metal oxide with certain electric conductivity.
5. the method that electroreduction processing low concentration uranium-bearing wastewater according to claim 1 produces uranium oxide, its feature exists
In：It is described by control voltage, reduction time, uranium-containing waste water mixing speed, specifically include：Control dc source or
It in 0.33 V to the reduction time between 2.5 V, control be 1-10 h that person's pulse power output voltage, which is, controls uranium-bearing useless
Water mixing speed is at 5 revolutions per seconds to 100 revolutions per seconds.
6. the method that electroreduction processing low concentration uranium-bearing wastewater according to claim 1 produces uranium oxide, its feature exists
In：Described to remove cathode electrode material by high temperature burning handling, detailed process includes：In atmosphere, 300 to 1800 DEG C
Under the conditions of, reacted negative electrode 1-10 h are heat-treated, its incendivity material is fully burnt, leaves incombustible solid uranium oxygen
Compound.
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| CN106448790B (en) * | 2016-11-11 | 2017-12-22 | 东华理工大学 | A kind of uranium-containing waste water electrochemical process for treating |
| CN111004934B (en) * | 2019-12-19 | 2021-03-23 | 西南科技大学 | Method for extracting uranium by using coupling device of wind power generation and uranium extraction from seawater |
| CN110952107B (en) * | 2019-12-19 | 2020-10-30 | 西南科技大学 | Method for extracting uranium from seawater by using metal oxide containing oxygen vacancy |
| CN111627588B (en) * | 2020-06-15 | 2021-08-10 | 华北电力大学 | Application of graphene aerogel in removing uranium through photocatalysis |
| CN112877709A (en) * | 2020-12-30 | 2021-06-01 | 中国原子能科学研究院 | Device for preparing tetravalent uranium through continuous electrolysis |
| CN114134349B (en) * | 2021-12-06 | 2023-03-28 | 西北工业大学 | Process for recovering uranium in water through photocatalytic reduction fixation, electrooxidation enrichment and precipitation separation |
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| US3961027A (en) * | 1973-10-18 | 1976-06-01 | Westinghouse Electric Corporation | Cyclic process for re-use of waste water generated during the production of UO2 |
| JP5386215B2 (en) * | 2009-04-08 | 2014-01-15 | 日揮株式会社 | Method and apparatus for treating radioactive liquid waste |
| CN101597113A (en) * | 2009-06-27 | 2009-12-09 | 南华大学 | A kind of treatment process of uranium-containing waste water |
| CN104835545B (en) * | 2015-03-19 | 2017-03-29 | 西南科技大学 | A kind of deep purifying and recovery method of the fluorine-containing uranium radioactive liquid waste of high salt |
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