CN110526455A - The uranium recovery method of uranium-containing waste water - Google Patents
The uranium recovery method of uranium-containing waste water Download PDFInfo
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- CN110526455A CN110526455A CN201910896570.6A CN201910896570A CN110526455A CN 110526455 A CN110526455 A CN 110526455A CN 201910896570 A CN201910896570 A CN 201910896570A CN 110526455 A CN110526455 A CN 110526455A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
- C22B60/0278—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries by chemical methods
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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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/463—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrocoagulation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/006—Radioactive compounds
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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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- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
A kind of uranium recovery method of uranium-containing waste water, belongs to water-treatment technology field.The uranium recovery method of uranium-containing waste water includes: under conditions of pH value is not higher than 3, uranium-containing waste water and uranyl ion organic ligand are mixed to get liquid to be processed, under acid condition of the pH value not less than 3, treats treatment fluid progress electric flocculation and handle to obtain except uranium waste water and uranium-bearing precipitate.Uranium-bearing precipitating is impregnated with cleaning solution, washing is obtained except uranium precipitating and uranium-bearing concentrate, the heating resolution of uranium-bearing concentrate concentrated nitric acid is obtained into uranium-bearing residue, cleaning solution contains sodium carbonate and hydrogen peroxide.Uranium-bearing residue is reacted into 1.5-2.5h under the solution environmental that pH value is 8-9.8 with ammonia source, obtains ammonium diuranate precipitating.Can in higher efficiency, the low concentration uranium that is selectively removed in uranium-containing waste water, while can be realized the resource utilization to uranium.
Description
Technical field
This application involves water-treatment technology fields, in particular to a kind of uranium recovery method of uranium-containing waste water.
Background technique
Nuclear power because its cleaning, efficiently, low-carbon due to become the main energy sources provisioning policy first developed current various countries, nuclear power
Devoting Major Efforts To Developing, popularization and use are necessarily increased to its main fuel --- the demand of natural uranium.Currently, natural uranium main source
In land mineral products uranium resource, the exploitation of land mineral products uranium resource generates a large amount of uranium-containing waste water with smelting process is selected, seriously threatens
The health of uranium mine location resident and the sustainable development of ecological environment.What the exploitation of land mineral products uranium resource generated contains
Uranium waste water is mainly derived from mine water, Tailings Dam dump leaching water outlet, and comprehensive 0.5~3.0mg/L of uranium concentration belongs to low concentration uranium-bearing wastewater
Scope.Radioactive uranium is easy to migrate and form combined pollution in low concentration uranium-bearing wastewater, and furthermore uranium concentration is low, associated metal type is numerous
More, the improvement of the waste water becomes one of emphasis and difficulties of uranium mine ecological environmental protection.
Uranium in uranium-containing waste water exists in the form of uranyl ion with counter anion complexing, practical uranium mine uranium-containing waste water
Processing mostly uses weak-base anion-exchange resin to capture fixed uranyl ion and anion complex, though there is uranium to retain efficiency
High, the strong feature of selectivity, but the problems such as be easily poisoned there are ion exchange resin, in addition, the processing method is difficult to realize to useless
Abandon the resource utilization of uranium resource.
Summary of the invention
A kind of uranium recovery method for being designed to provide uranium-containing waste water of the application, can in higher efficiency, selectively
The low concentration uranium in uranium-containing waste water is removed, while can be realized the resource utilization to uranium.
Embodiments herein is achieved in that
The embodiment of the present application provides a kind of uranium recovery method of uranium-containing waste water, comprising:
Under conditions of pH value is not higher than 3, uranium-containing waste water and uranyl ion organic ligand are mixed to get liquid to be processed, In
Under acid condition of the pH value not less than 3, treats treatment fluid progress electric flocculation and handle to obtain except uranium waste water and uranium-bearing precipitate.
Uranium-bearing precipitating is impregnated with cleaning solution, obtains washing except uranium precipitating and uranium-bearing concentrate, by uranium-bearing concentrate with dense
Nitration acid heat is cleared up to obtain uranium-bearing residue, and cleaning solution contains sodium carbonate and hydrogen peroxide.
1.5-2.5h is reacted after the pH value of uranium-bearing residue is adjusted to 8-9.8 with ammonia source, obtains ammonium diuranate precipitating.
In above-mentioned technical proposal, using electric flocculation handle in the flocculation presoma that generates to the uranyl ion in uranium-containing waste water
Adsorption-flocculation is carried out, processing cost is low, high-efficient and selectivity is strong.For inventor the study found that during electric flocculation, pH value is too low
When be unfavorable for the metal ion of metal anode dissolution and form flocculation presoma, be unfavorable for when pH value is excessively high the metal of metal anode from
The dissolution of son carries out electric flocculation processing under acid condition of the pH value not less than 3, and treatment effeciency is high, flocculating effect is good.Due to containing
Uranium in uranium waste water exists in the form of uranyl ion with counter anion complexing, under conditions of pH value is not higher than 3, uranium-containing waste water
In with the uranyl ion of anion complexing can be dissociated into monomer uranyl ion, monomer uranyl ion can effectively with uranyl from
Sub- organic ligand cooperatively forms uranyl ion organic chelate.The positive electricity on uranyl ion surface is reduced by the coordination of organic ligand
Property, and increase the weight and chain length of uranium-bearing material, enable in electric flocculation treatment process electric flocculation presoma to uranyl from
Sub- organic chelate carries out abundant and efficient adsorption-flocculation, guarantees that electric flocculation processing can be realized abundant and efficiently remove uranium.
The form separation that uranyl ion in uranium-containing waste water is precipitated with uranium-bearing, convenient for precipitating the resource for carrying out uranium using uranium-bearing
Change recycling.Inventor can effectively dissolve and contain the study found that by uranium-bearing precipitating is impregnated containing the cleaning solution of sodium carbonate and hydrogen peroxide
Uranyl ion organic chelate in uranium precipitating, so as to isolated washing except uranium precipitating and uranium-bearing concentrate.Meanwhile it soaking
During bubble, hydrogen peroxide can destroy matching between uranyl ion and uranyl ion organic ligand in uranyl ion organic chelate
Position effect cooperates further concentrated nitric acid resolution that can effectively remove uranyl ion organic ligand, to obtain mainly containing list
The uranium-bearing residue of body uranyl ion.Obtained uranium-bearing residue is further reacted into certain time with ammonia source under certain alkaline condition
Ammonium diuranate precipitating can be obtained, to realize the resource utilization to uranium.
In some optional embodiments, in cleaning solution, the concentration of sodium carbonate is 0.4-0.6mol/L, hydrogen peroxide it is dense
Degree is 0.4-0.6mol/L.
In above-mentioned technical proposal, when sodium carbonate and hydrogen peroxide have above-mentioned concentration in cleaning solution, cleaning solution precipitates uranium-bearing
Dissolution degree it is suitable, guarantee fully by uranium-bearing precipitate in uranyl ion organic chelate be dissolved in solution while,
Electric flocculation presoma is avoided to be dissolved in solution.Meanwhile cleaning solution also has oxidation susceptibility appropriate, can effectively destroy uranium
Coordination between acyl ion organic ligand.
In some optional embodiments, the solid-to-liquid ratio of uranium-bearing precipitating and cleaning solution is 1g:10-12mL.
In above-mentioned technical proposal, carry out the immersion that precipitates to uranium-bearing of cleaning solution according to above-mentioned solid-to-liquid ratio, can fully by
Uranyl ion organic chelate is dissolved in solution.
In some optional embodiments, before uranium-bearing precipitating is impregnated with cleaning solution, uranium-bearing is first deposited in 35-45
DEG C temperature under the conditions of dry.
In above-mentioned technical proposal, uranium-bearing precipitating dry under the conditions of above-mentioned temperature, can effectively remove and contain
Extra moisture and the part organic impurities ingredient of its attachment in uranium precipitating.Uranium-bearing precipitating is carried out using cleaning solution after drying
It impregnates, also makes in soaking process solid-to-liquid ratio control more accurate, advantageously ensure that immersion effect.
In some optional embodiments, it is 220- that uranium-bearing concentrate, which is heated the heating temperature cleared up with concentrated nitric acid,
250℃；Optionally, the volume ratio of the liquid before heating resolution and the residue after heating resolution is 1:0.01-0.02.
In above-mentioned technical proposal, uranium-bearing concentrate is heated under the conditions of above-mentioned temperature using concentrated nitric acid, Neng Gouyou
Effect eliminates the uranyl ion organic ligand in solution and obtains the higher uranium-bearing residue of uranyl ion purity, guarantees the recycling of uranium
It recycles obtained ammonium diuranate and precipitates purity with higher.When uranium-bearing concentrate is cleared up under the conditions of above-mentioned temperature,
The liquid of heating resolution front and back reaches above-mentioned volume ratio, guarantees that the uranyl ion organic ligand in solution can fully be disappeared
It removes.
In some optional embodiments, the concentration of concentrated nitric acid is 4-6mol/L.
It in above-mentioned technical proposal, is cleared up using the concentrated nitric acid of above-mentioned concentration, so that the oxidation effectiveness in digestion process
It is more suitable, it not only can guarantee that the uranyl ion organic ligand in solution was fully eliminated, but also be avoided that solution is excessively oxidated.
In some optional embodiments, after uranium-bearing precipitating is impregnated with cleaning solution, washing is removed into uranium precipitating cleaning solution
It is rinsed, collects the liquid for impregnating and rinsing and obtain uranium-bearing concentrate；Optionally, uranium-bearing precipitating and the amount ratio of cleaning solution are
The volume ratio of 1g:10-12mL, uranium-bearing concentrate and concentrated nitric acid is 1:0.25-0.35.
In above-mentioned technical proposal, washing is removed into uranium precipitating and is cleaned with cleaning solution, removes the washing except uranium precipitation surface
The uranium-bearing material of attachment guarantees that washing can carry out harmless discharge, green, environmental protection except uranium precipitating in the form of uranium-free.It will
Impregnate and the liquid that rinses collects together after be used as the resource utilization of uranium-bearing concentrate progress uranium, avoid because impregnating and rinsing
The discharge of uranium-bearing liquid, and cause uranium pollution and uranium resourceization recycling loss.According to above-mentioned amount ratio using cleaning solution to washing
Except uranium precipitating is cleaned, while guaranteeing cleaning effect, cleaning solution is avoided to influence subsequent resolution effect using excessive.It presses
It is cleared up according to above-mentioned volume ratio using concentrated nitric acid, guaranteeing can be by uranyl ion organic ligand substantially more in digestion process
It eliminates.
In some optional embodiments, after uranium-bearing concentrate is heated resolution with concentrated nitric acid, it is diluted with water and is contained
Uranium residue, the volume ratio for diluting front and back is 0.01-0.02:1.
In above-mentioned technical proposal, the uranium-bearing concentrate after resolution is diluted according to above-mentioned volume ratio, so that uranium-bearing is residual
There is appropriate uranyl ion concentration in slag, preferably react to obtain ammonium diuranate precipitating with ammonia source convenient for subsequent.
In some optional embodiments, before uranium-containing waste water is mixed with uranyl ion organic ligand, first by uranium-bearing
The pH value of waste water is adjusted to 2.8-3.
And/or before treating treatment fluid progress electric flocculation processing, the pH value of liquid to be processed is first adjusted to 6.4-6.7.
In above-mentioned technical proposal, uranium waste water is mixed with uranyl ion organic ligand under above-mentioned pH value condition, uranyl from
Son can fully carry out cooperatively forming uranyl ion organic chelate with uranyl ion organic ligand in the form of monomer.Upper
Progress electric flocculation processing is stated under pH value condition, metal anode can be fully dissolved out and be formed electric flocculation presoma, guarantee pair
Uranyl ion organic chelate carries out more abundant and efficient adsorption-flocculation.
In some optional embodiments, uranyl ion organic ligand in iminodiacetic acid and alizarin red one
Kind, optionally, uranyl ion organic ligand is alizarin red.
And/or electric flocculation processing middle-jiao yang, function of the spleen and stomach extremely iron electrode, to electrode be graphite electrode.
In above-mentioned technical proposal, there is preferable mating reaction to uranyl ion in iminodiacetic acid and alizarin red, and obtain
The uranyl ion organic chelate arrived can be sufficiently and efficiently by electric flocculation presoma institute adsorption-flocculation.Using iron electrode conduct
When anode, graphite electrode are used as to electrode, the Fe (OH) that is formed after iron ion dissolution3、Fe2O3Electric flocculation presoma can be abundant
Adsorption-flocculation uranyl ion organic chelate, and electric flocculation handle except uranium waste water is without dissolubility iron ion, therefore will not
Other metal ions are introduced in except uranium waste water due to electric flocculation treatment process.
Detailed description of the invention
Technical solution in ord to more clearly illustrate embodiments of the present application, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only some embodiments of the application, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
When Fig. 1 is that the uranium recovery method for the uranium-containing waste water that the embodiment of the present application 1 provides handles uranium-containing waste water, resulting washing
Except the SEM figure of uranium precipitating；
When Fig. 2 is that the uranium recovery method for the uranium-containing waste water that the embodiment of the present application 1 provides handles uranium-containing waste water, resulting washing
Except the x-ray photoelectron spectroscopy figure of uranium precipitating；
When Fig. 3 is that the uranium recovery method for the uranium-containing waste water that the embodiment of the present application 1 provides handles uranium-containing waste water, resulting heavy uranium
The exterior appearance figure of sour ammonium product；
When Fig. 4 is that the uranium recovery method for the uranium-containing waste water that the embodiment of the present application 1 provides handles uranium-containing waste water, resulting heavy uranium
The XRD spectra of sour ammonium product and the PDF standard card comparative diagram of ammonium diuranate；
The uranium recovery method processing for the uranium-containing waste water that Fig. 5 is the embodiment of the present application 1, embodiment 8, comparative example 1-3 are provided contains
Uranium concentration line chart when uranium waste water, in electric flocculation treatment process in liquid to be processed；
The uranium recovery method for the uranium-containing waste water that Fig. 6 is the embodiment of the present application 1, embodiment 9, embodiment 11 provide handles uranium-bearing
Concentration of metal ions line chart when waste water, in electric flocculation treatment process in liquid to be processed.
Specific embodiment
It, below will be in the embodiment of the present application to keep the purposes, technical schemes and advantages of the embodiment of the present application clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The uranium recovery method of the uranium-containing waste water of the embodiment of the present application is specifically described below.
It should be noted that the "and/or" in the application, such as " option A and/or option b ", each meaning individually to be
Option A is individually option b, option A+option b, three kinds of modes.
The embodiment of the present application provides a kind of uranium recovery method of uranium-containing waste water, comprising:
S1. under conditions of pH value is not higher than 3, uranium-containing waste water is mixed to get with uranyl ion organic ligand to be processed
Liquid treats treatment fluid progress electric flocculation and handles to obtain except uranium waste water and uranium-bearing precipitate under acid condition of the pH value not less than 3.
The initial pH value of uranium-containing waste water is about 7.2, therefore the uranium in the uranium-containing waste water of uranium mining generation, with uranyl ion
Form and counter anion complexing exist.Under conditions of pH value is not higher than 3, in uranium-containing waste water with the uranyl of anion complexing from
Son can be dissociated into monomer uranyl ion (UO2 2+), monomer uranyl ion effectively can cooperate shape with uranyl ion organic ligand
At uranyl ion organic chelate, reduces the electropositive on uranyl ion surface and increase the weight and chain length of uranium-bearing material, mention
The high electric flocculation absorption property of uranyl ion.
Illustratively, the hybrid manipulation packet of uranium-containing waste water and uranyl ion organic ligand under conditions of pH value is not higher than 3
It includes: the pH value of uranium-containing waste water being adjusted to not higher than 3 using acid, be then added to uranyl ion organic ligand after adjusting pH value
Uranium-containing waste water in.
In some optional embodiments, the pH value of uranium-containing waste water is adjusted using nitric acid or sulfuric acid, illustratively, is used
Concentration be 1.5-2.5mol/L nitric acid, the concentration of nitric acid be such as, but not limited to 1.5mol/L, 1.8mol/L, 2mol/L,
Any one of 2.2mol/L, 2.5mol/L or any range between the two, so that the uranyl ion energy with anion complexing
It is enough to be sufficiently dissociated into monomer uranyl ion, while avoiding introducing other anion for being difficult to remove.
Further, when adjusting the pH value of uranium-containing waste water, the pH value of uranium-containing waste water is adjusted to 2.8-3 or 2.9-3, example
It is such as, but not limited to, any one of 2.8,2.9,3 or any range between the two.
In some possible embodiments, uranyl ion organic ligand is selected from iminodiacetic acid (full name in English
Iminodiacetic Acid, English abbreviation IDA) and alizarin red (full name in English Mordant Red 3, English abbreviation ALR) in
One kind.Further, the molar ratio of uranyl ion organic ligand and uranyl ion is 2.5-3.5:1 or 2.8-3.2:1, example
It is such as, but not limited to, any one of 2.5:1,2.8:1,3:1,3.2:1,3.5:1 or any range between the two.
Illustratively, uranyl ion organic ligand is alizarin red, and the molar ratio of alizarin red and uranyl ion is 3:1.Invention
People is the study found that the content for removing the uranium in uranium waste water after ion exchange resin treatment is typically only capable to reach about in the prior art
0.3mg/L, and cooperated using alizarin red as uranyl ion organic ligand with monomer uranyl ion, electric wadding is carried out under given conditions
Solidifying processing, what is obtained (is no more than except the content of uranium Uranium in Waste Water can reach emission limit as defined in the drinking water standard of cities and towns
It 0.05mg/L) requires, uranium significant effect is removed to uranium-containing waste water.
Treatment fluid is treated using electric flocculation to be handled, using electric flocculation handle in the flocculation presoma that generates it is useless to uranium-bearing
Uranyl ion in water carries out adsorption-flocculation, and processing cost is low, high-efficient and selectivity is strong, can effectively realize low concentration and contain
The removal of uranium Uranium in Waste Water, the uranium mine waste water of mine of the useless for example comprehensive 0.5~3.0mg/L of uranium concentration of low concentration uranium-bearing.Electricity wadding
During solidifying, metal anode dissolves out metal ion, and metal ion generates the monokaryon hydrogen with flocculating effect using hydrolysis, polymerization
As electric flocculation presoma, electric flocculation presoma is organic with the uranyl ion in liquid to be processed again for oxide and multicore hydroxide
Chelate cohesion generates large volume flocculate, so that the uranyl ion removed in liquid to be processed by way of uranium-bearing precipitates is organic
Chelate.The form separation that uranyl ion in uranium-containing waste water is precipitated with uranium-bearing, convenient for precipitating the resource for carrying out uranium using uranium-bearing
Change recycling.For inventor the study found that when pH value is lower than 3, the metal ion for being unfavorable for metal anode dissolution forms monokaryon hydrogen-oxygen
Compound and multicore hydroxide；And under alkaline condition, metal anode be easy to happen passivation and make the dissolution of metal ion by
To inhibition, metal ion and hydroxide ion also primarily form soluble hydroxide under alkaline condition, are equally unfavorable for
Flocculation to uranyl ion organic chelate.Electric flocculation processing, treatment effeciency are carried out under acid condition of the pH value not less than 3
Height, flocculating effect are good.
In some optional embodiments, treat before treatment fluid carries out electric flocculation processing, using alkali or alkaline matter,
The pH value of liquid to be processed is first adjusted to 6.4-6.7 or 6.4-6.6, any in such as, but not limited to 6.4,6.5,6.6,6.7
Person or any range between the two.
In some optional embodiments, in electric flocculation treatment process, using the sacrifices metal anode such as iron, magnesium, aluminium.
Illustratively, anode is iron electrode, is graphite electrode, the Fe (OH) that the iron ion of iron electrode dissolution is formed to electrode3、Fe2O3Energy
Enough abundant adsorption-flocculation uranyl ion organic chelates, and iron ion will not be introduced in except uranium waste water after the completion of electric flocculation, because
This will not introduce other metal ions because of electric flocculation processing in except uranium waste water.
Optionally, the electrolyte of electric flocculation processing is sodium sulphate, and the mass concentration of sodium sulphate is illustrative in liquid to be processed
It is 5%, the electric conductivity of liquid to be processed can be enhanced, so that the output rate of electric flocculation presoma increases, promotes flocculation ability.
Further, the time of electric flocculation processing is 20-30min, to guarantee to uranyl ion organic chelate fully
Adsorption-flocculation.
S2. uranium-bearing precipitating is impregnated with cleaning solution, obtains washing except uranium precipitating and uranium-bearing concentrate, uranium-bearing concentrate is used
Concentrated nitric acid heating resolution obtains uranium-bearing residue, and cleaning solution contains sodium carbonate and hydrogen peroxide.
Containing the cleaning solution of sodium carbonate and hydrogen peroxide impregnate uranium-bearing precipitating, can effectively dissolve uranium-bearing precipitating in uranyl from
Sub- organic chelate, so that by the operation being separated by solid-liquid separation washing can be obtained except uranium precipitating and uranium-bearing concentrate, washing removes uranium
Electric flocculation presoma after precipitating predominantly removal uranyl ion organic chelate, can carry out nothing directly in the form of uranium-free
Evilization discharge.Hydrogen peroxide in cleaning solution can destroy in uranyl ion organic chelate uranyl ion and uranyl ion is organic matches
Coordination between body cooperates further concentrated nitric acid resolution that can effectively remove uranyl ion organic ligand, to obtain
Mainly contain the uranium-bearing residue of monomer uranyl ion.
In some optional embodiments, the time that cleaning solution impregnates uranium-bearing precipitating is 4-6h, such as, but not limited to
The range of any one of 4h, 5h, 6h or any between the two, with allow wash liquid to sufficiently by uranium-bearing precipitate in uranyl from
Sub- organic chelate is dissolved, while guaranteeing that hydrogen peroxide can fully destroy uranyl ion in uranyl ion organic chelate
With the coordination between uranyl ion organic ligand.
Further, in cleaning solution, the concentration of sodium carbonate is 0.4-0.6mol/L or 0.5-0.6mol/L；Hydrogen peroxide
Concentration is 0.4-0.6mol/L or 0.5-0.6mol/L.The concentration of the two optionally for 0.4mol/L, 0.5mol/L,
Any one of 0.6mol/L or any range between the two.For example, in cleaning solution, the concentration of sodium carbonate and hydrogen peroxide it is dense
The ratio between degree is 1:1.
Illustratively, uranium-bearing precipitating and the solid-to-liquid ratio of cleaning solution are 1g:10-12mL or 1g:10.5-11.5mL, such as but
It is not limited to any one of 1g:10mL, 1g:10.5mL, 1g:11mL, 1g:11.5mL, 1g:12mL or any model between the two
It encloses.
In some optional embodiments, before uranium-bearing precipitating is impregnated with cleaning solution, uranium-bearing is first deposited in 35-45
DEG C temperature under the conditions of dry, drying temperature be such as, but not limited in 35 DEG C, 35 DEG C, 38 DEG C, 40 DEG C, 42 DEG C, 45 DEG C appoint
One or any range between the two.Drying course carries out in an oven, and drying to constant weight.
In some optional embodiments, after uranium-bearing precipitating is impregnated with cleaning solution, washing is removed into uranium precipitating cleaning solution
It is rinsed, collects the liquid for impregnating and rinsing and obtain uranium-bearing concentrate.Further, the amount ratio of uranium-bearing precipitating and cleaning solution
For 1g:10-12mL or 1g:10.5-11.5mL, such as, but not limited to 1g:10mL, 1g:10.5mL, 1g:11mL, 1g:
Any one of 11.5mL, 1g:12mL or any range between the two.
Concentrated nitric acid has stronger oxidation, has preferable resolution effect to uranyl ion organic ligand.Using washing
After washing liquid immersion, cooperate further concentrated nitric acid resolution that can effectively remove uranyl ion organic ligand, to mainly be contained
There is the uranium-bearing residue of monomer uranyl ion.
In some optional embodiments, it is 220- that uranium-bearing concentrate, which is heated the heating temperature cleared up with concentrated nitric acid,
Any one of 250 DEG C or 230-250 DEG C, such as, but not limited to 220 DEG C, 230 DEG C, 240 DEG C, 250 DEG C or any the two
Between range.Illustratively, heating resolution carries out on graphite electric heating plate, homogeneous heating, temperature control are accurate, anticorrosive property is good,
It is energy-efficient.
Further, the body of the liquid before heating resolution and the residue (predominantly uranium-bearing residue) after heating resolution
It accumulates and compares for 1:0.01-0.02, such as, but not limited to any one of 1:0.01,1:0.015,1:0.02 or any between the two
Range.
In some optional embodiments, the concentration of concentrated nitric acid is 4-6mol/L, such as, but not limited to 4mol/L,
Any one of 4.5mol/L, 5mol/L, 5.5mol/L, 6mol/L or any range between the two.Optionally, contain uranium enrichment
The volume ratio of liquid and concentrated nitric acid is 1:0.25-0.35 or 1:0.28-0.32, such as, but not limited to 1:0.25,1:0.28,1:
0.3, any one of 1:0.32,1:0.35 or any range between the two.
Further, after uranium-bearing concentrate being heated resolution with concentrated nitric acid, natural cooling is diluted with water after cooling and is contained
Uranium residue, the volume ratio for diluting front and back is 0.01-0.02:1, such as, but not limited in 0.01:1,0.015:1,0.02:1
Any one or any range between the two.Dilution dissolves uranium-bearing residue in advance, carries out according to above-mentioned volume ratio
Dilution is so that the uranium-bearing residue after dilution contains uranium concentration with appropriate, and the pH value after dilution is generally 1-2, so that uranium-bearing
Uranium in residue mainly exists in the form of monomer uranyl ion.
S3. uranium-bearing residue is reacted into 1.5-2.5h in the case where pH value is adjusted to the solution environmental of 8-9.8 with ammonia source, obtains weight uranium
Sour ammonium ((NH4)2U4O13·7H2O it) precipitates.
The uranium that inventor studies uranium-bearing residue mainly exists in the form of monomer uranyl ion, and inventor, which will study discovery, to be contained
Uranium residue further reacts certain time under certain alkaline condition with ammonia source can obtain ammonium diuranate precipitating, thus realization pair
The resource utilization of uranium.
It should be noted that ammonia source refers to be mixed under solution environmental with uranium-bearing residue in embodiments herein
Afterwards, it is capable of providing NH3·H2The substance of O.The ammonia source for example can be ammonium hydroxide, be also possible to ammonia.
In some optional embodiments, the pH value of the uranium-bearing residue after being adjusted with ammonia source, such as, but not limited to 8,
8.5, any one of 9,9.5,9.8 or any range between the two；After the completion of pH value is adjusted, the reaction time is for example but unlimited
In for any one of 90min, 100min, 110min, 120min, 130min, 140min, 150min or any between the two
Range.Optionally, reaction carries out under conditions of standing, obtains sticky yellow milk, i.e. ammonium diuranate after the reaction was completed
Precipitating.
Illustratively, it is washed with water twice according to the solid-to-liquid ratio of 1:10 after the reaction was completed, then in natural under room temperature
It air-dries, final recycling obtains ammonium diuranate product.
The feature of the application and performance are described in further detail with reference to embodiments.
Embodiment 1
A kind of uranium recovery method of uranium-containing waste water, comprising:
S1. the uranium concentration and pH value of uranium-containing waste water are tested；Using concentration is the nitric acid of 2mol/L by the pH value of uranium-containing waste water
It is adjusted to 3；It is 3 according to the molar ratio of uranyl ion organic ligand and uranyl ion using alizarin red as uranyl ion organic ligand:
1 ratio adds uranyl ion organic ligand into uranium-containing waste water and is mixed to get liquid to be processed；The pH value of liquid to be processed is adjusted
To 6.5, with sodium sulphate (mass concentration 5%) be electrolyte, with ferroelectricity extremely anode, with graphite electrode be to be treated to electrode
Treatment fluid carries out electric flocculation and handles to obtain except uranium waste water and uranium-bearing precipitate.
S2., uranium-bearing is deposited in 40 DEG C of baking ovens to drying to constant weight；It with the concentration of sodium carbonate is 0.5mol/L, hydrogen peroxide
The solution that concentration is 0.5mol/L is cleaning solution, and the uranium-bearing precipitating after taking 9g to dry impregnates 5h with 100mL cleaning solution；Filtration treatment
Filter residue and filtrate are obtained, filter residue is rinsed as cleaning solution using 100mL clear water, flushing liquor is collected and is mixed to get uranium-bearing with filtrate
Concentrate, the filter residue after flushing is as washing except uranium precipitates；The nitric acid that 50mL concentration is 5mol/L is added into uranium-bearing concentrate,
It uses graphite electric heating plate set temperature for 240 DEG C of heating resolutions to residue residue 4mL, is diluted with water to after natural cooling
250mL obtains uranium-bearing residue.
S3. reaction 2h is stood after the pH value of uranium-bearing residue solution being adjusted to 9.5 with ammonium hydroxide, filtration treatment obtains sticky
Yellow milk；Yellow milk is washed with water twice according to the solid-to-liquid ratio of 1:10, then in natural air drying under room temperature,
Final recycling obtains ammonium diuranate product.
Embodiment 2
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that, S1 step is specific:
S1. the uranium concentration and pH value of uranium-containing waste water are tested；Using concentration is the nitric acid of 1.5mol/L by the pH of uranium-containing waste water
Value is adjusted to 3；Using alizarin red as uranyl ion organic ligand, the molar ratio according to uranyl ion organic ligand and uranyl ion is
The ratio of 2.5:1 adds uranyl ion organic ligand into uranium-containing waste water and is mixed to get liquid to be processed；By the pH value of liquid to be processed
Be adjusted to 6.7, with sodium sulphate (mass concentration 5%) be electrolyte, with ferroelectricity extremely anode, with graphite electrode be to electrode,
Treatment fluid progress electric flocculation is treated to handle to obtain except uranium waste water and uranium-bearing precipitate.
Embodiment 3
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that, S1 step is specific:
S1. the uranium concentration and pH value of uranium-containing waste water are tested；Using concentration is the nitric acid of 2.5mol/L by the pH of uranium-containing waste water
Value is adjusted to 2.8；Using alizarin red as uranyl ion organic ligand, according to the molar ratio of uranyl ion organic ligand and uranyl ion
For the ratio of 3.5:1, uranyl ion organic ligand is added into uranium-containing waste water and is mixed to get liquid to be processed；By the pH of liquid to be processed
Value is adjusted to 6.4, with sodium sulphate (mass concentration 5%) be electrolyte, with ferroelectricity extremely anode, with graphite electrode be to electricity
Pole treats treatment fluid progress electric flocculation and handles to obtain except uranium waste water and uranium-bearing precipitate.
Embodiment 4
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that, S2 step is specific:
S2., uranium-bearing is deposited in 40 DEG C of baking ovens to drying to constant weight；It with the concentration of sodium carbonate is 0.4mol/L, hydrogen peroxide
The solution that concentration is 0.4mol/L is cleaning solution, and the uranium-bearing precipitating after taking 9g to dry impregnates 6h with 110mL cleaning solution；Filtration treatment
Filter residue and filtrate are obtained, filter residue is rinsed as cleaning solution using 90mL clear water, flushing liquor is collected and is mixed to get uranium-bearing with filtrate
Concentrate, the filter residue after flushing is as washing except uranium precipitates；The nitric acid that 50mL concentration is 6mol/L is added into uranium-bearing concentrate,
It uses graphite electric heating plate set temperature for 240 DEG C of heating resolutions to residue residue 4mL, is diluted with water to after natural cooling
250mL obtains uranium-bearing residue.
Embodiment 5
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that, S2 step is specific:
S2., uranium-bearing is deposited in 40 DEG C of baking ovens to drying to constant weight；It with the concentration of sodium carbonate is 0.6mol/L, hydrogen peroxide
The solution that concentration is 0.6mol/L is cleaning solution, and the uranium-bearing precipitating after taking 9g to dry impregnates 4h with 90mL cleaning solution；Filtration treatment
Filter residue and filtrate are obtained, filter residue is rinsed as cleaning solution using 110mL clear water, flushing liquor is collected and is mixed to get uranium-bearing with filtrate
Concentrate, the filter residue after flushing is as washing except uranium precipitates；The nitric acid that 50mL concentration is 4mol/L is added into uranium-bearing concentrate,
It uses graphite electric heating plate set temperature for 240 DEG C of heating resolutions to residue residue 5mL, is diluted with water to after natural cooling
250mL obtains uranium-bearing residue.
Embodiment 6
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that, S3 step is specific:
S3. reaction 2.5h is stood after the pH value of uranium-bearing residue solution being adjusted to 8.5 with ammonium hydroxide, filtration treatment obtains sticky
Yellow milk；Yellow milk is washed with water twice according to the solid-to-liquid ratio of 1:10, then in natural wind under room temperature
Dry, final recycling obtains ammonium diuranate product.
Embodiment 7
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that, S3 step is specific:
S3. reaction 1.5h is stood after the pH value of uranium-bearing residue solution being adjusted to 9.8 with ammonium hydroxide, filtration treatment obtains sticky
Yellow milk；Yellow milk is washed with water twice according to the solid-to-liquid ratio of 1:10, then in natural wind under room temperature
Dry, final recycling obtains ammonium diuranate product.
Embodiment 8
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that: using iminodiacetic acid as uranium
Acyl ion organic ligand.
Embodiment 9
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that: using magnesium electrode as anode.
Embodiment 10
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that: using iminodiacetic acid as uranium
Acyl ion organic ligand, using magnesium electrode as anode.
Embodiment 11
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that: using aluminium electrode as anode.
Embodiment 12
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that: using iminodiacetic acid as uranium
Acyl ion organic ligand, using aluminium electrode as anode.
Comparative example 1
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that: it is not added into uranium-containing waste water
The ligand of uranyl ion.
Comparative example 2
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that: uranium is added into uranium-containing waste water
Acyl cationic inorganic ligand, the uranyl ion mineral ligand are containing CO3 2-Substance.
Comparative example 3
A kind of uranium recovery method of uranium-containing waste water, difference from example 1 is that: uranium is added into uranium-containing waste water
Acyl cationic inorganic ligand, the uranyl ion mineral ligand are containing PO4 3-Substance.
Test example
Uranium recovery processing test, the uranium-containing waste water of every group of test are carried out by uranium-containing waste water of Jiangxi uranium mine waste water of mine
Dosage is 500L, test before detection obtain the initial uranium concentration of the uranium-containing waste water be 2.973mg/L, pH value 7.3.
It is tested using the uranium recovery method of embodiment 1, embodiment 8-12, comparative example the 1-3 uranium-containing waste water provided.Electricity
During flocculation treatment, it is 0.2cm, pole plate spacing 5cm that the substrate area of anode and cathode, which is 10cm × 10cm, thickness,
Current density 2.4mA/cm2, electric flocculation processing time 24min.
Test example 1
The pattern and photoelectron energy that the washing that the uranium recovery method of uranium-containing waste water using embodiment 1 obtains is precipitated except uranium
Spectrum is detected, and Fig. 1 is SEM figure of the washing except uranium precipitating, and Fig. 2 is x-ray photoelectron spectroscopy figure of the washing except uranium precipitating.
As can be seen from FIG. 1, in embodiment 1, the washing obtained after being impregnated using cleaning solution has cotton-shaped shape except uranium precipitates
Looks.As can be seen from FIG. 2, the washing obtained after being impregnated using cleaning solution is only 0.04% except the weight percent of uranium in uranium precipitating,
The content is extremely low, it is believed that is not present, illustrates that the method for impregnating uranium-bearing precipitating using cleaning solution can effectively realize uranium
With the dissociation of electric flocculation presoma, the washing after washing can harmless discharge due to not having radioactive uranium except uranium precipitating.
The exterior appearance of ammonium diuranate product and X obtain to the uranium recovery method of the uranium-containing waste water using embodiment 1 is penetrated
Line diffraction is analyzed, and Fig. 3 is the exterior appearance figure of ammonium diuranate product, is substantially in yellow powder, and Fig. 4 is ammonium diuranate production
The XRD spectra of product and the PDF standard card comparative diagram of ammonium diuranate.
As can be seen from FIG. 3, in embodiment 1, obtained ammonium diuranate product is yellow powder, is had with ammonium diuranate identical
Exterior appearance.As can be seen from FIG. 4, in embodiment 1, the X-ray diffraction spectrogram and ammonium diuranate of obtained ammonium diuranate product
PDF standard card match.The ammonium diuranate product illustrated is ammonium diuranate ((NH really4)2U4O13·7H2O)。
The ammonium diuranate product obtained to the uranium recovery method of the uranium-containing waste water using embodiment 1 weighs, and weighs knot
Fruit is 1.988g, and the rate of recovery of uranium is up to 96.32%.
To the uranium recovery method of the uranium-containing waste water using embodiment 1 obtain except the uranium concentration of uranium waste water detects, it is flat
Row carries out two groups of tests, and the result of two groups of tests is respectively 0.023mg/L, 0.019mg/L, has reached cities and towns drinking water standard
Defined emission limit (being no more than 0.05mg/L) requires, and the uranium removal rate of uranium-containing waste water respectively reaches 99.23%, 99.36%.
Test example 2
Blank example 1: being tested using the uranium recovery method of uranium-containing waste water that embodiment 1 provides, using equivalent go from
Sub- water replaces uranium-containing waste water.
Blank example 2: being tested using the uranium recovery method of uranium-containing waste water that embodiment 9 provides, using equivalent go from
Sub- water replaces uranium-containing waste water.
Blank example 3: being tested using the uranium recovery method of uranium-containing waste water that embodiment 11 provides, using equivalent go from
Sub- water replaces uranium-containing waste water.
Each group test for embodiment 1, embodiment 8-12, comparative example 1-3, takes 20mg uranium-bearing precipitating to be scattered in respectively
In 100mL deionized water.Each group test for blank example 1-3, the precipitating for taking 20mg electric flocculation to obtain respectively are scattered in 100mL
In deionized water.The concentrated nitric acid that 25mL concentration is 5mol/L is added to be dissolved to obtain solution, corresponding solution is tested to each group
Composition checked that and calculate the uranium content of precipitating, the results are shown in Table 1.
Table 1 is at being grouped as and precipitate uranium content statistical form
According to table 1, when other conditions are identical, with the molar fraction highest of uranium in the embodiment of ferroelectricity extremely anode；
When other conditions are identical, using alizarin red as the molar fraction highest of uranium in the embodiment of the ligand of uranyl ion.
Test example 3
In electric flocculation treatment process, to the uranium concentration in liquid to be processed in embodiment 1, embodiment 8, comparative example 1-3 into
Row detection, result are as shown in Figure 5.
As can be seen from FIG. 5, use alizarin red for the ligand of uranyl ion, it is obvious to the removal of uranium in electric flocculation treatment process
Better than other schemes.
Test example 4
It is dense to the metal ion in liquid to be processed in embodiment 1, embodiment 9, embodiment 11 in electric flocculation treatment process
Degree is detected, and result is as shown in Figure 6.
As can be seen from FIG. 6, electric flocculation processing is carried out with ferroelectricity extremely anode, without dissolubility Fe in water outlet3+, Fe3+Content is not
Increase, other metal ions will not be introduced because of electric flocculation processing.Electric flocculation processing is carried out using magnesium electrode and aluminium electrode as anode, it is right
The Mg answered2+、Al3+Content increases, and can introduce other metal ions because of electric flocculation.
Embodiments described above is some embodiments of the present application, instead of all the embodiments.The reality of the application
The detailed description for applying example is not intended to limit claimed scope of the present application, but is merely representative of the selected implementation of the application
Example.Based on the embodiment in the application, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall in the protection scope of this application.
Claims (10)
1. a kind of uranium recovery method of uranium-containing waste water characterized by comprising
Under conditions of pH value is not higher than 3, uranium-containing waste water and uranyl ion organic ligand are mixed to get liquid to be processed, in pH value
Under acid condition not less than 3, electric flocculation is carried out to the liquid to be processed and handles to obtain except uranium waste water and uranium-bearing precipitate；
The uranium-bearing precipitating is impregnated with cleaning solution, obtains washing except uranium precipitating and uranium-bearing concentrate, by the uranium-bearing concentrate
Uranium-bearing residue is obtained with concentrated nitric acid heating resolution, the cleaning solution contains sodium carbonate and hydrogen peroxide；
The uranium-bearing residue is reacted into 1.5-2.5h under the solution environmental that pH value is 8-9.8 with ammonia source, it is heavy to obtain ammonium diuranate
It forms sediment.
2. the uranium recovery method of uranium-containing waste water according to claim 1, which is characterized in that in the cleaning solution, the carbon
The concentration of sour sodium is 0.4-0.6mol/L, and the concentration of the hydrogen peroxide is 0.4-0.6mol/L.
3. the uranium recovery method of uranium-containing waste water according to claim 2, which is characterized in that the uranium-bearing precipitating is washed with described
The solid-to-liquid ratio for washing liquid is 1g:10-12mL.
4. the uranium recovery method of uranium-containing waste water according to claim 3, which is characterized in that will be described in uranium-bearing precipitating use
Before cleaning solution impregnates, first the uranium-bearing is deposited under the conditions of 35-45 DEG C of temperature and is dried.
5. the uranium recovery method of uranium-containing waste water according to claim 1, which is characterized in that by the uranium-bearing concentrate institute
The heating temperature for stating concentrated nitric acid heating resolution is 220-250 DEG C；Optionally, after the liquid before heating resolution and heating are cleared up
Residue volume ratio be 1:0.01-0.02.
6. the uranium recovery method of uranium-containing waste water according to claim 1-5, which is characterized in that the concentrated nitric acid
Concentration is 4-6mol/L.
7. the uranium recovery method of uranium-containing waste water according to claim 6, which is characterized in that the uranium-bearing precipitating is washed described in
After washing liquid immersion, the washing is removed into uranium precipitating and is rinsed with cleaning solution, the liquid for collecting immersion and flushing obtains described contain
Uranium enrichment liquid；Optionally, the amount ratio of uranium-bearing precipitating and the cleaning solution is 1g:10-12mL, the uranium-bearing concentrate with
The volume ratio of the concentrated nitric acid is 1:0.25-0.35.
8. the uranium recovery method of uranium-containing waste water according to claim 5, which is characterized in that by the uranium-bearing concentrate institute
It after stating concentrated nitric acid heating resolution, is diluted with water to obtain the uranium-bearing residue, the volume ratio for diluting front and back is 0.01-0.02:1.
9. the uranium recovery method of uranium-containing waste water according to claim 1, which is characterized in that by the uranium-containing waste water with it is described
Before the mixing of uranyl ion organic ligand, the pH value of the uranium-containing waste water is first adjusted to 2.8-3；
And/or before carrying out electric flocculation processing to the liquid to be processed, the pH value of the liquid to be processed is first adjusted to 6.4-
6.7。
10. according to claim 1 or the uranium recovery method of uranium-containing waste water described in 9, which is characterized in that the uranyl ion is organic
Ligand is selected from one of iminodiacetic acid and alizarin red, and optionally, the uranyl ion organic ligand is alizarin red；
And/or electric flocculation processing middle-jiao yang, function of the spleen and stomach extremely iron electrode, to electrode be graphite electrode.
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| CN115557578A (en) * | 2022-09-28 | 2023-01-03 | 中核四0四有限公司 | Device and method for treating organic phase in uranium-containing nitric acid waste liquid through electro-flotation-electro-flocculation |
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| US4243638A (en) * | 1978-06-15 | 1981-01-06 | Westinghouse Electric Corp. | Iron EDTA chelate catalyzed oxidation of uranium |
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| US4243638A (en) * | 1978-06-15 | 1981-01-06 | Westinghouse Electric Corp. | Iron EDTA chelate catalyzed oxidation of uranium |
| CN102277499A (en) * | 2011-08-11 | 2011-12-14 | 杭州凯大催化金属材料有限公司 | Method for recovering rhodium from organic waste liquid produced in carbonyl synthesis reaction |
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| CN115557578A (en) * | 2022-09-28 | 2023-01-03 | 中核四0四有限公司 | Device and method for treating organic phase in uranium-containing nitric acid waste liquid through electro-flotation-electro-flocculation |
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