CN109741849A - A kind of deep-purifying method of the uranium purifying conversion fluorine-containing waste liquid of uranium-bearing - Google Patents
A kind of deep-purifying method of the uranium purifying conversion fluorine-containing waste liquid of uranium-bearing Download PDFInfo
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- CN109741849A CN109741849A CN201811608740.8A CN201811608740A CN109741849A CN 109741849 A CN109741849 A CN 109741849A CN 201811608740 A CN201811608740 A CN 201811608740A CN 109741849 A CN109741849 A CN 109741849A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
A kind of deep-purifying method of the uranium purifying conversion fluorine-containing waste liquid of uranium-bearing, comprising the following steps: S1: reagent prepares and prepare S2: uranium-bearing fluoride waste pre-processes S3: neutralize S4: separation organic phase S5: micro-filtration, nanofiltration S6: ion exchange removes uranium S7: lime precipitation S8: filtering S9: ion exchange fluorine removal S10: qualification discharge.
Description
Technical field
The invention belongs to uranium to purify conversion field, and in particular to a kind of deep purifying of the uranium purifying conversion fluorine-containing waste liquid of uranium-bearing
Method.
Background technique
In China, uranium purifying conversion production line is with U3O8Prepare UF6During can generate uranium-bearing, fluorine and CO3 2-、Cl?、
NO3 ?、Na+The radioactive liquid waste of plasma, a small amount of TBP.Currently, the waste water treatment process of the production line using solvent extraction, from
Son exchanges, the method for chemical precipitation removes uranium, using lime precipitation fluorine removal.
It is above-mentioned except in uranium technique solvent extraction be for the uranium-bearing waste liquid containing nitric acid and TBP generated in uranium purification process
Processing method, its acidity is deployed first to 3mol/L or so with NaOH, then with TBP from nitric acid solution Extraction of Nitric Acid uranium
Acyl makes metallic uranium separate, purify with other metal impurities, later again using 1mol/L nitric acid as detergent, to uranium-bearing organic phase
It is washed, the trace metal impurities for being extracted or carrying secretly is eluted from organic phase, finally again with dust technology metal
Uranium back extraction is to water phase, and strip liquor return uranium purifying production line recycling, raffinate water is as discharging of waste liquid after purification.
Ion-exchange is to contain F for what is generated in uranium conversion process-、CO3 2-Alkaline uranium-bearing waste liquid processing method,
Using strong basicity quaternary ammonium type anion exchange resin (201 × 7 type) adsorption treatment, uranium concentration can be reduced to 1mg/L after absorption
Left and right.
Chemical precipitation method is for the high concentration uranium-bearing generated in ion exchange resin stripping liquid and uranium purifying conversion process
The processing method of waste liquid is that solid sodium hydroxide is added in uranium-bearing waste liquid, is allowed to generate sodium diuranate precipitating, recycle therein
Metallic uranium.
Waste liquid after except uranium uses lime precipitation fluorine removal again, and superfluous lime is added in the waste liquid, makes wherein F-With
Lime reaction generates CaF2Precipitating, then be separated by solid-liquid separation by plate and frame filter press, discharging of waste liquid to evaporation tank, solid waste is temporary.
For uranium purifying conversion waste water after the fluorine removal is except uranium process, uranium content is 1~2mg/L, is not achieved 50 μ g/L's
Discharge index；The discharge index of 10mg/L is not achieved in 100mg/L or so in fluorine content.
Summary of the invention
It is an object of the invention to: the depth for providing a kind of uranium-bearing fluoride waste generated for uranium purifying conversion process is net
Change method, so that uranium concentration in relief liquor is small after the fluorine-containing uranium-containing waste water of uranium purifying conversion process generation is treated by the present method
In 50 μ g/L, fluorine content is less than 10mg/L.
Technical scheme is as follows: a kind of deep-purifying method of the uranium purifying conversion fluorine-containing waste liquid of uranium-bearing, including with
Lower step:
S1: reagent prepares and prepares
5%Na2CO3Solution, 10%HCl solution, 4%NaOH solution, 10% polymeric aluminum chlorides solution, 1% polyacrylamide
Solution；
S2: uranium-bearing fluoride waste pretreatment
The uranium content that conversion production line generates is purified to uranium by solvent extraction, ion-exchange and chemical precipitation method
Waste water higher than 50mg/L is pre-processed, and is allowed to uranium content and is reduced to 50 μ g/L~50mg/L；
S3: it neutralizes
All waste water generated in S2 are neutralized, waste liquid is in acidity after neutralization；
S4: separation organic phase
With oily water separating equipment by S3 generate waste liquid in organic phase make the organic phase content in water phase be reduced to 1ppm with
Under；
S5: micro-filtration, nanofiltration
Waste water after removal organic phase is concentrated with nanofiltration membrane again after micro-filtration removes larger particles；
S6: ion exchange removes uranium
Adsorption cleaning is carried out to the concentrate that nanofiltration generates；Efflux uranium is collected by letdown tank；Ion exchange resin absorption
It after saturation, is desorbed, generated stripping liquid recycles uranium using chemical precipitation method；
S7: lime precipitation
Excessive lime is added in letdown tank waste water, generates CaF2Precipitating removes fluorinion in waste water.
S8: filtering
The waste water after precipitating is separated by solid-liquid separation with filter press, filtered solution is further filtered with ultrafiltration membrane；Ultra-filtration process
The concentrate of generation returns to S7 and handles again；
S9: ion exchange fluorine removal
After liquid pH after the filter of ultrafiltration membrane is adjusted to 1~6 with 10%HCl solution, inhaled with Natural zeolite exchanger resin
Attached purification；After Natural zeolite exchanger resin adsorption saturation, resin is desorbed with 4%NaOH solution, generated desorption
Liquid return step 7 is handled again.
S10: qualification discharge
Through uranium concentration in S9 treated waste liquid less than 50 μ g/L, Funing tablet is less than 10mg/L, using NaOH by its pH value
It is discharged after adjustment.
In the S2, ion-exchange uses 201 × 7 type resins.
In the S4, the useless organic phase isolated is temporary with container, periodically transports outward.
In the S5, nanofiltration membrane precision uses 300 dalton.
In the S5, the clear liquid uranium concentration that final nanofiltration generates is reduced to 0.05mg/L hereinafter, being collected by letdown tank.
In the S6, inhaled with the concentrate that the bright TP260 resin cation for containing chemical production of Germany generates nanofiltration
Attached purification.
In the S6, adsorption cleaning is carried out to the concentrate that nanofiltration generates with TP107 resin anion (R.A.).
In the S6, before purification according to the absorption environment 10%HCl solution of resin or NaOH to the pH value of the waste liquid into
Row adjustment；Efflux uranium concentration can be reduced to 0.05mg/L or less.
In the S8, produced material residue barrelling outward transport.
In the S8, its pH value is adjusted to discharging after 6~9 using NaOH.
Remarkable result of the invention is:
(1) uranium is a kind of important radionuclide, releases alpha ray, will cause radioactivity irradiation damage to human body, lure
Send out disease various, in addition, uranium or a kind of valuable metal resource, therefore, the relation technological researching of removal and recycling uranium is increasingly
It is taken seriously.Uranium recycles the harm not only reduced to environment, also reduces the cost of uranium purifying conversion.Utilize the technology
The uranium content in the uranium-containing waste water for relating to the generation of uranium industry can be made to be down to 50 μ g/L hereinafter, being effectively protected around She You factory
Water quality.
(2) fluorine ion can polluted underground water, people's long-term drinking fluorinated water will lead to that den tal fluorosis, sclerotin be crisp, anchylosis
Even paralyse.The content of fluoride ion in the fluoride waste for relating to the generation of fluorine industry can be made to be down to 10mg/L hereinafter, reaching using the technology
To national emission standard, it is effectively protected water quality around She Fu factory.
Detailed description of the invention
Fig. 1 is the deep-purifying method schematic diagram of the uranium of the present invention purifying conversion fluorine-containing waste liquid of uranium-bearing；
Specific embodiment
A kind of deep-purifying method of the uranium purifying conversion fluorine-containing waste liquid of uranium-bearing, comprising the following steps:
S1: reagent prepares and prepares
5%Na2CO3Solution, 10%HCl solution, 4%NaOH solution, 10%PAC (aluminium polychloride) solution, 1%PAM
(polyacrylamide) solution；
S2: uranium-bearing fluoride waste pretreatment
Conversion production is purified to uranium by solvent extraction, ion-exchange (201 × 7 type resin) and chemical precipitation method
Waste water of the uranium content that line generates higher than 50mg/L is pre-processed, and is allowed to uranium content and is reduced to 50 μ g/L~50mg/L；
S3: it neutralizes
All waste water generated in S2 are neutralized, waste liquid is in acidity after neutralization；
S4: separation organic phase
With oily water separating equipment by S3 generate waste liquid in organic phase make the organic phase content in water phase be reduced to 1ppm with
Under；The useless organic phase isolated is temporary with container, periodically transports outward；
S5: micro-filtration, nanofiltration
Waste water after removal organic phase is concentrated with nanofiltration membrane again after micro-filtration removes larger particles.Nanofiltration membrane precision
Using 300 dalton, the clear liquid uranium concentration that final nanofiltration generates can be reduced to 0.05mg/L hereinafter, being collected by letdown tank.
S6: ion exchange removes uranium
The concentration that nanofiltration is generated with the bright TP260 resin cation for containing chemical production of Germany or TP107 resin anion (R.A.)
Liquid carries out adsorption cleaning.Needed before purification according to the absorption environment 10%HCl solution of resin or NaOH to the pH value of the waste liquid into
Row adjustment.Efflux uranium concentration can be reduced to 0.05mg/L hereinafter, being collected by letdown tank.After ion exchange resin adsorption saturation,
It need to be desorbed, generated stripping liquid recycles uranium using chemical precipitation method.
S7: lime precipitation
Excessive lime is added in letdown tank waste water, generates CaF2Precipitating removes fluorinion in waste water.
S8: filtering
The waste water after precipitating is separated by solid-liquid separation with filter press, produced material residue barrelling outward transport, filtered solution ultrafiltration membrane
Further filtering.The concentrate return step 7 that ultra-filtration process generates is handled again.
S9: ion exchange fluorine removal
After liquid pH after the filter of ultrafiltration membrane is adjusted to 1~6 with 10%HCl solution, inhaled with Natural zeolite exchanger resin
Attached purification.After Natural zeolite exchanger resin adsorption saturation, resin is desorbed with 4%NaOH solution, generated desorption
Liquid return step 7 is handled again.
S10: qualification discharge
Through uranium concentration in S9 treated waste liquid less than 50 μ g/L, Funing tablet is less than 10mg/L, using NaOH by its pH value
It adjusts to discharging after 6~9.
Claims (10)
1. a kind of deep-purifying method of the uranium purifying conversion fluorine-containing waste liquid of uranium-bearing, it is characterised in that: the following steps are included:
S1: reagent prepares and prepares
5%Na2CO3Solution, 10%HCl solution, 4%NaOH solution, 10% polymeric aluminum chlorides solution, 1% polyacrylamide are molten
Liquid；
S2: uranium-bearing fluoride waste pretreatment
The uranium content that conversion production line generates is purified to uranium by solvent extraction, ion-exchange and chemical precipitation method to be higher than
The waste water of 50mg/L is pre-processed, and is allowed to uranium content and is reduced to 50 μ g/L~50mg/L；
S3: it neutralizes
All waste water generated in S2 are neutralized, waste liquid is in acidity after neutralization；
S4: separation organic phase
S3, which is generated the organic phase in waste liquid, with oily water separating equipment makes the organic phase content in water phase be reduced to 1ppm or less；
S5: micro-filtration, nanofiltration
Waste water after removal organic phase is concentrated with nanofiltration membrane again after micro-filtration removes larger particles；
S6: ion exchange removes uranium
Adsorption cleaning is carried out to the concentrate that nanofiltration generates；Efflux uranium is collected by letdown tank；Ion exchange resin adsorption saturation
Afterwards, it is desorbed, generated stripping liquid recycles uranium using chemical precipitation method；
S7: lime precipitation
Excessive lime is added in letdown tank waste water, generates CaF2Precipitating removes fluorinion in waste water.
S8: filtering
The waste water after precipitating is separated by solid-liquid separation with filter press, filtered solution is further filtered with ultrafiltration membrane；Ultra-filtration process generates
Concentrate return S7 handle again；
S9: ion exchange fluorine removal
After liquid pH after the filter of ultrafiltration membrane is adjusted to 1~6 with 10%HCl solution, adsorb with Natural zeolite exchanger resin net
Change；After Natural zeolite exchanger resin adsorption saturation, resin is desorbed with 4%NaOH solution, generated stripping liquid returns
Step 7 is returned to handle again.
S10: qualification discharge
Through uranium concentration in S9 treated waste liquid less than 50 μ g/L, Funing tablet is less than 10mg/L, is adjusted its pH value using NaOH
After discharge.
2. a kind of deep-purifying method of uranium purifying conversion fluorine-containing waste liquid of uranium-bearing according to claim 1, it is characterised in that:
In the S2, ion-exchange uses 201 × 7 type resins.
3. a kind of deep-purifying method of uranium purifying conversion fluorine-containing waste liquid of uranium-bearing according to claim 1, it is characterised in that:
In the S4, the useless organic phase isolated is temporary with container, periodically transports outward.
4. a kind of deep-purifying method of uranium purifying conversion fluorine-containing waste liquid of uranium-bearing according to claim 1, it is characterised in that:
In the S5, nanofiltration membrane precision uses 300 dalton.
5. a kind of deep-purifying method of uranium purifying conversion fluorine-containing waste liquid of uranium-bearing according to claim 4, it is characterised in that:
In the S5, the clear liquid uranium concentration that final nanofiltration generates is reduced to 0.05mg/L hereinafter, being collected by letdown tank.
6. a kind of deep-purifying method of uranium purifying conversion fluorine-containing waste liquid of uranium-bearing according to claim 1, it is characterised in that:
In the S6, adsorption cleaning is carried out to the concentrate that nanofiltration generates with Germany's bright TP260 resin cation for containing chemical production.
7. a kind of deep-purifying method of uranium purifying conversion fluorine-containing waste liquid of uranium-bearing according to claim 1, it is characterised in that:
In the S6, adsorption cleaning is carried out to the concentrate that nanofiltration generates with TP107 resin anion (R.A.).
8. a kind of deep-purifying method of uranium purifying conversion fluorine-containing waste liquid of uranium-bearing according to claim 1, it is characterised in that:
In the S6, the pH value of the waste liquid is adjusted according to the absorption environment 10%HCl solution or NaOH of resin before purification；Stream
Liquid uranium concentration can be reduced to 0.05mg/L or less out.
9. a kind of deep-purifying method of uranium purifying conversion fluorine-containing waste liquid of uranium-bearing according to claim 1, it is characterised in that:
In the S8, produced material residue barrelling outward transport.
10. a kind of deep-purifying method of uranium purifying conversion fluorine-containing waste liquid of uranium-bearing according to claim 1, feature exist
In: in the S8, its pH value is adjusted to discharging after 6~9 using NaOH.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112708759A (en) * | 2020-11-27 | 2021-04-27 | 核工业北京化工冶金研究院 | Method for enriching uranium from sulfuric acid leaching solution |
| CN113387412A (en) * | 2021-05-19 | 2021-09-14 | 中核四0四有限公司 | Ion exchange device for uranium-containing wastewater treatment under nitric acid and carbonic acid mixed system |
| CN113406115A (en) * | 2021-04-28 | 2021-09-17 | 中国辐射防护研究院 | Method for analyzing uranium isotope content in calcium fluoride slag |
| CN115385492A (en) * | 2022-09-30 | 2022-11-25 | 中核四0四有限公司 | Process for treating uranium-containing fluorine-containing wastewater by combination of pretreatment and deep uranium removal |
| CN117059294A (en) * | 2023-08-16 | 2023-11-14 | 西南科技大学 | Deep purification and uranium fluoride resource recovery method for ultra-high fluorine uranium-containing wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112708759A (en) * | 2020-11-27 | 2021-04-27 | 核工业北京化工冶金研究院 | Method for enriching uranium from sulfuric acid leaching solution |
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