CN104437348A - Uranium removing material for treating uranium-containing groundwater in situ and preparation method thereof - Google Patents
Uranium removing material for treating uranium-containing groundwater in situ and preparation method thereof Download PDFInfo
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- CN104437348A CN104437348A CN201410634545.8A CN201410634545A CN104437348A CN 104437348 A CN104437348 A CN 104437348A CN 201410634545 A CN201410634545 A CN 201410634545A CN 104437348 A CN104437348 A CN 104437348A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/06—Contaminated groundwater or leachate
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a uranium removing material for treating uranium-containing groundwater in situ. The uranium removing material is in a powder form and comprises illite particles and nano zero-valent iron, wherein the illite particles serve as support materials, and the nano zero-valent iron is attached to the surfaces of the illite particles. The uranium removing material can be used for overcoming the defects of the background art, and the uranium removing material can achieve a good effect of treating and repairing the low-concentration uranium-containing groundwater due to the good adsorbability of the illite and the strong reducibility of the nano zero-valent iron. The uranium removing material is capable of effectively removing more than 98% of the uranium in the groundwater. The invention further discloses a preparation method of the uranium removing material. The preparation method of the uranium removing material is simple and easy to operate and has no special requirement for external environmental conditions. The raw materials used for preparing the uranium removing material are easily available and are low in cost, and the product synthesized by adopting the preparation method has high quality and good stability.
Description
Technical field
The invention provides a kind of for underground water except the material of uranium, particularly relate to a kind of can in-situ treatment uranium-bearing underground water except uranium material, and the preparation method of this material, belongs to functional material preparing technical field.
Background technology
In order to the health of the mankind and the development of society, countries in the world have launched the research to uranium-containing waste water treatment technology.Wherein the suction-operated of clay mineral, the adsorption precipitation effect of chemical agent, microorganism treatment, macromolecular material treatment technology and crops are mainly concentrated on to the adsorption effect of uranium to the research of low concentration uranium-bearing groundwater treatment technology.There is the drawback that cost is high, efficiency is low, repairing efficiency is long and secondary pollution has a big risk in current existing treatment technology.The reducing metal ions of high-valence state in solution can be lower valency by nano zero valence iron, be widely used in the repairing research of environmental contaminants, it has the feature that particle is little, specific area is large, but nano zero valence iron is very easily reunited, cause reducing its surface area, thus affect its repairing effect to pollutant.
Summary of the invention
The invention provides a kind of for in-situ treatment uranium-bearing underground water except uranium material, solve the deficiency in background technology, this material is in the groundwater remediation process of low concentration uranium, and gathered the strong reducing property of the good absorption property of illite and nano zero valence iron, treatment effect is good.This material effectively can remove the uranium in underground water, and clearance can reach more than 98%.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
For in-situ treatment uranium-bearing underground water except a uranium material, described material is Powdered, comprise as backing material illite particle and be attached to the nano zero valence iron of illite particle surface.
Described illite particle is 1250 orders, and its particle size is 0.1 ~ 10 μm.
The present invention additionally provides simultaneously and a kind ofly prepares the above-mentioned method except uranium material, comprises the following steps: (1), ground by illite, is sized to below 1250 orders, then puts it into drying box, dry at 75 ~ 85 DEG C, for subsequent use after dry;
(2), illite powder dried in upper step is added in container, and configuration concentration is the iron salt solutions of 0.143mol/L ~ 0.716mol/L in a reservoir, mechanical agitation 10 ~ 15min when logical nitrogen, iron salt solutions is fully mixed with illite powder, and illite powder is dispersed in iron salt solutions;
(3), in container, drip sodium borohydride or solution of potassium borohydride that concentration is 0.187mol/L ~ 0.935mol/L, whole course of reaction continue to pass into nitrogen and violent mechanical agitation until reaction terminate, reaction terminate rear continuation stirring 15 ~ 20min;
(4), stir stop after, vacuum filtration immediately, filters the complete filter cake ethanolic solution obtained and carries out filtration washing, then carry out filtration washing with absolute ethyl alcohol, obtain black solid after washing;
(5), by the black solid obtained in upper step transfer to vacuum drying in vacuum drying chamber immediately, baking temperature is 60 ~ 70 DEG C, namely obtain after drying for in-situ treatment uranium-bearing underground water except uranium material.
In step (2), the compound method of iron salt solutions is: by iron salt dissolved in ethanolic solution, the concentration of iron salt solutions is 1.44 ~ 7.16mol/L, and described molysite is the one in iron chloride/ferrous iron, ferric sulfate/ferrous iron, ferric nitrate/ferrous iron and water crystallization state thereof.
Step controls the rate of addition of sodium borohydride or solution of potassium borohydride in (3), guarantees that solution dropwises in 20 ~ 30min.
The uranium material that removes provided by the present invention is suitable for processing the underground water that uranium content is 100 ~ 500 μ g/L, when processing, above-mentioned material is added in underground water, addition is 0.05g/L ~ 0.1g/L, reaction time continues within 3 hours, effectively to remove the uranium in underground water, and clearance is greater than 98%.
In the present invention, because clay mineral has good absorption property, the ion in energy adsorption aqueous solution is fixed on clay mineral surface and interlayer.Illite is extensively present in occurring in nature as the one in three large clay minerals, and it has good bearing capacity, stability, easily obtains cheap, is applicable to pollution amelioration engineering and uses, and can not cause secondary pollution.Illite top layer is laminated structure, for the support of Zero-valent Iron provides the useful space.Above-mentioned material with sodium borohydride be reducing agent iron ion is reduced into nano zero valence iron be attached to illite surface make.As backing material, nano zero valence iron is supported with illite, the reunion of nano zero valence iron can be improved, increase specific area, improve the stability of nano zero valence iron.In course of reaction, adopt pretreated illite as backing material, the nano zero valence iron Granular composite utilizing illite laminated structure that reaction is produced also is attached on illite, passes into inert gas simultaneously, strengthens the peptizaiton of nano zero valence iron particle.The nano zero valence iron that illite supports is active strong, and bearing capacity is high, good stability, domain size distribution evenly; Illite supports nano zero valence iron can as permeable reactive barrier active filler, for heavy metal pollution underground water provide safer, economical, efficient method.
Generally speaking, the present invention compared with prior art has the following advantages: 1, relative to existing process uranium-bearing groundwater treatment technology, the reproducibility of illitic good adsorption properties and nano zero valence iron of collection of material prepared by the present invention, treatment effeciency improves greatly, and reduces secondary pollution risk.
2, relative to nano zero valence iron, the present invention's illite supports nano zero valence iron, and improve the problem that it is easily reunited, Zero-valent Iron is not easily oxidized, more stable, and bearing capacity improves, and can be used for underground water in-situ immobilization.
3, material provided by the present invention can synthesize in laboratory conditions, and preparation method is simple to operation, and raw materials used cheap and easy to get, environmental condition is without particular/special requirement to external world, and synthetic product quality is high, good stability.
Accompanying drawing explanation
Fig. 1 is that the SEM except uranium material prepared in the embodiment of the present invention schemes;
Fig. 2 is the XRD scintigram except uranium material prepared in the embodiment of the present invention;
Fig. 3 is prepared except uranium material is to the removal efficiency comparison diagram of uranium in the aqueous solution in the embodiment of the present invention;
Fig. 4 is prepared except uranium material is to the removal efficiency of uranium in aqueous solution variation diagram in time in the embodiment of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, detailed specific description is done to the present invention, but protection scope of the present invention is not limited to following examples.
Embodiment 1
The uranium material that removes provided in the present embodiment adopts following methods preparation, and illite grinds by (1), is sized to below 1250 orders, then illite is put into drying box, and 80 DEG C of dryings, are stored in drier for subsequent use;
(2) the illite 2g obtained in step (1) is taken stand-by in 500mL there-necked flask, configuration 50mL iron salt solutions is poured in there-necked flask, iron salt concentration is 0.2mol/L, the mechanical agitation mixture 10min when logical nitrogen, iron salt solutions is fully mixed with illite, and illite is dispersed in iron salt solutions;
Iron salt solutions collocation method is that 0.072-0.358mol molysite is dissolved in 50ml ethanolic solution (ethanol and water volume ratio are 4:1), and molysite is the one in iron chloride (ferrous iron), ferric sulfate (ferrous iron), ferric nitrate (ferrous iron) and water crystallization state thereof.
(3) the sodium borohydride solution 100mL of 0.5mol/L is configured in Brown Glass Brown glass bottles and jars only, adopt peristaltic pump to control rate of addition, in there-necked flask, dropwise drip sodium borohydride, whole process lasts passes into nitrogen and violent mechanical agitation, after question response terminates, continue to stir 15min;
The rate of addition of sodium borohydride solution remains on 4mL/min-5mL/min, ensures to dropwise in sodium borohydride solution 20-30min.
(4) stop after stirring, rapid vacuum suction filtration, filters the complete filter cake obtained and carries out filtration washing with the ethanol 100mL of 30% again, then carry out filtration washing with absolute ethyl alcohol 100mL;
(5) black solid that step (4) obtains is transferred to vacuum drying chamber 65 DEG C of vacuum drying immediately, can obtain except uranium material.
As shown in Figure 1, nano zero valence iron is attached on illite particle surface the figure of the SEM except uranium material prepared in the present embodiment as can be seen from Figure 1.The XRD scintigram except uranium material prepared by the present embodiment as shown in Figure 2.
The uranium-bearing underground water that initial concentration is 100-200 μ g/L is chosen in the present embodiment, get 20mL in 50mL centrifuge tube with cover, add above-mentioned except uranium material 2mg, be placed in air constant temperature oscillator, shake with 250r/min rotating speed, concussion case temperature controls at 25 DEG C, and 3h is to ensure that reaction reaches balance in concussion.Also with nano zero valence iron and illite material sample in contrast in the present embodiment.Then in differential responses time sampling, acquisition reaction time and initial concentration solution are on the provided impact of removing the reaction of the uranium in underground water except uranium material.Concentration and other compositions of uranium in solution is detected by icp ms.
Figure 3 shows in variable concentrations uranium solution, it is of the present invention except uranium material is to the removal effect of uranium and nano zero valence iron and illitic contrast, the result display uranium can efficiently removed except uranium material in the aqueous solution of the present invention, change removal effect with initial concentration is stablized, and is better than the performance of nano zero valence iron.
Fig. 4 shows illite and nano zero valence iron Theoretical Mass than for prepared except uranium material during 1:1, process initial concentration is the uranium-bearing underground water of 200 μ g/L, react removal efficiency curve over time in 3 hours, show in Fig. 4, above-mentioned except after uranium material and uranium-bearing underground water reacts 3 hours, in solution, the clearance of uranium reaches 98.3%.
Embodiment 2
The uranium material that removes provided in the present embodiment adopts following methods preparation, and illite grinds by (1), is sized to below 1250 orders, then illite is put into drying box, and 75 DEG C of dryings, are stored in drier for subsequent use;
(2) the illite 2g obtained in step (1) is taken stand-by in 500mL there-necked flask, configuration 40mL iron salt solutions is poured in there-necked flask, iron salt concentration is 0.4mol/L, the mechanical agitation mixture 13min when logical nitrogen, iron salt solutions is fully mixed with illite, and illite is dispersed in iron salt solutions;
Iron salt solutions collocation method is that 0.072-0.358mol molysite is dissolved in 50ml ethanolic solution (ethanol and water volume ratio are 4:1), and molysite is the one in iron chloride (ferrous iron), ferric sulfate (ferrous iron), ferric nitrate (ferrous iron) and water crystallization state thereof.
(3) the sodium borohydride solution 100mL of 0.2mol/L is configured in Brown Glass Brown glass bottles and jars only, adopt peristaltic pump to control rate of addition, in there-necked flask, dropwise drip sodium borohydride, whole process lasts passes into nitrogen and violent mechanical agitation, after question response terminates, continue to stir 17min;
Control rate of addition, ensure to dropwise in sodium borohydride solution 20-30min.
(4) stop after stirring, rapid vacuum suction filtration, filters the complete filter cake obtained and carries out filtration washing with the ethanol 100mL of 30% again, then carry out filtration washing with absolute ethyl alcohol 100mL;
(5) black solid that step (4) obtains is transferred to vacuum drying chamber 70 DEG C of vacuum drying immediately, can obtain except uranium material.
Embodiment 3
The uranium material that removes provided in the present embodiment adopts following methods preparation, and illite grinds by (1), is sized to below 1250 orders, then illite is put into drying box, and 85 DEG C of dryings, are stored in drier for subsequent use;
(2) the illite 2g obtained in step (1) is taken stand-by in 500mL there-necked flask, configuration 30mL iron salt solutions is poured in there-necked flask, iron salt concentration is 0.7mol/L, the mechanical agitation mixture 15min when logical nitrogen, iron salt solutions is fully mixed with illite, and illite is dispersed in iron salt solutions;
Iron salt solutions collocation method is that 0.072-0.358mol molysite is dissolved in 50ml ethanolic solution (ethanol and water volume ratio are 4:1), and molysite is the one in iron chloride (ferrous iron), ferric sulfate (ferrous iron), ferric nitrate (ferrous iron) and water crystallization state thereof.
(3) the solution of potassium borohydride 100mL of 0.8mol/L is configured in Brown Glass Brown glass bottles and jars only, adopt peristaltic pump to control rate of addition, in there-necked flask, dropwise drip sodium borohydride, whole process lasts passes into nitrogen and violent mechanical agitation, after question response terminates, continue to stir 20min;
Control rate of addition, ensure to dropwise in solution of potassium borohydride 20-30min.
(4) stop after stirring, rapid vacuum suction filtration, filters the complete filter cake obtained and carries out filtration washing with the ethanol 100mL of 30% again, then carry out filtration washing with absolute ethyl alcohol 100mL;
(5) black solid that step (4) obtains is transferred to vacuum drying chamber 80 DEG C of vacuum drying immediately, can obtain except uranium material.
Claims (6)
1. for in-situ treatment uranium-bearing underground water except a uranium material, it is characterized in that: described except uranium material be Powdered, comprise as backing material illite particle and be attached to the nano zero valence iron of illite particle surface.
2. according to claim 1 for in-situ treatment uranium-bearing underground water except uranium material, it is characterized in that: described illite particle is 1250 orders, its particle size is 0.1 ~ 10 μm.
3. to prepare described in claim 1 except the method for uranium material, it is characterized in that comprising the following steps: (1), illite is ground, be sized to below 1250 orders, then put it into drying box, dry at 75 ~ 85 DEG C, for subsequent use after dry;
(2), illite powder dried in upper step is added in container, and configuration concentration is the iron salt solutions of 0.143mol/L ~ 0.716mol/L in a reservoir, mechanical agitation 10 ~ 15min when logical nitrogen, iron salt solutions is fully mixed with illite powder, and illite powder is dispersed in iron salt solutions;
(3), in container, drip sodium borohydride or solution of potassium borohydride that concentration is 0.187mol/L ~ 0.935mol/L, whole course of reaction continue to pass into nitrogen and mechanical agitation until reaction terminate, reaction terminate rear continuation stirring 15 ~ 20min;
(4), stir stop after, vacuum filtration immediately, filters the complete filter cake ethanolic solution obtained and carries out filtration washing, then carry out filtration washing with absolute ethyl alcohol, obtain black solid after washing;
(5), by the black solid obtained in upper step transfer to vacuum drying in vacuum drying chamber immediately, baking temperature is 60 ~ 70 DEG C, namely obtain after drying for in-situ treatment uranium-bearing underground water except uranium material.
4. preparation method according to claim 3, it is characterized in that: in step (2), the compound method of iron salt solutions is: by iron salt dissolved in ethanolic solution, the concentration of iron salt solutions is 1.44 ~ 7.16mol/L, and described molysite is the one in iron chloride/ferrous iron, ferric sulfate/ferrous iron, ferric nitrate/ferrous iron and water crystallization state thereof.
5. preparation method according to claim 3, is characterized in that: step controls the rate of addition of sodium borohydride or solution of potassium borohydride in (3), guarantees that solution dropwises in 20 ~ 30min.
6. the uranium-bearing Groundwater Treatment Methods based on material described in claim 1, it is characterized in that: be add except uranium material in the underground water of 100 ~ 500 μ g/L at uranium content, addition is 0.05g/L ~ 0.1g/L, reaction time effectively can remove uranium in underground water after continuing 3 hours, and clearance is greater than 98%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105810278A (en) * | 2016-05-23 | 2016-07-27 | 绍兴文理学院 | Purification detection and purification device of uranium-polluted underground water |
| CN108927100A (en) * | 2018-08-15 | 2018-12-04 | 南华大学 | A kind of preparation method and application of nano zero-valence iron composite material |
| CN109821508A (en) * | 2019-01-15 | 2019-05-31 | 华北电力大学 | The preparation method and application of dictyophora phalloidea load vulcanization nano zero valence iron |
| CN110097992A (en) * | 2019-05-09 | 2019-08-06 | 东华理工大学 | A kind of method that high-strength flour cladding nano zero valence iron removes uranium in nuclear waste |
| CN113104921A (en) * | 2021-03-31 | 2021-07-13 | 核工业北京化工冶金研究院 | Method for treating uranium-containing wastewater |
| CN114733491A (en) * | 2022-03-07 | 2022-07-12 | 南华大学 | Phosphated chitosan loaded magnetic nano-iron composite material and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105810278A (en) * | 2016-05-23 | 2016-07-27 | 绍兴文理学院 | Purification detection and purification device of uranium-polluted underground water |
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| CN108927100A (en) * | 2018-08-15 | 2018-12-04 | 南华大学 | A kind of preparation method and application of nano zero-valence iron composite material |
| CN109821508A (en) * | 2019-01-15 | 2019-05-31 | 华北电力大学 | The preparation method and application of dictyophora phalloidea load vulcanization nano zero valence iron |
| CN110097992A (en) * | 2019-05-09 | 2019-08-06 | 东华理工大学 | A kind of method that high-strength flour cladding nano zero valence iron removes uranium in nuclear waste |
| CN113104921A (en) * | 2021-03-31 | 2021-07-13 | 核工业北京化工冶金研究院 | Method for treating uranium-containing wastewater |
| CN114733491A (en) * | 2022-03-07 | 2022-07-12 | 南华大学 | Phosphated chitosan loaded magnetic nano-iron composite material and preparation method and application thereof |
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Application publication date: 20150325 |