CN113060780B - Method for rapidly removing uranium in water by aging modified zero-valent iron - Google Patents

Method for rapidly removing uranium in water by aging modified zero-valent iron Download PDF

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CN113060780B
CN113060780B CN202110243037.7A CN202110243037A CN113060780B CN 113060780 B CN113060780 B CN 113060780B CN 202110243037 A CN202110243037 A CN 202110243037A CN 113060780 B CN113060780 B CN 113060780B
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valent iron
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uranium
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modified zero
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CN113060780A (en
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梁丽萍
吴倩
奚芬芬
谭为绶
孟旭
王斌
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University of Shaoxing
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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
    • 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
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • 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
    • 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
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
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Abstract

The invention improves the activity of zero-valent iron by aging in water after the zero-valent iron is vulcanized and modified, and provides a method for quickly removing uranium (VI) in water by aging and modifying the zero-valent iron. Compared with the prior art, the method is simple, rapid and convenient to operate, and the reaction process is easy to control.

Description

Method for rapidly removing uranium in water by aging modified zero-valent iron
Technical Field
The invention belongs to the technical field of water treatment, relates to a wastewater treatment method, and particularly relates to a method for treating uranium (VI) containing wastewater by aging modified zero-valent iron.
Background
Under the pressure of global energy shortage, countries in the world invest huge capital for research and development of new energy projects, and obtaining energy through large-scale nuclear energy development is an effective means for dealing with energy crisis. The large-scale development of nuclear energy inevitably generates a large amount of uranium-containing radioactive wastewater, and poses great threat to the natural environment. Because uranium is a heavy metal element with radioactivity and chemical toxicity, the uranium is exposed in a uranium-containing environment for a long time, and the uranium is easy to cause functional damage to the liver, the kidney and the like of people and even death. Meanwhile, uranium and compounds thereof can enter the water body through various ways and are extremely difficult to discharge out of the water body, and the uranium elements can form long-term radioactive internal irradiation in a human body, thereby causing great harm to the health of the human body.
Uranium in water exists in 3 valence states: u (0), U (IV) and U (VI), wherein U (0) and U (IV) are not easy to migrate and have small influence on the water environment; and U (VI) can coordinate with various ions in water, has higher mobility and has larger influence on the environment. At present, the method for treating uranium-containing wastewater mainly comprises chemistry (mixing)Coagulation), precipitation, ion exchange, microorganisms and the like, can achieve better pollution control effect. However, each treatment method has its own disadvantages, such as higher cost, poor removal efficiency, complex operation, risk of secondary pollution, discharge failure even reaching standards, or generation of radioactive sludge which is difficult to dispose, so that it is difficult to obtain a good treatment effect by using only a single treatment method. The zero-valent iron has low price, high reaction activity and no secondary pollution, and is favored by many researchers. Although the zero-valent iron technology has been widely used, it has certain limitations in practical applications, for example, a passivation film is formed on the surface of zero-valent iron during the production and manufacturing process, and this passivation film can prevent the direct contact between zero-valent iron and pollutants, and reduce the reactivity of zero-valent iron. And corrosion products of zero-valent iron formed during the reaction, e.g. iron oxides/hydroxides, e.g. Fe 2 O 3 ，Fe 3 O 4 FeOOH and Fe (OH) 3 Etc., which gradually accumulate on the surface, the reactivity of which gradually decreases with the accumulation of corrosion products on the surface, and some contaminants also have a passivating effect on zero-valent iron.
In order to improve the reaction activity of the zero-valent iron and effectively relieve the passivation of the zero-valent iron, scholars at home and abroad improve the zero-valent iron by methods such as pretreatment, nano-iron development, metal modification, load modification, weak magnetic field and the like. Although these methods can improve the activity of zero-valent iron to some extent, they still have the disadvantages of high cost, complex operation, potential ecological toxicity, etc. in practical application.
Disclosure of Invention
In order to solve the problems in the background art, the invention improves the activity of zero-valent iron by aging in water after the zero-valent iron is vulcanized and modified, and provides a method for quickly removing uranium (VI) in water by aging and modifying the zero-valent iron.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for rapidly removing uranium (U (VI)) in water by aging modified zero-valent iron comprises the following steps:
s1: modification: under the inert gas atmosphere, adding ferrous sulfate solid powder into stirred distilled water, then adding micron-sized zero-valent iron particles with the particle size, dropwise adding a sodium sulfide solution in the stirring process, stirring and reacting for 1-3 h after dropwise adding is completed, carrying out vacuum filtration, and drying at low temperature to obtain modified zero-valent iron, wherein the molar ratio of ferrous sulfate to sodium sulfide to the micron-sized zero-valent iron particles is 1: 1: 9-50;
s2: aging: placing the modified zero-valent iron in a non-closed container filled with distilled water, standing and aging to obtain an aged modified zero-valent iron solution;
s3: removing uranium: adding the aging modified zero-valent iron solution into uranium-containing wastewater to react and remove uranium; wherein the pH value of the uranium-containing wastewater is 3-8.
The modified zero-valent iron in the prior art can reduce the effect of wastewater treatment after aging, but the invention adopts micron-level zero-valent iron for modification, and then the modified zero-valent iron is subjected to standing aging in a container of non-closed distilled water, so that the uranium removal effect can be improved.
As further preferable in the present technical solution: and in the step S1, the particle size of the zero-valent iron particles is 10-200 microns.
More preferably: the particle size of the zero-valent iron particles in the step S1 is 50 microns.
As further preferable in the present technical solution: the molar ratio of the ferrous sulfate to the sodium sulfide to the micron zero-valent iron particles is 1: 1: 30.
as further preferable in the present technical solution: the molar ratio of Fe to S in the modified zero-valent iron in the step S1 is 30: 1.
As further preferable in the present technical solution: the concentration of the aging modified zero-valent iron solution in the step S2 is 30 g/L-60 g/L.
Further, the concentration of the aging modified zero-valent iron solution in the step S2 is 50 g/L.
As further preferable in the present technical solution: and the standing and aging time in the step S2 is 1 d-20 d.
Further, the standing and aging time in the step S2 is 1 d-15 d.
As further preferable in the present technical solution: the pH of the uranium-containing wastewater in the step S3 is 6.
0.1M MES buffer solution is added in the step S3 to maintain the pH of the uranium-containing wastewater.
As further preferable in the present technical solution: and in the step S3, the addition amount of the aged and modified zero-valent iron in the aged and modified zero-valent iron solution is 0.4-1.5 g per liter of uranium-containing wastewater.
Furthermore, the addition amount of the aging modified zero-valent iron in the aging modified zero-valent iron solution is 1g per liter of uranium-containing wastewater.
As further preferable in the present technical solution: a method for rapidly removing uranium in water by aging modified zero-valent iron comprises the following steps:
s1: modification: under the inert gas atmosphere, adding ferrous sulfate solid powder into stirred distilled water, then adding zero-valent iron particles with the particle size of 50 microns, stirring at the speed of 150-200 r/min, dropwise adding a sodium sulfide solution, completing the dropwise adding within 30min, stirring for 2h after the completion, carrying out vacuum filtration, and drying at low temperature to obtain modified zero-valent iron, wherein the molar ratio of Fe to S in the modified zero-valent iron is 30: 1;
s2: aging: placing the modified zero-valent iron in a non-closed container filled with distilled water, standing and aging for 1d to obtain 50g/L aged modified zero-valent iron solution;
s3: removing uranium: adding the aged and modified zero-valent iron solution into uranium-containing wastewater with the pH of 6, the temperature of 25 ℃ and the concentration of 25-100 mg/L, and stirring at 400r/min to remove uranium; wherein the addition amount of the aging modified zero-valent iron is 1g per liter of uranium-containing wastewater.
Furthermore, the concentration of the uranium-containing wastewater is 50 mg/L.
The concentration of the uranium-containing wastewater which can be treated by the method is higher than that of the uranium-containing wastewater treated by the prior art, the wastewater with the concentration of less than 10mg/L is treated by the prior art, and the modified aged zero-valent iron solution can be directly added into the uranium-containing wastewater to treat the uranium-containing wastewater with the concentration of 25-100 mg/L.
Compared with the prior art, the invention has the beneficial effects that:
(1) compared with the prior art, the activity, the stability in water and the selectivity of target pollutants of the zero-valent iron are greatly improved through the modification and aging process of the micron-sized zero-valent iron.
(2) Compared with the prior art, the micron-sized zero-valent iron is used, the cost is lower, and the modified aged zero-valent iron material is more stable and easy to store.
(3) Compared with the prior art, the invention has the advantages of quick U (VI) removal effect and high removal rate, and well solves the problem of U (VI) pollution.
(4) Compared with the prior art, the method is simple, rapid and convenient to operate, and the reaction process is easy to control.
Drawings
FIG. 1 is a graph comparing the effect of removing U (VI) from zero-valent iron and modified zero-valent iron;
FIG. 2 is a graph showing the comparison of the effect of removing U (VI) from modified zero-valent iron with different S/Fe ratios;
FIG. 3 is a graph comparing the effect of removing U (VI) from modified zero-valent iron and aged modified zero-valent iron;
FIG. 4 is a graph comparing the effect of modified zero valent iron on U (VI) removal for different aging times.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Modified zero-valent iron (1: 9):
at room temperature, adding 150mL of distilled water into a 250mL four-neck flask, stirring by a mechanical stirrer, controlling the rotating speed to be 200r/min, introducing nitrogen in the whole process to control the dissolved oxygen to be 0, and then adding 2.78g (0.01mol) of ferrous sulfate solid powder and stirring for 15 min; then 5g (0.09mol) of 10-micron zero-valent iron particles are added and stirred for 10min, sodium sulfide solution is dropwise added within 30min, the mass of sodium sulfide is 2.40g (0.01mol), after the dropwise addition, anaerobic stirring reaction is continued for 2h, vacuum filtration and low-temperature drying are carried out, and a modified zero-valent iron product is obtained;
aging of modified zero-valent iron:
0.3g of the modified zero-valent iron is put into 10mL of water for aging to form an aged modified zero-valent iron solution.
Removing uranium:
1) and adding the aged modified zero-valent iron solution into 500mL of U (VI) wastewater, stirring for reaction, and quickly removing U (VI) within 10min, wherein the removal rate is over 99.9%.
2) 0.3g of modified zero-valent iron is put into 10mL of water for aging, the aged 7d modified zero-valent iron is filtered and added into 500mLU (VI) wastewater, the pH value is 6, U (VI) can be removed within 45min, and the removal rate is more than 99.9%.
3) 0.3g of modified zero-valent iron is added into 500mLU (VI) wastewater, the pH value is 6, U (VI) can be removed within 60min, and the removal rate is more than 99.9%.
The result is shown in fig. 3, and it can be seen that the activity, stability in water and selectivity of target pollutants of the modified zero-valent iron are greatly improved after the modified zero-valent iron is aged in water, U (VI) can be removed within 10min, and the removal rate is more than 99.9%, so that the operation is simple, rapid and convenient.
Example 2
Modified zero valent iron (1: 15):
at room temperature, adding 150mL of distilled water into a 250mL four-neck flask, stirring by a mechanical stirrer, controlling the rotating speed to be 200r/min, introducing inert gas in the whole process to control the dissolved oxygen to be 0, and then adding 1.67g (0.006mol) of ferrous sulfate solid powder and stirring for 15 min; then adding 5g (0.09mol) of 10-micron zero-valent iron particles, stirring for 10min, dropwise adding a sodium sulfide solution within 30min, continuing anaerobic stirring reaction for 1h after dropwise adding, carrying out vacuum filtration, and drying at low temperature to obtain a modified zero-valent iron product;
aging of modified zero-valent iron:
0.5g of the modified zero-valent iron is put into 10mL of water for aging to form an aged modified zero-valent iron solution.
Example 3
Modified zero-valent iron (1: 30):
at room temperature, adding 150mL of distilled water into a 250mL four-neck flask, stirring by a mechanical stirrer, controlling the rotating speed to be 200r/min, introducing inert gas in the whole process to control the dissolved oxygen to be 0, and then adding 0.83g (0.003mol) of ferrous sulfate solid powder and stirring for 15 min; then adding 5g (0.09mol) of 10-micron zero-valent iron particles, stirring for 10min, dropwise adding a sodium sulfide solution within 30min, continuing anaerobic stirring reaction for 3h after dropwise adding, carrying out vacuum filtration, and drying at low temperature to obtain a modified zero-valent iron product;
aging of modified zero-valent iron:
0.5g of the modified zero-valent iron is put into 10mL of water for aging to form an aged modified zero-valent iron solution.
Example 4
Modified zero valent iron (1: 50):
at room temperature, adding 150mL of distilled water into a 250mL four-neck flask, stirring by a mechanical stirrer, controlling the rotating speed to be 200r/min, introducing inert gas in the whole process to control the dissolved oxygen to be 0, and then adding 0.55g (0.002mol) of ferrous sulfate solid powder and stirring for 15 min; then adding 5g (0.09mol) of 10-micron zero-valent iron particles, stirring for 10min, dropwise adding a sodium sulfide solution within 30min, continuously carrying out anaerobic stirring reaction for 3h after dropwise adding, carrying out vacuum filtration, and drying at low temperature to obtain a modified zero-valent iron product;
aging of modified zero-valent iron:
0.5g of the modified zero-valent iron is put into 10mL of water for aging to form an aged modified zero-valent iron solution.
Example 5
Modification: under an inert gas atmosphere, adding ferrous sulfate solid powder into stirred distilled water, then adding zero-valent iron particles with the particle size of 50 microns, stirring at the speed of 150-200 r/min, dropwise adding a sodium sulfide solution, completing the dropwise adding within 30min, stirring for 2h after the completion, carrying out vacuum filtration, and drying at a low temperature to obtain modified zero-valent iron, wherein the molar ratio of Fe to S in the modified zero-valent iron is 30: 1;
aging: placing the modified zero-valent iron in a non-closed container filled with distilled water, standing and aging for 1d to obtain 50g/L aged modified zero-valent iron solution;
removing uranium: adding the aged and modified zero-valent iron solution into uranium-containing wastewater with the pH value of 6, the temperature of 25 ℃ and the concentration of 50mg/L, and stirring at 400r/min to remove uranium; wherein the addition amount of the aging modified zero-valent iron is 1g per liter of uranium-containing wastewater.
Example 6
Modified zero-valent iron (1: 30) treatment U:
adding 1g/L of synthesized modified zero-valent iron (1: 30) material into a 500mL complete mixing reactor, stirring, rotating speed at 400r/min, temperature at 25 ℃, adding uranium-containing wastewater, controlling pH to be 6.0 by using 0.1M MES buffer solution, adding 0.01M NaCl as background ion, and reacting for 1 hour to remove U (VI).
Unmodified zero-valent iron treatment U:
and the unmodified zero-valent iron is used under the same conditions, and only about 4.9 percent of the iron is removed after 1 hour of reaction.
The results are shown in fig. 1, and it can be seen that the modified zero-valent iron aged by the method improves the reactivity of the zero-valent iron, and greatly accelerates the removal of U (VI); but the removal effect of the ordinary zero-valent iron which is not modified is poor.
Example 7
The U (VI) is treated by different modified zero-valent iron and the removal effect is detected, the treatment result is shown in figure 2, the effect of the modified zero-valent iron (1: 30) is optimal, the U (VI) can be removed within 60min, and the removal rate is over 99.9 percent.
0.5g of modified zero-valent iron (1: 30) is placed in 10mL of water for aging, the aging is carried out for 1d, 7d, 15d and 30d respectively, the aged modified zero-valent iron solution is added into the U (VI) wastewater respectively, and uranium removal is carried out according to the uranium removal method in the embodiment 5, the effect is shown in figure 4, as can be seen from the figure, the modified zero-valent iron removal effect is best within 1-15 days after aging, and uranium (VI) in the wastewater can be completely removed within 10 min.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. A method for rapidly removing uranium in water by aging modified zero-valent iron is characterized by comprising the following steps:
s1: modification: under the inert gas atmosphere, adding ferrous sulfate solid powder into stirred distilled water, then adding micron-sized zero-valent iron particles, dropwise adding a sodium sulfide solution in the stirring process, stirring and reacting for 1-3 h after dropwise adding is completed, carrying out vacuum filtration, and drying at low temperature to obtain modified zero-valent iron, wherein the molar ratio of ferrous sulfate to sodium sulfide to the micron-sized zero-valent iron particles is 1: 1: 9-50;
s2: aging: placing the modified zero-valent iron in a non-closed container filled with distilled water, standing and aging to obtain an aged modified zero-valent iron solution;
s3: removing uranium: adding the aged and modified zero-valent iron solution into uranium-containing wastewater to react and remove uranium; wherein the pH value of the uranium-containing wastewater is 3-8.
2. The method for rapidly removing uranium from water through aging modified zero-valent iron according to claim 1, wherein the particle size of the zero-valent iron particles in the step S1 is 10-200 microns.
3. The method for rapidly removing uranium in water by aging modified zero-valent iron according to claim 1, wherein the molar ratio of the ferrous sulfate, the sodium sulfide and the micron zero-valent iron particles is 1: 1: 30.
4. the method for rapidly removing uranium from water by aging modified zero-valent iron according to claim 1, wherein the molar ratio of Fe to S in the modified zero-valent iron in the step S1 is 30: 1.
5. The method for rapidly removing uranium from water by aging modified zero-valent iron according to claim 1, wherein the concentration of the aging modified zero-valent iron solution in the step S2 is 30 g/L-60 g/L.
6. The method for rapidly removing uranium from water by aging modified zero-valent iron according to claim 1, wherein the standing aging time in the step S2 is 1 d-15 d.
7. The method for rapidly removing uranium from water by aging modified zero-valent iron according to claim 1, wherein the pH of the uranium-containing wastewater in the step S3 is 6.
8. The method for rapidly removing uranium from water by aging modified zero-valent iron according to claim 7, wherein 0.1M MES buffer solution is added in the step S3 to maintain the pH of uranium-containing wastewater.
9. The method for rapidly removing uranium from water by aging modified zero-valent iron according to claim 1, wherein the addition amount of the aging modified zero-valent iron in the aging modified zero-valent iron solution in the step S3 is 0.4g to 1.5g per liter of uranium-containing wastewater.
10. The method for rapidly removing uranium in water by aging modified zero-valent iron according to claim 1, which is characterized by comprising the following steps:
s1: modification: under the inert gas atmosphere, adding ferrous sulfate solid powder into stirred distilled water, then adding zero-valent iron particles with the particle size of 50 microns, stirring at the speed of 150-200 r/min, dropwise adding a sodium sulfide solution, completing the dropwise adding within 30min, stirring for 2h after the completion, carrying out vacuum filtration, and drying at low temperature to obtain modified zero-valent iron, wherein the molar ratio of Fe to S in the modified zero-valent iron is 30: 1;
s2: aging: placing the modified zero-valent iron in a non-closed container filled with distilled water, standing and aging for 1d to obtain 50g/L aged modified zero-valent iron solution;
s3: removing uranium: adding the aged and modified zero-valent iron solution into uranium-containing wastewater with the pH value of 6, the temperature of 25 ℃ and the concentration of 50mg/L, and stirring at 400r/min to remove uranium; wherein the addition amount of the aging modified zero-valent iron is 1g per liter of uranium-containing wastewater.
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