CN115159598B - Preparation method and application of sodium oxalate doped modified nano zero-valent iron - Google Patents
Preparation method and application of sodium oxalate doped modified nano zero-valent iron Download PDFInfo
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- CN115159598B CN115159598B CN202210892801.8A CN202210892801A CN115159598B CN 115159598 B CN115159598 B CN 115159598B CN 202210892801 A CN202210892801 A CN 202210892801A CN 115159598 B CN115159598 B CN 115159598B
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- sodium oxalate
- valent iron
- nano zero
- modified nano
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 65
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 title claims abstract description 46
- 229940039790 sodium oxalate Drugs 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- 239000008239 natural water Substances 0.000 claims description 6
- 238000003911 water pollution Methods 0.000 claims description 6
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005067 remediation Methods 0.000 claims 1
- 230000009257 reactivity Effects 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 235000006408 oxalic acid Nutrition 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a preparation method of sodium oxalate doped modified nano zero-valent iron, which belongs to the technical field of nano material preparation and water purification environment, and comprises the following steps: s1: preparation of FeSO 4 A solution; s2: preparing sodium oxalate solution; s3: preparation of NaBH 4 A solution; s4: preparation of NaBH 4 Sodium oxalate mixed solution; s5: under the condition of nitrogen protection and no oxygen, naBH is added 4 Dropwise adding sodium oxalate mixed solution into FeSO 4 Fully stirring and reacting for 20min in the solution; s6: separating a black precipitate; s7: washing; s8: vacuum drying to obtain modified nanometer zero-valent iron; the invention also discloses application of the sodium oxalate doped modified nano zero-valent iron; compared with nano zero-valent iron, the sodium oxalate doped modified nano zero-valent iron has better reactivity and recycling property, and the treatment efficiency of Cr (VI) in the water phase is obviously improved.
Description
Technical Field
The invention belongs to the technical field of nano material preparation and water purification environment, and particularly relates to a preparation method and application of sodium oxalate doped modified nano zero-valent iron.
Background
The nano zero-valent iron has the advantages of high activity, large specific surface area, easy preparation, magnetism, convenient recycling and the like, and has rapid development in the field of natural water pollution restoration of groundwater and the like in recent years.
However, the nano particles have larger specific surface area and higher surface energy, so that nano zero-valent iron is easy to oxidize in air to form a surface oxide film, and the material is seriously passivated, so that the repairing effect in natural water pollution is affected.
In view of the above, a sodium oxalate doped modified nano zero-valent iron is designed to improve the reactivity and the reusability of the nano zero-valent iron so as to achieve the purpose of remarkably improving the restoration efficiency in natural water pollution and solve the problems.
Disclosure of Invention
To solve the problems set forth in the background art. The invention provides a preparation method and application of sodium oxalate doped modified nano zero-valent iron, which have the characteristics of better reactivity and reusability and remarkably improve the treatment efficiency of Cr (VI) in a water phase.
The invention further aims to provide an application of the sodium oxalate doped modified nano zero-valent iron.
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method of the sodium oxalate doped modified nano zero-valent iron comprises the following steps:
s1: weighing FeSO 4 ·7H 2 O is dissolved in oxygen-free water to prepare FeSO 4 A solution;
s2: weighing sodium oxalate and dissolving in oxygen-free water to prepare sodium oxalate solution;
s3: weighing NaBH 4 Dissolving in oxygen-free water to obtain NaBH 4 A solution;
s4: naBH is carried out 4 Mixing the solution with sodium oxalate solution, stirring thoroughly for 20min to obtain NaBH 4 Sodium oxalate mixed solution;
s5: feSO is carried out 4 The solution is placed in a three-neck flask with mechanical stirring, and NaBH is added under the condition of nitrogen protection and no oxygen 4 Dropwise adding sodium oxalate mixed solution into FeSO 4 Fully stirring and reacting for 20min in the solution;
s6: using a magnet to separate black precipitate in the three-neck flask;
s7: washing the black precipitate by using oxygen-free water and absolute ethyl alcohol;
s8: and (3) immediately placing the washed black precipitate into a vacuum drying oven for drying to obtain the modified nano zero-valent iron.
Preferably, in the step S1, feSO 4 ·7H 2 The mass volume ratio of O to the anaerobic water is 1.2:30 (g: mL).
Preferably, in the step S3, naBH 4 The mass volume ratio of the water to the anaerobic water is 0.38:20 (g: mL).
Preferably, in the step S4 and the step S5, the stirring speed is 200-300r/min.
Preferably, in the step S7, the number of times of washing is three.
Preferably, in the step S8, the drying temperature of the vacuum drying oven is 60 ℃ and the drying time is 12 hours.
The modified nano zero-valent iron prepared by the preparation method of sodium oxalate doped modified nano zero-valent iron.
An application of the modified nano zero-valent iron in natural water pollution restoration.
Compared with the prior art, the invention has the beneficial effects that:
compared with nano zero-valent iron, the sodium oxalate doped modified nano zero-valent iron has better reactivity and recycling property, and the treatment efficiency of Cr (VI) in the water phase is obviously improved.
Drawings
FIG. 1 is a flow chart of a method for preparing sodium oxalate doped modified nano zero-valent iron;
FIG. 2 is an X-ray diffraction pattern of modified nano zero-valent iron of the present invention and comparative examples with different oxalic acid doping ratios;
FIG. 3 shows the Cr (VI) removal effect of modified nano zero-valent iron with different oxalic acid doping ratios;
FIG. 4 is a graph showing the change of the second order kinetic constants of modified nano zero-valent iron with different oxalic acid doping ratios for Cr (VI) removal;
FIG. 5 is a graph showing the effect of the modified nano zero-valent iron material of the present invention in the Cr (VI) removal process.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1-5, the present invention provides the following technical solutions: the preparation method of the sodium oxalate doped modified nano zero-valent iron comprises the following steps:
s1: 1.2g of FeSO is weighed out 4 ·7H 2 O is dissolved in 30mL of anaerobic water to prepare FeSO 4 A solution;
s2: weighing 0.02g of sodium oxalate and dissolving in 30mL of oxygen-free water to prepare sodium oxalate solution;
s3: 0.38g of NaBH was weighed 4 Dissolving in 20mL of oxygen-free water to obtain NaBH 4 A solution;
s4: naBH is carried out 4 Mixing the solution with sodium oxalate solution, stirring at 200-300r/min for 20min to obtain NaBH 4 Sodium oxalate mixed solution;
s5: feSO is carried out 4 The solution is placed in a three-neck flask with mechanical stirring, and NaBH is added under the condition of nitrogen protection and no oxygen 4 Dropwise adding sodium oxalate mixed solution into FeSO 4 Fully stirring the solution at a stirring speed of 200-300r/min for reacting for 20min;
s6: using a magnet to separate black precipitate in the three-neck flask;
s7: washing the black precipitate three times by using oxygen-free water and absolute ethyl alcohol;
s8: and (3) immediately placing the washed black precipitate into a vacuum drying oven, and drying the black precipitate for 12 hours at a drying temperature of 60 ℃ in the vacuum drying oven to obtain the modified nano zero-valent iron.
The modified nano zero-valent iron prepared by the preparation method of sodium oxalate doped modified nano zero-valent iron.
An application of modified nano zero-valent iron in natural water pollution restoration.
C in modified nano zero-valent iron prepared in this example 2 O 4 2- And FeSO 4 The molar ratio of (2) is 1:29, so the modified nano zero-valent iron is marked as nFe oxa (1/29)。
Example 2
The difference between this embodiment and embodiment 1 is that:
0.01g of sodium oxalate was weighed and dissolved in 30mL of oxygen-free water to prepare a sodium oxalate solution.
C in modified nano zero-valent iron prepared in this example 2 O 4 2- And FeSO 4 The molar ratio of (2) is 1:58, so the modified nano zero-valent iron is marked as nFe oxa (1/58)。
Example 3
The difference between this embodiment and embodiment 1 is that:
0.03g of sodium oxalate was weighed and dissolved in 30mL of oxygen-free water to prepare a sodium oxalate solution.
C in modified nano zero-valent iron prepared in this example 2 O 4 2- And FeSO 4 The molar ratio of (2) is 1:19, so the modified nano zero-valent iron is marked as nFe oxa (1/19)。
Example 4
The difference between this embodiment and embodiment 1 is that:
0.04g of sodium oxalate was weighed and dissolved in 30mL of oxygen-free water to prepare a sodium oxalate solution.
C in modified nano zero-valent iron prepared in this example 2 O 4 2- And FeSO 4 The molar ratio of (2) is 1:14, so the modified nano zero-valent iron is marked as nFe oxa (1/14)。
Comparative example
SA: 1.2g of FeSO is weighed out 4 ·7H 2 O is dissolved in 30mL of anaerobic water to prepare FeSO 4 A solution;
SB: 0.38g of NaBH was weighed 4 Dissolving in 20mL of oxygen-free water to obtain NaBH 4 A solution;
SC: feSO is carried out 4 The solution is placed in a three-neck flask with mechanical stirring, and NaBH is added under the condition of nitrogen protection and no oxygen 4 Drop-wise addition of solution to FeSO 4 Fully reacting in the solution for 20min at a stirring speed of 200-300r/min to obtain nano zero-valent iron, which is marked as nFe 0 。
The XRD spectra of the modified nano zero-valent iron material and the comparative example are shown in figure 2 of the specification, the mineral components and crystallinity of the modified nano zero-valent iron material and the comparative example can be compared, the modified nano zero-valent iron material and the comparative example both have obvious diffraction peaks of zero-valent iron at 44.6 degrees, and Fe can be seen in the XRD spectra of the comparative example 3 O 4 Weak characteristic diffraction peaks, indicating a thinner layer of Fe on the surface of the comparative example 3 O 4 The oxide layer, but no corresponding magnetite diffraction peak appears in the modified nano zero-valent iron material, which indicates that the doping of oxalic acid can erode the oxide layer on the surface of the comparative example, thereby delaying the passivation process.
Reactive comparative experiments:
1g/L of the examples 1, 2, 3, 4 and comparative examples were added to Cr (VI) having a concentration of 10mg/L at a reaction temperature of 10.+ -. 2 ℃ to adjust the pH of the solution to 6, and the reaction was carried out under aerobic conditions;
as shown in fig. 3 of the specification, it can be seen that the reaction activity of the prepared example 1 is highest when the molar ratio of oxalic acid to Fe is 1/29, cr (VI) is completely removed within 20min, 68.5% is removed within 20min in the comparative example under the same conditions, the removal efficiency of Cr (VI) by the reaction 1h is only 88.7%, so that the removal efficiency of Cr (VI) by the modified nano zero-valent iron material doped and modified by oxalic acid is generally higher than that of the unmodified comparative example, and the doping amount of oxalic acid has a significant effect on the modified nano zero-valent iron;
further carrying out secondary dynamics fitting on the data of the attached drawing 3 in the specification, and the fitting result is shown in the attached drawing 4 in the specification, it can be seen that the doping amount of oxalic acid is not linearly related to the reactivity of the modified nano zero-valent iron, but the removal rate of Cr (VI) is in a process of increasing and then decreasing and keeping stable along with the increase of the doping amount of oxalic acid.
Repeated usability experiment:
the magnetic recovery of the adsorption-balanced modified nano zero-valent iron material is repeated for 5 times for Cr (VI) removal, and the experimental result is shown in the attached figure 5 of the specification, and it can be seen that the removal efficiency of the modified nano zero-valent iron for Cr (VI) in 1h gradually decreases with the continuous increase of the repeated use times, the removal effect of the modified nano zero-valent iron after the repeated use for 5 times is reduced by nearly 50% compared with that of the newly prepared material, and FeS modified nFe reported in the prior art 0 After three cycles, the Cr (VI) removal rate of the material is reduced to 33.4 percent, and nFe alone 0 The removal efficiency of Cr (VI) after three repeated use is 19.8%, and the result shows that the modified nano zero-valent iron has better recycling property in the aspect of Cr (VI) removal.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The preparation method of the sodium oxalate doped modified nano zero-valent iron is characterized by comprising the following steps of:
s1: weighing FeSO 4 ·7H 2 O is dissolved in oxygen-free water to prepare FeSO 4 A solution;
s2: weighing sodium oxalate and dissolving in oxygen-free water to prepare sodium oxalate solution;
s3: weighing NaBH 4 Dissolving in oxygen-free water to obtain NaBH 4 A solution;
s4: naBH is carried out 4 Mixing the solution with sodium oxalate solution, stirring thoroughly for 20min to obtain NaBH 4 Sodium oxalate mixed solution;
s5: feSO is carried out 4 The solution is placed in a three-neck flask with mechanical stirring, and NaBH is added under the condition of nitrogen protection and no oxygen 4 Dropwise adding sodium oxalate mixed solution into FeSO 4 Fully stirring and reacting for 20min in the solution;
s6: using a magnet to separate black precipitate in the three-neck flask;
s7: washing the black precipitate by using oxygen-free water and absolute ethyl alcohol;
s8: and (3) immediately placing the washed black precipitate into a vacuum drying oven for drying to obtain the modified nano zero-valent iron.
2. The method for preparing sodium oxalate doped modified nano zero-valent iron according to claim 1, which is characterized in that: in the step S1, feSO 4 ·7H 2 The mass volume ratio of O to the anaerobic water is 1.2:30 (g: mL).
3. The method for preparing sodium oxalate doped modified nano zero-valent iron according to claim 1, which is characterized in that: in the step S3, naBH 4 The mass volume ratio of the water to the anaerobic water is 0.38:20 (g: mL).
4. The method for preparing sodium oxalate doped modified nano zero-valent iron according to claim 1, which is characterized in that: in the step S4 and the step S5, the stirring speed is 200-300r/min.
5. The method for preparing sodium oxalate doped modified nano zero-valent iron according to claim 1, which is characterized in that: in the step S7, the number of times of washing is three.
6. The method for preparing sodium oxalate doped modified nano zero-valent iron according to claim 1, which is characterized in that: in the step S8, the drying temperature of the vacuum drying oven is 60 ℃ and the drying time is 12 hours.
7. A modified nano zero-valent iron prepared by the method for preparing the sodium oxalate doped modified nano zero-valent iron according to any one of claims 1 to 6.
8. Use of the modified nano zero-valent iron of claim 7 in natural water pollution remediation.
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