CN112456597A - Method for removing hexavalent chromium in underground water by loading nano zero-valent iron on modified cellulose filter paper - Google Patents
Method for removing hexavalent chromium in underground water by loading nano zero-valent iron on modified cellulose filter paper Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229920002678 cellulose Polymers 0.000 title claims abstract description 42
- 239000001913 cellulose Substances 0.000 title claims abstract description 42
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 title claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 5
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 229920003043 Cellulose fiber Polymers 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 238000005067 remediation Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 230000001360 synchronised effect Effects 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 description 11
- 239000011651 chromium Substances 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000003895 groundwater pollution Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000008575 Iron Assay Methods 0.000 description 1
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A method for removing hexavalent chromium in underground water by loading nano zero-valent iron on modified cellulose filter paper. The nano zero-valent iron has high specific surface area and high reducibility, has excellent performance on solving the problem of water environment pollution remediation, but has the problems of high reaction activity, easy oxidation, easy agglomeration and the like. After the cellulose filter paper is modified by NaOH, cellulose fibers swell, so that the attachment area of the nano zero-valent iron is increased, the surface of the cellulose filter paper can be provided with hydroxyl, and the load capacity of the cellulose filter paper on the nano zero-valent iron is improved. The composite material has good reducing and adsorbing synchronous removing effects on hexavalent chromium in underground water. The method has the advantages of simple operation process, no need of nitrogen protection in the preparation process, relatively low requirement on equipment, low cost of used materials, environmental protection and reproducibility, and is a good method for removing hexavalent chromium in water.
Description
Technical Field
The invention belongs to the technical field of treatment of heavy metal pollutants in water, and particularly relates to a method for removing hexavalent chromium in underground water by adopting a modified cellulose filter paper loaded with a nano zero-valent iron material.
Background
Due to the rapid development of industry and urbanization, groundwater in most areas of China is polluted to different degrees. In the past decades, China has been dedicated to the prevention and treatment of groundwater pollution to achieve certain effect, but the situation of groundwater pollution is still severe. According to the current trend, the expert scholars predict that many cities in China will abandon underground water as drinking water source within 10 years.
The nanometer zero-valent iron (NZVI) can effectively restore pollutants such as halogenated hydrocarbon, chlorine-containing organic matters, heavy metals and the like by reduction, and is widely applied to the treatment of water body pollution. The chromium removal of NZVI is carried out by reducing Cr (VI) to Cr (III), hydrolyzing to Cr (OH)3The precipitate was separated from the water.
However, the NZVI particles have high surface energy and magnetism, and are easy to agglomerate when used alone, so that the defects of reduced reaction activity and the like are caused, and the application and development of the NZVI particles are greatly limited. Therefore, in order to make nano-iron practically usable for cr (vi) contamination remediation in water, it is necessary to modify the nano-particles to effectively inhibit agglomeration and increase removal efficiency.
Cellulose as the most abundant natural high molecular compound accounts for about 50% of global biomass, and annual output can reach 10%11Ton, a low cost renewable material with biodegradability, high strength and high thermal stability. The cellulose Filter Paper (FP) can be used as a cheap adsorbent and is also suitable to be used as a carrier of a pollution adsorbent. Modifying the cellulose filter paper by adopting a NaOH swelling method; the cellulose fiber can be swelled to increase the attachment area of the nano zero-valent iron, and the surface of the cellulose filter paper can be provided with hydroxyl, so that the load capacity of the cellulose filter paper on the nano zero-valent iron is improved, and the reduction and adsorption capacity of the cellulose filter paper on Cr (VI) is improved.
According to the invention, the mechanism of removing hexavalent chromium in water by the modified cellulose full-duty load nano zero-valent iron material has not only a chemical reduction effect, but also an adsorption effect, and compared with the single effect of the nano zero-valent iron material, the stability is higher, and the removal effect is better.
Disclosure of Invention
The invention aims to provide a preparation method of a supported nano zero-valent iron material, which is characterized in that NaOH is used for modifying cellulose filter paper, and the modified cellulose filter paper is used for supporting nano zero-valent iron, so that the stability and the dispersibility of the nano zero-valent iron are improved, and the material has an adsorption effect and a chemical reduction effect and can quickly and efficiently remove hexavalent chromium in water.
In order to realize the aim, the technical scheme adopted by the invention is a method for removing hexavalent chromium in underground water by loading nano zero-valent iron (FP-OH-NZVI) on modified cellulose filter paper, which comprises the following steps:
1. a preparation method of a modified cellulose filter paper loaded nano zero-valent iron composite material is characterized by comprising the following steps:
(1) 0.1mol/L NaOH solution is prepared, and the ashless cellulose filter paper is soaked in the solution, taken out after 30 to 60 minutes and washed by ultrapure water.
(2) Preparing 0.5mol/L ethanol solution of ferric chloride hexahydrate, completely soaking the product obtained in the step (1) in the solution for 40-60 minutes, and then air-drying to obtain yellow filter paper.
(3) Completely immersing the product obtained in (2) in 0.25mol/L NaBH4In solution for 45-60 minutes, black magnetic paper is produced.
(4) And (4) thoroughly cleaning the composite material obtained in the step (4) by using deionized water and absolute ethyl alcohol, and finally carrying out vacuum drying.
2. Further, ashless cellulose filter paper with the aperture of 8 mu m is adopted in the step (1).
3. Further, the composite material is placed in a freeze drying oven for vacuum drying for 10-15 h.
4. A method for removing hexavalent chromium in water by loading nano zero-valent iron on modified cellulose filter paper is characterized by comprising the following steps:
when the initial concentration of hexavalent chromium in the solution is 5-40mg/L, NaOH and HCl solution with the mass fraction of 1% is adopted for adjustment to keep the pH value between 3 and 5, a prepared composite material is added at 25 ℃, the reaction time is 120-240min, and the content of hexavalent chromium is measured after the reaction is finished.
The invention has the beneficial effects that:
(1) the modified cellulose filter paper loaded nano zero-valent iron material has good adsorption performance and chemical reduction effect, good stability and dispersibility, high removal efficiency of hexavalent chromium in water, and 97.5% removal rate when the iron loading amount of the cellulose filter paper is 11.45%.
(2) Compared with other methods for modifying the nano zero-valent iron, the preparation method does not need nitrogen protection, has relatively low requirements on equipment, and has relatively simple principle; the method has the biggest advantages of rapid reaction and rapid preparation, can generate iron powder in a short time, and the prepared sample is not obviously oxidized; and has the advantages of high removal efficiency and high removal speed.
Drawings
Fig. 1(a) is a scanning electron micrograph of the modified cellulose filter paper loaded with the nano zero-valent iron material.
FIG. 1(b) is a second scanning electron microscope image of the modified cellulose filter paper loaded with the nano zero-valent iron material.
FIG. 2 is a Fourier infrared spectrum of FP and FP-OH-NZVI.
FIG. 3(a) is a full scan of FP, FP-OH-NZVI and FP-OH-NZVI @ Cr; FIG. 3(b) is a narrow spectrum scan of FP-OH-NZVI with Fe2p
FIG. 4 shows the iron loading of the nano zero-valent iron material loaded on the Fe solution modified cellulose filter paper with different concentrations
FIG. 5 shows the hexavalent chromium removing effect of the Fe solution modified cellulose filter paper loaded with the nano zero-valent iron material with different concentrations
FIG. 6 shows the effect of the modified cellulose filter paper loaded with the nano zero-valent iron material on removing hexavalent chromium with different initial concentrations
FIG. 7 is a diagram showing the actual effect of removing hexavalent chromium by using a modified cellulose filter paper loaded with a nano zero-valent iron material
Detailed Description
Example one:
0.4g of NaOH was dissolved in 100ml of ultrapure water, and an ashless cellulose filter paper was immersed in the solution for 30 minutes and then taken out and washed with ultrapure water for use. 0.1, 0.2, 0.5, 0.8 and 1.0mol/L ferric chloride hexahydrate solution is prepared, specifically, 1.08g, 2.16g,5.4g,8.64g and 10.8g ferric chloride hexahydrate are dissolved in 40ml ethanol solvent, and the treated filter paper is immersed in the solution for 40 minutes and then dried in the air to obtain yellow filter paper. Then 0.25mol/L NaBH is taken4100ml of the solution, each of which will be coated with Fe3+Directly immersing the cellulose filter paper in NaBH4In solution for 45 minutes, a black magnetic paper (FP-OH-NZVI) was produced. And (3) thoroughly cleaning the composite material by using deionized water and absolute ethyl alcohol, and finally putting the composite material in a freeze drying box for vacuum drying for 10 hours.
The final product obtained in this way had the following characteristics:
referring to fig. 1, an SEM image of the modified cellulose filter paper loaded with the nano zero-valent iron material is observed, wherein the nano zero-valent iron has a particle size of 50 to 80nm, is loaded on the surface of the cellulose filter paper, and has good dispersibility.
Referring to FIG. 2, the composite material was analyzed by Fourier Infrared Spectroscopy, as shown at 3317cm-1、2893cm-1、1653cm-1And 1049cm-1Characteristic peaks of FP, which are assigned to-OH stretch, -CH, respectively, are observed2Stretching, H-O-H stretching and C-O, C-C stretching, and is consistent with the characteristic peaks of cellulose fibers. However, when NZVI was loaded into FP matrices, FP-OH-NZVI was 1653cm-1The peak at (a) disappeared. At 1743cm-1And 1691cm-1A new peak appears, which can be seen as an asymmetric stretching of the carboxyl groups. Some research reports indicate that the shape of the-COO-frequency and the stretch band change when carboxylic acids and their salts form complexes with metals. Thus, the FT-IR results indicate that NZVI has been successfully embedded in the FP. However, cellulose was in 1049cm-1The C-O and C-C bonds remain nearly unchanged, indicating that there is no substantial change in the ring structure of the cellulose filter paper.
Referring to FIG. 3(a), when XPS full spectrum scans of FP, FP-OH-NZVI and FP-OH-NZVI @ Cr are observed, about 286.08eV and 531.2eV appear in all 3 samplesDue to C1s and O1s, respectively, whereas the electron binding energies Fe2p at 711.08eV and 725.1eV are observed in the resolved scan when the filter paper is loaded with iron, which is the photoelectron energy measured when the 2p orbital electron of the iron atom is excited. To better explore the form of iron present in FP-OH-NZVI, XPS was used to scan the peak of iron photoelectrons in FIG. 3(b), which is Fe at a binding energy of 710.2eV and 723.8eV, respectively2+The corresponding 2p3/2 peak and 2p1/2 characteristic peak are Fe at 711.7eV and 723.3eV respectively3+The corresponding 2p3/2 peak and 2p1/2 characteristic peak are Fe at 707.0eV and 720.1eV of binding energy0The corresponding characteristic peak indicates Fe0Well fixed on the surface of the filter paper.
Preparing 60ml of a mixture with the proportion of 1: 2, respectively soaking the filter paper prepared by the 5 kinds of filter paper with different iron concentrations in the hydrochloric acid solution, placing the filter paper at a rotating speed of 120r/min, shaking for 1 hour, and taking out the filter paper to ensure that the iron powder in the filter paper completely falls off. The sample was taken in a 100ml quantitative flask, treated by the o-phenanthroline iron assay and the absorbance was measured. Finally, the iron loading on the filter paper was calculated separately, see fig. 4.
Preparing 200mL of solution with hexavalent chromium initial concentration of 15mg/L, adjusting the pH value to be 4, reacting for 210min, respectively adding the 5 cellulose filter paper composite materials with different iron concentrations, and slowly oscillating in a water bath at normal temperature under the condition of 130 r/min. The sample was taken out from a 50mL quantitative flask, treated with diphenylcarbodihydrazide spectrophotometry and the absorbance was measured. Finally, the hexavalent chromium removal effect is calculated, please refer to fig. 5.
Example two:
respectively preparing 200mL of hexavalent chromium solution with the initial concentration range of 5-40mg/L, adjusting the pH value to 4, reacting for 120min, respectively adding one FP-OH-NZVI composite material prepared from 0.5mol/L ferric chloride hexahydrate, wherein the iron carrying amount is about 65mg, and slowly oscillating in a water bath at the normal temperature of 130 r/min. The sample was taken out from a 50mL quantitative flask, treated with diphenylcarbodihydrazide spectrophotometry and the absorbance was measured. Finally, the hexavalent chromium removal rate is calculated, please refer to fig. 6. The hexavalent chromium removal effect actually exhibited in the experiment is shown in fig. 7.
Claims (4)
1. A preparation method of a modified cellulose filter paper loaded nano zero-valent iron composite material is characterized by comprising the following steps:
(1) preparing 0.1mol/L NaOH solution, soaking the ashless cellulose filter paper in the solution, taking out the solution after 30-60 minutes, and washing the solution with ultrapure water;
(2) preparing 0.5mol/L ferric chloride hexahydrate ethanol solution, completely soaking the product obtained in the step (1) in the solution for 40-60 minutes, and then air-drying to obtain yellow filter paper;
(3) completely immersing the product obtained in (2) in 0.25mol/L NaBH4Generating black magnetic paper in the solution for 45-60 minutes;
(4) and (4) thoroughly cleaning the composite material obtained in the step (4) by using deionized water and absolute ethyl alcohol, and finally carrying out vacuum drying.
2. The preparation method of the modified cellulose filter paper loaded nano zero-valent iron composite material according to claim 1, characterized in that, ashless cellulose filter paper with 8 μm pore diameter is adopted in the step (1).
3. The preparation method of the modified cellulose filter paper loaded nano zero-valent iron composite material according to claim 1, characterized in that the composite material is placed in a freeze drying oven for vacuum drying for 10-15 h.
4. A method for removing hexavalent chromium in water by loading nano zero-valent iron on modified cellulose filter paper is characterized by comprising the following steps:
when the initial concentration of hexavalent chromium in the solution is 5-40mg/L, NaOH and HCl solution with the mass fraction of 1% is adopted for adjustment to keep the pH value between 3 and 5, a prepared composite material is added at 25 ℃, the reaction time is 120-240min, and the content of hexavalent chromium is measured after the reaction is finished.
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| CN114259993A (en) * | 2021-12-02 | 2022-04-01 | 苏州中晟环境修复有限公司 | Process for repairing chromium-polluted underground water by adopting micro-nano composite particles |
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