CN109110901B - Method for efficiently removing heavy metal pollutants based on zero-valent iron fluoride - Google Patents
Method for efficiently removing heavy metal pollutants based on zero-valent iron fluoride Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000003344 environmental pollutant Substances 0.000 title claims abstract description 26
- 231100000719 pollutant Toxicity 0.000 title claims abstract description 26
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011737 fluorine Substances 0.000 claims abstract description 13
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 13
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006011 modification reaction Methods 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- 235000013024 sodium fluoride Nutrition 0.000 claims description 3
- 239000011775 sodium fluoride Substances 0.000 claims description 3
- ABDBNWQRPYOPDF-UHFFFAOYSA-N carbonofluoridic acid Chemical compound OC(F)=O ABDBNWQRPYOPDF-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- VPFNWSAQNWQCNX-UHFFFAOYSA-N CCCCCCCCCCCCC[Na] Chemical compound CCCCCCCCCCCCC[Na] VPFNWSAQNWQCNX-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 abstract description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 9
- 229910052804 chromium Inorganic materials 0.000 description 9
- 239000011651 chromium Substances 0.000 description 9
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000005067 remediation Methods 0.000 description 3
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- CACJZDMMUHMEBN-UHFFFAOYSA-M sodium;tridecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCS([O-])(=O)=O CACJZDMMUHMEBN-UHFFFAOYSA-M 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Images
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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- 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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- 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)
- Removal Of Specific Substances (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention relates to a method for efficiently removing heavy metal pollutants based on zero-valent iron fluoride. The zero-valent iron fluoride is characterized in that: part of the hydroxyl groups on the surface of the zero-valent iron are replaced by fluorine or fluorine-containing groups and sulfonic acid surfactant groups. The using method comprises the following steps: and adding the zero-valent iron fluoride into a heavy metal pollutant water body to remove heavy metals. The zero-valent iron fluoride provided by the invention has the advantages of good transmission capability, high electron selectivity, high utilization rate, higher pollutant removal efficiency, simple operation, economy and high efficiency when being used for removing heavy metal pollutants.
Description
Technical Field
The invention belongs to the field of environmental material preparation and pollutant remediation in water, and particularly relates to preparation of zero-valent iron fluoride and application of the zero-valent iron fluoride in pollutant removal.
Background
Compared with other chromium pollution remediation technologies, the zero-valent iron technology has the characteristics of low cost, environmental friendliness, simplicity in operation and the like, and is increasingly emphasized in the field of remediation of heavy metal chromium-polluted water bodies. After more than 20 years of basic research and application development, the zero-valent iron technology has excellent effect on treating heavy metal chromium ions in some practical water bodies, but the wide application of the zero-valent iron technology still has challenges. For example, micron-sized zero-valent iron has a problem of low activity, which is manifested by low electron transfer efficiency, poor electron selectivity, slow dissolution of ferrous ions, and the like. The reasons for this problem are: during the preparation, storage or use process of the zero-valent iron, a ferrite/hydroxide shell layer is generated on the surface of the zero-valent iron, and a typical core-shell structure is formed. Although the existence of the shell layer can prevent the continuous oxidation of the zero-valent iron, the contact of the zero-valent iron and the pollutants can be possibly hindered, the electron transfer and mass transfer processes of the system are influenced, and the pollutant removal efficiency of the zero-valent iron is further reduced; in addition, hydroxyl on the surface of the zero-valent iron is a hydrophilic group and is easy to combine with water molecules, so that the surface of the zero-valent iron is surrounded by the water molecules, and electrons generated by corrosion of the zero-valent iron are directly transferred to the water molecules instead of pollutants. In response to the above problems, researchers have developed various improvement strategies to improve the activity and electron selectivity of zero-valent iron. For example, researchers prepare nanoscale zero-valent iron to replace micron-sized zero-valent iron for removing pollutants, the shell layer of the nanoscale zero-valent iron is relatively thin, and the reduction capability and the reaction rate of the nanoscale zero-valent iron are found to be high, so that heavy metals can be efficiently removed; applying a weak magnetic field or pre-magnetizing the zero-valent iron in advance to generate a non-uniform induction magnetic field on the surface of the zero-valent iron, so that the thickening of a shell layer in the reaction process can be slowed down, the corrosion effect of the zero-valent iron is strengthened, more iron ions are generated, and the efficiency of removing heavy metal pollutants by the zero-valent iron is improved; the shell layer part on the surface of the zero-valent iron can be removed by the methods of acid washing, hydrogen pretreatment, ultrasonic treatment and the like, so that the zero-valent iron is directly exposed in the water body, and the pollutant removing efficiency of the zero-valent iron is further improved; the sulfuration modification method is adopted to prepare the sulfuration zero-valent iron, and the pollutant removal capability and the electron selectivity of the zero-valent iron can be obviously improved. However, the above zero-valent iron improvement techniques involve complicated operations, require additional equipment, or fail to improve the electron selectivity of zero-valent iron.
Disclosure of Invention
The invention aims to provide the fluorinated zero-valent iron with simple operation and low cost, and the preparation method and the application thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
provided is a fluorinated zero-valent iron, wherein a part of hydroxyl groups on the surface of the zero-valent iron are replaced by fluorine or fluorine-containing groups, and sulfonic acid surfactant groups.
Provides a preparation method of novel zero-valent iron fluoride, which mainly comprises the following steps: firstly, preparing a fluorine-containing substance solution, then mixing a sulfonic acid surfactant solution with a certain concentration, and adding zero-valent iron to perform a modification reaction to obtain the zero-valent iron fluoride material.
According to the scheme, the concentration of the fluorine source substance solution is 0.001-1M, the concentration of the stable transmission agent solution is 0.0001-0.001M, and the dosage of the zero-valent iron is 0.56-5.6 g/L.
According to the scheme, the modification reaction time is 0.5-2.5h, and the modification reaction temperature is 20-27 ℃. According to the scheme, after the modification reaction, the post-treatment is carried out: washing with deionized water and ethanol for several times, and vacuum drying.
According to the scheme, the fluoride comprises perfluorocarboxylic acid, hydrofluoric acid, sodium fluoride and the like.
According to the scheme, the sulfonic acid surfactant comprises sodium tridecyl sulfonate, sodium dodecyl benzene sulfonate, sodium petroleum sulfonate and the like.
The method for efficiently removing the heavy metal pollutants based on the zero-valent iron fluoride is characterized in that the zero-valent iron fluoride is added into a heavy metal pollutant water body to remove the heavy metals.
According to the scheme, when the heavy metal is removed, the pollutants are stirred or not stirred.
According to the scheme, the adding amount of the zero-valent iron fluoride is 0.5-3 g/L.
The invention has the beneficial effects that:
the fluorine-containing group of the fluorinated zero-valent iron obtained by the invention partially replaces hydroxyl on the surface of the zero-valent iron, so that the electronic selectivity of the material for removing pollutants is weakened, and the electronic selectivity is greatly improved, meanwhile, the hydrophobic property of the material can be enhanced by matching with the addition of part of sulfonic acid surfactant groups as a stable transmission agent, the charge distribution on the surface of the zero-valent iron is changed, and the stability and the transmission capability of the modified fluorinated zero-valent iron, namely the migration capability in a water body, are remarkably improved, as shown in figure 1. As can be seen from the attached figure 2, the corrosion potential of the modified material is more negative, which shows that the material is easier to corrode, can release electrons more quickly, is high in selectivity of removing electrons for heavy metal pollutants, high in utilization rate, can remove heavy metal ions more economically and efficiently, does not need to control the dissolved oxygen of a system, and has the heavy metal removal rate of more than 99%.
The whole modification process of the obtained zero-valent iron fluoride is simple to operate and has low requirements on instruments and equipment.
Drawings
FIG. 1 is a graph showing the contact angle results of original zero-valent iron (A) and zero-valent iron (B) after modification in example 3;
FIG. 2 is a Tafel plot of zero-valent iron before and after modification in example 3, wherein: a, original zero-valent iron, and b, the modified zero-valent iron in the embodiment;
FIG. 3 is a graph showing the chromium removal effect of virgin zero-valent iron and modified zero-valent iron of example 1, example 2 and example 3.
Detailed Description
Example 1, first 50mL of 0.01M sodium fluoride solution was prepared and added to a 100mL beaker, 0.005M sodium petroleum sulfonate solution was added and 0.56g of zero-valent iron was added. Reacting for 60min at 25 ℃, washing for 3 times by using deionized water and ethanol respectively, filtering a sample, and drying for 18h at 25 ℃ in a vacuum drying oven; under the aerobic condition, the rotating speed is 200 r/min, the initial concentration of hexavalent chromium is 2mg/L, the adding amount of the zero-valent iron fluoride is 2g/L, after 90min of reaction, the removal rate of chromium reaches 99%, the electron selectivity of the original zero-valent iron is about 2.3%, the electron selectivity after modification reaches 23%, and the removal rate of chromium after 5 times of circulation still reaches 95%.
Example 2, first, 50mL of 1M hydrofluoric acid solution was prepared and added to a 100mL beaker, 0.001M sodium dodecylbenzenesulfonate solution was added, and 3g of zero-valent iron was added. Reacting for 90min at 25 ℃, then washing for 3 times by using deionized water and ethanol respectively, and filtering and drying a sample for 12h at 25 ℃ in a vacuum drying oven; under the aerobic condition, the rotating speed is 200 r/min, the initial concentration of hexavalent chromium is 10mg/L, the adding amount of the zero-valent iron fluoride is 2g/L, the removal rate of chromium reaches 99 percent after reaction for 30min, the electron selectivity of the original zero-valent iron is about 2.3 percent, the electron selectivity after modification reaches 25 percent, and the removal rate of chromium after 5 times of circulation still reaches 93 percent.
Example 3A 0.05M trifluoroacetic acid solution (50 mL) was prepared in a 100mL beaker, and a 0.0001M sodium tridecylsulfonate solution was added thereto, followed by addition of 5.6g of zero-valent iron. Reacting at 25 ℃ for 120min, washing with deionized water and ethanol for 3 times respectively, filtering the sample, and drying in a vacuum drying oven at 25 ℃ for 16 h; under the aerobic condition, the rotating speed is 200 r/min, the initial concentration of hexavalent chromium is 5mg/L, the adding amount of the zero-valent iron fluoride is 2g/L, the removal rate of chromium reaches 99 percent after the reaction is carried out for 30min, the electron selectivity of the original zero-valent iron is about 2.3 percent, the electron selectivity after the modification is as high as 32 percent, and the removal rate of chromium after 5 times of circulation is still as high as 96 percent.
The zero-valent iron of examples 1-3 above was micron-sized zero-valent iron.
The contact angle results of the original zero-valent iron and the modified zero-valent iron (B) are shown in a graph of FIG. 1; the Tafel plot of zero-valent iron before and after modification is shown in FIG. 2; the chromium removal effect of the original zero-valent iron and the modified zero-valent iron of example 1, example 2 and example 3 is shown in fig. 3.
The results show that: the fluorine-containing group of the fluorinated zero-valent iron obtained by the invention partially replaces hydroxyl on the surface of the zero-valent iron, so that the hydrophilic performance of the material is weakened, and meanwhile, the addition of the matched sulfonic acid surfactant not only obviously improves the stability and the transmission capability of the zero-valent iron, but also enhances the hydrophobic performance of the material, as shown in figure 1; as can be seen from the attached figure 2, the corrosion potential of the modified material is more negative, which indicates that the material is easier to corrode and can release electrons more quickly; the electronic selectivity of the modified zero-valent iron fluoride material for removing pollutants (the proportion of the number of electrons used for removing pollutants in the total number of electrons released in the zero-valent iron corrosion process is determined by the valence state change and mass conservation of iron and pollutants) is greatly improved (the electronic selectivity of original zero-valent iron is about 2.3%, the electronic selectivity of the modified zero-valent iron fluoride in embodiment 3 of the invention is about 32%, and the capacity of removing heavy metals is greatly improved, as shown in fig. 3.
Claims (9)
1. A zero-valent iron fluoride, characterized by: part of hydroxyl groups on the surface of the micron-sized zero-valent iron are replaced by fluorine or fluorine-containing groups and sulfonic acid surfactant groups.
2. The method for producing zero-valent iron fluoride according to claim 1, wherein: the method mainly comprises the following steps: firstly, preparing a fluorine source substance solution, then mixing a sulfonic acid surfactant solution with a certain concentration, and adding micron-sized zero-valent iron for modification reaction to obtain a zero-valent iron fluoride material, wherein the concentration of the fluorine source substance solution is 0.001-1M, the concentration of the sulfonic acid surfactant solution is 0.0001-0.001M, and the using amount of the zero-valent iron is 0.56-5.6 g/L.
3. The method of claim 2, wherein: the modification reaction time is 0.5-2.5h, and the modification reaction temperature is 20-27 ℃.
4. The method of claim 2, wherein: carrying out post-treatment after the modification reaction: washing with deionized water and ethanol for several times, and vacuum drying.
5. The method of claim 2, wherein: the fluorine source substance is selected from one or more of perfluorocarboxylic acid, hydrofluoric acid and sodium fluoride.
6. The method of claim 2, wherein: the sulfonic acid surfactant is one or more of tridecyl sodium sulfonate, sodium dodecyl benzene sulfonate and petroleum sodium sulfonate.
7. The method for efficiently removing heavy metal pollutants based on the zero-valent iron fluoride according to claim 1, which is characterized in that: the method comprises the step of adding the zero-valent iron fluoride according to claim 1 into a heavy metal pollutant water body to remove heavy metals.
8. The method of claim 7, wherein: when the heavy metal is removed, the pollutants are stirred or not stirred.
9. The method of claim 7, wherein: the addition amount of the zero-valent iron fluoride is 0.5-3 g/L.
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| CN110713242B (en) * | 2019-08-09 | 2020-12-01 | 中国科学院地理科学与资源研究所 | Zero-valent iron material Fe @ iron fluoride and preparation method thereof |
| CN112139508A (en) * | 2020-09-23 | 2020-12-29 | 中国科学院地理科学与资源研究所 | Amphoteric surface micron zero-valent iron, and preparation method and application thereof |
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| CN104310726A (en) * | 2014-09-30 | 2015-01-28 | 湖南大学 | Method for removing heavy metal chromium in bottom mud by using modified nano zero-valent iron |
| CN108002518A (en) * | 2017-12-16 | 2018-05-08 | 傲自然成都生物科技有限公司 | A kind of bioelectrochemical system and purification method for purifying drinking water nitrate |
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| CN104310726A (en) * | 2014-09-30 | 2015-01-28 | 湖南大学 | Method for removing heavy metal chromium in bottom mud by using modified nano zero-valent iron |
| CN108002518A (en) * | 2017-12-16 | 2018-05-08 | 傲自然成都生物科技有限公司 | A kind of bioelectrochemical system and purification method for purifying drinking water nitrate |
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Application publication date: 20190101 Assignee: Wuhan Nanwang Environmental Protection Technology Research Co.,Ltd. Assignor: CENTRAL CHINA NORMAL University Contract record no.: X2023980053268 Denomination of invention: A method for efficient removal of heavy metal pollutants based on zero valent iron fluoride Granted publication date: 20210720 License type: Common License Record date: 20231220 |
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