CN115703058A - Iron-carbon nano composite and preparation method and application thereof - Google Patents
Iron-carbon nano composite and preparation method and application thereof Download PDFInfo
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- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 150000008282 halocarbons Chemical class 0.000 claims abstract description 17
- 150000001323 aldoses Chemical class 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000003763 carbonization Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000000376 reactant Substances 0.000 claims abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 229960002089 ferrous chloride Drugs 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 238000011109 contamination Methods 0.000 claims 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 abstract description 30
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 abstract description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 30
- 239000000463 material Substances 0.000 description 12
- 229910052742 iron Inorganic materials 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- 239000003344 environmental pollutant Substances 0.000 description 8
- 231100000719 pollutant Toxicity 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- -1 carboxyl activated carbon Chemical compound 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003673 groundwater Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000012612 commercial material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
The invention provides an iron-carbon nano composite and a preparation method and application thereof. The preparation method comprises the steps of dissolving ferrous salt and aldose with the molar ratio of 1-5 to 1-10 in an ethanol water solution to form a reactant solution, and carrying out hydrothermal reaction or microwave heating reaction and carbonization to obtain the iron-carbon nano composite. The invention also provides an iron-carbon nano composite obtained by the preparation method. The invention also provides application of the iron-carbon nano composite in treating halogenated hydrocarbon pollution. The iron-carbon nano composite provided by the invention has simple and convenient preparation process, the used raw materials are cheap and easy to obtain, and halogenated hydrocarbon organic pollutants such as carbon tetrachloride, trichloroethylene and the like in underground water can be effectively removed.
Description
Technical Field
The invention relates to the technical field of material synthesis, and relates to an iron-carbon nano composite, and a preparation method and application thereof.
Background
The pollutant components in petrochemical wastewater are complex, and the wastewater contains many refractory organic pollutants such as halogenated hydrocarbons (aliphatic hydrocarbons/aromatic hydrocarbons) besides oil, sulfur, phenol, cyanide and COD. Most halogenated hydrocarbons have higher density than water and lower surface tension and viscosity coefficient than water, and when groundwater is seriously polluted, they are concentrated at the bottom of aquifer, so that the halogenated hydrocarbons are also classified as non-aqueous heavy liquids. The treatment of halogenated hydrocarbons in ground water has attracted general attention and interest.
At present, a new field based on nano materials, such as carbon nano tubes, activated carbon, graphite-coated nano metal ions and the like, is developed in the carbon world on the basis of the traditional carbon material. However, carbon materials such as activated carbon only have the effect of concentration and enrichment in the pollutant treatment process, and the purpose of effectively removing or degrading pollutants cannot be achieved.
The nanometer zero-valent iron (nZVI) has high reaction activity, so that the method becomes a very active hot technology in the fields of material synthesis, environmental remediation, medicine and the like at present. However, the non-modified zero-valent iron particles have agglomeration property, which limits the wide application in various fields of the scientific field.
In order to improve the dispersibility and stability of the nano-iron particles and effectively remove pollutants, the methods of adding a dispersing agent, preparing coated nano-iron particles and the like are currently researched to improve the dispersibility and stability of the nano-iron particles so as to effectively remove the pollutants, but the two methods are complex and are not easy to implement. Therefore, a more green and convenient method for producing the iron-carbon composite material is needed to meet the requirements of repairing underground water halogenated hydrocarbons.
Disclosure of Invention
In order to solve the above problems, the present invention aims to provide an iron-carbon nanocomposite, and a preparation method and an application thereof. The iron-carbon nano-composite has a good treatment effect when being applied to degradation treatment of halogenated hydrocarbon organic pollutants.
In order to achieve the purpose, the invention provides a preparation method of an iron-carbon nano composite, which comprises the steps of dissolving ferrous salt and aldose with the molar ratio of 1-5.
In the preparation method, the carbon load material (aldose) is used for adsorbing ferrous ions to become a nucleation center of mineralized substances (iron nano particles), and then the carbon load material is crystallized and grown to obtain a precursor of the carbon load material/iron-containing mineral compound, and the precursor is carbonized at high temperature to obtain the carboxyl activated carbon/iron-containing nano material. The carboxyl activated carbon can be obtained by conversion of a carbon-supported material, and the carboxyl activated carbon not only has an adsorption effect on halogenated hydrocarbon pollutants, but also can enhance the dispersibility and stability of nanoparticles. Compared with a physical and chemical method for modifying the nano iron particles, the preparation method of the iron-carbon nano composite provided by the invention is more convenient and more environment-friendly.
In the above preparation method, preferably, the molar ratio of the ferrous salt to the aldose is 1-5.
In the above preparation method, preferably, the ferrous salt includes ferrous sulfate (FeSO) 4 ) And/or ferrous chloride (FeCl) 2 ). In particular embodiments, hydrates of ferrous salts, such as FeSO, may also be employed 4 ·7H 2 O, and the like.
In the above production method, aldose is selected as the carbon-supporting material, and the carbon-supporting material can be subjected to hydrothermal reaction and carbonization to produce a carboxyl-based activated carbon. Preferably, the aldose sugar comprises glucose.
In the above preparation method, preferably, in the reactant solution, the molar concentration of the ferrous salt is 0.1mol/L to 1mol/L, and the molar concentration of the aldose is 0.25mol/L to 1mol/L.
In the above production method, preferably, in the aqueous ethanol solution, the volume ratio of ethanol to water is 1.
In the above preparation method, preferably, the temperature of the hydrothermal reaction is 150 ℃ to 230 ℃ (e.g., 180 ℃ to 200 ℃), and the time of the hydrothermal reaction is 5h to 24h (e.g., 5h to 20h, 15 h).
In the preparation method, the reaction is carried out in a microwave heating mode, and compared with the traditional hydrothermal method, the preparation method has the advantages of simplicity, convenience, rapidness, high efficiency, greenness and the like. Preferably, the temperature of the microwave heating reaction is 280-350 ℃, the time of the microwave heating reaction is 0.5-1 h, and the microwave power can be controlled to be about 30 KW.
In the above production method, preferably, the temperature of the carbonization is 600 ℃ to 750 ℃ (e.g., 650 ℃ to 720 ℃), and the time of the carbonization is 5h to 10h (e.g., 6h to 8 h).
According to a specific embodiment of the present invention, in the above preparation method, before carbonization, the preparation method further comprises cooling, washing and drying the product of the hydrothermal reaction, and the product obtained after drying may be referred to as a precursor of the iron-carbon nanocomposite. Specifically, the drying temperature is generally controlled to be 40-50 ℃, the drying time is generally controlled to be 180-540 min, and the washing can comprise centrifugal washing by using ethanol.
The invention also provides an iron-carbon nano composite obtained by the preparation method. In a specific embodiment, the iron-carbon nanocomposite contains nano zero valent iron. In some embodiments, the nano zero valent iron can have a particle size of 20nm to 60nm.
According to a specific embodiment of the present invention, the iron-carbon nanocomposite can be used for removing halogenated hydrocarbons, for example, the iron-carbon nanocomposite can remove carbon tetrachloride with a carbon tetrachloride removal rate of 50%.
The invention also provides application of the iron-carbon nano composite in treating halogenated hydrocarbon pollution. In some embodiments, the mass ratio of the iron-carbon nanocomposite to the halogenated hydrocarbon can be from 25 to 100, for example 25. The removal rate of the iron-carbon nano composite to halogenated hydrocarbons such as carbon tetrachloride can reach more than 50%.
The invention has the beneficial effects that:
1. the invention adopts ethanol solution to synthesize the carboxyl-rich iron-carbon nano composite, has simple and convenient preparation process, cheap and easily obtained raw materials, no special requirements on external environmental conditions, small occupied space and no secondary pollution.
2. The iron-carbon nano composite provided by the invention has the adsorption effect of a carbon material and the strong reduction performance of nano zero-valent iron, can avoid the easy agglomeration phenomenon caused by high magnetism and van der Waals force among nano iron particles, and can effectively remove halogenated hydrocarbon organic pollutants such as carbon tetrachloride, trichloroethylene and the like in underground water.
Drawings
Fig. 1 is an SEM image of the iron-carbon nanocomposite of example 1.
Fig. 2 is an XRD pattern of the iron-carbon nanocomposite of example 1.
Fig. 3 is an infrared spectrum of the iron-carbon nanocomposite of example 1.
Fig. 4 shows the results of the carbon tetrachloride degradation experiment by commercial zero-valent iron powder (a picture) and commercial activated carbon material (b picture).
Fig. 5 shows the result of the carbon tetrachloride degradation experiment by the iron-carbon nanocomposite of example 1.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
1. Mixing 8.60gFeSO of (2) 4 ·7H 2 Dissolving O and 16.78g of glucose in a 100mL beaker of ethanol water (ethanol: water volume ratio of 1;
2. placing 80mL of reactant solution into a polytetrafluoroethylene sleeve with the volume of 100mL, and outputting microwave power by using a microwave heating device: 30KW, the sleeve is heated to 350 ℃ for 10min and kept for 1h. Then cooling the reaction product at room temperature, centrifugally washing the reaction product by using absolute ethyl alcohol, reserving the precipitate, and drying the reaction product in a vacuum drying oven at the temperature of 50 ℃ for 6 hours to obtain an iron-carbon composite precursor;
3. and (3) placing the iron-carbon composite precursor in a tubular furnace, introducing nitrogen into the tubular furnace, carbonizing at 680 ℃ for 6 hours, and cooling to room temperature to obtain the iron-carbon nano composite.
Fig. 1 is an SEM image of the product prepared in this example, and fig. 2 is an XRD image of the iron-carbon nanocomposite. The white circles in fig. 1 are zero-valent iron nanoparticles, and as can be seen from fig. 1, the nano-sized zero-valent iron in the product is attached to the carbon nano-material, no agglomeration occurs between the nanoparticles, the dispersibility is good, the nano-zero-valent iron is uniformly distributed on the surface of the porous nano-activated carbon, and the particle size of the iron nanoparticles is 20nm-60nm. As can be seen from fig. 2, the XRD results showed that the peaks at 44.5 °,65 °,85 ° in 2 θ were mainly characteristic peaks of zero-valent iron. This indicates that more zero valent iron is present in the composite nanomaterial.
The pH value of the aqueous solution (mass concentration of 8.6 wt%) of the iron-carbon nanocomposite of example 1 was measured, and it was found to be 6.1. Infrared spectroscopy of the iron-carbon nanocomposite was performed, and the results are shown in fig. 3, where table 1 shows peak positions associated with carboxyl groups. From FIG. 3 it can be seen that the material is 1690cm -1 The absorption peak in the vicinity is a carboxyl group stretching vibration peak (CH) 2 C = O in the form of a-CH-COOH di-associated complex, the absorption position of which is shifted to a low wave number due to the influence of hydrogen bonding), demonstrating that the material contains a carboxyl group.
TABLE 1
Test example 1
The test example provides a carbon tetrachloride degradation performance test using the iron-carbon nanocomposite prepared in example 1, commercial zero-valent iron powder (manufactured by shin-hong metallic material limited, the model of which is JR-Fe-T01), and commercial activated carbon (manufactured by changzhou zhiguan activated carbon limited, the model of which is 8-16 mesh coconut shell activated carbon) as samples to be tested. The test procedure was as follows:
1. 0.1g of sample to be tested is added into 100mL of carbon tetrachloride (16 mg/L) solution and placed in a shaking table (25 ℃ at 125 r/min) for degradation experiment, and at least 3 parallel controls are arranged on each group of sample to be tested. Sampling is carried out at intervals of 30min by taking carbon tetrachloride as a single pollutant for 5 times in total, the reaction time lasts for 150min, and the degradation effect of the iron-carbon nano composite is inspected by a gas chromatography.
Fig. 4 is a result of an experiment of degrading carbon tetrachloride with commercial zero-valent iron powder (a diagram) and a commercial activated carbon material (b diagram), fig. 5 is a result of an experiment of degrading carbon tetrachloride with the iron-carbon nanocomposite of example 1, and a peak area and a carbon tetrachloride removal rate are obtained by integrating the chromatographic results of fig. 4 and 5. Comparing fig. 4 and fig. 5, it can be seen that when the reaction time reaches 150min, the removal rate of carbon tetrachloride in the solution treated by the commercial zero-valent iron powder and the commercial activated carbon is only 12% and 30%. But the removal rate of the iron-carbon nano composite prepared by the method to carbon tetrachloride reaches 50 percent and is obviously higher than that of the two commercial materials. The iron-carbon nano composite provided by the invention has excellent pollutant adsorption and degradation effects and can be suitable for degradation operation of halogenated hydrocarbon.
Claims (12)
1. A preparation method of an iron-carbon nano composite comprises the steps of dissolving ferrous salt and aldose in a molar ratio of 1-5.
2. The preparation method according to claim 1, wherein the molar ratio of the ferrous salt to the aldose is 1-5.
3. The production method according to claim 1 or 2, wherein the ferrous salt includes ferrous sulfate and/or ferrous chloride.
4. The production method according to any one of claims 1 to 3, wherein the aldose includes glucose.
5. The production method according to any one of claims 1 to 4, wherein the molar concentration of the ferrous salt is 0.1 to 1mol/L and the molar concentration of the aldose is 0.25 to 1mol/L in the reactant solution.
6. The process according to claim 1, wherein in the aqueous ethanol solution, the volume ratio of ethanol to water is from 1.
7. The preparation method according to claim 1, wherein the temperature of the hydrothermal reaction is 150-230 ℃, and the time of the hydrothermal reaction is 5-24 h; the temperature of the microwave heating reaction is 280-350 ℃, and the time of the microwave heating reaction is 0.5-1 h;
preferably, the temperature of the hydrothermal reaction is 180-200 ℃, and the time of the hydrothermal reaction is 5-20 h, more preferably 15h.
8. The preparation method according to claim 1, wherein the temperature of the carbonization is 600 ℃ to 750 ℃, and the time of the carbonization is 5h to 10h;
preferably, the temperature of the carbonization is 650-720 ℃, and the time of the carbonization is 6-8 h.
9. The production method according to any one of claims 1 to 8, wherein the production method further comprises cooling, washing and drying the product of the hydrothermal reaction before carbonization;
preferably, the drying temperature is 40-50 ℃, the drying time is 180-540 min, and the washing comprises centrifugal washing by ethanol.
10. An iron-carbon nanocomposite obtained by the production method according to any one of claims 1 to 9.
11. The iron-carbon nanocomposite as claimed in claim 10, wherein the iron-carbon nanocomposite contains nano zero valent iron; preferably, the particle size of the nanometer zero-valent iron is 20nm-60nm.
12. Use of the iron-carbon nanocomposite of claim 10 or 11 for treating halocarbon contamination;
preferably, the mass ratio of the iron-carbon nano-composite to the halogenated hydrocarbon is 25-100, preferably 25.
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