CN114192080A - Nano iron-based particles and preparation method and application thereof - Google Patents
Nano iron-based particles and preparation method and application thereof Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 51
- 239000002245 particle Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000012153 distilled water Substances 0.000 claims abstract description 21
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- PGWMQVQLSMAHHO-UHFFFAOYSA-N sulfanylidenesilver Chemical compound [Ag]=S PGWMQVQLSMAHHO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 239000007795 chemical reaction product Substances 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 230000001590 oxidative effect Effects 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000010865 sewage Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 229960002089 ferrous chloride Drugs 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical group Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 claims description 3
- 235000019252 potassium sulphite Nutrition 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 57
- 230000004048 modification Effects 0.000 abstract description 7
- 238000012986 modification Methods 0.000 abstract description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052709 silver Inorganic materials 0.000 abstract description 6
- 239000004332 silver Substances 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000009257 reactivity Effects 0.000 abstract description 4
- 229910052717 sulfur Inorganic materials 0.000 abstract description 4
- 239000011593 sulfur Substances 0.000 abstract description 4
- 239000012670 alkaline solution Substances 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- -1 iron ions Chemical class 0.000 abstract 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract 1
- 229910001448 ferrous ion Inorganic materials 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 239000013043 chemical agent Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 208000032420 Latent Infection Diseases 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000002155 anti-virotic effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 208000037771 disease arising from reactivation of latent virus Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
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- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/003—Wastewater from hospitals, laboratories and the like, heavily contaminated by pathogenic microorganisms
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
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Abstract
The invention belongs to the technical field of functional nano materials, and particularly relates to a nano iron-based particle and a preparation method and application thereof, wherein the preparation method comprises the following steps: fe preparation by utilizing ferrous ions, citric acid, ethanol and oxygen-free distilled water2+A hydroalcoholic solution of the complex; then adding low-sulfite alkaline solution into the above hydroalcoholic solution to reduce iron ions toForming iron sulfide on the surface of the nanoscale zero-valent iron to finish the preparation of the sulfur-modified nano iron-based particles; and then adding a silver ion solution, reducing silver ions into zero-valent silver by zero-valent iron, combining the silver ions with the surface of the nano iron-based particles, and filtering, washing and drying in vacuum to obtain the silver-sulfur modified nano iron-based particles. The invention adopts low-sulfite alkaline solution as a reducing agent and Fe2+The complex is a precursor, synchronously completes the generation of the nano zero-valent iron substrate and the modification of the sulfur on the surface of the nano zero-valent iron substrate, reduces the production cost, reduces the environmental hazard, and improves the reactivity and the killing capacity.
Description
Technical Field
The invention belongs to the technical field of functional nano materials, and particularly relates to a nano iron-based particle and a preparation method and application thereof.
Background
The medical sewage is mainly sewage discharged from diagnosis and treatment rooms, laboratory rooms, ward rooms, laundry rooms, X-ray photography rooms, operating rooms and the like of hospitals, contains a large amount of pathogenic bacteria, viruses and chemical agents, has very complex sources and components, and has the characteristics of space pollution, acute infection and latent infection. The traditional treatment methods such as a membrane treatment method, a chlorine disinfection method, an ultraviolet ray method and an ozone method have high requirements on equipment, have poor long-term sterilization effect, cannot synchronously complete disinfection and drug degradation, and can be accompanied with the problems of toxic byproducts and safety.
The nano iron-based particles are a novel material for environmental remediation, have the characteristics of small volume, strong removal capacity, high reactivity and the like, and can further improve the reactivity of the nano particles after certain surface modification is carried out on the nano iron-based particles. The strong reducibility of the zero-valent iron substrate and strong oxidizing free radicals generated in water can synchronously remove pathogenic microorganisms and chemical agents difficult to degrade, the modification of sulfur can improve the degradation capability and the degradation range of organic matters, and the modification of silver can enable the iron-based particles to have stronger antivirus capability. In the prior art, many ways of preparing nano iron-based particles have been reported, but most methods are accompanied by expensive equipment and harsh production environments. The liquid phase reduction method for preparing the nano iron-based particles has the characteristics of low cost, small investment, large output and the like, but the method usually relates to an expensive and toxic reducing agent sodium borohydride, so that the method is not applied in a large quantity.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a nano iron-based particle and a preparation method and application thereof.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a method for preparing nano iron-based particles comprises the following steps:
1) preparing an oxidizing solution: measuring a certain amount of anaerobic distilled water and absolute ethyl alcohol, and uniformly mixing to obtain a water-alcohol solution; weighing a certain mass of iron source, dissolving the iron source in a hydroalcoholic solution, adding a certain mass of citric acid under the stirring condition, and generating Fe in the hydroalcoholic solution2+To obtain an oxidation solution;
2) preparation of reducing liquid: weighing a certain amount of sodium hydroxide, dissolving the sodium hydroxide in distilled water, releasing a large amount of heat at the moment, adding a certain amount of low sulfite into the distilled water, and controlling the water temperature to be 50-70 ℃ to prepare reducing liquid;
3) preparing the nano iron-based particles: heating the oxidizing solution prepared in the step 1) to the same temperature as the reducing solution prepared in the step 2), adding the reducing solution into the oxidizing solution under the condition of stirring, reacting for 20-40 min, and gradually turning the solution into grey black, so that sulfur-modified nano iron-based particles are generated; after the reaction is finished, stopping heating, keeping stirring, slowly adding the silver nitrate solution into the reaction system, and stopping stirring after continuously stirring for a period of time; and filtering the cooled reaction product under the protection of nitrogen, repeatedly washing the reaction product by using oxygen-free distilled water until the pH value is neutral, and drying the reaction product in vacuum to obtain the silver-sulfur modified nano iron-based particles.
Further, in the preparation method of the iron-based nanoparticle, in the step 1), the volume ratio of the oxygen-free distilled water to the absolute ethyl alcohol in the water-alcohol solution is 7: 3-3: 7.
Further, in the preparation method of the iron-based nanoparticle, in step 1), the iron source is ferrous chloride or ferrous sulfate, and the concentration of the iron element after dissolving in the hydroalcoholic solution is 0.3-0.7 mol/L.
Further, the preparation method of the nano iron-based particles as described above, in step 1), the mole number of the citric acid is Fe2+1.3 times of the total weight of the powder.
Further, in the method for preparing the nano iron-based particles, in the step 2), the concentration of the sodium hydroxide dissolved in the distilled water is 1mol/L, and the mole number of the sodium hydroxide is Fe2+5 times of the total weight of the powder.
Further, in the method for preparing the nano iron-based particles, step 2), the low sulfite is sodium sulfite or potassium sulfite, and the mole number of the low sulfite ions is Fe2+1.5 times of the total weight of the powder.
Further, in the method for preparing the nano iron-based particles, in the step 3), the silver nitrate solution has a concentration of 0.2mol/L and Ag2+With Fe2+In a molar ratio of 1: 5.
Further, in the method for preparing the nano iron-based particles as described above, in the step 3), the temperature for vacuum drying is 60 ℃.
A nanometer iron-based particle is prepared by the preparation method. The nano iron-based particles are of a core-shell structure, the core layer comprises zero-valent iron, and the shell layer comprises iron sulfide and zero-valent silver. The average particle size of the nano iron-based particles is 50-100 nm. The nano iron-based particles can be applied to medical sewage treatment.
The invention has the beneficial effects that:
in the invention, Fe is adopted2+The citric acid complex is used as a precursor, so that the transfer path of electrons under an alkaline condition is improved, and the substrate of the generated nano particles is zero-valent iron; adopts low-sulfite alkaline solution as a reducing agent and completes the processThe generation of the nano zero-valent iron substrate and the modification of the sulfur on the surface of the nano zero-valent iron substrate are achieved, the production cost is reduced, and the environmental hazard in the production process of the traditional nano iron-based particles is reduced; the nonmetal and metal modification of the sulfur and the silver is carried out on the surface of the zero-valent iron, so that the reactivity and the killing capability of the zero-valent iron are improved, and the zero-valent iron has a good effect in the treatment of medical sewage.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for preparing nano iron-based particles comprises the following steps:
1) preparing an oxidizing solution: uniformly mixing oxygen-free distilled water and absolute ethyl alcohol according to the volume ratio of 7: 3-3: 7 to obtain a water-alcohol solution; weighing ferrous chloride or ferrous sulfate in certain weight, dissolving in water alcohol solution to control Fe2+The concentration of the hydroalcoholic solution is 0.3-0.7 mol/L. Adding a certain mass of citric acid with the mol number of Fe under the stirring condition2+1.3 times of that of the solution, Fe is generated in the hydroalcoholic solution2+To obtain an oxidation solution.
2) Preparation of reducing liquid: sodium hydroxide is weighed, the mole number of the sodium hydroxide is Fe2+5 times of the amount of the sodium hydroxide solution, 1mol/L of the sodium hydroxide solution is prepared, a large amount of heat is released at the time, and a certain amount of low sulfite, the mol number of which is Fe, is added into the sodium hydroxide solution2+1.5 times of the reduction solution, and controlling the water temperature to be 50-70 ℃ to prepare the reduction solution.
3) Preparing the nano iron-based particles: and heating the oxidizing solution to the same temperature as the reducing solution, adding the reducing solution into the oxidizing solution under the stirring condition, reacting for 20-40 min, and gradually turning the solution into grey black, so that the sulfur-modified nano iron-based particles are generated. After the reaction is finished, the addition is stoppedHeating, keeping stirring, slowly adding 0.2mol/L silver nitrate solution into the reaction system, and controlling Fe2+With Ag2+The molar ratio of the silver-sulfur-modified nano iron-based particles to the reaction product is 5:1, stirring is stopped after continuous stirring for 20min, the cooled reaction product is filtered under the protection of nitrogen, and is repeatedly washed by oxygen-free distilled water until the pH value is neutral, and the silver-sulfur-modified nano iron-based particles with the average particle size of 50-100 nm are obtained after vacuum drying at 60 ℃.
The following embodiments are relevant to the present invention:
example 1
And (3) uniformly mixing the oxygen-free distilled water and the absolute ethyl alcohol in a volume ratio of 6:4 to obtain a water-alcohol solution. 198.81g of FeCl were weighed2·4H2O was dissolved in 2L of the above hydroalcoholic solution. Adding 250g of citric acid under the stirring condition to prepare 0.5mol/L Fe2+The complex is a water-alcohol solution, i.e. an oxidation solution. 200g of sodium hydroxide was weighed and dissolved in 5L of distilled water, a large amount of heat was released, 261.16g of sodium hydrosulfite was added thereto, and the temperature of water was controlled at 60 ℃ to prepare a reducing solution. And (3) similarly heating the reducing solution to 60 ℃, adding the reducing solution into the oxidizing solution under the condition of stirring, reacting for 30min, and gradually turning the solution into grey black, so that the sulfur-modified nano iron-based particles are generated. And after the reaction is finished, stopping heating, keeping stirring, slowly adding 40ml of 0.2mol/L silver nitrate solution into the reaction system, continuously stirring for 20min, stopping stirring, filtering the cooled reaction product under the protection of nitrogen, repeatedly washing the reaction product by using oxygen-free distilled water until the pH value is neutral, and drying the reaction product in vacuum at the temperature of 60 ℃ to obtain the silver-sulfur modified nano iron-based particles with the average particle size of 90 nm.
Example 2
And (3) uniformly mixing the oxygen-free distilled water and the absolute ethyl alcohol in a volume ratio of 4:6 to obtain a water-alcohol solution. 16.68g of FeSO are weighed4·7H2O was dissolved in 100ml of the above hydroalcoholic solution. Adding 15g of citric acid under stirring to obtain 0.6mol/L Fe2+The complex is a water-alcohol solution, i.e. an oxidation solution. 12g of sodium hydroxide was weighed and dissolved in 300ml of distilled water, a large amount of heat was released, 18.57g of low potassium sulfite was added thereto, and the water temperature was controlled at 65 ℃ to prepare a reducing solution. The reducing solution is heated to 65 ℃ in the same way, and the reducing solution is stirredAdding the solution into the oxidizing solution, reacting for 30min, and gradually turning the solution into grey black, so that the sulfur-modified nano iron-based particles are generated. And after the reaction is finished, stopping heating, keeping stirring, slowly adding 2.5ml of 0.2mol/L silver nitrate solution into the reaction system, continuously stirring for 20min, stopping stirring, filtering the cooled reaction product under the protection of nitrogen, repeatedly washing the reaction product by using oxygen-free distilled water until the pH value is neutral, and drying the reaction product in vacuum at the temperature of 60 ℃ to obtain the silver-sulfur modified nano iron-based particles with the average particle size of 60 nm.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A method for preparing nano iron-based particles is characterized by comprising the following steps:
1) preparing an oxidizing solution: measuring a certain amount of anaerobic distilled water and absolute ethyl alcohol, and uniformly mixing to obtain a water-alcohol solution; weighing a certain mass of iron source, dissolving the iron source in a hydroalcoholic solution, adding a certain mass of citric acid under the stirring condition, and generating Fe in the hydroalcoholic solution2+To obtain an oxidation solution;
2) preparation of reducing liquid: weighing a certain amount of sodium hydroxide, dissolving the sodium hydroxide in distilled water, releasing a large amount of heat at the moment, adding a certain amount of low sulfite into the distilled water, and controlling the water temperature to be 50-70 ℃ to prepare reducing liquid;
3) preparing the nano iron-based particles: heating the oxidizing solution prepared in the step 1) to the same temperature as the reducing solution prepared in the step 2), adding the reducing solution into the oxidizing solution under the condition of stirring, reacting for 20-40 min, and gradually turning the solution into grey black, so that sulfur-modified nano iron-based particles are generated; after the reaction is finished, stopping heating, keeping stirring, slowly adding the silver nitrate solution into the reaction system, and stopping stirring after continuously stirring for a period of time; and filtering the cooled reaction product under the protection of nitrogen, repeatedly washing the reaction product by using oxygen-free distilled water until the pH value is neutral, and drying the reaction product in vacuum to obtain the silver-sulfur modified nano iron-based particles.
2. The method of claim 1, wherein: in the step 1), the volume ratio of the oxygen-free distilled water to the absolute ethyl alcohol in the water-alcohol solution is 7: 3-3: 7.
3. The method of claim 1, wherein: in the step 1), the iron source is ferrous chloride or ferrous sulfate, and the concentration of the iron element after dissolving in the hydroalcoholic solution is 0.3-0.7 mol/L.
4. The method of claim 1, wherein: in the step 1), the mole number of the citric acid is Fe2+1.3 times of the total weight of the powder.
5. The method of claim 1, wherein: in the step 2), the concentration of the sodium hydroxide dissolved in the distilled water with the concentration is 1mol/L, and the mole number of the sodium hydroxide is Fe2+5 times of the total weight of the powder.
6. The method of claim 1, wherein: in the step 2), the low sulfite is low sodium sulfite or low potassium sulfite, and the mole number of the low sulfite ions is Fe2+1.5 times of the total weight of the powder.
7. The method of claim 1, wherein: in the step 3), the concentration of the silver nitrate solution is 0.2mol/L, and Ag is2+With Fe2+In a molar ratio of 1: 5.
8. The method of claim 1, wherein: in step 3), the temperature for vacuum drying is 60 ℃.
9. A nano iron-based particle prepared by the method of any one of claims 1 to 8.
10. Use of the nano iron-based particles according to claim 9 in medical sewage treatment.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101336070A (en) * | 2008-08-06 | 2008-12-31 | 长沙矿冶研究院 | Nano composite alpha-Fe for wave-absorbing material and preparation method thereof |
| CN102259192A (en) * | 2011-07-27 | 2011-11-30 | 南京师范大学 | Method for preparing nanometer zero-valent iron based on liquid-phase complexation reduction method |
| CN102284706A (en) * | 2011-08-15 | 2011-12-21 | 华南理工大学 | Nanoscale zero-valent iron stable in air and preparation method for the same |
| CN104609531A (en) * | 2015-02-02 | 2015-05-13 | 中国地质大学（武汉） | Method for preparing citrate nano zero-valent iron and method of activated persulfate thereof for treating organic wastewater |
| CN105081340A (en) * | 2014-05-07 | 2015-11-25 | 沈阳农业大学 | Dispersed nano iron particle and preparation method thereof |
| CN106927547A (en) * | 2017-04-05 | 2017-07-07 | 同济大学 | A kind of method that magnetic iron-based material reduction contact break removes complex state heavy metal |
| CN106955667A (en) * | 2017-03-31 | 2017-07-18 | 中国科学院城市环境研究所 | A kind of composite of activated carbon supported nano zero valence iron and silver metal cluster and preparation method thereof |
| JP2019050104A (en) * | 2017-09-08 | 2019-03-28 | 太平洋セメント株式会社 | Method for manufacturing positive electrode active material composite for lithium ion secondary battery |
| CN110449188A (en) * | 2019-08-15 | 2019-11-15 | 苏州大学 | Silver citrate/silver composite nano materials and its preparation method and application |
| US20210269311A1 (en) * | 2018-07-13 | 2021-09-02 | University Of Delaware | Methods for producing silver-amended carbon materials |
-
2021
- 2021-12-09 CN CN202111498032.5A patent/CN114192080B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101336070A (en) * | 2008-08-06 | 2008-12-31 | 长沙矿冶研究院 | Nano composite alpha-Fe for wave-absorbing material and preparation method thereof |
| CN102259192A (en) * | 2011-07-27 | 2011-11-30 | 南京师范大学 | Method for preparing nanometer zero-valent iron based on liquid-phase complexation reduction method |
| CN102284706A (en) * | 2011-08-15 | 2011-12-21 | 华南理工大学 | Nanoscale zero-valent iron stable in air and preparation method for the same |
| CN105081340A (en) * | 2014-05-07 | 2015-11-25 | 沈阳农业大学 | Dispersed nano iron particle and preparation method thereof |
| CN104609531A (en) * | 2015-02-02 | 2015-05-13 | 中国地质大学（武汉） | Method for preparing citrate nano zero-valent iron and method of activated persulfate thereof for treating organic wastewater |
| CN106955667A (en) * | 2017-03-31 | 2017-07-18 | 中国科学院城市环境研究所 | A kind of composite of activated carbon supported nano zero valence iron and silver metal cluster and preparation method thereof |
| CN106927547A (en) * | 2017-04-05 | 2017-07-07 | 同济大学 | A kind of method that magnetic iron-based material reduction contact break removes complex state heavy metal |
| JP2019050104A (en) * | 2017-09-08 | 2019-03-28 | 太平洋セメント株式会社 | Method for manufacturing positive electrode active material composite for lithium ion secondary battery |
| US20210269311A1 (en) * | 2018-07-13 | 2021-09-02 | University Of Delaware | Methods for producing silver-amended carbon materials |
| CN110449188A (en) * | 2019-08-15 | 2019-11-15 | 苏州大学 | Silver citrate/silver composite nano materials and its preparation method and application |
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