CN112047449A - Manganese ferrite nano powder, preparation thereof and method for treating hexavalent chromium-containing sewage by using manganese ferrite nano powder - Google Patents
Manganese ferrite nano powder, preparation thereof and method for treating hexavalent chromium-containing sewage by using manganese ferrite nano powder Download PDFInfo
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 145
- 239000011572 manganese Substances 0.000 title claims abstract description 145
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 145
- 239000011858 nanopowder Substances 0.000 title claims abstract description 136
- 238000000034 method Methods 0.000 title claims abstract description 61
- 239000010865 sewage Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 title abstract description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 33
- 239000010935 stainless steel Substances 0.000 claims abstract description 33
- 239000002245 particle Substances 0.000 claims abstract description 30
- 150000002500 ions Chemical class 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 20
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 16
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 15
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 15
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 15
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000011565 manganese chloride Substances 0.000 claims abstract description 15
- 235000002867 manganese chloride Nutrition 0.000 claims abstract description 15
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 14
- 239000002351 wastewater Substances 0.000 claims abstract description 12
- 238000003795 desorption Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 12
- 241001388119 Anisotremus surinamensis Species 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 239000011651 chromium Substances 0.000 abstract description 87
- 238000005054 agglomeration Methods 0.000 abstract description 10
- 230000002776 aggregation Effects 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 37
- 239000000047 product Substances 0.000 description 17
- 239000000843 powder Substances 0.000 description 14
- 239000012535 impurity Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 231100000331 toxic Toxicity 0.000 description 4
- 230000002588 toxic effect Effects 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 231100000243 mutagenic effect Toxicity 0.000 description 1
- 230000003505 mutagenic effect Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 239000011686 zinc sulphate Substances 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- 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)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Removal Of Specific Substances (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Manganese ferrite nano powder, preparation thereof and a method for treating hexavalent chromium-containing sewage by using the same. The technical scheme is as follows: dissolving manganous chloride solid-four water and ferric trichloride in ethylene glycol, magnetically stirring, adding anhydrous sodium acetate and polyethylene glycol, and stirring; and adding the mixture solution obtained by stirring into a sealed container, transferring the sealed container into a stainless steel high-pressure kettle, transferring into a hydrothermal oven, preserving heat, taking out, washing and drying to obtain the manganese ferrite nano powder. Adding manganese ferrite nano powder into sewage containing Cr (VI) according to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) of 1: 5-30; the absorption-desorption equilibrium is achieved under the dark room condition, and then the wastewater is transferred to a microwave reactor to be heated to 60-200 ℃, and the temperature is preserved, so that Cr (VI) ions in the wastewater containing Cr (VI) are all reduced into Cr (III) ions. The invention has low cost and simple process, and the prepared manganese ferrite nano powder has small particle agglomeration and uniform particle size distribution, and has good effect and short time for treating sewage containing Cr (VI).
Description
Technical Field
The present invention belongs to the field of superfine inorganic non-metal material powder technology. In particular to manganese ferrite nano powder, a preparation method thereof and a method for treating hexavalent chromium-containing sewage by using the manganese ferrite nano powder.
Background
The chromium-containing wastewater is from different industrial processes such as printing and dyeing, medicine, spinning, metallurgy, electroplating, tanning and the like. Cr (VI) and Cr (III) are two common valence states of chromium compounds. Of these, hexavalent chromium (cr (vi)) has carcinogenic and mutagenic properties and is considered second to the second common inorganic contaminant of lead (Pb). Compared with Cr (VI), Cr (III) has lower toxicity and fluidity, and can be used as nutrient substance of organism at low concentration. Therefore, the reduction of Cr (VI) to Cr (III) is an effective method for treating chromium-containing wastewater.
At present, the method for treating the chromium-containing wastewater comprises the following steps: biological reduction, electrochemical reduction, photocatalytic reduction, and the like. The biological reduction method is an environment-friendly technology, has simple equipment and low investment, plays an increasingly important role in the reduction of Cr (VI), and has low reduction efficiency, low speed and weak capability. The electrochemical reduction method has the advantages of good selectivity, high efficiency, flexible operation, good environmental compatibility and the like, but the defect of high cost limits the application in large-scale treatment of industrial wastewater. In addition, the electrochemical reduction method also has certain risks, such as overvoltage and secondary pollution, which can cause potential harm to human bodies; the photocatalytic reduction method is considered as the most promising method for removing the wastewater containing Cr (VI) due to the characteristics of high efficiency, economy, environmental protection and the like, but most of photocatalytic systems are not suitable for emergency treatment of the wastewater containing Cr (VI) due to long reaction time (>60 min).
Manganese ferrite (MnFe)2O4) Is a magnetic spinel structure material used as waste waterA physical catalyst. Compared with other catalysts, manganese ferrite has attracted extensive attention because of its advantages of high catalytic activity, stable chemical properties, easy magnetic separation, etc.
The chemical coprecipitation method is to use MnSO4◆4H2O，ZnSO4◆7H2O，FeCl3◆6H2Using excessive KOH, NaOH and the like as a precipitator by using O as a raw material, and preparing single-crystal-phase manganese ferrite powder by filtering, washing, drying and calcining; the method has simple manufacturing process, but is easy to introduce impurities, and colloidal precipitate is often generated in the precipitation process, so the filtering and washing are difficult. The self-propagating high-temperature synthesis method (SHS) is a process technology which relies on the self-heat release of substance reaction and synthesizes target products in a very short time, and although the self-propagating high-temperature synthesis method has the advantages of simple equipment, low energy consumption, high efficiency and short reaction time, the powder obtained by the method has large particles and serious agglomeration and the reaction process is difficult to control. The Sol-gel method (Sol-gel) is to solidify metal organic or inorganic compounds through solution, Sol and gel, and then to form oxide or other compound solid through heat treatment; although the method has simple process, short reaction period, low reaction temperature and low sintering temperature, the formed gel precursor is easy to deliquesce, hard agglomeration is easy to form after drying, and the shrinkage is large during drying.
In summary, the conventional manganese ferrite powder (MnFe)2O4) The preparation technology has the following defects: high cost, low purity of the synthesized powder, uneven particle size distribution of the powder particles, easy agglomeration of the powder particles and the like. The existing Cr (VI) reducing system has the following defects: long reaction time, low catalyst utilization rate and easy secondary pollution to environment.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide the preparation method of the manganese ferrite powder with low cost and simple process.
In order to realize the purpose, the technical scheme for preparing the manganese ferrite powder is as follows:
step one, dissolving 0.2-1 part by mass of manganous chloride diamond-solid and 0.5-1.5 parts by mass of ferric trichloride in 85-91 parts by mass of ethylene glycol, and magnetically stirring at the rotating speed of 1000-1200 r/min for 20-40 min to obtain a light yellow solution; and adding 6.5-7.5 parts by mass of anhydrous sodium acetate and 1-5 parts by mass of polyethylene glycol into the light yellow solution, and stirring at the rotating speed of 1000-1200 r/min for 60-70 min to obtain a mixture solution.
Step two, adding the mixture solution into a sealed container according to the volume ratio of the mixture solution to the sealed container being 0.55-0.65: 1, wherein the lining of the sealed container is made of polytetrafluoroethylene; moving the sealed container into a stainless steel high-pressure autoclave, moving the stainless steel high-pressure autoclave into a hydrothermal oven, and preserving heat for 15-24 hours at 160-220 ℃; and then taking out the stainless steel autoclave, and naturally cooling to obtain a black product.
And step three, washing the black product with ethanol for 2-4 times, and drying for 6-8 hours at the temperature of 60-70 ℃ in an air atmosphere to obtain the manganese ferrite nano powder.
The manganese ferrite nano powder is in a pompon shape, and the particle size of the manganese ferrite nano powder is less than or equal to 500 nm; the manganese ferrite nano powder is more than industrial pure.
In the above technical scheme:
MnCl in the manganous chloride water2·4H2The content of O is more than or equal to 99.0 wt%;
FeCl in the ferric trichloride3·6H2The content of O is more than or equal to 99.0 wt%;
of the ethylene glycol (CH)2OH)2The content is more than or equal to 99.5 wt%;
the NaAc content in the anhydrous sodium acetate is more than or equal to 99.0 wt%;
the average molecular weight of the polyethylene glycol is 380-430.
The method for treating the sewage containing Cr (VI) by using the manganese ferrite nano powder prepared by the technical scheme comprises the following steps:
adding the manganese ferrite nano powder into the sewage containing Cr (VI) according to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) of 1: 5-30, and adjusting the pH value to 2-6; and then the absorption-desorption balance is achieved under the dark room condition, the mixture is transferred to a microwave reactor, the microwave is heated to 60-200 ℃, the microwave is insulated for 5-25 min, and Cr (VI) ions in the sewage containing Cr (VI) are all reduced into Cr (III) ions.
Compared with the prior art, the invention has the following positive effects and prominent characteristics due to the adoption of the technical scheme:
1. the invention takes manganous chloride and ferric trichloride as raw materials, has wide source and low price, and the prepared manganese ferrite nano powder has low production cost.
2. Dissolving manganous chloride diamond-solid and ferric trichloride diamond-solid in ethylene glycol, magnetically stirring, adding anhydrous sodium acetate and polyethylene glycol, and stirring; then adding the manganese ferrite powder into a sealed container, moving the container into a stainless steel high-pressure kettle, moving the container into a hydrothermal oven, preserving heat, taking out the container, washing and drying the container to obtain manganese ferrite nano powder, so that the preparation process is simple; in addition, the components are uniformly mixed according to the mass ratio in the preparation process, the pH value of the mixed solution does not need to be accurately adjusted, and the synthesis process is simple.
3. The invention is beneficial to removing impurities in the reaction process and the subsequent cleaning process of the manganese ferrite nano powder; the invention adopts the glycol as the solvent, has low boiling point, can obtain higher pressure and can avoid the influence of the introduction of impurities on the product; high purity reactant, no impurity phase and high purity.
4. The manganese ferrite powder prepared by the invention is uniformly dispersed in ethylene glycol, and the occurrence of agglomeration phenomenon after dissolution and washing is greatly reduced. The prepared manganese ferrite nano powder is in a pompon shape, the particles are free from agglomeration, and the average particle size of the manganese ferrite nano powder is less than or equal to 500 nm; the manganese ferrite nano powder is more than industrial pure and has high purity.
5. According to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) being 1: 5-30, the manganese ferrite nano powder prepared by the invention is added into the sewage containing Cr (VI), and is completely reduced into Cr (III) liquid under the microwave condition within 20 minutes, so that the treatment effect is good, and the method is particularly suitable for emergency treatment of toxic Cr (VI) wastewater.
6. The manganese ferrite nano powder synthesized by the method has strong magnetism, is easy to recover after being used for treating sewage containing Cr (VI), and avoids secondary pollution to a water body.
Therefore, the method has the characteristics of low cost and simple process, the manganese ferrite nano powder prepared by the method has small particle agglomeration, uniform powder particle size distribution and high purity, the effect of treating the sewage containing Cr (VI) by using the prepared manganese ferrite nano powder is high, the time is short, the recovery is easy, no secondary pollution is caused, and the method is particularly suitable for emergently treating the toxic Cr (VI) wastewater.
Drawings
FIG. 1 is an XRD spectrum of a manganese ferrite nanopowder prepared in the present invention;
fig. 2 is an SEM photograph of the manganese ferrite nanopowder shown in fig. 1.
Detailed Description
The invention is further described with reference to the following figures and detailed description, without limiting its scope.
In order to avoid repetition, the raw materials related to this specific embodiment are uniformly described as follows, and are not described in detail in the embodiments:
MnCl in the manganous chloride water2·4H2The content of O is more than or equal to 99.0 wt%;
FeCl in the ferric trichloride3·6H2The content of O is more than or equal to 99.0 wt%;
of the ethylene glycol (CH)2OH)2The content is more than or equal to 99.5 wt%;
the NaAc content in the anhydrous sodium acetate is more than or equal to 99.0 wt%.
Example 1
Manganese ferrite nano powder, preparation thereof and a method for treating hexavalent chromium-containing sewage by using the same. The method of the embodiment comprises the following steps:
preparation method of manganese ferrite nano powder
Step one, dissolving 0.5 parts by mass of manganous chloride diamond-solid and 1.0 part by mass of ferric trichloride in 90 parts by mass of ethylene glycol, and magnetically stirring for 30min at the rotating speed of 1100r/min to obtain a light yellow solution; and adding 7.0 parts by mass of anhydrous sodium acetate and 3.0 parts by mass of polyethylene glycol into the light yellow solution, and stirring at the rotating speed of 1100r/min for 65min to obtain a mixture solution.
Step two, adding the mixture solution into a sealed container according to the volume ratio of the mixture solution to the sealed container of 0.55: 1, wherein the inner liner of the sealed container is made of polytetrafluoroethylene; moving the sealed container into a stainless steel high-pressure autoclave, moving the stainless steel high-pressure autoclave into a hydrothermal oven, and preserving heat for 22 hours at the temperature of 200 ℃; and then taking out the stainless steel autoclave, and naturally cooling to obtain a black product.
And step three, washing the black product with ethanol for 2 times, and drying for 6 hours at the temperature of 60 ℃ in the air atmosphere to obtain the manganese ferrite nano powder.
The manganese ferrite nano powder is in a pompon shape, particles are not agglomerated, and the average particle size of the manganese ferrite nano powder is 105 nm; the manganese ferrite nano powder is more than industrial pure and has high purity.
The polyethylene glycol has an average molecular weight of 380.
Method for treating sewage containing Cr (VI) by using prepared manganese ferrite nano powder
Adding the manganese ferrite nano powder into the sewage containing Cr (VI) according to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) of 1: 30, and adjusting the pH value to 6; then the absorption-desorption equilibrium is achieved under the condition of a darkroom, and the sewage is transferred to a microwave reactor, the microwave is heated to 180 ℃, the microwave is insulated for 20min, and the Cr (VI) ions in the sewage containing Cr (VI) are all reduced into Cr (III) ions.
The manganese ferrite nanopowder described in the second embodiment is the manganese ferrite nanopowder prepared by the preparation method of the manganese ferrite nanopowder described in the first embodiment.
Example 2
Manganese ferrite nano powder, preparation thereof and a method for treating hexavalent chromium-containing sewage by using the same. The method of the embodiment comprises the following steps:
preparation method of manganese ferrite nano powder
Step one, dissolving 1 part by mass of manganous chloride diamond-solid and 1.5 parts by mass of ferric trichloride in 87 parts by mass of ethylene glycol, and magnetically stirring for 40min at the rotating speed of 1000r/min to obtain a light yellow solution; and adding 7.5 parts by mass of anhydrous sodium acetate and 5 parts by mass of polyethylene glycol into the light yellow solution, and stirring at the rotating speed of 1000r/min for 60min to obtain a mixture solution.
Step two, adding the mixture solution into a sealed container according to the volume ratio of the mixture solution to the sealed container of 0.65: 1, wherein the inner liner of the sealed container is made of polytetrafluoroethylene; moving the sealed container into a stainless steel high-pressure autoclave, moving the stainless steel high-pressure autoclave into a hydrothermal oven, and preserving heat for 20 hours at the temperature of 180 ℃; and then taking out the stainless steel autoclave, and naturally cooling to obtain a black product.
And step three, washing the black product with ethanol for 3 times, and drying for 6 hours at the temperature of 65 ℃ in the air atmosphere to obtain the manganese ferrite nano powder.
The manganese ferrite nano powder is in a pompon shape, particles are not agglomerated, and the average particle size of the manganese ferrite nano powder is 210 nm; the manganese ferrite nano powder is more than industrial pure and has high purity.
The polyethylene glycol has an average molecular weight of 400.
Method for treating sewage containing Cr (VI) by using prepared manganese ferrite nano powder
Adding the manganese ferrite nano powder into the sewage containing Cr (VI) according to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) of 1: 25, and adjusting the pH value to 5; then the absorption-desorption equilibrium is achieved under the condition of a darkroom, and the sewage is transferred to a microwave reactor, the microwave is heated to 160 ℃, the microwave is kept for 18min, and the Cr (VI) ions in the sewage containing Cr (VI) are all reduced into Cr (III) ions.
The manganese ferrite nanopowder described in the second embodiment is the manganese ferrite nanopowder prepared by the preparation method of the manganese ferrite nanopowder described in the first embodiment.
Example 3
Manganese ferrite nano powder, preparation thereof and a method for treating hexavalent chromium-containing sewage by using the same. The method of the embodiment comprises the following steps:
preparation method of manganese ferrite nano powder
Step one, dissolving 0.2 parts by mass of manganous chloride diamond-solid and 0.5 parts by mass of ferric trichloride in 85 parts by mass of ethylene glycol, and magnetically stirring at the rotating speed of 1200r/min for 20min to obtain a light yellow solution; and adding 7.1 parts by mass of anhydrous sodium acetate and 1.0 part by mass of polyethylene glycol into the light yellow solution, and stirring at the rotating speed of 1200r/min for 70min to obtain a mixture solution.
Step two, adding the mixture solution into a sealed container according to the volume ratio of the mixture solution to the sealed container of 0.60: 1, wherein the inner liner of the sealed container is made of polytetrafluoroethylene; moving the sealed container into a stainless steel high-pressure autoclave, moving the stainless steel high-pressure autoclave into a hydrothermal oven, and preserving heat for 18 hours at the temperature of 210 ℃; and then taking out the stainless steel autoclave, and naturally cooling to obtain a black product.
And step three, washing the black product with ethanol for 4 times, and drying for 7 hours at 70 ℃ in an air atmosphere to obtain the manganese ferrite nano powder.
The manganese ferrite nano powder is in a pompon shape, particles are not agglomerated, and the average particle size of the manganese ferrite nano powder is 315 nm; the manganese ferrite nano powder is more than industrial pure and has high purity.
The polyethylene glycol has an average molecular weight of 400.
Method for treating sewage containing Cr (VI) by using prepared manganese ferrite nano powder
Adding the manganese ferrite nano powder into the sewage containing Cr (VI) according to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) of 1: 20, and adjusting the pH value to 3; then the absorption-desorption equilibrium is achieved under the dark room condition, and the sewage is transferred to a microwave reactor, the microwave is heated to 140 ℃, the microwave is insulated for 15min, and the Cr (VI) ions in the sewage containing Cr (VI) are all reduced into Cr (III) ions.
The manganese ferrite nanopowder described in the second embodiment is the manganese ferrite nanopowder prepared by the preparation method of the manganese ferrite nanopowder described in the first embodiment.
Example 4
Manganese ferrite nano powder, preparation thereof and a method for treating hexavalent chromium-containing sewage by using the same. The method of the embodiment comprises the following steps:
preparation method of manganese ferrite nano powder
Step one, dissolving 0.8 part by mass of manganous chloride-tetrahydrate and 1.4 parts by mass of ferric trichloride in 89 parts by mass of ethylene glycol, and magnetically stirring at the rotating speed of 1100r/min for 40min to obtain a light yellow solution; and adding 7.4 parts by mass of anhydrous sodium acetate and 2.5 parts by mass of polyethylene glycol into the light yellow solution, and stirring at the rotating speed of 1100r/min for 70min to obtain a mixture solution.
Step two, adding the mixture solution into a sealed container according to the volume ratio of the mixture solution to the sealed container of 0.65: 1, wherein the inner liner of the sealed container is made of polytetrafluoroethylene; moving the sealed container into a stainless steel high-pressure autoclave, moving the stainless steel high-pressure autoclave into a hydrothermal oven, and preserving heat for 24 hours at the temperature of 200 ℃; and then taking out the stainless steel autoclave, and naturally cooling to obtain a black product.
And step three, washing the black product with ethanol for 3 times, and drying for 8 hours at the temperature of 60 ℃ in an air atmosphere to obtain the manganese ferrite nano powder.
The manganese ferrite nano powder is in a pompon shape, particles are not agglomerated, and the average particle size of the manganese ferrite nano powder is 350 nm; the manganese ferrite nano powder is more than industrial pure and has high purity.
The polyethylene glycol has an average molecular weight of 420.
Method for treating sewage containing Cr (VI) by using prepared manganese ferrite nano powder
Adding the manganese ferrite nano powder into the sewage containing Cr (VI) according to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) of 1: 15, and adjusting the pH value to 4; then the absorption-desorption equilibrium is achieved under the condition of a darkroom, and the sewage is transferred to a microwave reactor, the microwave is heated to 120 ℃, the microwave is kept for 13min, and the Cr (VI) ions in the sewage containing Cr (VI) are all reduced into Cr (III) ions.
The manganese ferrite nanopowder described in the second embodiment is the manganese ferrite nanopowder prepared by the preparation method of the manganese ferrite nanopowder described in the first embodiment.
Example 5
Manganese ferrite nano powder, preparation thereof and a method for treating hexavalent chromium-containing sewage by using the same. The method of the embodiment comprises the following steps:
preparation method of manganese ferrite nano powder
Step one, dissolving 0.4 parts by mass of manganous chloride diamond-solid and 1.3 parts by mass of ferric trichloride in 88 parts by mass of ethylene glycol, and magnetically stirring at the rotating speed of 1000r/min for 40min to obtain a light yellow solution; and adding 7.3 parts by mass of anhydrous sodium acetate and 2 parts by mass of polyethylene glycol into the light yellow solution, and stirring at the rotating speed of 1000r/min for 65min to obtain a mixture solution.
Step two, adding the mixture solution into a sealed container according to the volume ratio of the mixture solution to the sealed container of 0.60: 1, wherein the inner liner of the sealed container is made of polytetrafluoroethylene; moving the sealed container into a stainless steel high-pressure autoclave, moving the stainless steel high-pressure autoclave into a hydrothermal oven, and preserving heat for 20 hours at the temperature of 200 ℃; and then taking out the stainless steel autoclave, and naturally cooling to obtain a black product.
And step three, washing the black product with ethanol for 2 times, and drying for 7 hours at the temperature of 65 ℃ in the air atmosphere to obtain the manganese ferrite nano powder.
The manganese ferrite nano powder is in a pompon shape, particles are not agglomerated, and the average particle size of the manganese ferrite nano powder is 420 nm; the manganese ferrite nano powder is more than industrial pure and has high purity.
The polyethylene glycol has an average molecular weight of 420.
Method for treating sewage containing Cr (VI) by using prepared manganese ferrite nano powder
Adding the manganese ferrite nano powder into the sewage containing Cr (VI) according to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) of 1: 10, and adjusting the pH value to 3; then the absorption-desorption equilibrium is achieved under the condition of a darkroom, and the sewage is transferred to a microwave reactor, the microwave is heated to 100 ℃, the microwave is insulated for 10min, and the Cr (VI) ions in the sewage containing Cr (VI) are all reduced into Cr (III) ions.
The manganese ferrite nanopowder described in the second embodiment is the manganese ferrite nanopowder prepared by the preparation method of the manganese ferrite nanopowder described in the first embodiment.
Example 6
Manganese ferrite nano powder, preparation thereof and a method for treating hexavalent chromium-containing sewage by using the same. The method of the embodiment comprises the following steps:
preparation method of manganese ferrite nano powder
Step one, dissolving 0.6 mass part of manganous chloride diamond-solid and 1.2 mass parts of ferric trichloride in 91 mass parts of ethylene glycol, and magnetically stirring at the rotating speed of 1200r/min for 40min to obtain a light yellow solution; and adding 6.5 parts by mass of anhydrous sodium acetate and 4 parts by mass of polyethylene glycol into the light yellow solution, and stirring at the rotating speed of 1200r/min for 60min to obtain a mixture solution.
Step two, adding the mixture solution into a sealed container according to the volume ratio of the mixture solution to the sealed container of 0.55: 1, wherein the inner liner of the sealed container is made of polytetrafluoroethylene; moving the sealed container into a stainless steel high-pressure autoclave, moving the stainless steel high-pressure autoclave into a hydrothermal oven, and preserving heat for 18 hours at 190 ℃; and then taking out the stainless steel autoclave, and naturally cooling to obtain a black product.
And step three, washing the black product with ethanol for 4 times, and drying for 8 hours at 70 ℃ in an air atmosphere to obtain the manganese ferrite nano powder.
The manganese ferrite nano powder is in a pompon shape, particles are not agglomerated, and the average particle size of the manganese ferrite nano powder is 495 nm; the manganese ferrite nano powder is more than industrial pure and has high purity.
The polyethylene glycol has an average molecular weight of 430.
Method for treating sewage containing Cr (VI) by using prepared manganese ferrite nano powder
Adding the manganese ferrite nano powder into the sewage containing Cr (VI) according to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) of 1: 5, and adjusting the pH value to 2; then the absorption-desorption equilibrium is achieved under the condition of a darkroom, and the sewage is transferred to a microwave reactor, the microwave is heated to 60 ℃, the microwave is insulated for 10min, and the Cr (VI) ions in the sewage containing Cr (VI) are all reduced into Cr (III) ions.
The manganese ferrite nanopowder described in the second embodiment is the manganese ferrite nanopowder prepared by the preparation method of the manganese ferrite nanopowder described in the first embodiment.
Compared with the prior art, the specific implementation mode has the following positive effects and outstanding characteristics:
1. the specific embodiment takes manganous chloride and ferric trichloride as raw materials, the source is wide, the price is low, and the production cost of the prepared manganese ferrite nano powder is low.
2. Dissolving manganous chloride-tetrahydrate and ferric trichloride-hexahydrate in ethylene glycol, magnetically stirring, adding anhydrous sodium acetate and polyethylene glycol, and stirring; then adding the manganese ferrite powder into a sealed container, moving the container into a stainless steel high-pressure kettle, moving the stainless steel high-pressure kettle into a hydrothermal oven, preserving heat, taking out the stainless steel high-pressure kettle, washing and drying the stainless steel high-pressure kettle to obtain manganese ferrite nano powder, so that the preparation process is simple; in addition, the components are uniformly mixed according to the mass ratio in the preparation process, the pH value of the mixed solution does not need to be accurately adjusted, and the synthesis process is simple.
3. The specific embodiment is beneficial to removing impurities in the reaction process and the subsequent cleaning process of the manganese ferrite nano powder; the specific embodiment adopts the ethylene glycol as the solvent, has low boiling point, can obtain higher pressure, and can avoid the influence of the introduction of impurities on the product; high purity reactant, no impurity phase and high purity.
4. The manganese ferrite nano powder prepared by the specific embodiment is uniformly dispersed in ethylene glycol, so that the agglomeration phenomenon after dissolution and washing is greatly reduced. Therefore, the prepared manganese ferrite nano powder is in a pompon shape, the particles are not agglomerated, and the average particle size of the manganese ferrite nano powder is less than or equal to 500 nm; the manganese ferrite nano powder is more than industrial pure and has high purity. The prepared manganese ferrite nano powder is shown in the attached drawing, fig. 1 is an XRD (X-ray diffraction) spectrum of the manganese ferrite nano powder prepared in example 4, and fig. 2 is an SEM (scanning Electron microscope) picture of the manganese ferrite nano powder shown in fig. 1. As can be seen from FIG. 1, the synthesized manganese ferrite nano-powder has high purity and good crystallinity; as can be seen from FIG. 2, the synthesized manganese ferrite nanopowder has high sphericity, no particle agglomeration and an average particle size of 350 nm.
5. According to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) being 1: 5-30, the manganese ferrite nano powder prepared by the embodiment is added into the sewage containing Cr (VI), and is completely reduced into a Cr (III) solution within 20 minutes under the microwave condition, so that the treatment effect is good, and the method is particularly suitable for emergency treatment of toxic Cr (VI) wastewater. In addition, the sewage containing Cr (VI) is light yellow before treatment, and after the treatment method of the specific embodiment is adopted, the liquid containing Cr (III) is colorless and odorless transparent liquid.
6. The manganese ferrite nano powder synthesized by the specific embodiment has strong magnetism, is easy to recover after being used for treating sewage containing Cr (VI), and avoids secondary pollution to a water body.
Therefore, the embodiment has the characteristics of low cost and simple process, the manganese ferrite nano powder prepared by the method has small particle agglomeration, uniform powder particle size distribution and high purity, the effect of treating the sewage containing Cr (VI) by using the prepared manganese ferrite nano powder is high, the time is short, the recovery is easy, no secondary pollution is caused, and the method is particularly suitable for emergently treating the toxic sewage containing Cr (VI).
Claims (8)
1. A preparation method of manganese ferrite nano powder is characterized by comprising the following steps:
step one, dissolving 0.2-1 part by mass of manganous chloride diamond-solid and 0.5-1.5 parts by mass of ferric trichloride in 85-91 parts by mass of ethylene glycol, and magnetically stirring at the rotating speed of 1000-1200 r/min for 20-40 min to obtain a light yellow solution; adding 6.5-7.5 parts by mass of anhydrous sodium acetate and 1-5 parts by mass of polyethylene glycol into the light yellow solution, and stirring at the rotating speed of 1000-1200 r/min for 60-70 min to obtain a mixture solution;
step two, adding the mixture solution into a sealed container according to the volume ratio of the mixture solution to the sealed container being 0.55-0.65: 1, wherein the lining of the sealed container is made of polytetrafluoroethylene; moving the sealed container into a stainless steel high-pressure autoclave, moving the stainless steel high-pressure autoclave into a hydrothermal oven, and preserving heat for 15-24 hours at 160-220 ℃; then taking out the stainless steel autoclave, and naturally cooling to obtain a black product;
and step three, washing the black product with ethanol for 2-4 times, and drying for 6-8 hours at the temperature of 60-70 ℃ in an air atmosphere to obtain the manganese ferrite nano powder.
2. The method for preparing manganese ferrite nanopowder according to claim 1, characterized in that said manganous chloride diamond-solid in tetrahydrate2·4H2The content of O is more than or equal to 99.0wt percent.
3. The method for preparing manganese ferrite nanopowder according to claim 1, characterized in that FeCl in the ferric trichloride3·6H2The content of O is more than or equal to 99.0wt percent.
4. The method for preparing manganese ferrite nanopowder according to claim 1, characterized in that said ethylene glycol (CH)2OH)2The content is more than or equal to 99.5 wt%.
5. The method for preparing the manganese ferrite nano powder according to claim 1, characterized in that the NaAc content in the anhydrous sodium acetate is more than or equal to 99.0 wt%.
6. The method for preparing the manganese ferrite nano powder according to claim 1, wherein the average molecular weight of the polyethylene glycol is 380-430.
7. A manganese ferrite nanopowder characterized in that it is prepared by the method of any one of claims 1 to 6;
the manganese ferrite nano powder is in a pompon shape, and the particle size of the manganese ferrite nano powder is less than or equal to 500 nm; the manganese ferrite nano powder is more than industrial pure.
8. A method for treating sewage containing Cr (VI) by using manganese ferrite nano powder is characterized in that: adding the manganese ferrite nano powder into the sewage containing Cr (VI) according to the mass ratio of the manganese ferrite nano powder to Cr (VI) ions in the sewage containing Cr (VI) of 1: 5-30, and adjusting the pH value to 2-6; then, the absorption-desorption balance is achieved under the dark room condition, the wastewater is transferred to a microwave reactor, the microwave is heated to 60-200 ℃, the microwave is insulated for 5-25 min, and Cr (VI) ions in the wastewater containing Cr (VI) are all reduced into Cr (III) ions;
the preparation method of the manganese ferrite nano powder comprises the following steps:
step one, dissolving 0.2-1 part by mass of manganous chloride diamond-solid and 0.5-1.5 parts by mass of ferric trichloride in 85-91 parts by mass of ethylene glycol, and magnetically stirring at the rotating speed of 1000-1200 r/min for 20-40 min to obtain a light yellow solution; adding 6.5-7.5 parts by mass of anhydrous sodium acetate and 1-5 parts by mass of polyethylene glycol into the light yellow solution, and stirring at the rotating speed of 1000-1200 r/min for 60-70 min to obtain a mixture solution;
step two, adding the mixture solution into a sealed container according to the volume ratio of the mixture solution to the sealed container being 0.55-0.65: 1, wherein the lining of the sealed container is made of polytetrafluoroethylene; moving the sealed container into a stainless steel high-pressure autoclave, moving the stainless steel high-pressure autoclave into a hydrothermal oven, and preserving heat for 15-24 hours at 160-220 ℃; then taking out the stainless steel autoclave, and naturally cooling to obtain a black product;
and step three, washing the black product with ethanol for 2-4 times, and drying for 6-8 hours at the temperature of 60-70 ℃ in an air atmosphere to obtain the manganese ferrite nano powder.
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