CN105771877A - Method for preparing composite adsorption material MnO2-Fe3O4 with core-shell structure - Google Patents

Abstract

The invention discloses a method for preparing a core-shell composite adsorption material MnO2-Fe3O4, relates to a method for preparing a composite adsorption material MnO2-Fe3O4 with a core-shell structure, and aims to solve the technical problems that the adsorption material MnO2 is small in particle size, low in apparent density, difficult to separate and recycle, and high in probability of causing secondary pollution. The method for preparing the core-shell composite adsorption material comprises the following steps: at normal temperature, adding 0.51 g of KMnO4 to 40 mL of deionized water; dropwise adding 0.8 mL of HCl (37wt%), stirring for 15 minutes, and then adding 0.35 g of Fe3O4 (nanoscale) to obtain a mixture; transferring the mixture to a 50 mL high pressure reaction kettle to react for 6 hours at 110 DEG C; centrifugally separating the solution, and repeatedly washing precipitate with deionized water and alcohol for four times, and drying in a vacuum drying oven at 60 DEG C for 12 hours, to obtain the composite adsorption material MnO2-Fe3O4; subsequently, a method for applying a magnetic field can be used for separating the composite adsorption material adsorbing heavy metals from the water body, and has high operability.

Description

Nucleocapsid structure composite adsorbing material MnO2-Fe3O4Preparation method

Technical field

The present invention relates to the composite adsorbing material MnO of a kind of nucleocapsid structure₂-Fe₃O₄Preparation method.

Background technology

Absorption method, because its floor space is little, technique is simple and convenient to operate, heavy metal treatment effeciency high, receives much concern in water processes.But adsorbing material particle diameter is little, apparent density is low, difficult separation and recycling, easily causes secondary pollution, and when processing low concentration heavy metal water, treatment effect is the best, sensible less than GB discharge.Therefore, research be not only able to process the effective and easily separated adsorbing material recycled of low-concentration heavy metal imperative.Compound adsorbing material is a kind of new thinking of development, it is possible to the shortcoming making up two or more single adsorbing materials itself, while ensureing adsorbance, makes NEW TYPE OF COMPOSITE regneration of adsorbent material program simple, and easy recycling reaches the purpose of economical and efficient.In various types of adsorbents, research worker finds that the metal-oxide with hydrolysising property has good chemical affinity with heavy metal, this quasi-metal oxides includes Mn, Fe, Al, Zn etc., and compare with other metal-oxides, to have specific surface area big because of it for Mn oxide, the features such as isoelectric point, IP is low, and surface hydroxyl is abundant, have the strongest absorbability to the heavy metal in water.And Fe₃O₄Not only there is absorption property, the most certain magnetic, it is possible to use its magnetic reclaims, therefore select MnO₂And Fe₃O₄Mainly comprise composition as composite adsorbing material, make compound after material be not only able to the low-concentration heavy metal treatment effect that had, while can also carry out magnetic recovery.

Summary of the invention

One nucleocapsid structure composite adsorbing material MnO of the present invention₂-Fe₃O₄Preparation method carry out according to the following steps:

(a). under room temperature, by 0.51gKMnO₄Join in the deionized water of 40mL, be added dropwise over the HCl(37wt% of 0.8mL), stir 15min, be subsequently adding 0.35g Fe₃O₄(nanoscale)；

(b). more above-mentioned mixed liquor is transferred to 110 DEG C of reaction 6h in the autoclave of 50mL；

(c). centrifugation, by precipitate deionized water and ethanol cyclic washing 4 times, it is dried 12h at 60 DEG C of vacuum drying ovens；Finally give composite adsorbing material MnO₂-Fe₃O₄。

Accompanying drawing explanation

Fig. 1 is the apparent figure that composite adsorbing material is mixed in water and Magneto separate.

Fig. 2 is for pure compound MnO₂、Fe₃O₄With composite MnO₂-Fe₃O₄FTIR(fourier conversion infrared spectrum analysis, resolution: standard 0.5cm^-1；) comparison collection of illustrative plates.

Fig. 3 is composite MnO₂-Fe₃O₄And Fe₃O₄XRD(X x ray diffraction analysis x) comparison chart.

Fig. 4 is composite MnO₂-Fe₃O₄Scanning electron microscope (SEM) photograph.

Fig. 5 is composite MnO₂-Fe₃O₄Transmission electron microscope picture.

Detailed description of the invention

Now the specific embodiment of the present invention is reported in rear.Embodiment 1, in the present embodiment, core-shell composite material MnO₂-Fe₃O₄Preparation method carry out according to the following steps: (1). under room temperature, by 0.51gKMnO₄Join in the deionized water of 40mL, be added dropwise over the HCl(37wt% of 0.8mL), stir 15min, be subsequently adding 0.35g Fe₃O₄(nanoscale).(2). more above-mentioned mixed liquor is transferred to 110 DEG C of reaction 6h in the autoclave of 50mL.(3). centrifugation, by precipitate deionized water and ethanol cyclic washing 4 times, it is dried 12h at 60 DEG C of vacuum drying ovens, finally gives composite adsorbing material MnO₂-Fe₃O₄(such as Fig. 2 and Fig. 3).

Adsorbing material prepared by present embodiment method is a kind of by MnO₂And Fe₃O₄The material (Fig. 2) being composited, even particle size distribution, at about 70nm (such as Fig. 4)；MnO₂With armorphous existence, (in Fig. 3, XRD figure spectrum does not has MnO₂The existence of peak spectrum)；This composite has nucleocapsid structure (Fig. 5)；This composite has good dispersibility (Fig. 1 is left) and superior Magneto separate (Fig. 1 is right) in water.

Can be by this composite of the experimental verification removal effect to low-concentration heavy metal: in an experiment, Cu in water body²⁺Initial concentration be 10mg/L, the present embodiment composite adsorbing material MnO₂-Fe₃O₄Dosage be 1g/L, final Cu²⁺Clearance be 99.81%.

Claims (1)

1. a nucleocapsid structure composite adsorbing material MnO₂-Fe₃O₄Preparation method, it is characterised in that there is following process and step:

(a). at normal temperatures, by 0.51g KMnO₄Join in the deionized water of 40mL, be added dropwise over the HCl(37wt% of 0.8mL), stir 15min, be subsequently adding 0.35g Fe₃O₄(nanoscale)；

(b). more above-mentioned mixed liquor is transferred to 110 DEG C of reaction 6h in the autoclave of 50mL；

(c). centrifugation, by precipitate deionized water and ethanol cyclic washing 4 times, it is dried 12h at 60 DEG C of vacuum drying ovens；Finally give composite adsorbing material MnO₂-Fe₃O₄。