CN114436389A - Preparation method and application of magnetically separable zero-valent aluminum-ferroferric oxide compound - Google Patents

Preparation method and application of magnetically separable zero-valent aluminum-ferroferric oxide compound Download PDF

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Publication number
CN114436389A
CN114436389A CN202210129711.3A CN202210129711A CN114436389A CN 114436389 A CN114436389 A CN 114436389A CN 202210129711 A CN202210129711 A CN 202210129711A CN 114436389 A CN114436389 A CN 114436389A
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zero
ferroferric oxide
valent aluminum
ball milling
aluminum
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王文豪
赵子轩
马青
甄树聪
张婷婷
方学友
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Yancheng Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/70Treatment of water, waste water, or sewage by reduction
    • C02F1/705Reduction by metals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009Magnetic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/22Chromium or chromium compounds, e.g. chromates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Compounds Of Iron (AREA)

Abstract

The invention discloses a preparation method and application of a magnetically separable zero-valent aluminum-ferroferric oxide compound, wherein the preparation method of the zero-valent aluminum-ferroferric oxide compound comprises the following steps: mixing micron zero-valent aluminum and nano ferroferric oxide, pouring the mixture into a ball milling tank filled with zirconia balls with different particle diameters, sealing the ball milling tank, putting the ball milling tank into a planetary ball mill for fixing and pressing without vacuum extraction and inert gas protection, carrying out ball milling, regularly changing the clockwise and anticlockwise rotation directions, adding a magnetic field outside the tank after ball milling, inverting the tank to separate the zirconia balls by gravity, and collecting the residual product, namely the zero-valent aluminum-ferroferric oxide compound. The preparation method is carried out at normal temperature and normal pressure, is simple to operate, short in time consumption and suitable for industrial production; the zero-valent aluminum-ferroferric oxide compound overcomes the defect of surface passivation of zero-valent aluminum, the zero-valent aluminum passivated again after practical application is convenient to recover and restore activity, and the compound has good removal efficiency on heavy metal Cr (VI) in water within a wide pH range.

Description

Preparation method and application of magnetically separable zero-valent aluminum-ferroferric oxide compound
Technical Field
The invention belongs to the technical field of water treatment functional materials, and particularly relates to a preparation method and application of a magnetically separable zero-valent aluminum-ferroferric oxide compound.
Background
The heavy metal Cr (VI) is one of typical heavy metal pollutants in water, and is reduced into low-toxicity Cr (III) which is one of common means, however, the common reducing agent cannot effectively reduce Cr (VI) under neutral conditions, so that the toxicity of Cr (VI) is difficult to eliminate. The zero-valent aluminum can provide electrons under the conditions of acid and alkali to play a role in reduction due to the amphoteric property of the zero-valent aluminum, so that the zero-valent aluminum is applied to the field of water treatment, and researches show that the zero-valent aluminum can effectively remove organic pollution and inorganic pollutants such As Cr (VI), As (III) and the like in water under the wide pH condition. But the low oxidation-reduction potential of the zero-valent aluminum makes the aluminum easy to react with O in the air2Or H2O reacts to form a compact oxide layer (Al) on the surface2O3) And the electron conduction is seriously hindered, and the removal efficiency of the electron conduction on pollutants in water is greatly reduced.
In order to destroy the surface passivation layer of the zero-valent aluminum and overcome the defects of the zero-valent aluminum in practical application, researchers try a series of pre-activation (acid washing, ball milling and the like) measures or compound the zero-valent aluminum with other substances based on the principle of a primary battery, so that the electronic conductivity is effectively enhanced, and the removal efficiency of the zero-valent aluminum to pollutants is improved. However, during the use of the preactivated zero-valent aluminum or the zero-valent aluminum-based composite, as the reaction occurs, the surface of the composite can be covered by the generated (hydro) aluminum oxide, so that the internal electrons can not be released, and the corrosion process of the composite is stopped and is inactivated. Therefore, how to rapidly recover and reactivate the passivated zero-valent aluminum after use is an important problem in the field of water treatment.
At present, the solid substances can be separated from the liquid phase rapidly by means of magnetization. Therefore, the rapid separation and recovery of the zero-valent aluminum from the water can be realized by doping or loading the magnetic substance in the zero-valent aluminum under the action of an external magnetic field. The more common aluminum-based composite with magnetism is iron-aluminum bimetal, but the iron-aluminum bimetal has higher activity, which causes a plurality of side reactions, and the iron-aluminum bimetal is generally prepared by a chemical deposition method, which has the following disadvantages: (1) zero-valent aluminum needs acid washing activation, which causes the consumption of the zero-valent aluminum; (2) the preparation process is relatively complicated; (3) a large amount of wastewater is generated in the preparation process.
Disclosure of Invention
Aiming at the defects pointed out in the background technology, the invention provides a preparation method and application of a magnetically separable zero-valent aluminum-ferroferric oxide compound, and aims to solve the problems in the prior art in the background technology.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a magnetically separable zero-valent aluminum-ferroferric oxide compound comprises the steps of firstly mixing micron-sized zero-valent aluminum and nano-sized ferroferric oxide, pouring the obtained mixed raw materials into a ball milling tank filled with zirconia balls with different particle sizes, capping the ball milling tank, carrying out ball milling, changing the forward and reverse rotation directions of the ball milling once every 5min, adding a magnetic field outside the ball milling tank after ball milling, inverting the tank to separate the zirconia balls by gravity, and obtaining a residual product, namely the zero-valent aluminum-ferroferric oxide compound in the tank.
Preferably, the mass ratio of the micron zero-valent aluminum to the nano ferroferric oxide is as follows: 4: 1-1: 2, wherein when the mass ratio is 2:1, the zero-valent aluminum-ferroferric oxide compound has the best effect of removing Cr (VI).
Preferably, the particle size of the micron zero-valent aluminum is 10-50 μm, and the particle size of the nano ferroferric oxide is 150-250 nm.
Preferably, the rotating speed is 200r/min-350r/min in the ball milling process; the ball milling time is 0.5h-2.0 h. But comprehensively considering the product performance, time and energy consumption cost, and selecting the rotation speed of 300r/min and the ball milling time of 1.5h as the optimal ball milling factor of the synthetic material.
The invention further provides application of the prepared magnetically separable zero-valent aluminum-ferroferric oxide compound, and the zero-valent aluminum-ferroferric oxide compound can effectively remove Cr (VI) in water. Removing Cr (VI) in water, performing magnetic separation and recovery by using an external magnetic field, and performing ball milling on the passivated product after recovery, thereby recovering the activity of removing Cr (VI) in water.
Compared with the defects and shortcomings of the prior art, the invention has the following beneficial effects:
(1) the raw materials for preparing the zero-valent aluminum-ferroferric oxide compound are low in price and convenient to obtain.
(2) The preparation method of the zero-valent aluminum-ferroferric oxide compound provided by the invention is carried out at normal temperature and normal pressure, the product can be obtained by ball milling, the preparation process does not need vacuum pumping treatment or inert gas protection, the operation is simple, the time consumption is short, and the preparation method is suitable for industrial production.
(3) The zero-valent aluminum-ferroferric oxide compound overcomes the defect of surface passivation of the zero-valent aluminum, and the zero-valent aluminum which is passivated again after practical application can be magnetically separated and recovered.
(4) Compared with the existing micron zero-valent aluminum for removing pollutants in water, the zero-valent aluminum-ferroferric oxide greatly improves the removal efficiency of the pollutants, and can absorb and reduce heavy metals Cr (VI) in the water in a wide pH range.
Drawings
Fig. 1(a) and (b) are scanning electron micrographs of zerovalent aluminum and zerovalent aluminum-ferroferric oxide provided in the embodiment of the present invention, respectively, and fig. 1(c) and (d) are scanning electron micrographs of zerovalent aluminum-ferroferric oxide at different magnifications.
Fig. 2 is a hysteresis loop diagram of a compound of ferroferric oxide and zero-valent aluminum-ferroferric oxide according to an embodiment of the present invention.
FIG. 3 is a diagram illustrating the effect of removing Cr (VI) from a mixture of Al-zero, Fe-oxide and Fe-zero-valent Al-Fe-oxide.
Fig. 4 is a graph of the effect of the zerovalent aluminum-ferroferric oxide composite on removing cr (vi) under different initial pH conditions according to the embodiment of the present invention.
Fig. 5 is a graph showing the trend of the concentrations of cr (vi) and total chromium along with the reaction time in the process of removing cr (vi) from zerovalent aluminum-ferrosoferric oxide according to the embodiment of the present invention.
Fig. 6 is an XPS result graph (fig. 6(a)) before and after a Cr (vi) removal reaction of zerovalent aluminum-ferrosoferric oxide and an XPS result graph (fig. 6(b)) of Cr in particles after the reaction, which are provided in an embodiment of the present invention.
FIG. 7 is a performance diagram of the zero-valent aluminum-ferroferric oxide composite according to the present invention for Cr (VI) removal by circulation, magnetic separation, recovery, and ball milling.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Firstly, preparing a magnetically separable zero-valent aluminum-ferroferric oxide compound
1. Mixing about 20 mu m of zero-valent aluminum and about 200nm of ferroferric oxide, wherein the mass ratio of the zero-valent aluminum to the ferroferric oxide is 2:1, the total weight is 3g, pouring the mixed raw materials into a 50mL ball milling tank filled with zirconia balls with different particle sizes, wherein the zirconia balls with different particle sizes are 1mm, 5mm and 10mm, and adding according to the mass ratio of 3g to 15g to 10 g. And (4) capping the ball milling tank, not extracting vacuum, not arranging inert gas protection, and then symmetrically putting the ball milling tank into a planetary ball mill for fixing and pressing.
2. Setting a ball milling program: the rotating speed is 300r/min, the ball milling time is 1.5h, and the ball milling forward and backward rotating direction is changed once every 5 min.
3. Starting the equipment, carrying out ball milling at normal temperature, adding a magnetic field outside a ball milling tank body after ball milling, inverting the tank body to separate the zirconia balls by gravity, and collecting the rest product in the tank, namely the zero-valent aluminum-ferroferric oxide compound for later use.
SEM test is carried out on the prepared zero-valent aluminum-ferroferric oxide compound, meanwhile SEM test is carried out on untreated zero-valent aluminum, and the result is shown in figure 1, and it can be seen that ferroferric oxide nano particles are covered on the surface of the zero-valent aluminum. The hysteresis loops of the ferriferrous oxide and the zerovalent aluminum-ferriferrous oxide compound are measured respectively, as shown in fig. 2, it can be seen that the zerovalent aluminum-ferriferrous oxide compound has a certain magnetic responsiveness, and the magnetic attraction effect of the magnetic zerovalent aluminum-ferriferrous oxide compound can be seen visually from the photograph of fig. 2.
Method for removing Cr (VI) in water by using secondary and zero-valent aluminum-ferroferric oxide compound
1. Preparing 200mL of Cr (VI) solution with the initial concentration of 10mg/L and 10mM sodium chloride ion background by using analytically pure potassium dichromate, pouring the prepared solution into a three-neck flask, removing dissolved oxygen in the solution by using nitrogen and continuously aerating the nitrogen, adding 3g/L of zero-valent aluminum-ferroferric oxide compound into the solution, and then mechanically stirring (the room temperature is 25 +/-1 ℃, and the rotating speed is 300 r/min).
2. Taking about 2mL of water sample by using a 5mL syringe at different time intervals, filtering the water sample by using a 0.22-micron acetate fiber membrane, collecting the water sample in a 10mL centrifuge tube, and then carrying out quantitative analysis by using an ultraviolet spectrophotometry; meanwhile, untreated zero-valent aluminum and ferroferric oxide are used as controls for the test. The results are shown in fig. 3, so that only a small amount of Cr (VI) can be removed in 50min by using the single zero-valent aluminum and the single ferroferric oxide, but 10mg/L of Cr (VI) can be completely removed in 30min by using the magnetic zero-valent aluminum-ferroferric oxide composite prepared by the invention, which indicates that the high activity of the zero-valent aluminum-ferroferric oxide composite can effectively remove the Cr (VI) in the water.
3. The initial pH values of the Cr (VI) solution are adjusted to 3.0, 5.0, 7.0, 9.0 and 11.0 by using sodium hydroxide and hydrochloric acid, and the test process for removing Cr (VI) in water is repeated, the removal result is shown in fig. 4, and it can be seen that within 50min, the zero-valent aluminum-ferroferric oxide compound can completely remove Cr (VI) with different initial pH values, which indicates that the zero-valent aluminum-ferroferric oxide compound can remove inorganic pollutants such as Cr (VI) in water within a wide pH range.
4. FIG. 5 shows the variation of Cr (VI) and total chromium concentration with reaction time during the process of removing Cr (VI) from a zero-valent aluminum-ferroferric oxide, FIG. 6 shows XPS results before and after the reaction of removing Cr (VI) from a zero-valent aluminum-ferroferric oxide and XPS results of Cr in particles after the reaction, and FIGS. 5 and 6 show that Cr (VI) is removed by reduction from a zero-valent aluminum-ferroferric oxide compound.
5. Fig. 7 is a graph of the performance of the zero-valent aluminum-ferroferric oxide compound for removing cr (vi) by circulation and removing cr (vi) by magnetic separation, recovery and ball milling, and it can be seen that the efficiency of the zero-valent aluminum-ferroferric oxide compound for removing cr (vi) is reduced after three times of circulation, but the efficiency of the zero-valent aluminum-ferroferric oxide compound for removing cr (vi) can be recovered after recovery and ball milling.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (6)

1. A preparation method of a magnetically separable zero-valent aluminum-ferroferric oxide compound is characterized by firstly mixing micron zero-valent aluminum and nano ferroferric oxide, pouring the obtained mixed raw materials into a ball milling tank filled with zirconia balls with different particle sizes, capping the ball milling tank, then carrying out ball milling, changing the ball milling in the forward and reverse rotation direction once every 5min, adding a magnetic field outside the ball milling tank after ball milling, inverting the tank body to separate the zirconia balls by gravity, and obtaining the residual product, namely the zero-valent aluminum-ferroferric oxide compound, in the tank.
2. The preparation method of the magnetically separable zero-valent aluminum-ferroferric oxide compound according to claim 1, wherein the mass ratio of the micro-zero-valent aluminum to the nano-ferroferric oxide is as follows: 4: 1-1: 2.
3. The preparation method of the magnetically separable zero-valent aluminum-ferroferric oxide compound according to claim 2, wherein the mass ratio of the micron zero-valent aluminum to the nano ferroferric oxide is as follows: 2:1.
4. The method for preparing a magnetically separable zero-valent aluminum-ferroferric oxide compound according to claim 1, wherein the particle size of the micron zero-valent aluminum is about 10-50 μm, and the particle size of the nano ferroferric oxide is about 150-250 nm.
5. The method for preparing a magnetically separable zero-valent aluminum-ferroferric oxide composite according to claim 4, wherein during the ball milling process, the rotation speed is 200r/min to 350 r/min; the ball milling time is 0.5h-2.0 h.
6. The application of the magnetically separable zero-valent aluminum-ferroferric oxide compound according to any one of claims 1 to 5, wherein the application of the zero-valent aluminum-ferroferric oxide compound in the removal of Cr (VI) in water is characterized in that the zero-valent aluminum-ferroferric oxide compound is separated and recovered under the action of an external magnetic field in the process of removing Cr (VI) in water for reuse, and the activity of the passivated products is recovered by means of ball milling again after recovery.
CN202210129711.3A 2022-02-11 2022-02-11 Preparation method and application of magnetically separable zero-valent aluminum-ferroferric oxide compound Withdrawn CN114436389A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102623692A (en) * 2012-03-21 2012-08-01 新疆大学 Method for preparing anode material of ferroferric oxide and carbon composite lithium battery
KR20130037131A (en) * 2011-10-05 2013-04-15 에코랜드 주식회사 Environment enhanced functional soil paving method applying oxidation and reduction
CN108793371A (en) * 2018-06-25 2018-11-13 河南师范大学 A kind of Na2EDTA couples Fe0/Fe3O4The method that composite material removes Cr (VI) in water body
CN108862537A (en) * 2018-06-25 2018-11-23 河南师范大学 Hydroxy functionalized Modified lift Fe0/Fe3O4Method of the composite material to Cr in waste water (VI) removal capacity
CN110282717A (en) * 2019-07-03 2019-09-27 中国海洋大学 A kind of method of mechanical ball mill activation zeroth order aluminium removal water pollutant
CN111995035A (en) * 2020-08-11 2020-11-27 中国海洋大学 Mechanochemical dry preparation method and application of all-solid-phase Fenton reagent
CN113292150A (en) * 2021-05-01 2021-08-24 河南师范大学 Preparation of Fe by ball milling-calcining method3O4-CuxMethod for degrading LVF in organic wastewater by using O
CN113976117A (en) * 2021-10-28 2022-01-28 南京大学 Preparation method and application of zero-valent aluminum/iron-containing clay composite material for catalyzing persulfate to oxidize organic matters

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20130037131A (en) * 2011-10-05 2013-04-15 에코랜드 주식회사 Environment enhanced functional soil paving method applying oxidation and reduction
CN102623692A (en) * 2012-03-21 2012-08-01 新疆大学 Method for preparing anode material of ferroferric oxide and carbon composite lithium battery
CN108793371A (en) * 2018-06-25 2018-11-13 河南师范大学 A kind of Na2EDTA couples Fe0/Fe3O4The method that composite material removes Cr (VI) in water body
CN108862537A (en) * 2018-06-25 2018-11-23 河南师范大学 Hydroxy functionalized Modified lift Fe0/Fe3O4Method of the composite material to Cr in waste water (VI) removal capacity
CN110282717A (en) * 2019-07-03 2019-09-27 中国海洋大学 A kind of method of mechanical ball mill activation zeroth order aluminium removal water pollutant
CN111995035A (en) * 2020-08-11 2020-11-27 中国海洋大学 Mechanochemical dry preparation method and application of all-solid-phase Fenton reagent
CN113292150A (en) * 2021-05-01 2021-08-24 河南师范大学 Preparation of Fe by ball milling-calcining method3O4-CuxMethod for degrading LVF in organic wastewater by using O
CN113976117A (en) * 2021-10-28 2022-01-28 南京大学 Preparation method and application of zero-valent aluminum/iron-containing clay composite material for catalyzing persulfate to oxidize organic matters

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