CN107281999A - A kind of ferriferous oxide/manganese dioxide nano-composite material and preparation method and application - Google Patents
A kind of ferriferous oxide/manganese dioxide nano-composite material and preparation method and application Download PDFInfo
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- CN107281999A CN107281999A CN201710387568.7A CN201710387568A CN107281999A CN 107281999 A CN107281999 A CN 107281999A CN 201710387568 A CN201710387568 A CN 201710387568A CN 107281999 A CN107281999 A CN 107281999A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid 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
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid 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
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid 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 form
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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
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- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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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
- C02F2101/00—Nature of the contaminant
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Abstract
A kind of ferriferous oxide/manganese dioxide nano-composite material and preparation method and application, belongs to technical field of composite materials.Soluble ferrite and manganous salt are added in ethanol water, then sal volatile is added, reaction obtains ferrimanganic compound precursor, and ferrimanganic compound precursor is added in liquor potassic permanganate and reacted, the microballoon with loose structure being made up of nano particle is obtained.For adsorbing the heavy metal ion in water.
Description
Technical field
The present invention relates to a kind of ferriferous oxide/manganese dioxide composite material and preparation method and application, belong to composite wood
Expect technical field.
Background technology
Heavy metal ion content exceeds national security drinking water standard in the underground water in many areas of China, seriously threatens people
Life and health.Nano adsorber heavy metal ion has good removal effect, has there is many kind nanometers at present
Material is applied in water process.
Iron is one of content most abundant element in the earth's crust, and ferro element is environment-friendly, the iron oxide energy of nanostructured
Contaminated place is enough directly applied to without causing secondary pollution.Meanwhile, nano-iron oxide has high specific surface area
With good heavy metal ion compatibility, and cost is low, safety non-toxic, be the most frequently used water pollutant remove material it
One.Widely studied NFeOs includes goethite (alpha-feooh), bloodstone (α-Fe2O3), amorphous hydrated ferric oxide, maghemite
(-Fe2O3), magnetic iron ore (Fe3O4) and iron/iron oxide (Fe@FexOy) etc..In in the past few decades, the manganese oxidation of nanostructured
Thing is also exploited for adsorbing the cation or anionic pollutant such as heavy metal ion, arsenate and phosphate in water.Wherein
Widely studied Mn oxide includes hydrated manganese oxide (HMO) and nanoporous/nano tunnel manganese oxide.Manganese dioxide has
Redox characteristic, can react with water pollutant, and the heavy metal ion oxidation that can adsorb toxicity disaster is also
It is former into the relatively low ion for being more easy to absorption of toxicity.
Composite is prepared using the synergy between each component, is that the feasibility for improving nano material combination property is arranged
Apply.Due to usually containing contents of many kinds of heavy metal ion in underground water, by the way that iron oxide and manganese dioxide are combined, one is prepared
Plant safe and efficient multi-functional material for water treatment significant to reduction preparation cost and simplified technique.Meanwhile, differently
Heavy metal ion in Qu Shui is different, realizes that the regulation of its absorption property also will by simply regulating and controlling the composition of sorbing material
Improve application of the material in water process.
The content of the invention
It is an object of the invention to provide a kind of composite of ferriferous oxide/manganese dioxide and its method
The method that what the present invention was provided prepare ferriferous oxide/manganese dioxide composite material, comprises the following steps：
(1) a certain amount of soluble ferrite and manganous salt are weighed for 2/8~8/2 by the mol ratio of iron and manganese and added
Into the mixed liquor of second alcohol and water, stirring and dissolving obtains solution A；Ferrous salt and manganous salt concentration range are in solution
0.025~0.1mmol/L；The volume ratio of preferred water and ethanol is 7 in the mixed liquor of second alcohol and water:1；
(2) ammonium carbonate is added to the water stirring and dissolving, obtains the ammonium carbonate solution B that concentration is 0.01~0.1mol/L；
(3) under agitation, ammonium carbonate solution B is added to and (preferably rapidly joined, the time that adds is 1~10 s)
In solution A, continue to stir 2~4h, preferably 3h, the precipitation of brown can be obtained after obtaining ferrimanganic compound precursor dispersion liquid, standing
Thing；Washing precipitate, obtains ferrimanganic compound precursor after 60~100 DEG C of dryings；
(4) take after being reacted 10~20 hours in the compound precursor addition liquor potassic permanganate obtained by step (3), separation is washed
Sediment is washed, final product is obtained after 60~100 DEG C of dryings.
In the preparation method, divalent iron salt can mix for one or both of frerrous chloride or green vitriol
Close；Manganese salt can be one or more combinations in manganese sulfate, manganese chloride, manganese nitrate.
The total moles ratio of ammonium carbonate and iron and manganese is 1 in step (3):(1-4), preferably 1:3；
The concentration of step (4) liquor potassic permanganate is 0.02-0.05mol/L；It is preferred that per 10ml potassium permanganate solutions pair
1-300mg compound precursors should be added；
In wherein further step (1), the mol ratio of iron and manganese can obtain compound structure when being Fe/Mn=7/3 is
FeOOH/MnO2；The mol ratio of iron and manganese is Fe/Mn=5:The structure that compound is can obtain when 5 is Fe2O3/MnO2；Fe/Mn=
3:Iron oxide is undefined structure when 7.
Step (1) stirring, temperature is room temperature, and the time is not less than 5min, specially 10-40min；
Ferriferous oxide/manganese dioxide composite material that the present invention is provided be it is a kind of by nano particle constitute have porous knot
The microballoon of structure.
Ferriferous oxide/the manganese dioxide prepared using the above method is used to adsorb the heavy metal ion in water.Such as：Lead from
At least one of son, cadmium ion, mercury ion, arsenic acid radical ion.
The invention provides a kind of safe, simple and economic method for preparing ferriferous oxide/manganese dioxide composite material.
Compared with existing other technologies, have the characteristics that：
1) in the present invention, reaction condition is gentle, can complete at room temperature, and material preparation process is simple, safety, energy consumption
It is low, be easy to implement large-scale production.
2) raw material economics of the invention used, environmental protection, the addition of surfactant is not related to.
3) composite material surface obtained by the present invention is the loose structure being made up of nano particle, thus specific surface area
It is very high.
4) in preparation process of the present invention by simply regulate and control material rate can obtain different institutions constitute ferriferous oxide/
Manganese dioxide composite material
5) ferriferous oxide/manganese dioxide composite material that the present invention is obtained shows excellent synchronization in water treatment procedure
Remove the ability of contents of many kinds of heavy metal ion.
Brief description of the drawings
Fig. 1 is that the X-ray powder diffraction patterns of different Fe/Mn ratios products therefroms is respectively adopted in embodiment 1-3
(XRD).Curve 1,2,3 represents the diffracting spectrum of product resulting when Fe/Mn ratios are 7/3,1/1 and 3/7 respectively.
Fig. 2 shines for the SEM (SEM) of different Fe/Mn ratios products therefroms is respectively adopted in embodiment 1-3
Piece.Wherein picture (a) (b) (c) is respectively the SEM photograph of product resulting when Fe/Mn ratios are 7/3,1/1 and 3/7.
Fig. 3 be respectively adopted in embodiment 1-3 different Fe/Mn ratios products therefroms to pollutant lead ion and arsenate from
The adsorption isothermal curve of son.Wherein figure (a) and (b) are respectively ferriferous oxide/manganese dioxide composite material to lead ion and arsenic acid
The adsorption isothermal curve of root.
Embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Institute
It is conventional method unless otherwise instructed to state method.The raw material can be obtained from open commercial sources unless otherwise instructed.
Embodiment 1
7mmol green vitriols and the chloride hydrate manganese of 3mmol tetra- is taken to add the mixed of 70 milliliters of water and 10 milliliters of ethanol
Close in liquid, stirring and dissolving obtains solution A.30mmol ammonium carbonate is added in 70 milliliters of water, stirring and dissolving obtains solution B.
Under the conditions of stirring at normal temperature, solution B is quickly poured into solution A, continues to stir 3h, obtains ferrimanganic compound precursor dispersion liquid, it is quiet
The sediment of brown can be obtained by postponing.Washing precipitate, obtains ferrimanganic compound precursor standby after 60 DEG C of dryings.200mg ferrimanganics are taken to answer
It is in the liquor potassic permanganate that 0.032M, volume are 10mL after reaction 12 hours, to centrifuge solid that polymer precursor, which adds concentration,
With deionized water by solid washes clean, dried at 60 DEG C, obtain FeOOH/MnO2Brown solid powder.
The sign of nano material：X-ray diffractometer analysis determines FeOOH/MnO2Structure, as a result such as the institute of curve 1 in Fig. 1
Show.
Scanning electron microscopic picture display gained composite is the chondritic of about 2 μm of diameter, and its surface is by nano particle group
Into being loose structure；As a result as shown in Fig. 2 (a).
Embodiment 2
By identical process in embodiment 1, but the addition of reactant green vitriol and four chloride hydrate manganese is equal
For 5mmol.
The sign of nano material：X-ray diffractometer analysis determines Fe2O3/MnO2Structure, as a result such as the institute of curve 2 in Fig. 1
Show.
Scanning electron microscopic picture display gained composite is the chondritic of about 2 μm of diameter, and its surface is by nano particle group
Into surface roughness is small compared with products therefrom in embodiment 1, is loose structure；As a result as shown in Fig. 2 (b).
Embodiment 3
Divide by the addition of identical process in embodiment 1, but reactant green vitriol and four chloride hydrate manganese
Wei not 3mmol and 7mmol.
The sign of nano material：X-ray diffractometer analysis shows that iron oxide is undefined structure, as a result such as curve 3 in Fig. 1
It is shown.
Scanning electron microscopic picture display gained composite is the chondritic of about 2 μm of diameter, and its surface is by nano particle group
Into its surface is made up of nano particle, and surface roughness is small compared with products therefrom in embodiment 2, is loose structure；As a result such as Fig. 2
(c) shown in.
Embodiment 4
Lead ion in ferriferous oxide/manganese dioxide nano-composite material absorption water.With plumbi nitras (Pb (NO3)2) and go from
Sub- water configuration lead ion (Pb2+) concentration be respectively 10-200mg/L lead ion solution for standby.
Various concentrations 20mL Pb is measured respectively2+The aqueous solution, then thereto will add any systems of 5mg embodiments 1-3
Standby gained iron oxide/manganese dioxide nano-composite material.At room temperature after stirring 12h, separation of solid and liquid is carried out to mixed liquor, collects clear
Liquid.Using Pb in inductively coupled plasma atomic emission spectrum detection solution2+Concentration.It is molten according to heavy metal ion before and after absorption
Degree is poor, can calculate each adsorbent to Pb2+Maximal absorptive capacity.As a result it is as shown in table 1.
Embodiment 5
Arsenic acid radical ion in ferriferous oxide/manganese dioxide nano-composite material absorption water.Use natrium arsenicum
(Na2HAsO4.12H2O) and deionized water configuration arsenic acid ion concentration be respectively 10-200mg/L solution for standby.It is specific to inhale
Attached process be the same as Example 4.
As a result it is as shown in table 1.
The absorption testing result of table 1, iron oxide/manganese dioxide nano-composite material
Note：Fe/ in embodiment 1-3 reactants is represented in table 1 with Fe/Mn-3/7, Fe/Mn-1/1 and Fe/Mn-7/3 respectively
Iron oxide/the manganese dioxide nano-composite material obtained when the amount of Mn materials is than being respectively 3/7,1/1 and 7/3.
As it can be seen from table 1 iron oxide/manganese dioxide nano-composite material for providing of the present invention, to heavy metal in water from
Sub- lead ion and arsenic acid radical ion has excellent removal effect, can be used as practical adsorbent for heavy metal.
Claims (8)
1. a kind of preparation method of ferriferous oxide/manganese dioxide composite material, it is characterised in that comprise the following steps：
(1) a certain amount of soluble ferrite and manganous salt are weighed for 2/8~8/2 by the mol ratio of iron and manganese and is added to second
In the mixed liquor of alcohol and water, stirring and dissolving obtains solution A；In solution ferrous salt and manganous salt concentration range be 0.025~
0.1mmol/L；The volume ratio of preferred water and ethanol is 7 in the mixed liquor of second alcohol and water:1；
(2) ammonium carbonate is added to the water stirring and dissolving, obtains the ammonium carbonate solution B that concentration is 0.01~0.1mol/L；
(3) under agitation, ammonium carbonate solution B is added in solution A, continues to stir 2~4h, preferably stir 3h, obtain
To ferrimanganic compound precursor dispersion liquid, the sediment of brown can be obtained after standing；Washing precipitate, obtains iron after 60~100 DEG C of dryings
Manganese compound precursor；
(4) take after being reacted 10~20 hours in the compound precursor addition liquor potassic permanganate obtained by step (3), separating, washing sinks
Starch, obtains final product after 60~100 DEG C of dryings.
2. according to the method for claim 3, it is characterised in that ammonium carbonate solution B is added rapidly in solution A, during addition
Between be 1~10s.
3. according to the method for claim 3, it is characterised in that divalent iron salt is one in frerrous chloride or green vitriol
Plant or two kinds of mixing；Manganese salt is one or more combinations in manganese sulfate, manganese chloride, manganese nitrate.
4. according to the method for claim 3, it is characterised in that the total moles ratio of ammonium carbonate and iron and manganese is 1 in step (3):(1-
4), preferably 1:3.
5. according to the method for claim 3, it is characterised in that the concentration of step (4) liquor potassic permanganate is 0.02-0.05mol/
L；It is preferred that adding 1-300mg compound precursors per 10ml potassium permanganate solutions correspondence.
6. according to the method for claim 3, it is characterised in that the mol ratio of iron and manganese obtains compound when being Fe/Mn=7/3
Structure is FeOOH/MnO2；The mol ratio of iron and manganese is Fe/Mn=5:The structure that compound is obtained when 5 is Fe2O3/MnO2；Fe/
Mn=3:Iron oxide is undefined structure when 7.
7. the application of the composite described in claim 1 or 2, it is characterised in that as adsorbent, for adsorbing the weight in water
Metal ion.
8. according to the method for claim 9, it is characterised in that heavy metal ion is lead ion, cadmium ion, mercury ion, arsenate
At least one of ion.
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Cited By (7)
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| CN110911652A (en) * | 2018-09-17 | 2020-03-24 | 浙江浙能中科储能科技有限公司 | Nano spherical alpha-MnO 2 /Bi 2 O 3 Material, preparation method and application thereof |
| CN112264096A (en) * | 2020-11-23 | 2021-01-26 | 陕西科技大学 | Magnetic Fenton-like catalyst based on chitosan and preparation method and application thereof |
| CN112387246A (en) * | 2020-11-27 | 2021-02-23 | 宁夏医科大学 | Ferroferric oxide-manganese dioxide/molybdenum sulfide complex and preparation method and application thereof |
| CN113786799A (en) * | 2021-09-17 | 2021-12-14 | 辽宁大学 | Preparation method of manganese dioxide/ferric oxide hydroxide loaded three-dimensional silicon dioxide adsorbent and application of adsorbent in adsorption of As (III) |
| CN114534683A (en) * | 2022-02-14 | 2022-05-27 | 华侨大学 | Core-shell type magnetic nano material and preparation method and application thereof |
| CN115029139A (en) * | 2022-04-29 | 2022-09-09 | 中南大学 | Heavy metal contaminated soil stabilizing agent and preparation method and application thereof |
| CN115301194A (en) * | 2022-07-22 | 2022-11-08 | 南开大学 | Nano composite material and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110911652A (en) * | 2018-09-17 | 2020-03-24 | 浙江浙能中科储能科技有限公司 | Nano spherical alpha-MnO 2 /Bi 2 O 3 Material, preparation method and application thereof |
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| CN112264096A (en) * | 2020-11-23 | 2021-01-26 | 陕西科技大学 | Magnetic Fenton-like catalyst based on chitosan and preparation method and application thereof |
| CN112264096B (en) * | 2020-11-23 | 2023-02-03 | 陕西科技大学 | Magnetic Fenton-like catalyst based on chitosan and preparation method and application thereof |
| CN112387246A (en) * | 2020-11-27 | 2021-02-23 | 宁夏医科大学 | Ferroferric oxide-manganese dioxide/molybdenum sulfide complex and preparation method and application thereof |
| CN113786799A (en) * | 2021-09-17 | 2021-12-14 | 辽宁大学 | Preparation method of manganese dioxide/ferric oxide hydroxide loaded three-dimensional silicon dioxide adsorbent and application of adsorbent in adsorption of As (III) |
| CN114534683A (en) * | 2022-02-14 | 2022-05-27 | 华侨大学 | Core-shell type magnetic nano material and preparation method and application thereof |
| CN114534683B (en) * | 2022-02-14 | 2023-12-12 | 华侨大学 | Core-shell type magnetic nano material and preparation method and application thereof |
| CN115029139A (en) * | 2022-04-29 | 2022-09-09 | 中南大学 | Heavy metal contaminated soil stabilizing agent and preparation method and application thereof |
| CN115029139B (en) * | 2022-04-29 | 2023-12-05 | 中南大学 | Heavy metal contaminated soil stabilization medicament and preparation method and application thereof |
| CN115301194A (en) * | 2022-07-22 | 2022-11-08 | 南开大学 | Nano composite material and preparation method and application thereof |
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