CN106268616A - Based on retaining Armco magnetic iron manganio cubic nanometer material and application thereof prepared by template - Google Patents
Based on retaining Armco magnetic iron manganio cubic nanometer material and application thereof prepared by template Download PDFInfo
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- CN106268616A CN106268616A CN201610655193.3A CN201610655193A CN106268616A CN 106268616 A CN106268616 A CN 106268616A CN 201610655193 A CN201610655193 A CN 201610655193A CN 106268616 A CN106268616 A CN 106268616A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
- B01J20/02—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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- 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
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/28009—Magnetic properties
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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Abstract
The invention belongs to environment and Material Field, be specifically related to a kind of based on retaining Armco magnetic iron manganio cubic nanometer material and application thereof prepared by template.The present invention is with three hydration six cyanogen ferrum (II) acid potassium (K4[Fe(CN)6]·3H2O), polyvinylpyrrolidone K 30, the nanometer Prussian Blue of hydrochloric acid synthesis of cubic structure, then by mix different amounts of KMnO4As Mn source, by centrifugation, wash sample, after drying it is sintered, finally give Armco magnetic iron manganio cubic nanometer material.The Armco magnetic iron manganio cubic nanometer material that the present invention prepares, it is possible to the Pb in absorption industrial wastewater effectively2+, Pb in realizing active adsorption waste liquid2+While, it is easy to and the separation that disposes waste liquid, it is easy to reclaim, waste liquid is not resulted in secondary pollution.Its preparation method is simple, with low cost, has good economic benefit and environmental benefit.
Description
Technical field
The invention belongs to environment and Material Field, be specifically related to a kind of Armco magnetic iron manganio prepared based on reservation template and stand
Side's nano material and application thereof.
Background technology
Nowadays, along with the progress and development of science and technology, the living standard of the mankind is more and more higher, but water environment is heavy metal-polluted
Dye increases the weight of the most day by day.Therefore find the heavy metal ion during effective method disposes waste liquid, become problem demanding prompt solution.Use
It is a kind of effective means that the granular materials of hollow microsize or Nano type carries out absorption.Because the knot that granular materials is unique
Structure makes it have good application prospect in many fields.
In recent years, nanometer Fe2O3Because having, surface charge is high, specific surface area is big, heavy metal has the strongest energy of adsorption
Power, wide material sources, toxicity are little, be difficult to cause environment the features such as secondary pollution, and by the extensive concern of researcher, are inhaling
The fields such as attached, catalysis, air-sensitive are widely used.And for Mn oxide, though it can effective weight in Adsorption water
Metal ion, but owing to particle diameter is less, be easy to run off so that it is apply limited.
In the prior art, formwork structure is often some Organic Ingredientss so that sample can be to ring during using
Secondary pollution is caused in border.And Prussian blue (metal organic frame) is as the template of Armco magnetic iron manganio cubic nanometer structural material,
Then do not result in secondary pollution.And, Prussian blue have the best stereoeffect, in many territories
To relatively broad application, utilizing the Prussian blue iron sesquioxide as templated synthesis, this material still is able to keep Prussia
Blue cubic structure, adulterate different Mn2+, obtained iron sesquioxide/Mn oxide, it still is able to keep cubic structure.I
Prepared Prussian blue by hydro-thermal method, and by mixing the Mn of different content, obtain mixing manganese under different Fe, Mn molar ratio
Modified Prussian blue sample, finally, is sintered it, then can obtain Armco magnetic iron manganio cubic nanometer structural material.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of based on retaining Armco magnetic iron prepared by template
Manganio cubic nanometer material and application thereof.The present invention utilizes the Prussian blue Armco magnetic iron manganio cubic nanometer material as templated synthesis
Material can keep Prussian blue cubic structure, and Pb in active adsorption waste liquid well2+, thus solution Organic substance is as mould
The secondary pollution problem that plate synthetic adsorbent is in use caused.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of based on retaining Armco magnetic iron manganio cubic nanometer material prepared by template, comprise the following steps:
(1) preparation of the nanometer Prussian Blue template of cubic structure:
A certain amount of three hydration six cyanogen ferrum (II) acid potassium and polyvinylpyrrolidone are put in beaker, then adds in beaker
Aqueous hydrochloric acid solution, obtains mixed system；Then mixed system stirring is completely dissolved to raw material, obtains mixed solution；Again will mixing
Solution supersound process 30 minutes；Then gained solution is poured in reactor, react 24 h in 80 DEG C；Finally by reactor
Sample centrifuge washing, 70 DEG C be dried 12 h, i.e. obtain Prussian blue template；The concentration of aqueous hydrochloric acid solution is 0.1 mol/L,
Consumption is 50 mL；Polyvinylpyrrolidone model is K-30, and consumption is 3.8 g；The consumption of three hydration six cyanogen ferrum (II) acid potassium is
0.11 g；
(2) preparation of Armco magnetic iron manganio cubic nanometer structural material:
By dispersed to ethanol solution for the Prussian blue template obtained by (1), stirring is navy blue to solution, obtains mixing
Solution；Then potassium permanganate solution is poured in mixed solution slowly, stir 1 h；Then it is centrifuged reactant liquor separating,
Washing；Sample after washing is put into and baking oven is incubated at 70 DEG C 12 h dries, obtain mixing modified Prussian blue of manganese；
Finally, the Prussian blue of manganese modification of mixing of gained is put in Muffle furnace, is incubated 6 hours at 350 DEG C-650 DEG C, heating rate
It is 0.3 DEG C/min-0.5 DEG C/min, finally gives the Armco magnetic iron manganio cubic nanometer structural material retaining template.
Wherein, the concentration of potassium permanganate solution is 1g/L, and in ethanol solution, the volume ratio of deionized water and ethanol is: 3:2
~8:2。
In obtained Armco magnetic iron manganio cubic nanometer material, ferrum, the mol ratio of manganese are 1:1 ~ 10:1.
The beneficial effects of the present invention is:
1) present invention uses the Prussian blue preparation being combined cubic nanometer structural material as templated synthesis Armco magnetic iron manganio, due to
The incorporation of Mn can control surface topography so that material can keep Prussian blue had cubic structure；Institute after sintering
The Armco magnetic iron Mn-based material cube porous obtained, has preferable absorption property, and due to ferromagnetic existence so that it is can
Magnetic separation technique is utilized to propose from waste liquid, it is simple to reclaim, and do not cause secondary pollution；
2) equipment and material required for the preparation method of the present invention are easily obtained, and technological operation is simple, and process conditions are uncomplicated,
There is low cost, safety, the advantage that efficiency is high, it is easy to popularization and application.
Accompanying drawing explanation
Fig. 1 is the Prussian blue microscopic appearance of undoped sintering processes in the implementation case；
Fig. 2 is Prussian blue in comparative example 1 to sinter the Fe obtained at 650 DEG C2O3Scanning microgram；
The microscopic appearance of the Armco magnetic iron manganio cubic nanometer material of 650 DEG C of sintering when Fig. 3 is Fe:Mn=1:1 in embodiment 1；
Fig. 4 is Fe:Mn=10:1 in embodiment 2, the unsintered Prussian blue microscopic appearance mixing manganese modification；
Fig. 5 is Fe:Mn=10:1 in embodiment 2, the microscopic appearance of the Armco magnetic iron manganio cubic nanometer material of 650 DEG C of sintering；
Fig. 6 is Armco magnetic iron manganio nano material (Fe:Mn=1:1(s) in Application Example 1), mix the Prussian blue (Fe:Mn after manganese
=1:1(I), Fe:Mn=10:1(I)) and the Prussian blue Fe sintered into for template2O3These four material adsorbs Pb according to it2+
The scattergram that effect is drawn；
Fig. 7 is Armco magnetic iron manganio nano material (Fe:Mn=1:1(s) in Application Example 2), mix the Prussian blue (Fe:Mn after manganese
=1:1(I), Fe:Mn=10:1(I)) and the Prussian blue Fe sintered into for template2O3These four material adsorbs Zn according to it2+
The scattergram that drawn of effect；
Fig. 8 is Armco magnetic iron manganio nano material (Fe:Mn=1:1(s) in Application Example 3), mix the Prussian blue (Fe:Mn after manganese
=1:1(I), Fe:Mn=10:1(I)), the Prussian blue Fe sintered into for template2O3Fe with commercial use2O3, adsorb according to it
Pb2+、Zn2+The scattergram that drawn of effect；
After Fig. 9 is liquid waste processing, magnetic separation technique is utilized to process forward and backward design sketch.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing i.e. embodiment, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.If additionally, technical characteristic involved in each embodiment of invention described below
The conflict that do not constitutes each other just can be in conjunction with.
Embodiment 1
A kind of based on retaining Armco magnetic iron manganio cubic nanometer material prepared by template, concretely comprise the following steps:
1) preparation Prussian blue (PB):
(K4[Fe(CN)6]·3H2O), PVP, hydrochloric acid, mix and blend, in yellow, it is carried out ultrasonic 30 min process after, will
Solution is poured in water heating kettle 80 DEG C into and is incubated 24 hours, and finally by the sample centrifuge washing in reactor, 70 DEG C are dried 12 h, i.e.
Obtain Prussian blue template；
It is 2) Prussian blue (PB) that to mix manganese modified:
By dispersed for the 0.05 Prussian blue sample of g to (volume ratio of deionized water and ethanol is 8:2) in ethanol solution, stir
Mixing to solution is navy blue, adds a certain amount of potassium permanganate solution (1g/L) prepared in advance, stirs 1 hour, wash sample, is dried
Obtain mixing the Prussian blue of manganese modification；Wherein the mol ratio of Fe, Mn is 1:1；
3) the ferrimanganic base (Fe that manganese is modified is mixed2O3/KMn8O16) synthesis:
Install the sample obtained in (2) with monkey and build, putting it in Muffle furnace, heating rate is 0.5 DEG C/
Min, at 650 DEG C, sinters 6h.Finally give and mix the ferrimanganic base (Fe that manganese is modified2O3/ KMn8O16).
Embodiment 2
A kind of based on retaining Armco magnetic iron manganio cubic nanometer material prepared by template, concretely comprise the following steps:
1) preparation Prussian blue (PB):
(K4[Fe(CN)6]·3H2O), PVP, hydrochloric acid, mix and blend, in yellow, it is carried out ultrasonic 30 min process after, will
Solution is poured in water heating kettle 80 DEG C into and is incubated 24 hours, and finally by the sample centrifuge washing in reactor, 70 DEG C are dried 12 h, i.e.
Obtain Prussian blue template；
It is 2) Prussian blue (PB) that to mix manganese modified:
By dispersed for the 0.05 Prussian blue sample of g to (volume ratio of deionized water and ethanol is 8:2) in ethanol solution, stir
Mixing to solution is navy blue, adds a certain amount of potassium permanganate solution (1g/L) prepared in advance, stirs 1 hour, wash sample, is dried
Obtain mixing the Prussian blue of manganese modification；Wherein the mol ratio of Fe, Mn is 10:1；
3) the ferrimanganic base (Fe that manganese is modified is mixed2O3/ KMn8O16) synthesis:
Install the sample obtained in (2) with monkey and build, putting it in Muffle furnace, heating rate is 0.5 DEG C/
Min, at 650 DEG C, sinters 6h.Finally give and mix the ferrimanganic base (Fe that manganese is modified2O3/ KMn8O16).
Comparative example 1
A kind of Fe2O3Preparation method, concretely comprise the following steps:
1) preparation Prussian blue (PB):
(K4[Fe(CN)6]·3H2O), PVP, hydrochloric acid, mix and blend, in yellow, it is carried out ultrasonic 30 min process after, will
Solution is poured in water heating kettle 80 DEG C into and is incubated 24 hours, and finally by the sample centrifuge washing in reactor, 70 DEG C are dried 12 h, i.e.
Obtain Prussian blue template；
2) sintering processes of Prussian blue template:
Install the sample obtained in (1) with monkey and build, putting it in Muffle furnace, heating rate is 0.5 DEG C/
Min, at 650 DEG C, sinters 6h.Finally give cubic Fe2O3。
Adsorption experiment
Application Example 1
Weigh the sample (Fe that 10 mg comparative examples 1 prepare respectively2O3), and embodiment Fe:Mn=10:1(I), Fe:Mn=1:1
(I) mix modified Prussian blue of manganese, Fe:Mn=1:1(s) Armco magnetic iron manganio cubic nanometer material；Compound concentration is 40ppm
Self-control Pb2+Solution；
Above four kinds of samples are made by oneself Pb respectively with 50 ml, 40 ppm2+Solution mixes, stirring；Start at adsorption experiment respectively
After 1 min, 5 min, 10 min, 15 min, 30 min, 45 min, 60 min be sampled, be then placed in centrifuge,
Rotating speed is 12000 r/min, centrifugal 2 min；Centrifugal liquid carries out Atomic Absorption test, and the sampling of each time period surveys three respectively
Secondary, take its meansigma methods.
Application Example 2
Weigh the sample (Fe that 10 mg comparative examples 1 prepare respectively2O3), and Fe:Mn=10:1(I), Fe:Mn=1:1(I) mix
Modified Prussian blue of manganese, Fe:Mn=1:1(s) Armco magnetic iron manganio cubic nanometer material；Compound concentration is the self-control of 40 ppm
Zn2+Solution；
Above four kinds of samples are made by oneself Zn respectively with 50 ml, 40 ppm2+Solution mixes, stirring；Start at adsorption experiment respectively
After 1 min, 5 min, 10 min, 15 min, 30 min, 45 min, 60 min be sampled, be then placed in centrifuge,
Rotating speed is 12000 r/min, centrifugal 2 min；Finally, after being diluted the solution after centrifugation processing (diluting five times),
Carrying out Atomic Absorption test, the sampling of each time period is surveyed three times respectively, takes its meansigma methods.
Application Example 3
Weigh the sample (Fe that 10 mg comparative examples 1 prepare respectively2O3), and Fe:Mn=10:1(I), Fe:Mn=1:1(I) mix
Modified Prussian blue of manganese, Fe:Mn=1:1(s) Armco magnetic iron manganio cubic nanometer material, and the Fe of commercial use2O3；Preparation
Pb2+、Zn2+Concentration is the mixed solution of 40ppm；
Above five kinds of samples are made by oneself Pb respectively with 50 ml, 40 ppm2+、Zn2+Mixed solution mixes, stirring；Respectively in absorption
Experiment start after 1 min, 5 min, 10 min, 15 min, 30 min, 45 min, 60 min be sampled, be then placed in from
In scheming, rotating speed is 12000 r/min, centrifugal 2 min；First centrifugal liquid is carried out Pb2+Mensuration；Then centrifugal liquid is carried out dilute
After releasing process (diluting five times), then carry out Zn2+Mensuration.
As it will be easily appreciated by one skilled in the art that the preferred embodiments that the foregoing is only the present invention, not in order to limit
The present invention processed, all any amendment, equivalent and improvement made within the spirit and principles in the present invention, should be included in this
Within the protection domain of invention.
Claims (8)
1. the method for the Armco magnetic iron manganio cubic nanometer material prepared based on reservation template, it is characterised in that: general cube
The nanometer Prussian Blue of structure is dispersed to ethanol solution, and stirring to mixed solution is navy blue；Then by potassium permanganate
Solution adds to mixed solution, under agitation reacts 1 h；Then it is centrifuged reactant liquor separating, washing, after washing
Sample is dried 12 h at 70 DEG C, obtains mixing the Prussian blue of manganese modification；Then Muffle is put into by mixing the Prussian blue of manganese modification
In stove, being incubated 6 hours at 350 DEG C-650 DEG C, heating rate is 0.3 DEG C/min-0.5 DEG C/min, obtains Armco magnetic iron manganio and stands
Side's nano material；In wherein obtained nano material, ferrum, the mol ratio of manganese are 1:1 ~ 10:1.
The most according to claim 1 a kind of based on the side retaining Armco magnetic iron manganio cubic nanometer material prepared by template
Method, it is characterised in that: in described ethanol solution, the volume ratio of deionized water and ethanol is: 3:2 ~ 8:2.
The most according to claim 1 a kind of based on the side retaining Armco magnetic iron manganio cubic nanometer material prepared by template
Method, it is characterised in that: the concentration of described potassium permanganate solution is 1g/L；Raw material potassium permanganate and Prussian blue mol ratio are
1:1~1:10。
The most according to claim 1 a kind of based on the side retaining Armco magnetic iron manganio cubic nanometer material prepared by template
Method, it is characterised in that: the nanometer Prussian Blue of described cubic structure is with three hydration six cyanogen ferrum (II) acid potassium, polyvinyl pyrrole
Alkanone and hydrochloric acid are raw material, are prepared from through hydrothermal synthesis method.
The most according to claim 4 a kind of based on the side retaining Armco magnetic iron manganio cubic nanometer material prepared by template
Method, it is characterised in that: the concrete preparation method of the nanometer Prussian Blue of cubic structure is:
1) a certain amount of three hydration six cyanogen ferrum (II) acid potassium and polyvinylpyrrolidone are put in beaker, be subsequently adding hydrochloric acid molten
Liquid, obtains mixed system；
2) mixed system stirring is completely dissolved to raw material, obtains mixed solution；
3) by after ultrasonic for mixed solution 30 minutes, pour in reactor, 80 DEG C of reaction 24h；Product is washed by centrifugation, 70 DEG C
It is dried 12 h, i.e. obtains Prussian blue.
The most according to claim 5 a kind of based on the side retaining Armco magnetic iron manganio cubic nanometer material prepared by template
Method, it is characterised in that: in step (1), the consumption of three hydration six cyanogen ferrum (II) acid potassium is 0.11 g, the use of polyvinylpyrrolidone
Amount is 3.8 g；The concentration of hydrochloric acid solution is 0.1 mol/L, and consumption is 50mL.
7. the Armco magnetic iron manganio cubic nanometer material that prepared by the method as described in any one of claim 1 ~ 6.
Armco magnetic iron manganio cubic nanometer material Pb in selective absorption waste liquid the most according to claim 72+Answering of aspect
With.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108706637A (en) * | 2018-06-21 | 2018-10-26 | 福州大学 | A kind of preparation method of the adjustable magnetic iron oxide mesomorphic material of size uniform |
| CN109437338A (en) * | 2018-11-30 | 2019-03-08 | 福州大学 | The preparation method of one type sawtooth pattern nickel cobalt iron Prussian blue analogue sintered oxide nano material |
| CN115430597A (en) * | 2022-11-03 | 2022-12-06 | 中国科学院宁波材料技术与工程研究所 | Super-hydrophilic nickel-based multilayer composite film material and preparation method and application thereof |
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| CN103193219A (en) * | 2013-04-09 | 2013-07-10 | 江西师范大学 | Preparation method of three-dimensional ordered porous carbon/Prussian blue nanocomposite |
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| CN103193219A (en) * | 2013-04-09 | 2013-07-10 | 江西师范大学 | Preparation method of three-dimensional ordered porous carbon/Prussian blue nanocomposite |
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| YOU-CUN CHEN等: ""Morphology controllable preparation of nanocube Mn3[Fe(CN)6]2•nH2O particles》", 《COLLOIDS AND SURFACES A: PHYSICOCHEM. ENG. ASPECTS》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108706637A (en) * | 2018-06-21 | 2018-10-26 | 福州大学 | A kind of preparation method of the adjustable magnetic iron oxide mesomorphic material of size uniform |
| CN109437338A (en) * | 2018-11-30 | 2019-03-08 | 福州大学 | The preparation method of one type sawtooth pattern nickel cobalt iron Prussian blue analogue sintered oxide nano material |
| CN109437338B (en) * | 2018-11-30 | 2021-03-02 | 福州大学 | Preparation method of sawtooth-like nickel-cobalt-iron Prussian blue sintered oxide nano material |
| CN115430597A (en) * | 2022-11-03 | 2022-12-06 | 中国科学院宁波材料技术与工程研究所 | Super-hydrophilic nickel-based multilayer composite film material and preparation method and application thereof |
| CN115430597B (en) * | 2022-11-03 | 2023-03-07 | 中国科学院宁波材料技术与工程研究所 | Super-hydrophilic nickel-based multilayer composite film material and preparation method and application thereof |
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