CN106268616B - Based on the magnetic ferrimanganic base cubic nanometer material and its application for retaining template preparation - Google Patents
Based on the magnetic ferrimanganic base cubic nanometer material and its application for retaining template preparation Download PDFInfo
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- CN106268616B CN106268616B CN201610655193.3A CN201610655193A CN106268616B CN 106268616 B CN106268616 B CN 106268616B CN 201610655193 A CN201610655193 A CN 201610655193A CN 106268616 B CN106268616 B CN 106268616B
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- 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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
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- 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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Abstract
The invention belongs to environment and Material Fields, and in particular to a kind of based on the magnetic ferrimanganic base cubic nanometer material for retaining template preparation and its application.The present invention is with three six cyanogen iron of hydration（Ⅱ）Sour potassium（K4[Fe(CN)6]·3H2O）, polyvinylpyrrolidone K 30, hydrochloric acid synthesis of cubic structure nanometer Prussian Blue, then pass through and mix different amounts of KMnO4Sample is washed, it is sintered after dry, finally obtains magnetic ferrimanganic base cubic nanometer material by centrifuging as the sources Mn.Magnetism ferrimanganic base cubic nanometer material produced by the present invention, can effectively adsorb the Pb in industrial wastewater2+, the Pb in realizing effectively absorption waste liquid2+While, it is easy to and the separation that disposes waste liquid, is easily recycled, secondary pollution will not be caused to waste liquid.Preparation method is simple, of low cost, with good economic efficiency and environmental benefit.
Description
Technical field
The invention belongs to environment and Material Fields, and in particular to a kind of vertical based on magnetic ferrimanganic base prepared by template is retained
Square nano material and its application.
Background technology
Nowadays, with advances in technology with development, the living standard of the mankind is higher and higher, but water environment is heavy metal-polluted
Dye but increasingly aggravates.Therefore effective method is found come the heavy metal ion in disposing waste liquid, become urgent problem to be solved.Using
It is a kind of effective means that the granular materials of hollow microsize or Nano type, which carries out absorption,.Because of the unique knot of granular materials
Structure makes it have good application prospect in many fields.
In recent years, nanometer Fe2O3Cause is with surface charge height, large specific surface area, to heavy metal with very strong adsorption energy
Power, derive from a wealth of sources, small toxicity, the features such as being not easy to cause secondary pollution to environment, are inhaling and by the extensive concern of researcher
The fields such as attached, catalysis, air-sensitive are widely used.And for Mn oxide, though it can be weighed in effective Adsorption water
Metal ion, but since grain size is smaller, be easy to run off, keep its application limited.
In the prior art, formwork structure is often some Organic Ingredients so that sample during use can be to ring
Cause secondary pollution in border.And it is Prussian blue（Metal organic frame）As the template of magnetic ferrimanganic base cubic nanometer structural material,
Secondary pollution will not then be caused.Moreover, Prussian blue have better stereoeffect, in many territories
To relatively broad application, using Prussian blue as the di-iron trioxide of templated synthesis, which still is able to keep Prussia
Blue cubic structure, adulterates different Mn2+, obtained di-iron trioxide/Mn oxide, still be able to keep cubic structure.I
Prepared by hydro-thermal method it is Prussian blue, and by mix different content Mn, obtain mixing manganese under different Fe, Mn molar ratios
Modified Prussian blue sample is finally sintered it, then can obtain magnetic ferrimanganic base cubic nanometer structural material.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of based on the Armco magnetic iron for retaining template preparation
Manganese base cubic nanometer material and its application.The present invention is using Prussian blue as the magnetic ferrimanganic base cubic nanometer material of templated synthesis
Material can keep Prussian blue cubic structure well, and effectively adsorb Pb in waste liquid2+, thus solution uses organic matter as mould
Plate synthetic adsorbent in use caused by secondary pollution problem.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of magnetic ferrimanganic base cubic nanometer material prepared based on reservation template, is included the following steps：
（1）The preparation of the nanometer Prussian Blue template of cubic structure：
It is hydrated six cyanogen iron by a certain amount of three（Ⅱ）Sour potassium and polyvinylpyrrolidone are put into beaker, then into beaker
Aqueous hydrochloric acid solution is added, obtains mixed system；Then mixed system is stirred to raw material and is completely dissolved, obtain mixed solution；Again will
Mixed solution is ultrasonically treated 30 minutes；Then acquired solution is poured into reaction kettle, reacts 24 h in 80 DEG C；It finally will reaction
Sample centrifuge washing in kettle, 70 DEG C of 12 h of drying are to get to Prussian blue template；A concentration of the 0.1 of aqueous hydrochloric acid solution
Mol/L, dosage are 50 mL；Polyvinylpyrrolidone model K-30, dosage are 3.8 g；Three six cyanogen iron of hydration（Ⅱ）Sour potassium
Dosage is 0.11 g；
（2）The preparation of magnetic ferrimanganic base cubic nanometer structural material：
It will（1）In obtained Prussian blue template it is evenly dispersed in ethanol solution, stirring to solution is in navy blue, is obtained
Mixed solution；Then liquor potassic permanganate is slowly poured into mixed solution, stirs 1 h；Then reaction solution is centrifuged
Separation, washing；Sample after washing is put into baking oven and keeps the temperature 12 h at 70 DEG C and is dried, obtains the Pu Lu for mixing manganese modification
Scholar is blue；Finally, by Prussian blue being put into Muffle furnace for mixing manganese modification of gained, 6 hours is kept the temperature at 350 DEG C -650 DEG C, is risen
Warm rate is 0.3 DEG C/min-0.5 DEG C/min, finally obtains the magnetic ferrimanganic base cubic nanometer structural material for retaining template.
Wherein, a concentration of 1g/L of liquor potassic permanganate, in ethanol solution, the volume ratio of deionized water and ethyl alcohol is：3:2
~8:2。
In obtained magnetic ferrimanganic base cubic nanometer material, iron, manganese molar ratio be 1:1 ~10:1.
The beneficial effects of the present invention are：
1）The present invention uses the Prussian blue preparation as the compound cubic nanometer structural material of templated synthesis magnetism ferrimanganic base,
Since the incorporation of Mn can be with control surface pattern so that material can keep Prussian blue possessed cubic structure；Sintering
The Armco magnetic iron Mn-based material cube obtained afterwards is porous, has preferable absorption property, and due to ferromagnetic presence, make it
It can be proposed from waste liquid using magnetic separation technique, convenient for recycling, without causing secondary pollution；
2）The required equipment of preparation method and material of the present invention is easily obtained, and technological operation is simple, and process conditions are not
Complexity has at low cost, safety, efficient advantage, application easy to spread.
Description of the drawings
Fig. 1 is the Prussian blue microscopic appearance of undoped sintering processes in the implementation case；
Fig. 2 is the Prussian blue Fe being sintered at 650 DEG C in comparative example 12O3Scan microgram；
Fig. 3 is Fe in embodiment 1:Mn=1:The microcosmic shape of the magnetic ferrimanganic base cubic nanometer material of 650 DEG C of sintering when 1
Looks；
Fig. 4 is Fe in embodiment 2:Mn=10:1, the unsintered Prussian blue microscopic appearance for mixing manganese modification；
Fig. 5 is Fe in embodiment 2:Mn=10:The microcosmic shape of the magnetic ferrimanganic base cubic nanometer material of 1,650 DEG C of sintering
Looks；
Fig. 6 is magnetic ferrimanganic based nano-material in Application Example 1（Fe:Mn=1:1（s））, mix it is Prussian blue after manganese
（Fe:Mn=1:1（I）、Fe:Mn=10:1（I））And the Prussian blue Fe sintered into for template2O3These four materials are inhaled according to it
Attached Pb2+The scattergram that effect is obtained；
Fig. 7 is magnetic ferrimanganic based nano-material in Application Example 2（Fe:Mn=1:1（s））, mix it is Prussian blue after manganese
（Fe:Mn=1:1（I）、Fe:Mn=10:1（I））And the Prussian blue Fe sintered into for template2O3These four materials are inhaled according to it
Attached Zn2+The scattergram that is obtained of effect；
Fig. 8 is magnetic ferrimanganic based nano-material in Application Example 3（Fe:Mn=1:1（s））, mix it is Prussian blue after manganese
（Fe:Mn=1:1（I）、Fe:Mn=10:1（I））, the Prussian blue Fe sintered into for template2O3With the Fe of commercial use2O3, according to
It adsorbs Pb2+、Zn2+The scattergram that is obtained of effect；
After Fig. 9 is liquid waste processing, forward and backward design sketch is handled using magnetic separation technique.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, right below in conjunction with attached drawing, that is, embodiment
The present invention is further elaborated.It 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.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can combine.
Embodiment 1
A kind of magnetic ferrimanganic base cubic nanometer material prepared based on reservation template, the specific steps are：
1）It is Prussian blue（PB）Preparation：
（K4[Fe(CN)6]·3H2O）, PVP, hydrochloric acid is mixed, and is in yellow, and ultrasonic 30 min processing are being carried out to it
Afterwards, solution is poured into water heating kettle and keeps the temperature 24 hours for 80 DEG C, finally by the sample centrifuge washing in reaction kettle, 70 DEG C of dryings 12
H is to get to Prussian blue template；
2）It is Prussian blue（PB）Mix manganese modification：
The Prussian blue samples of 0.05 g is evenly dispersed in ethanol solution（Deionized water and the volume ratio of ethyl alcohol are 8:
2）, stirring to solution is in navy blue, and a certain amount of liquor potassic permanganate prepared in advance is added（1g/L）, stir 1 hour, wash
Sample is dried to obtain and mixes the Prussian blue of manganese modification；Wherein the molar ratio of Fe, Mn are 1:1；
3）Mix the modified ferrimanganic base of manganese（Fe2O3/KMn8O16）Synthesis：
It is installed with small crucible（2）Obtained in sample and cover, put it into Muffle furnace, heating rate 0.5
DEG C/min, at 650 DEG C, it is sintered 6h.It finally obtains and mixes the modified ferrimanganic base of manganese（Fe2O3/ KMn8O16）.
Embodiment 2
A kind of magnetic ferrimanganic base cubic nanometer material prepared based on reservation template, the specific steps are：
1）It is Prussian blue（PB）Preparation：
（K4[Fe(CN)6]·3H2O）, PVP, hydrochloric acid is mixed, and is in yellow, and ultrasonic 30 min processing are being carried out to it
Afterwards, solution is poured into water heating kettle and keeps the temperature 24 hours for 80 DEG C, finally by the sample centrifuge washing in reaction kettle, 70 DEG C of dryings 12
H is to get to Prussian blue template；
2）It is Prussian blue（PB）Mix manganese modification：
The Prussian blue samples of 0.05 g is evenly dispersed in ethanol solution（Deionized water and the volume ratio of ethyl alcohol are 8:
2）, stirring to solution is in navy blue, and a certain amount of liquor potassic permanganate prepared in advance is added（1g/L）, stir 1 hour, wash
Sample is dried to obtain and mixes the Prussian blue of manganese modification；Wherein the molar ratio of Fe, Mn are 10:1；
3）Mix the modified ferrimanganic base of manganese（Fe2O3/ KMn8O16）Synthesis：
It is installed with small crucible（2）Obtained in sample and cover, put it into Muffle furnace, heating rate 0.5
DEG C/min, at 650 DEG C, it is sintered 6h.It finally obtains and mixes the modified ferrimanganic base of manganese（Fe2O3/ KMn8O16）.
Comparative example 1
A kind of Fe2O3Preparation method, the specific steps are：
1）It is Prussian blue（PB）Preparation：
（K4[Fe(CN)6]·3H2O）, PVP, hydrochloric acid is mixed, and is in yellow, and ultrasonic 30 min processing are being carried out to it
Afterwards, solution is poured into water heating kettle and keeps the temperature 24 hours for 80 DEG C, finally by the sample centrifuge washing in reaction kettle, 70 DEG C of dryings 12
H is to get to Prussian blue template；
2）The sintering processes of Prussian blue template：
It is installed with small crucible（1）Obtained in sample and cover, put it into Muffle furnace, heating rate 0.5
DEG C/min, at 650 DEG C, it is sintered 6h.Finally obtain cubic Fe2O3。
Adsorption experiment
Application Example 1
Sample made from 10 mg comparative examples 1 is weighed respectively（Fe2O3）And embodiment Fe:Mn=10:1（I）、Fe:Mn=1:
1（I）Mix manganese modification Prussian blue, Fe:Mn=1:1（s）Magnetic ferrimanganic base cubic nanometer material；Compound concentration is 40ppm
Self-control Pb2+Solution；
Above four kinds of samples are made by oneself Pb with 50 ml, 40 ppm respectively2+Solution mixes, stirring；It is opened respectively in adsorption experiment
1 min, 5 min, 10 min, 15 min, 30 min, 45 min, 60 min after beginning are sampled, and are then placed in centrifuge
In, rotating speed is 12000 r/min, centrifuges 2 min；Atomic absorption test, the sampling difference of each period are carried out to centrifugate
It surveys three times, takes its average value.
Application Example 2
Sample made from 10 mg comparative examples 1 is weighed respectively（Fe2O3）And Fe:Mn=10:1（I）、Fe:Mn=1:1（I）'s
Mix Prussian blue, the Fe of manganese modification:Mn=1:1（s）Magnetic ferrimanganic base cubic nanometer material；Compound concentration is oneself of 40 ppm
Zn processed2+Solution；
Above four kinds of samples are made by oneself Zn with 50 ml, 40 ppm respectively2+Solution mixes, stirring；It is opened respectively in adsorption experiment
1 min, 5 min, 10 min, 15 min, 30 min, 45 min, 60 min after beginning are sampled, and are then placed in centrifuge
In, rotating speed is 12000 r/min, centrifuges 2 min；Finally, processing is diluted to the solution after centrifugation（Five times of dilution）
Afterwards, Atomic absorption test is carried out, the sampling of each period is surveyed three times respectively, takes its average value.
Application Example 3
Sample made from 10 mg comparative examples 1 is weighed respectively（Fe2O3）And Fe:Mn=10:1（I）, Fe:Mn=1:1（I）'s
Mix Prussian blue, the Fe of manganese modification:Mn=1:1（s）Magnetic ferrimanganic base cubic nanometer material and commercial use Fe2O3；Match
Pb processed2+、Zn2+Concentration is the mixed solution of 40ppm；
Above five kinds of samples are made by oneself Pb with 50 ml, 40 ppm respectively2+、Zn2+Mixed solution mixes, stirring；Exist respectively
Adsorption experiment start after 1 min, 5 min, 10 min, 15 min, 30 min, 45 min, 60 min be sampled, then put
Enter in centrifuge, rotating speed is 12000 r/min, centrifuges 2 min；Pb first is carried out to centrifugate2+Measurement；Then by centrifugate into
Row dilution is handled（Five times of dilution）Afterwards, then Zn is carried out2+Measurement.
As it will be easily appreciated by one skilled in the art that the foregoing is merely the preferred embodiments of the present invention, not limiting
The system present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement, should be included in this
Within the protection domain of invention.
Claims (8)
1. a kind of based on the method for retaining the magnetic ferrimanganic base cubic nanometer material of template preparation, it is characterised in that：It will cube knot
The nanometer Prussian Blue of structure is evenly dispersed in ethanol solution, and stirring to mixed solution is in navy blue；Then potassium permanganate is molten
Liquid is added into mixed solution, reacts 1 h under stiring；Then reaction solution is centrifuged, washed, the sample after washing
Product dry 12 h at 70 DEG C obtain mixing the Prussian blue of manganese modification；Then the Prussian blue of manganese modification will be mixed and be put into Muffle furnace
In, 6 hours are kept the temperature at 350 DEG C -650 DEG C, heating rate is 0.3 DEG C/min-0.5 DEG C/min, obtains magnetic ferrimanganic base cube
Nano material；In wherein obtained nano material, iron, manganese molar ratio be 1:1~10:1.
2. a kind of method that magnetic ferrimanganic base cubic nanometer material is prepared based on reservation template according to claim 1,
It is characterized in that：In the ethanol solution, the volume ratio of deionized water and ethyl alcohol is：3:2~8:2.
3. a kind of method that magnetic ferrimanganic base cubic nanometer material is prepared based on reservation template according to claim 1,
It is characterized in that：A concentration of 1g/L of the liquor potassic permanganate；Raw material potassium permanganate and Prussian blue molar ratio are 1:1
~1:10。
4. a kind of method that magnetic ferrimanganic base cubic nanometer material is prepared based on reservation template according to claim 1,
It is characterized in that：The nanometer Prussian Blue of the cubic structure is with three six cyanogen iron of hydration（Ⅱ）Sour potassium, polyvinylpyrrolidine
Ketone and hydrochloric acid are raw material, are prepared through hydrothermal synthesis method.
5. a kind of method that magnetic ferrimanganic base cubic nanometer material is prepared based on reservation template according to claim 4,
It is characterized in that：The specific preparation method of the nanometer Prussian Blue of cubic structure is：
1）It is hydrated six cyanogen iron by a certain amount of three（Ⅱ）Sour potassium and polyvinylpyrrolidone are put into beaker, and it is molten that hydrochloric acid is then added
Liquid obtains mixed system；
2）Mixed system is stirred to raw material and is completely dissolved, mixed solution is obtained；
3）It after mixed solution ultrasound 30 minutes, pours into reaction kettle, 80 DEG C of reactions are for 24 hours；Reaction product is through centrifuge washing, 70 DEG C
Dry 12 h are to get to Prussian blue.
6. a kind of method that magnetic ferrimanganic base cubic nanometer material is prepared based on reservation template according to claim 5,
It is characterized in that：Step（1）In three hydration six cyanogen iron（Ⅱ）The dosage of sour potassium is 0.11 g, and the dosage of polyvinylpyrrolidone is
3.8 g；A concentration of 0.1 mol/L, dosage 50mL of hydrochloric acid solution.
7. a kind of magnetic ferrimanganic base cubic nanometer material prepared such as claim 1 ~ 6 any one of them method.
8. magnetism ferrimanganic base cubic nanometer material Pb in selective absorption waste liquid according to claim 72+Aspect is answered
With.
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| 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 |
| 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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| ""分子合金"类普鲁士蓝配合物Co0.25Mn1.25[Fe(CN)6]·5.9H2O的磁性研究";何云等;《广西师范大学学报:自然科学版》;20120930;第30卷(第3期);第201-206页 * |
| You-Cun Chen等."Morphology controllable preparation of nanocube Mn3[Fe(CN)6]2•nH2O particles》.《Colloids and Surfaces A: Physicochem. Eng. Aspects》.2013,第436卷第1140-1144页. * |
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