CN106925282A - NiFe/CeO is obtained by topology reducing process in situ2The method of nano composite material - Google Patents
NiFe/CeO is obtained by topology reducing process in situ2The method of nano composite material Download PDFInfo
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- CN106925282A CN106925282A CN201710119508.7A CN201710119508A CN106925282A CN 106925282 A CN106925282 A CN 106925282A CN 201710119508 A CN201710119508 A CN 201710119508A CN 106925282 A CN106925282 A CN 106925282A
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The present invention relates to a kind of dimensional thinlayer shape NiFe/CeO obtained by topology reducing process in situ2The method of nano composite material, specially：Be added in the pyroxylin film of conical flask pattern for Ni, the inorganic salt solution of Fe, Ce by the first step, and being put into after sealing carries out precipitation reaction in the beaker equipped with sodium hydroxide solution, obtain intermediate product, is centrifuged, washing, dries.Second step is reduced by topology reducing process in situ to the intermediate product for obtaining, and be centrifuged for sample after terminating by reaction, washs, and is dried to obtain final product for dimensional thinlayer shape NiFe/CeO2Nano composite material.The big nano composite material of specific surface area is prepared using the inventive method, with excellent magnetic and catalysis activity.The inventive method is simple to operation, and the treatment of easy to control and product is simple, is adapted to medium-scale industrial production.
Description
Technical field
Two dimension is obtained by topology reducing process in situ the invention belongs to technical field of inorganic nanometer material, more particularly to one kind
Lamelliform NiFe/CeO2The method of nano composite material.
Background technology
The characteristics of two-dimension nano materials are because of its thickness and two-dimension plane structure often has different from respective masses material
The electronic structure of material, is not only able to influence its intrinsic performance, moreover it is possible to produce some new properties, while it has theory very high
Specific surface area and electron mobility so that it rapidly becomes material science and the active study hotspot of chemical catalysis field.Two dimension
The synergy that structure is produced during composite nanoparticle, makes it show excellent performance in actual applications：Such as
During as li-ion electrode materials, two-dimensional nano composite has satisfactory electrical conductivity, and can improve electrode material with electrolysis
The diffusivity of matter boundary；When as sensor material, due to the support fixation of two-dimentional carbon material, nano-particle is in height
Curing is not susceptible under the condition of work of temperature to grow up, while the big specific surface area of two-dimensional material is beneficial to the diffusion and phase for improving gas
Interfacial reaction；As elctro-catalyst, while with preferable nano-particle dispersiveness, with electron mobility higher.Receive
Rice alloy particle can further improve the performance of material, widen inorganic metal nanometer significantly with being combined for dimensional thinlayer oxide
The range of application of particle and metal oxide.Nanoalloy particle modifies dimensional thinlayer oxide, and this can not only overcome nanometer
The huge Van der Waals force of piece interlayer, prevents the reunion of nanometer sheet, enables the peculiar property of the ultra-thin layer structure of metal oxide
Retain.By lamelliform CeO in this experiment2Nanometer sheet and NiFe nano-particles are effectively combined, and are formed two-dimensional nano and are combined
Structure.First, CeO2Easily it is reduced to CeO2-xSo that lamelliform CeO2Nanometer sheet carrier has a large amount of Ce3+, high electron density
Ce3+Absorption of the catalyst to hydrazine hydrate can be promoted as Lewis alkali, make the declines of N-H keys.Can also promote NiFe simultaneously
Alloy is preferentially broken N-H keys as activated centre, greatly improves the selectivity and activity of catalytic reaction.In addition, this two dimension is thin
Membrane structure also has larger specific surface area, can provide the avtive spot of more catalytic reactions, improves catalytic efficiency.
The content of the invention
Dimensional thinlayer shape NiFe/CeO is obtained by topology reducing process in situ it is an object of the invention to provide a kind of2Nanometer is multiple
The method of condensation material.
To achieve these goals, technical scheme is as follows：
One kind proposed by the present invention obtains dimensional thinlayer shape NiFe/CeO by topology reducing process in situ2The side of nano composite material
Method, comprises the following steps that：
（1）Ni, the inorganic salt solution of Fe, Ce are added in the pyroxylin film of conical flask pattern, are put into equipped with hydrogen-oxygen after sealing
Precipitation reaction is carried out in the beaker for changing sodium solution；Be centrifuged for sample after terminating, wash, drying by reaction, and calcining is obtained
Intermediate product；The mol ratio of the inorganic salts of Ni, Fe, Ce is 6:4:1；The molal quantity summation and hydrogen-oxygen of the Ni, Fe, Ce inorganic salts
The mol ratio for changing sodium solution is 11:40；
（2）By step（1）Obtain intermediate product ultrasound, dispersed with stirring in the ethylene glycol solution dissolved with sodium hydrate solid,
Reduction reaction is carried out in a kettle.；Be centrifuged for sample after terminating by reaction, washs, and dries, and obtains final product, i.e.,
Dimensional thinlayer shape NiFe/CeO2Nano composite material.
In the present invention, step（1）The solvent that the inorganic salt solution of middle preparation Ni, Fe, Ce is used is deionized water.
In the present invention, step（1）Described in the inorganic salts of Ni be nickel chloride, the inorganic salts of Fe are ferrous sulfate, the nothing of Ce
Machine salt is cerous nitrate, and its concentration is 0.025mol/L.
In the present invention, step（1）Described in sodium hydroxide solution concentration be 0.1mol/L.
In the present invention, step（1）Described in the precipitation reaction time be 1 hour.
In the present invention, step（1）Described in washing be using deionized water and absolute ethyl alcohol carry out alternately washing.
In the present invention, step（1）Described in centrifugation rotating speed be 6000 revs/min, the time be 5 minutes.
In the present invention, step（1）Described in drying be to dry 10h at 60 DEG C of vacuum drying chamber.
In the present invention, step（2）Described in the ethylene glycol solution dissolved with NaOH, its concentration be 0.25mol/L.
In the present invention, step（2）Described in the reduction reaction time be 12 hours.
In the present invention, step（2）Described in reduction reaction temperature be 140 DEG C -180 DEG C.
In the present invention, step（2）Described in washing be all using deionized water and absolute ethyl alcohol carry out alternately washing.
In the present invention, step（2）Described in centrifugation rotating speed be 6000 revs/min, the time be 5 minutes.
In the present invention, step（2）Described in drying be to dry 10h at 60 DEG C of vacuum drying chamber.
Due to using such scheme, the invention has the advantages that：
1st, the present invention realize using common nickel chloride, ferrous sulfate, cerous nitrate be reaction presoma, by co-precipitation-
Topology reducing process in situ, has synthesized dimensional thinlayer shape NiFe/CeO first2Nano composite material.
2nd, the method for the present invention has control very high to the pattern of product.
3rd, the present invention uses simple inorganic salts as reactant, with very strong versatility.
4th, there is product prepared by the present invention good Compounds with Hydrazine Hydrate Catalyzed to decompose the performance for producing hydrogen, can be urged as high-performance
Agent, there is more vast potential for future development and application space.
5th, process is simple of the invention, preparation condition is general, and product morphology stabilization, purity are high, and the convenient letter of product treatment
It is clean, it is suitable for medium-scale industrial production.
6th, the method for the present invention have mild condition, efficient energy-saving, it is easily controllable the features such as.
Brief description of the drawings
Fig. 1 is the SEM photograph of intermediate product obtained under the multiple of 500nm in embodiment 1.
Fig. 2 is the SEM photograph of product obtained under the multiple of 500nm in embodiment 1.
Fig. 3 is the TEM photos of intermediate product obtained under the multiple of 50nm in embodiment 1.
Fig. 4 is the TEM photos of product obtained under the multiple of 50nm in embodiment 1.
Fig. 5 is the XRD spectrum of the products therefrom of embodiment 1.
Fig. 6 is the EDS collection of illustrative plates of the products therefrom of embodiment 1.
Fig. 7 is the SEM photograph of intermediate product obtained under the multiple of 500nm in embodiment 2.
Fig. 8 is the XRD spectrum of the products therefrom of embodiment 3.
Fig. 9 is the SEM photograph of intermediate product obtained under the multiple of 500nm in embodiment 3.
Figure 10 is the XRD spectrum of the products therefrom of embodiment 4.
Specific embodiment
The present invention is further detailed explanation for illustrated embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The first step, accurately weighs 0.5942gNiCl2·6H2O, 100ml solution is configured to deionized water, and concentration is 25mmol/
L, accurately weighs 0.6950g FeSO4·7H2O, 100ml solution is configured to deionized water, and concentration is 25mmol/L, accurately
Weigh 1.0856g Ce (NO3)3·6H2O, 100ml solution is configured to deionized water, and concentration is 25mmol/L, Ni2+：Fe2+:
Ce3+According to 6:4:1 mol ratio is mixed, and cumulative volume is 110ml, is subsequently placed in the pyroxylin film of conical flask pattern, sealing
After be placed in 250ml beakers.
Second step, accurately weighs the NaOH of 0.400g, and 100ml solution is configured to deionized water, and concentration is
100mmol/L, is then poured into the beaker of the first step and is sealed beaker mouth with preservative film and reacted.
3rd step, reaction 1 hour after, collect pyroxylin film in solution and precipitation, be centrifuged and with absolute ethyl alcohol and go from
Sub- water washing for several times, is placed in vacuum drying chamber and dries, and obtains intermediate product.
4th step, accurately weighs the sodium hydrate solid of 0.200g, is placed in the beaker for filling 20ml ethylene glycol solutions, stirs
Mix to NaOH and be completely dissolved.
5th step, accurately weighs 20mg intermediate products, is added in the ethylene glycol solution of above-mentioned NaOH, and stirring is to complete
CL, transfers the solution into the reactor of 30ml, is reacted 12 hours at 160 DEG C.
6th step, question response kettle is cooled to room temperature, collects solution and solid in reactor, is centrifuged and with absolute ethyl alcohol and goes
Ion water washing for several times, is placed in vacuum drying chamber and dries.Obtain final product：Dimensional thinlayer shape NiFe/CeO2Nanometer is multiple
Condensation material.
Fig. 1 is the SEM pictures of intermediate product NiFeCe hydroxide obtained under the multiple of 500nm in embodiment 1；Figure
2 is the SEM pictures of product obtained under the multiple of 500nm in embodiment 1；Fig. 3 is the gained intermediate product of embodiment 1 in 50nm
Multiple under NiFeCe hydroxide TEM pictures；Fig. 4 is TEM picture of the products therefrom of embodiment 1 under the multiple of 50nm；
Fig. 5 is the XRD spectrum of embodiment 1 products therefrom, it was demonstrated that NiFe alloy and CeO2Nano thin-layer it is compound；Fig. 6 is embodiment 1
The EDS collection of illustrative plates of middle product indicates wherein Ni, the presence of Fe, Ce, O element.
Embodiment 2
The first step, accurately weighs 0.5942gNiCl2·6H2O, 100ml solution is configured to deionized water, and concentration is 25mmol/
L, accurately weighs 0.6950g FeSO4·7H2O, 100ml solution is configured to deionized water, and concentration is 25mmol/L, accurately
Weigh 1.0856g Ce (NO3)3·6H2O, 100ml solution is configured to deionized water, and concentration is 25mmol/L, Ni2+：Fe2+:
Ce3+According to 6:4:1 mol ratio is mixed, and cumulative volume is 110ml, is subsequently placed in the pyroxylin film of conical flask pattern, sealing
After be placed in 250ml beakers.
Second step, accurately weighs the NaOH of 0.400g, and 100ml solution is configured to deionized water, and concentration is
100mmol/L, is then poured into the beaker of the first step and is sealed beaker mouth with preservative film and reacted.
3rd step, after reacting 1 hour, collects the solution in pyroxylin film and precipitation is poured into 100 ml centrifuge tubes,
It is centrifuged and is washed for several times with absolute ethyl alcohol and deionized water, be placed in vacuum drying chamber and dry, obtains intermediate product.
4th step, accurately weighs the sodium hydrate solid of 0.200g, is placed in the beaker for filling 20ml ethylene glycol solutions, stirs
Mix to NaOH and be completely dissolved.
5th step, accurately weighs 20mg intermediate products, is added in the ethylene glycol solution of above-mentioned NaOH, and stirring is to complete
CL, transfers the solution into the reactor of 30ml, is reacted 12 hours at 140 DEG C.
6th step, question response kettle is cooled to room temperature, collects solution and solid in reactor, is centrifuged and with absolute ethyl alcohol and goes
Ion water washing for several times, is placed in vacuum drying chamber and dries, and obtains final product：Dimensional thinlayer shape NiFe/CeO2Nanometer is multiple
Condensation material.
Fig. 7 is the product NiFe/CeO obtained under the multiple of 500nm in embodiment 22The SEM photograph of nanometer sheet.By scheming
Piece can be seen that can still form dimensional thinlayer structure with this understanding, and simply the amount of crimp of film is larger, with respect to specific surface
Product is smaller.Fig. 8 is the XRD spectrum of the products therefrom of example 2, by picture as can be seen that reducing the product for obtaining with this understanding also
Former not abundant enough, Ni, Fe still exist in the form of the oxide.Reaction temperature reduction is illustrated, the reducing degree of product is impacted, nothing
Method obtains estimated NiFe alloy.
Embodiment 3
The first step, accurately weighs 0.5942gNiCl2·6H2O, 100ml solution is configured to deionized water, and concentration is 25mmol/
L, accurately weighs 0.6950g FeSO4·7H2O, 100ml solution is configured to deionized water, and concentration is 25mmol/L, accurately
Weigh 1.0856g Ce (NO3)3·6H2O, 100ml solution is configured to deionized water, and concentration is 25mmol/L, Ni2+：Fe2+:
Ce3+According to 6:4:1 mol ratio is mixed, and cumulative volume is 110ml, is subsequently placed in the pyroxylin film of conical flask pattern, sealing
After be placed in 250ml beakers.
Second step, accurately weighs the NaOH of 0.400g, and 100ml solution is configured to deionized water, and concentration is
100mmol/L, is then poured into the beaker of the first step and is sealed beaker mouth with preservative film and reacted.
3rd step, after reacting 1 hour, collects the solution in pyroxylin film and precipitation is poured into 100 ml centrifuge tubes,
It is centrifuged and is washed for several times with absolute ethyl alcohol and deionized water, be placed in vacuum drying chamber and dry, obtains intermediate product.
4th step, accurately weighs the sodium hydrate solid of 0.200g, is placed in the beaker for filling 20ml ethylene glycol solutions, stirs
Mix to NaOH and be completely dissolved.
5th step, accurately weighs 20mg intermediate products, is added in the ethylene glycol solution of above-mentioned NaOH, and stirring is to complete
CL, transfers the solution into the reactor of 30ml, is reacted 12 hours at 180 DEG C.
6th step, question response kettle is cooled to room temperature, collects solution and solid in reactor, is centrifuged and with absolute ethyl alcohol and goes
Ion water washing for several times, is placed in vacuum drying chamber and dries, and obtains final product：Dimensional thinlayer shape NiFe/CeO2Nanometer is multiple
Condensation material.
Fig. 9 is the product NiFe/CeO obtained under the multiple of 500nm in embodiment 32The SEM photograph of nanometer sheet.By scheming
It is not it is obvious that reunite obvious, after illustrate that reaction temperature is improved, to give birth to that piece can be seen that the laminate structure for being formed with this understanding
Speed long is accelerated to be difficult to generate dimensional thinlayer structure.Figure 10 is the XRD spectrum of embodiment 3 products therefrom, it was demonstrated that NiFe alloy
And CeO2Nano thin-layer it is compound.
The above-mentioned description to embodiment is to be understood that and apply this hair for ease of those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to implementation here
Example, in the modification made without departing from the scope of the invention all within protection scope of the present invention.
Claims (10)
1. it is a kind of that dimensional thinlayer shape NiFe/CeO is obtained by topology reducing process in situ2The method of nano composite material, its feature exists
In comprising the following steps that：
（1）Ni, the inorganic salt solution of Fe, Ce are added in the pyroxylin film of conical flask pattern, are put into equipped with hydrogen-oxygen after sealing
Precipitation reaction is carried out in the beaker for changing sodium solution；Be centrifuged for sample after terminating, wash, drying by reaction, and calcining is obtained
Intermediate product；The mol ratio of the inorganic salts of Ni, Fe, Ce is 6:4:1；The molal quantity summation and hydrogen-oxygen of the Ni, Fe, Ce inorganic salts
The mol ratio for changing sodium solution is 11:40；
（2）By step（1）Obtain intermediate product ultrasound, dispersed with stirring in the ethylene glycol solution dissolved with sodium hydrate solid,
Reduction reaction is carried out in a kettle.；Be centrifuged for sample after terminating by reaction, washs, and dries, and obtains final product, i.e.,
Dimensional thinlayer shape NiFe/CeO2Nano composite material.
2. one kind according to claim 1 obtains dimensional thinlayer shape NiFe/CeO by topology reducing process in situ2It is nano combined
The method of material, it is characterised in that：Step（1）The solvent that the inorganic salt solution of middle preparation Ni, Fe, Ce is used is deionization
Water.
3. one kind according to claim 1 obtains dimensional thinlayer shape NiFe/CeO by topology reducing process in situ2It is nano combined
The method of material, it is characterised in that：Step（1）Described in the inorganic salts of Ni be nickel chloride, the inorganic salts of Fe are ferrous sulfate, Ce
Inorganic salts be cerous nitrate, concentration is 0.025mol/L.
4. one kind according to claim 1 obtains dimensional thinlayer shape NiFe/CeO by topology reducing process in situ2It is nano combined
The method of material, it is characterised in that：Step（1）Described in sodium hydroxide solution concentration be 0.1mol/L.
5. a kind of dimensional thinlayer shape NiFe/CeO obtained by topology reducing process in situ according to claim 12Nanometer is multiple
The method of condensation material, it is characterised in that：Step（1）Described in the precipitation reaction time be 1 hour.
6. a kind of dimensional thinlayer shape NiFe/CeO obtained by topology reducing process in situ according to claim 12Nanometer is multiple
The method of condensation material, it is characterised in that：Step（1）And step（2）Described in washing all be use deionized water and anhydrous second
Alcohol carries out alternately washing.
7. a kind of dimensional thinlayer shape NiFe/CeO obtained by topology reducing process in situ according to claim 12Nanometer is multiple
The method of condensation material, it is characterised in that：Step（1）And step（2）Described in centrifugation rotating speed be 6000 revs/min,
Time is 5 minutes.
8. a kind of dimensional thinlayer shape NiFe/CeO obtained by topology reducing process in situ according to claim 12Nanometer is multiple
The method of condensation material, it is characterised in that：Step（1）And step（2）Described in drying be to be done at 60 DEG C of vacuum drying chamber
Dry 10h.
9. one kind according to claim 1 obtains dimensional thinlayer shape NiFe/CeO by topology reducing process in situ2It is nano combined
The method of material, it is characterised in that：Step（2）Described in the ethylene glycol solution dissolved with NaOH, its concentration is
0.25mol/L。
10. one kind according to claim 1 obtains dimensional thinlayer shape NiFe/CeO by topology reducing process in situ2Nanometer is multiple
The method of condensation material, it is characterised in that：Step（2）Described in the reduction reaction time be 12 hours, reaction temperature be 140 DEG C -180
℃。
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Cited By (2)
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| CN108479783A (en) * | 2018-03-13 | 2018-09-04 | 同济大学 | Two-dimensional ultrathin is from independent NiCu-SiO2Nanocomposite and its synthetic method |
| CN114944492A (en) * | 2022-01-28 | 2022-08-26 | 上海应用技术大学 | Preparation method of two-dimensional ultrathin nano composite material |
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Application publication date: 20170707 |