CN105931774B - The method that ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material is prepared using ferrous gluconate as single raw material - Google Patents
The method that ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material is prepared using ferrous gluconate as single raw material Download PDFInfo
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Abstract
The present invention provides a kind of method for preparing ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material, it is with single Fe2+Salt ferrous gluconate is source of iron and carbon source, H2O is solvent, and using hydro-thermal method, by controlling hydrothermal condition, a step is prepared for the Fe with high magnetic characteristics3O4With with similar graphene oxide structural carbon（LGO）Magnetic nanometer composite material Fe3O4/LGO.The method of the present invention is without other any additives（Such as alkaline precipitating agent, oxidant, catalyst, surfactant）, need not more carry out Fe3O4Under conditions of the surface modification of material, a step realizes Fe3O4, LGO generation and the two is effective compound, prepare the alternate Fe there are strong interaction3O4/ LGO magnetic composites, have outstanding advantages of technique is simple, flow is short, cost is low, environmentally protective, are conducive to industrialize.
Description
Technical field
The present invention relates to a kind of ferroso-ferric oxide/class graphene oxide（Fe3O4/LGO）The system of magnetic nanometer composite material
It is standby, more particularly to one kind is with ferrous gluconate Fe (OOC (CHOH)4CH2OH)2Fe is prepared for single one step of raw material3O4/ LGO magnetic
The method of property nanocomposite, belongs to technical field of nano material.
Background technology
The fast development of chemical science, while bringing huge materiality achievement to the mankind, also result in environment dirt
The negative effect such as dye, ecocrisis and energy waste, therefore, people advocate the theory of Green Chemistry：Safe and non-toxic, synthesis letter
It is single, product property is excellent etc., reduce the negative interaction to environment and the mankind as far as possible from source.
In recent years, Fe3O4/ C magnetic composites are being inhaled with its excellent magnetic property, absorption property and heat conductivility etc.
Enclosure material, electromagnetic shielding, microwave absorbing material, anti-corrosion of metal, stealth material etc. have a wide range of applications, therefore with non-
Often wide application prospect.
Generally, for Fe3O4The preparation of/C magnetic composites is except the Fe with stoichiometric ratio2+、Fe3+Salt or list
One Fe2+Or Fe3+Salt is cooked outside source of iron, also needs to introduce carbon source.It is in addition, single from formation Fe3O4The angle of phase is said, no matter using chemistry
Metering is than (1:2) Fe2+、Fe3+Salt, or with single Fe2+Or Fe3+Salt is cooked source of iron, and most of preparation method, which is removed, to be added
Add outside alkaline precipitating agent, also need addition oxidation or reducing agent, to realize conversion Fe2+→Fe3+Or Fe3+→Fe2+, so as to ensure to turn
Change Fe2++Fe3+→Fe3O4；Again because of Fe2+Easily it is oxidized to Fe3+, therefore the stringent control of experiment condition need to be carried out.Therefore, it is this kind of
The preparation method of composite material mostly there are preparation process is complicated, condition is difficult to strictly control, it is of high cost, easily cause environment dirt
Dye etc., and be difficult to purity height, the Fe of excellent performance is made3O4The shortcomings of.
The content of the invention
In order to solve the problems in the prior art, the purpose of the present invention is to, there is provided it is a kind of simple and direct, efficient, green, inexpensive
Prepare ferroso-ferric oxide/class graphene oxide（Fe3O4/LGO）The method of magnetic nanometer composite material.
First, Fe3O4The preparation of/LGO
The present invention prepares ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material（Fe3O4/LGO）Method, be
Ferrous gluconate is single raw material, and using water as solvent, 5 ~ 15 h are reacted at 180 ~ 220 DEG C（8~10h）；Reaction terminates
Centrifuge, wash afterwards, is dry, up to ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material.
The molar concentration of ferrous gluconate in a solvent is 0.0833 ~ 0.2083 mol/L.
The washing is to be washed successively using secondary, absolute ethyl alcohol.
The drying is dry 9 ~ 11 h at 90 ~ 100 DEG C in an oven.
2nd, Fe3O4The characterization of/LGO
The sample F e of gained will be prepared below with technologies such as XRD, IR, TEM, VSM3O4/ LGO is characterized, analyzed.
1st, XRD analysis
Fig. 1 a, b are given to be H2O solvents, under different hydrothermal temperatures, time conditions, the XRD knots of gained sample
Fruit.Should the result shows that, control hydrothermal temperature exists, and 180 ~ 220 DEG C of reaction time in 5 ~ 15 h, can obtain purity
Target components Fe high, crystal property is good3O4, that is, realize Fe3O4Controllable preparation.
2nd, IR is analyzed
The IR figures that Fig. 2 is sample F F/LGO prepared by the present invention.3400 cm-1Neighbouring Bao Fengyu-OH are related, it should return
In absorption water（See the XPS results of sample）；1700 cm-1Locate as the vibration absorption peak of carbonyl C=O, 1630 ~ 1300 cm-1Section
There is the eigen vibration absworption peak similar to conjugated alkene/aromatic ring frame.Should the result shows that：In hydrothermal condition and Fe2+In the presence of
Under conditions of, CH2OH(CHOH)4COO-Pass through dehydration（There occurs reduction reaction）（According to convention, it is also possible to exist to a certain degree
Decarboxylation phenomenon）, interchain it is a degree of crosslinking etc. and be carbonized, form the carbon materials containing polar group C=O and C=C conjugated structure
Material（Class graphene oxide composite material-LGO is called for the time being）.588 cm-1It is nearby the absworption peak of inorganic Fe-O.
With reference to the XRD results of sample, it is believed that：In the water-heat process, Fe (OOC (CHOH)4CH2OH)2Divided
Oxidation-reduction reaction in son, i.e. Fe2+ + CH2OH(CHOH)4COO-→Fe3O4 + LGO, it is achieved thereby that by single Fe2+Source
Under without other any additive existence conditions, Fe3O4It is prepared by one step of/LGO nanocomposites.
3rd, XPS analysis
The XPS that Fig. 3 is sample F F/LGO schemes.From score Fig. 3, contain tri- kinds of elements of C, O and Fe in sample.By width
And asymmetric Fe2pPeak proves that there are the Fe of different valence state in sample：Fe3+And Fe2+, which absolutely proves in the hydro-thermal mistake
Cheng Zhong, Fe2+It is partially converted into Fe3+（Fe2+→Fe3+, oxidation reaction occurs）, so as to ensure by single Fe2+To Fe3O4Conversion
（Fe2+→Fe3O4）.Equally, by folding discovery to the solution of C, O spectral peak：It is substantially C=O and C=C that the presence of C, which is formed, in LGO；Sample
O in product has 2 kinds：Lattice Oxygen O2-With ketonic oxygen C=O.Therefore, the XPS of C and O without-OH groups the result shows that deposit substantially in LGO
.
4、SEM
The SEM that Fig. 4 is sample F F/LGO-1 schemes.As can be seen that sample is Fe3O4With the good compound of carbon material, nothing
Fe3O4, i.e., should there are strong interaction between two-phase with the phase separation of carbon material.More importantly finding substantial amounts of sample is
Formed by layer-layer accumulation.Therefore, comprehensive IR, XPS, SEM as a result, we have reason the carbon material in composite material being known as
Class graphene.
5th, magnetic property is analyzed
Fig. 5 is the hysteresis graph of sample F F/LGO-1 ~ 4, inserts composition and magnetic intensity that table is sample.It can be obtained by Fig. 5,
Different Fe (OOC (CHOH)4CH2OH)2Under the conditions of initial concentration, the composite wood of good magnetic property can be obtained by hydro-thermal reaction
Expect Fe3O4/ LGO, and Fe3O4The magnetic property of/LGO is with Fe (OOC (CHOH)4CH2OH)2The increase of initial concentration and weaken.
With reference to the XRD results of sample, it is believed that Fe in sample3O4Crystal property should be influence its magnetic property principal element, knot
Brilliant performance is better, and magnetic property is stronger.In the range of the initial concentration studied, in relatively low Fe (OOC (CHOH)4CH2OH)2Just
Beginning concentration（0.0833 mol/L）Under the conditions of, the intensity of magnetization of gained sample is maximum, is 68.8 emu/g.In addition, by gained material
Expect Fe in FF/LGO-1 ~ 43O4Actual compound quantity vary less（40.5~41.2 %）（See illustration）, can further prove Fe
(OOC(CHOH)4CH2OH)2The oxidation-reduction reaction of intramolecular.
3rd, influence of the reaction condition to nanocomposite performance
In order to obtain the composite material of high-purity and good magnetic property, the present invention has investigated solvent（EtOH、H2O and EtOH+
H2O（1:1v/v）, 180 ~ 220 DEG C of solvent heat temperature, solvent heat time 5 ~ 5 h and Fe (OOC (CHOH)4CH2OH)2·2H2O's rubs
That concentration（0.0833 ~0.2083 mol/L）Influence for product property.
1st, solvent is to magnetic component Fe3O4Formation and magnetism of material can influence
By 1.9291g Fe (OOC (CHOH)4CH2OH)2·2H2O is dissolved separately in 48.00 mL EtOH, EtOH+H2O（1:
1v/v）And H2In O, ptfe autoclave is transferred to, 10 h are reacted at 200 DEG C；Solid product is centrifuged, is washed
Wash, is dry.It turns out that as solvent is by EtOH → EtOH+H2O→H2O, i.e., with H2The addition of O and its increase of amount, gained
The magnetic intensity of composite material（Gone to examine them magnetic with same magnet）By without → it is weak → strong.That is, solvent H2O is favourable
In the formation of magnetic material, therefore, the present invention selects H2O makees solvent.
2nd, hydrothermal temperature is to magnetic component Fe3O4Formation and magnetism of material can influence
By 1.9291 g Fe (OOC (CHOH)4CH2OH)2·2H2O is dissolved in 48.00 mL H2In O, respectively 180,
200th, 10 h are reacted at 220 DEG C, equally solid product is centrifuged, is washed, is dry, obtains sample（See Fig. 1 a）.Can by Fig. 1 a
Know, with the rise of hydrothermal temperature, non-magnetic impurity component Fe in product2O3Amount reduce, target magnetic component Fe3O4
Increase.That is low temperature is unfavorable for magnetic component Fe3O4Formation.Many experiments show, solvent heat temperature control 180 ~
220℃（It is preferred that 200 DEG C）, obtained composite material has good magnetic property.
3rd, the hydro-thermal time is to magnetic component Fe3O4Formation and magnetism of material can influence
At 200 DEG C, 5,10,15 h are reacted respectively, other to be same as above, the XRD of products therefrom is shown in Fig. 1 b.Can by Fig. 1 b
Know, when the hydro-thermal time is 5 h, there are substantial amounts of impurities phase Fe in product2O3；When hydro-thermal time lengthening is to 10 h, impurities phase
Fe2O3It is obvious to weaken, and continue increase change less with the hydro-thermal time.Consider the factor of cost and energy consumption, the hydro-thermal time is controlled
System is advisable in 8 ~ 10h.
4th, ferrous gluconate concentration is to magnetic component Fe3O4Formation and magnetism of material can influence
By 1.9291,2.8933,3.8575,4.8216 g Fe (OOC (CHOH)4CH2OH)2·2H2O（With Fe2+Mole
Concentration represents, is respectively 0.0833,0.1250,0.1667,0.2083 mol/L）It is added separately to 48.00 mL H2In O,
10 h of hydro-thermal reaction at 200 DEG C.Solid product is washed successively, is dry, resulting materials successively labeled as FF/LGO-1,
FF/LGO-2、FF/LGO-3、FF/LGO-4.The composition of the series of samples（Content）Determined by sour dissolving method, will be certain
The sample of amount soaks a few days in the HCl solution of 6 mol/L, to be completely dissolved metal oxide therein, before and after immersion
The change of quality, calculates Fe in the composite material3O4Actual compound quantity.Fig. 6 is present invention sample prepared with optimal conditions
The XRD diagram of product FF/LGO-1, FF/LGO-4.Found by the XRD of two samples in comparison diagram 6, Fe (OOC (CHOH)4CH2OH)2It is dense
Degree does not influence the phase of Gold Samples category oxide, but influences target phase-inverse spinel structure Fe3O4Diffraction peak intensity, i.e., its tie
Brilliant performance.With regard to concentration of raw material for the influence of the crystal property of sample, relatively low material concentration is conducive to the orientation of particle
The target components of the preferable crystal property of arrangement form.
4th, single Fe2+Salt forms target phase Fe3O4Principle
In order to study single Fe2+Salt forms target phase Fe3O4Principle, the present invention also investigated hydro-thermal atmosphere-air and
Nitrogen is to Fe3O4The influence of formation.The result shows that：Hydro-thermal atmosphere-air, nitrogen have substantially no effect on the composition of sample, that is,
Say, the dissolved oxygen in water is for converting Fe2+→Fe3+Influence it is little.Therefore, we with for：In the water-heat process of the present invention
In, in single raw material Fe (OOC (CHOH)4CH2OH)2In the presence of, it should it is glucose acid group CH2OH(CHOH)4COO-
Oxygen loss（See the IR of gained sample）, make Fe2+Ionic portions are oxidized into Fe3+Ion, so as to ensure that target phase Fe3O4Formation
（Fe2++Fe3+→Fe3O4）.
In conclusion the present invention is with single Fe2+Salt ferrous gluconate Fe (OOC (CHOH)4CH2OH)2For source of iron and carbon
Source, H2O is solvent, and using hydro-thermal method, by controlling hydrothermal condition, a step is prepared for the Fe with high magnetic characteristics3O4With with class
Like the magnetic nanometer composite material Fe of graphene oxide structural carbon (LGO)3O4/LGO.This method is without other any additives（Such as
Alkaline precipitating agent, oxidant, other carbon sources, surfactant etc.）, need not more carry out Fe3O4The condition of the surface modification of material
Under, a step realizes Fe3O4, LGO generation and the two is effective compound, prepare the alternate Fe there are strong interaction3O4/
LGO magnetic composites.Such composite material is in microwave absorption, electromagnetic shielding, super capacitor material, stealth material, air-sensitive
Material etc. is widely used.In addition, the present invention has, technique is simple, flow is short, cost is low, the protrusion such as environmentally protective is excellent
Point, is conducive to industrialize.
Brief description of the drawings
Fig. 1 is different hydrothermal temperatures, the XRD diagram of product is obtained under the time.
The IR that Fig. 2 is sample F F/LGO-1 schemes.
The XPS that Fig. 3 is sample F F/LGO schemes.
The TEM figures of Fig. 4 sample Fs F/LGO-1.
Fig. 5 is the B-H loop and the intensity of magnetization of sample F F/LGO-1 ~ 4.
Fig. 6 is the XRD diagram of sample F F/LGO-1, FF/LGO-4.
Embodiment
Below by specific embodiment to Fe of the present invention3O4The preparation of/LGO magnetic nanometer composite materials and its performance are made
Further illustrate.
Embodiment 1
By 1.9291 g Fe (OOC (CHOH)4CH2OH)2·2H2O（With Fe2+Molar concentration be expressed as 0.0833 mol/
L）It is added to 48.00 mL H2In O, after stirring and dissolving, it is transferred in ptfe autoclave, at 200 DEG C, reacts 10 h.
After reaction, solid product is placed on baking oven with absolute ethyl alcohol, secondary water washing, dry 9 ~ 11 at 90 ~ 100 DEG C
H, obtains composite material FF/LGO-1.
A certain amount of material is soaked into 24 h in the HCl solution of 6 mol/L, according to the change meter of quality before and after immersion
Calculate Fe in the composite material3O4Actual compound quantity be 41.2 %.The intensity of magnetization of the composite material is 68.8 emu/g.
Embodiment 2
Fe(OOC(CHOH)4CH2OH)2·2H2The addition of O is 2.8933 g（With Fe2+Molar concentration be expressed as
0.1250 mol/L）, other conditions are with embodiment 1, obtained composite material FF/LGO-2.Fe in the composite material3O4Reality
Compound quantity is 41.0 %；Its intensity of magnetization is 58.2 emu/g.
Embodiment 3
Fe(OOC(CHOH)4CH2OH)2·2H2The addition of O is 3.8575 g（With Fe2+Molar concentration be expressed as
0.1667 mol/L）, other conditions are with embodiment 1, obtained composite material FF/LGO-3.
Fe in the composite material3O4Actual compound quantity be 40.6 %；Its intensity of magnetization is 50.3 emu/g.
Embodiment 4
Fe(OOC(CHOH)4CH2OH)2·2H2The addition of O is 4.8216 g（With Fe2+Molar concentration be expressed as
0.2083 mol/L）, other conditions are with embodiment 1, obtained composite material FF/LGO-4.
Fe in the composite material3O4Actual compound quantity be 40.5 %；Its intensity of magnetization is 49.1 emu/g.
Claims (3)
1. the side of ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material is prepared using ferrous gluconate as single raw material
Method, is using ferrous gluconate as raw material, and water is solvent, 8 ~ 10 h of hydro-thermal reaction at 180 ~ 220 DEG C；Reaction terminates
Centrifuge, wash afterwards, is dry, up to ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material；
The molar concentration of the ferrous gluconate in a solvent is 0.0833 ~ 0.2083 mol/L.
2. it is magnetic to prepare ferroso-ferric oxide/class graphene oxide using ferrous gluconate as single raw material as claimed in claim 1
The method of nanocomposite, it is characterised in that：The washing is to be washed successively using secondary, absolute ethyl alcohol.
3. it is magnetic to prepare ferroso-ferric oxide/class graphene oxide using ferrous gluconate as single raw material as claimed in claim 1
The method of nanocomposite, it is characterised in that：The drying is dry 9 ~ 11 h at 90 ~ 100 DEG C in an oven.
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Denomination of invention: Method for preparing iron tetroxide/graphene oxide like magnetic nanocomposites using ferrous gluconate as a single raw material Effective date of registration: 20230904 Granted publication date: 20180413 Pledgee: Dongchen sub branch of Jiangsu Rugao Rural Commercial Bank Co.,Ltd. Pledgor: Jiangsu bangzheng New Material Co.,Ltd. Registration number: Y2023980054945 |