CN105931774A - Method for preparing ferroferric oxide/graphene oxide-like magnetic nanocomposite by taking ferrous gluconate as single raw material - Google Patents
Method for preparing ferroferric oxide/graphene oxide-like magnetic nanocomposite by taking ferrous gluconate as single raw material Download PDFInfo
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- CN105931774A CN105931774A CN201610295631.XA CN201610295631A CN105931774A CN 105931774 A CN105931774 A CN 105931774A CN 201610295631 A CN201610295631 A CN 201610295631A CN 105931774 A CN105931774 A CN 105931774A
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- ferrous gluconate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
Abstract
The invention provides a method for preparing a ferroferric oxide/graphene oxide-like magnetic nanocomposite by taking ferrous gluconate as a single raw material. The single Fe<2+> ferrous gluconate is taken as the iron source and the carbon source; H<2>O is taken as the solvent; the Fe<3>O<4> with high magnetic property and magnetic nanocomposite Fe<3>O<4>/LGO with the graphene oxide-like structure carbon (LGO) are prepared by one step through a hydrothermal method by controlling the hydrothermal conditions. According to the method, any other additive (such as an alkali precipitator, an oxidizing agent, a catalyst, a surfactant and the like) is not required; surface modification of the Fe<3>O<4> material is not required either; the generation and effective compounding of the Fe<3>O<4> and the LGO are realized in one step; the Fe<3>O<4>/LGO magnetic composite material with strong interphase interaction is prepared; and in addition, the magnetic nanocomposite has the outstanding advantages of simple process, short process, low cost, green and environment-friendly performance and the like, so that the industrialization of the magnetic nanocomposite can be promoted.
Description
Technical field
The present invention relates to a kind of ferroso-ferric oxide/class graphene oxide (Fe3O4/ LGO) system of magnetic nanometer composite material
Standby, particularly relate to a kind of with ferrous gluconate Fe (OOC (CHOH)4CH2OH)2Fe is prepared for single raw material one step3O4/ LGO magnetic
The method of property nano composite material, 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 dirty
The negative effect such as dye, ecocrisis and energy waste, therefore, people advocate the theory of Green Chemistry: safety non-toxic, synthesis letter
List, product property are excellent, reduce the negative interaction to environment and the mankind from source as far as possible.
In recent years, Fe3O4/ C magnetic composite, with its excellent magnetic property, absorption property and heat conductivility etc., is being inhaled
The aspects such as enclosure material, electromagnetic shielding, microwave absorbing material, anti-corrosion of metal, stealth material have a wide range of applications, and therefore have non-
The most wide application prospect.
Generally, for Fe3O4The preparation of/C magnetic composite is except with the Fe of stoichiometric proportion2+、Fe3+Salt or list
The Fe of one2+Or Fe3+Salt is cooked outside source of iron, also needs to introduce carbon source.It addition, it is single from forming Fe3O4The angle of phase is said, no matter using chemistry
Measure the Fe than (1:2)2+、Fe3+Salt, or with single Fe2+Or Fe3+Salt is cooked source of iron, and most of preparation method is except adding
Add outside alkaline precipitating agent, also need to add oxidation or reducing agent, to realize converting Fe2+→Fe3+Or Fe3+→Fe2+, thus ensure to turn
Change Fe2++Fe3+→Fe3O4；Again because of Fe2+Easily it is oxidized to Fe3+, therefore the strict control of experiment condition need to be carried out.Therefore, this kind of
The preparation method of composite exists that preparation process is complicated mostly, condition is difficult to strictly to control, cost is high, it is dirty to easily cause environment
Dye etc., and be difficult to prepare purity height, the Fe of excellent performance3O4Etc. shortcoming.
Summary of the invention
The problem that it is an object of the invention to exist for prior art, it is provided that one is simple and direct, efficient, green, prepared by low cost
Ferroso-ferric oxide/class graphene oxide (Fe3O4/ LGO) method of magnetic nanometer composite material.
One, Fe3O4The preparation of/LGO
The present invention prepares ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material (Fe3O4/ LGO) method, be grape
Saccharic acid ferrous iron is single raw material, with water as solvent, reacts 5 ~ 15 h(8 ~ 10h at 180 ~ 220 DEG C)；Reaction terminate after from
The heart, wash, be dried, obtain ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material.
Ferrous gluconate molar concentration in a solvent is 0.0833 ~ 0.2083 mol/L.
Described washing is to use secondary, absolute ethyl alcohol to wash successively.
Described being dried is in an oven, is dried 9 ~ 11 h at 90 ~ 100 DEG C.
Two, Fe3O4The sign of/LGO
Sample F e of gained will be prepared below with technology such as XRD, IR, TEM, VSM3O4/ LGO carries out characterizing, analyzing.
1, XRD analysis
Fig. 1 a, b give to be H2O solvent, under different hydrothermal temperatures, time conditions, the XRD result of gained sample.Should
Result shows, controls hydrothermal temperature and exists, and 180 ~ 220 DEG C of reaction time, at 5 ~ 15 h, all can get purity height, crystallization
Target components Fe that performance is good3O4, i.e. realize Fe3O4Controlled preparation.
2, IR analyzes
Fig. 2 is the IR figure of sample F F/LGO prepared by the present invention.3400 cm-1Neighbouring Bao Fengyu-OH is relevant, it should be attributed to inhale
Attached water (see the XPS result of sample)；1700 cm-1Place is the vibration absorption peak of carbonyl C=O, 1630 ~ 1300 cm-1Interval occur
It is similar to the eigen vibration absworption peak of conjugated alkene/aromatic ring frame.This result shows: at hydrothermal condition and Fe2+The bar existed
Under part, CH2OH(CHOH)4COO-By dehydration (there occurs reduction reaction) (according to convention, it is also possible to exist a certain degree of de-
Carboxylic phenomenon), a certain degree of crosslinking of interchain etc. and carbonization, formed containing polar group C=O and the material with carbon element of C=C conjugated structure
(being called class graphene oxide composite material-LGO for the time being).588 cm-1Near be the absworption peak of inorganic Fe-O.
In conjunction with the XRD of sample as a result, it is possible to think: in this water-heat process, Fe (OOC (CHOH)4CH2OH)2There occurs point
Oxidation-reduction reaction in son, i.e. Fe2+ + CH2OH(CHOH)4COO-→Fe3O4 + LGO, it is achieved thereby that by single Fe2+Source
Without under other any additive existence condition, Fe3O4Prepared by one step of/LGO nano composite material.
3, XPS analysis
Fig. 3 is the XPS figure of sample F F/LGO.From score Fig. 3, containing tri-kinds of elements of C, O and Fe in sample.By width not
Symmetrical Fe2pPeak proves to exist in sample the Fe:Fe of different valence state3+And Fe2+, this result absolutely proves in this water-heat process,
Fe2+It is partially converted into Fe3+(Fe2+→Fe3+, there is oxidation reaction), thus ensure by single Fe2+To Fe3O4Conversion (Fe2+→
Fe3O4).Equally, by finding the solution of C, O spectral peak is folded: in LGO, the existence of C forms substantially C=O and C=C；O in sample
There are 2 kinds: Lattice Oxygen O2-With ketonic oxygen C=O.Therefore, the XPS result of C and O shows substantially to exist without-OH group in LGO.
4、SEM
Fig. 4 is the SEM figure of sample F F/LGO-1.It can be seen that sample is Fe3O4With the good compound of material with carbon element, without Fe3O4
With being separated of material with carbon element, strong interaction i.e. between two-phase, should be there is.The more important thing is discovery substantial amounts of sample be by layer-
Layer stack is long-pending to be formed.Therefore, the result of comprehensive IR, XPS, SEM, we have reason the material with carbon element in composite is referred to as class graphite
Alkene.
5, magnetic property analysis
Fig. 5 is the hysteresis graph of sample F F/LGO-1 ~ 4, and slotting table is composition and the magnetic intensity of sample.Can be obtained by Fig. 5, in difference
Fe(OOC(CHOH)4CH2OH)2Under the conditions of initial concentration, the composite of good magnetic property can be obtained by hydro-thermal reaction
Fe3O4/ LGO, and Fe3O4The magnetic property of/LGO is with Fe (OOC (CHOH)4CH2OH)2The increase of initial concentration and weaken.Knot
Close the XRD of sample as a result, it is possible to think Fe in sample3O4Crystal property should be the principal element affecting its magnetic property, crystallization
Performance is the best, and magnetic property is the strongest.In the range of the initial concentration studied, at relatively low Fe (OOC (CHOH)4CH2OH)2Initially
Under the conditions of concentration (0.0833 mol/L), the intensity of magnetization of gained sample is maximum, is 68.8 emu/g.It addition, by resulting materials
Fe in FF/LGO-1 ~ 43O4Actual compound quantity vary less (40.5 ~ 41.2 %) (see illustration), Fe can be proved further
(OOC(CHOH)4CH2OH)2Intramolecular oxidation-reduction reaction.
Three, the reaction condition impact on nano composite material performance
In order to obtain high-purity and the composite of good magnetic property, the present invention has investigated solvent (EtOH, H2O and EtOH+H2O
(1:1v/v), solvent heat temperature 180 ~ 220 DEG C, solvent heat time 5 ~ 5 h and Fe (OOC (CHOH)4CH2OH)2·2H2O mole
Concentration (0.0833 ~ 0.2083 mol/L) is for the impact of product property.
1, solvent is to magnetic component Fe3O4Formation and magnetism of material can impact
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, proceed to polytetrafluoroethylene (PTFE) reactor, at 200 DEG C, react 10 h；Solid product is centrifuged, washs, does
Dry.It was found that along with solvent is by EtOH → EtOH+H2O→H2O, i.e. with H2O adds and the increase of amount, gained composite wood
The magnetic intensity (going to check they magnetic with same magnet) of material by without → weak → strong.It is to say, solvent H2O is conducive to magnetic
The formation of material, therefore, the present invention selects H2O makees solvent.
2, hydrothermal temperature is to magnetic component Fe3O4Formation and magnetism of material can impact
By 1.9291 g Fe (OOC (CHOH)4CH2OH)2·2H2O is dissolved in 48.00 mL H2In O, respectively 180,200,
React 10 h at 220 DEG C, equally solid product is centrifuged, washs, is dried, obtain sample (see Fig. 1 a).From Fig. 1 a, with
The rising of hydrothermal temperature, non-magnetic impurity component Fe in product2O3Amount reduce, target magnetic component Fe3O4Increasing
Greatly.That is low temperature is unfavorable for magnetic component Fe3O4Formation.Great many of experiments shows, solvent heat temperature controls 180 ~ 220
DEG C (preferably 200 DEG C), the composite obtained has good magnetic property.
3, the hydro-thermal time is to magnetic component Fe3O4Formation and magnetism of material can impact
At 200 DEG C, react 5,10,15 h respectively, other ibid, the XRD of products therefrom is shown in Fig. 1 b.From Fig. 1 b, when
When the hydro-thermal time is 5 h, product exists substantial amounts of impurity phase Fe2O3；When hydro-thermal time lengthening to 10 h, impurity phase Fe2O3
Substantially weaken, and it is little to increase change with the continuation of hydro-thermal time.Consider cost and the factor of energy consumption, the hydro-thermal time is controlled
8 ~ 10h is advisable.
4, ferrous gluconate concentration is to magnetic component Fe3O4Formation and magnetism of material can impact
By 1.9291,2.8933,3.8575,4.8216 g Fe (OOC (CHOH)4CH2OH)2·2H2O(is with Fe2+Molar concentration
Represent, respectively 0.0833,0.1250,0.1667,0.2083 mol/L) be added separately to 48.00 mL H2In O, 200
Hydro-thermal reaction 10 h at DEG C.Carrying out solid product successively washing, being dried, resulting materials is labeled as FF/LGO-1, FF/ successively
LGO-2、FF/LGO-3、FF/LGO-4.The composition (content) of this series of samples is determined by acid dissolving method, will be a certain amount of
Sample soaks a few days in the HCl solution of 6 mol/L, to be completely dissolved metal oxide therein, according to quality before and after soaking
Change, calculate Fe in this composite3O4Actual compound quantity.Fig. 6 is the present invention prepared sample with optimal conditions
The XRD of FF/LGO-1, FF/LGO-4.Found by the XRD of two samples in comparison diagram 6, Fe (OOC (CHOH)4CH2OH)2Concentration
Do not affect Gold Samples and belong to the phase of oxide, but affect target phase-inverse spinel structure Fe3O4Diffraction peak intensity, i.e. its crystallization
Performance.With regard to concentration of raw material for the impact of the crystal property of sample, relatively low material concentration is conducive to the orientation of particle to arrange
Row form the target components of preferable crystal property.
Four, single Fe2+Salt forms target phase Fe3O4Principle
In order to study single Fe2+Salt forms target phase Fe3O4Principle, the present invention has also investigated hydro-thermal atmosphere-air and nitrogen
To Fe3O4The impact formed.Result shows: hydro-thermal atmosphere-air, nitrogen have substantially no effect on the composition of sample, say, that water
In dissolved oxygen for convert Fe2+→Fe3+Impact little.Therefore, we think: in the water-heat process of the present invention, at list
One 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 is oxidized into Fe3+Ion, thus ensure that target phase Fe3O4Formation (Fe2++
Fe3+→Fe3O4).
In sum, the present invention is with single Fe2+Salt ferrous gluconate Fe (OOC (CHOH)4CH2OH)2For source of iron and carbon
Source, H2O is solvent, utilizes hydro-thermal method, and by controlling hydrothermal condition, a step is prepared for the Fe with high magnetic characteristics3O4With there is class
Magnetic nanometer composite material Fe like graphene oxide structural carbon (LGO)3O4/LGO.The method without other any additive (as
Alkaline precipitating agent, oxidant, other carbon source, surfactant etc.), more without carrying out Fe3O4The condition that the surface of material is modified
Under, a step achieves Fe3O4, the generation of LGO and the two is effectively compound, prepare the alternate Fe that there is strong interaction3O4/
LGO magnetic composite.Such composite is in microwave absorption, electromagnetic shielding, super capacitor material, stealth material, air-sensitive
The aspects such as material are widely used.It addition, the present invention has, technique is simple, flow process is short, low cost, environmental protection etc. are prominent excellent
Point, is conducive to industrialization.
Accompanying drawing explanation
Fig. 1 is different hydrothermal temperature, obtains the XRD of product under the time.
Fig. 2 is the IR figure of sample F F/LGO-1.
Fig. 3 is the XPS figure of sample F F/LGO.
The TEM figure of Fig. 4 sample F F/LGO-1.
Fig. 5 is B-H loop and the intensity of magnetization of sample F F/LGO-1 ~ 4.
Fig. 6 is the XRD of sample F F/LGO-1, FF/LGO-4.
Detailed description of the invention
Below by specific embodiment to Fe of the present invention3O4The preparation of/LGO magnetic nanometer composite material and its performance are made
Further illustrate.
Embodiment 1
By 1.9291 g Fe (OOC (CHOH)4CH2OH)2·2H2O(is with Fe2+Molar concentration be expressed as 0.0833 mol/L) add
Enter to 48.00 mL H2In O, after stirring and dissolving, proceed in polytetrafluoroethylene (PTFE) reactor, at 200 DEG C, react 10 h.Reaction
After end, solid product absolute ethyl alcohol, the washing of secondary water are placed on baking oven, at 90 ~ 100 DEG C, are dried 9 ~ 11 h,
To composite FF/LGO-1.
This material a certain amount of is soaked 24 h in the HCl solution of 6 mol/L, according to the change meter of quality before and after soaking
Calculate Fe in this composite3O4Actual compound quantity be 41.2 %.The intensity of magnetization of this composite is 68.8 emu/g.
Embodiment 2
Fe(OOC(CHOH)4CH2OH)2·2H2The addition of O is that 2.8933 g(are with Fe2+Molar concentration be expressed as 0.1250
Mol/L), other condition is with embodiment 1, the composite FF/LGO-2 obtained.Fe in this composite3O4Actual compound quantity
It is 41.0 %；Its intensity of magnetization is 58.2 emu/g.
Embodiment 3
Fe(OOC(CHOH)4CH2OH)2·2H2The addition of O is that 3.8575 g(are with Fe2+Molar concentration be expressed as 0.1667
Mol/L), other condition is with embodiment 1, the composite FF/LGO-3 obtained.
Fe in this composite3O4Actual 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 that 4.8216 g(are with Fe2+Molar concentration be expressed as 0.2083
Mol/L), other conditions are with embodiment 1, the composite FF/LGO-4 obtained.
Fe in this composite3O4Actual compound quantity be 40.5 %；Its intensity of magnetization is 49.1 emu/g.
Claims (5)
1. it is the side that ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material prepared by single raw material with ferrous gluconate
Method, is with ferrous gluconate as raw material, and water is solvent, hydro-thermal reaction 5 ~ 15 h at 180 ~ 220 DEG C；Reaction terminates
After be centrifuged, wash, be dried, obtain ferroso-ferric oxide/class graphene oxide magnetic nanometer composite material.
2. as claimed in claim 1 is that ferroso-ferric oxide/class graphene oxide magnetic prepared by single raw material with ferrous gluconate
The method of nano composite material, it is characterised in that: described ferrous gluconate molar concentration in a solvent is 0.0833 ~
0.2083 mol/L。
3. as claimed in claim 1 is that ferroso-ferric oxide/class graphene oxide magnetic prepared by single raw material with ferrous gluconate
The method of nano composite material, it is characterised in that: it is 8 ~ 10 h between described hydro-thermal reaction.
4. as claimed in claim 1 is that ferroso-ferric oxide/class graphene oxide magnetic prepared by single raw material with ferrous gluconate
The method of nano composite material, it is characterised in that: described washing is to use secondary, absolute ethyl alcohol to wash successively.
5. as claimed in claim 1 is that ferroso-ferric oxide/class graphene oxide magnetic prepared by single raw material with ferrous gluconate
The method of nano composite material, it is characterised in that: described being dried is in an oven, is dried 9 ~ 11 h at 90 ~ 100 DEG C.
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| CN107758655A (en) * | 2017-10-26 | 2018-03-06 | 华南师范大学 | A kind of porous graphite and preparation method and application |
| CN108751262A (en) * | 2018-06-14 | 2018-11-06 | 重庆科技学院 | It is a kind of to prepare Fe3O4Method |
| CN110164642A (en) * | 2019-04-23 | 2019-08-23 | 中北大学 | A kind of the hypergravity preparation method and device of graphene oxide modified magnetic nano material |
| CN113697863A (en) * | 2021-09-09 | 2021-11-26 | 华东理工大学 | Ferroferric oxide/carbon nanosheet composite material with excellent electromagnetic wave absorption performance and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107758655A (en) * | 2017-10-26 | 2018-03-06 | 华南师范大学 | A kind of porous graphite and preparation method and application |
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| CN110164642A (en) * | 2019-04-23 | 2019-08-23 | 中北大学 | A kind of the hypergravity preparation method and device of graphene oxide modified magnetic nano material |
| CN113697863A (en) * | 2021-09-09 | 2021-11-26 | 华东理工大学 | Ferroferric oxide/carbon nanosheet composite material with excellent electromagnetic wave absorption performance and preparation method and application thereof |
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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 |
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