CN103224255A - Preparation method of iron oxyhydroxide/graphene oxide composite material - Google Patents
Preparation method of iron oxyhydroxide/graphene oxide composite material Download PDFInfo
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- CN103224255A CN103224255A CN2013101125194A CN201310112519A CN103224255A CN 103224255 A CN103224255 A CN 103224255A CN 2013101125194 A CN2013101125194 A CN 2013101125194A CN 201310112519 A CN201310112519 A CN 201310112519A CN 103224255 A CN103224255 A CN 103224255A
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Abstract
The invention relates to a preparation method of iron oxyhydroxide/graphene oxide composites. The method uses an improved Hummers method to regulate a proportion of a saturated ferric salt aqueous solution for preparing a precursor sol with boiling water, and a concentration of a graphene oxide aqueous solution, thereby preparing the iron oxyhydroxide/graphene oxide composite material with monodisperse nanoparticles and a size of less than 10 nanometer, and without a surfactant. The iron oxyhydroxide/graphene oxide composite material prepared by the method has characteristics of small particle size of the iron oxyhydroxide, monodispersed iron oxyhydroxide on surfaces of the graphene oxide, and large specific surface area; and the method is low in equipment investment, few in synthesis steps, simple in operation technology, low in production cost, easy to realize industrial production and wide in application prospect.
Description
Technical field
The present invention relates to the preparation method of a kind of hydrous iron oxide/graphene oxide matrix material, belong to field of nanocomposite materials.
Background technology
Hydrous iron oxide is a kind of functional materials that is mainly used in environment protection and industrial production field; in environment protection, can be used to sulphur in the deaerated and the heavy metal of absorption in the trade effluent etc.; useful as catalysts, pigment etc. in industrial production, application prospect are very wide.Along with the development of nano material and nanotechnology, material will show more excellent and special nature has obtained proving fully under nanoscale.How being applied to the characteristic of nano material excellence in the middle of the reality is a difficult problem.Nano material makes it have bigger specific surface and higher surface energy owing to size is little, caused its excellent properties that is different from block materials and special nature.Simultaneously, because the surface energy height has also brought its shortcoming of reuniting easily, agglomeration makes the nano material size become big, makes excellent nano level characteristic decay, even disappears.At present, the preparation of nano material need be added tensio-active agent mostly, by the auxiliary following nano material of undersized nano material, particularly 10 nanometers that obtains of tensio-active agent; Simultaneously, need the coating of tensio-active agent and protection to avoid the generation of reuniting.But the coating of tensio-active agent has influence on the excellent properties of nano material itself again.Therefore, how to obtain that surfactant-free coats, the mono-dispersed nano particle is the nano material input huge challenge that practical application faced.
Summary of the invention
For solving problems of the prior art, the object of the present invention is to provide the preparation method of a kind of hydrous iron oxide/graphene oxide matrix material, size is coated less than the hydrous iron oxide particle surfactant-free of 10 nanometers, be distributed in the graphene oxide surface with monodisperse status.The present invention is by saturated molysite aqueous solution and the ratio of boiling water and the concentration of graphite oxide aqueous solution of regulation and control preparation precursor colloidal sol, obtain the matrix material that the nano-grade hydroxy ferric oxide is distributed in the graphene oxide surface, the hydrous iron oxide of preparation/graphene oxide matrix material has characteristics such as the hydrous iron oxide particle size is little, the hydrous iron oxide particle presents the monodisperse status distribution on the graphene oxide surface, specific surface area is big.This preparation method's facility investment is few, and synthesis step is few, and operating procedure is simple, and production cost is low, is easy to realize suitability for industrialized production.
The technical solution adopted in the present invention:
The preparation method of a kind of hydrous iron oxide/graphene oxide matrix material may further comprise the steps:
(1) powdered graphite of sheet structure and SODIUMNITRATE being joined massfraction is in 98% the vitriol oil, to stir 0.5 ~ 1h under 1 ~ 5 ℃ of condition;
(2) in solution, add potassium permanganate, be warming up to 35 ℃ and stir 1.5 ~ 3h;
(3) in solution, slowly add deionized water, be warming up to 90 ℃ and stir 1 ~ 2h;
(4) add deionized water once more, drip massfraction and be 30% hydrogen peroxide, transfer glassy yellow to by dark-brown until the color of solution;
(5) be that 5% hydrochloric acid and deionized water wash respectively 3 times with the product massfraction, centrifugation final vacuum drying obtains the graphene oxide powder;
(6) preparation concentration is the graphite oxide aqueous solution of 0.1 ~ 1g/L;
(7) saturated molysite aqueous solution is dripped in the ebullient deionized water, be heated to solution and become sorrel, obtain hydrous iron oxide precursor colloidal sol;
(8) the graphite oxide aqueous solution is mixed with hydrous iron oxide precursor colloidal sol, stir 0.5 ~ 1h;
(9) solution centrifugal after will stirring separates, and the product that obtains places the vacuum drying oven ageing, promptly gets hydrous iron oxide/graphene oxide matrix material.
The mass ratio of powdered graphite, SODIUMNITRATE, the vitriol oil is 1:(0.5 ~ 2 in the step (1)): (75 ~ 100).
The mass ratio of powdered graphite and potassium permanganate is 1:(5 ~ 10 in the step (2)).
The mass ratio of powdered graphite and deionized water is 1:(75 ~ 90 in the step (3)).
The mass ratio of powdered graphite and deionized water is 1:(180 ~ 210 in the step (4)).
Molysite in the step (7) in the saturated iron salt solutions is iron protochloride or ferrous sulfate or iron nitrate or ironic oxalate or ferric sulfate.
Saturated molysite aqueous solution is 1:(10 ~ 20 with the volume ratio of boiling deionized water in the step (7)).
The volume ratio of graphite oxide aqueous solution and hydrous iron oxide precursor colloidal sol is 1:(1 ~ 10 in the step (8)).
The ageing temperature is 40 ~ 60 ℃ in the step (9), and digestion time is 20 ~ 40h.
Beneficial effect of the present invention:
The present invention makes size less than 10 nanometers, surfactant-free, dispersed nano particulate hydrous iron oxide/graphene oxide matrix material by saturated molysite aqueous solution and the ratio of boiling water and the concentration of graphite oxide aqueous solution of improved Hummers method regulation and control preparation precursor colloidal sol.Hydrous iron oxide/graphene oxide the matrix material of this preparation method's preparation has characteristics such as the hydrous iron oxide particle size is little, the hydrous iron oxide particle presents the monodisperse status distribution on the graphene oxide surface, specific surface area is big, its facility investment is few, synthesis step is few, operating procedure is simple, production cost is low, be easy to realize suitability for industrialized production, be with a wide range of applications.
Description of drawings
X-ray diffraction (XRD) figure of the hydrous iron oxide that Fig. 1 prepares for the present invention/graphene oxide matrix material;
Transmission electron microscope (TEM) figure of the hydrous iron oxide that Fig. 2 prepares for the present invention/graphene oxide matrix material;
High-resolution-ration transmission electric-lens (HRTEM) figure of the hydrous iron oxide that Fig. 3 prepares for the present invention/graphene oxide matrix material.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Embodiment 1
The preparation method of a kind of hydrous iron oxide/graphene oxide matrix material may further comprise the steps:
(1) powdered graphite of 1g sheet structure and 1g SODIUMNITRATE being joined the 80g massfraction is in 98% the vitriol oil, to stir 0.5h under 5 ℃ of conditions;
(2) in solution, add 8g potassium permanganate, be warming up to 35 ℃ and stir 2h;
(3) in solution, slowly add the 80ml deionized water, be warming up to 90 ℃ and stir 1h;
(4) add the 200ml deionized water once more, drip massfraction and be 30% hydrogen peroxide, transfer glassy yellow to by dark-brown until the color of solution;
(5) be that 5% hydrochloric acid and deionized water wash respectively 3 times with the product massfraction, centrifugation final vacuum drying obtains the graphene oxide powder;
(6) preparation concentration is the graphite oxide aqueous solution of 1g/L;
(7) the saturated ferrous chloride aqueous solution of 100ml is dripped in ebullient 1000ml deionized water, be heated to solution and become sorrel, obtain hydrous iron oxide precursor colloidal sol;
(8) 10ml graphite oxide aqueous solution is mixed with 10ml hydrous iron oxide precursor colloidal sol, stir 1h;
(9) solution centrifugal after will stirring separates, and the product that obtains places 60 ℃ of ageing 24h of vacuum drying oven, promptly gets hydrous iron oxide/graphene oxide matrix material.
Gained hydrous iron oxide/graphene oxide matrix material is characterized, obtain X-ray diffraction (XRD) figure, as Fig. 1; Transmission electron microscope (TEM) figure is as Fig. 2; High-resolution-ration transmission electric-lens (HRTEM) figure is as Fig. 3.
Embodiment 2
The preparation method of a kind of hydrous iron oxide/graphene oxide matrix material may further comprise the steps:
(1) powdered graphite of 1g sheet structure and 0.5g SODIUMNITRATE being joined the 75g massfraction is in 98% the vitriol oil, to stir 1h under 1 ℃ of condition;
(2) in solution, add 5g potassium permanganate, be warming up to 35 ℃ and stir 3h;
(3) in solution, slowly add the 90ml deionized water, be warming up to 90 ℃ and stir 1h;
(4) add the 210ml deionized water once more, drip massfraction and be 30% hydrogen peroxide, transfer glassy yellow to by dark-brown until the color of solution;
(5) be that 5% hydrochloric acid and deionized water wash respectively 3 times with the product massfraction, centrifugation final vacuum drying obtains the graphene oxide powder;
(6) preparation concentration is the graphite oxide aqueous solution of 0.1g/L;
(7) the saturated ferrous sulfate aqueous solution of 100ml is dripped in 1200ml ebullient deionized water, be heated to solution and become sorrel, obtain hydrous iron oxide precursor colloidal sol;
(8) 10ml graphite oxide aqueous solution is mixed with 50ml hydrous iron oxide precursor colloidal sol, stir 0.5h;
(9) solution centrifugal after will stirring separates, and the product that obtains places 40 ℃ of ageing 40h of vacuum drying oven, promptly gets hydrous iron oxide/graphene oxide matrix material.
Embodiment 3
The preparation method of a kind of hydrous iron oxide/graphene oxide matrix material may further comprise the steps:
(1) powdered graphite of 1g sheet structure and 2g SODIUMNITRATE being joined the 100g massfraction is in 98% the vitriol oil, to stir 0.5h under 4 ℃ of conditions;
(2) in solution, add 10g potassium permanganate, be warming up to 35 ℃ and stir 1.5h;
(3) in solution, slowly add the 75ml deionized water, be warming up to 90 ℃ and stir 2h;
(4) add the 200ml deionized water once more, drip massfraction and be 30% hydrogen peroxide, transfer glassy yellow to by dark-brown until the color of solution;
(5) be that 5% hydrochloric acid and deionized water wash respectively 3 times with the product massfraction, centrifugation final vacuum drying obtains the graphene oxide powder;
(6) preparation concentration is the graphite oxide aqueous solution of 0.3g/L;
(7) the saturated iron nitrate aqueous solution of 100ml is dripped in 1000ml ebullient deionized water, be heated to solution and become sorrel, obtain hydrous iron oxide precursor colloidal sol;
(8) 10ml graphite oxide aqueous solution is mixed with 100ml hydrous iron oxide precursor colloidal sol, stir 1h;
(9) solution centrifugal after will stirring separates, and the product that obtains places 60 ℃ of ageing 20h of vacuum drying oven, promptly gets hydrous iron oxide/graphene oxide matrix material.
Embodiment 4
The preparation method of a kind of hydrous iron oxide/graphene oxide matrix material may further comprise the steps:
(1) powdered graphite of 1g sheet structure and 1.5g SODIUMNITRATE being joined the 80g massfraction is in 98% the vitriol oil, to stir 1h under 2 ℃ of conditions;
(2) in solution, add 6g potassium permanganate, be warming up to 35 ℃ and stir 2h;
(3) in solution, slowly add the 85ml deionized water, be warming up to 90 ℃ and stir 1h;
(4) add the 190ml deionized water once more, drip massfraction and be 30% hydrogen peroxide, transfer glassy yellow to by dark-brown until the color of solution;
(5) be that 5% hydrochloric acid and deionized water wash respectively 3 times with the product massfraction, centrifugation final vacuum drying obtains the graphene oxide powder;
(6) preparation concentration is the graphite oxide aqueous solution of 0.5g/L;
(7) 100ml saturated oxalic acid molten iron drips of solution is added in the 1500ml ebullient deionized water, is heated to solution and becomes sorrel, obtain hydrous iron oxide precursor colloidal sol;
(8) 10ml graphite oxide aqueous solution is mixed with 70ml hydrous iron oxide precursor colloidal sol, stir 1h;
(9) solution centrifugal after will stirring separates, and the product that obtains places 50 ℃ of ageing 30h of vacuum drying oven, promptly gets hydrous iron oxide/graphene oxide matrix material.
Embodiment 5
The preparation method of a kind of hydrous iron oxide/graphene oxide matrix material may further comprise the steps:
(1) powdered graphite of 1g sheet structure and 1.2g SODIUMNITRATE being joined the 90g massfraction is in 98% the vitriol oil, to stir 0.8h under 3 ℃ of conditions;
(2) in solution, add 8g potassium permanganate, be warming up to 35 ℃ and stir 2.5h;
(3) in solution, slowly add the 80ml deionized water, be warming up to 90 ℃ and stir 1.5h;
(4) add the 180ml deionized water once more, drip massfraction and be 30% hydrogen peroxide, transfer glassy yellow to by dark-brown until the color of solution;
(5) be that 5% hydrochloric acid and deionized water wash respectively 3 times with the product massfraction, centrifugation final vacuum drying obtains the graphene oxide powder;
(6) preparation concentration is the graphite oxide aqueous solution of 0.8g/L;
(7) the saturated ferric sulfate aqueous solution of 100ml is dripped in 2000ml ebullient deionized water, be heated to solution and become sorrel, obtain hydrous iron oxide precursor colloidal sol;
(8) 10ml graphite oxide aqueous solution is mixed with 30ml hydrous iron oxide precursor colloidal sol, stir 0.5h;
(9) solution centrifugal after will stirring separates, and the product that obtains places 50 ℃ of ageing 36h of vacuum drying oven, promptly gets hydrous iron oxide/graphene oxide matrix material.
Claims (9)
1. the preparation method of hydrous iron oxide/graphene oxide matrix material is characterized in that: may further comprise the steps:
(1) powdered graphite of sheet structure and SODIUMNITRATE being joined massfraction is in 98% the vitriol oil, to stir 0.5 ~ 1h under 1 ~ 5 ℃ of condition;
(2) in solution, add potassium permanganate, be warming up to 35 ℃ and stir 1.5 ~ 3h;
(3) in solution, slowly add deionized water, be warming up to 90 ℃ and stir 1 ~ 2h;
(4) add deionized water once more, drip massfraction and be 30% hydrogen peroxide, transfer glassy yellow to by dark-brown until the color of solution;
(5) be that 5% hydrochloric acid and deionized water wash respectively 3 times with the product massfraction, centrifugation final vacuum drying obtains the graphene oxide powder;
(6) preparation concentration is the graphite oxide aqueous solution of 0.1 ~ 1g/L;
(7) saturated molysite aqueous solution is dripped in the ebullient deionized water, be heated to solution and become sorrel, obtain hydrous iron oxide precursor colloidal sol;
(8) the graphite oxide aqueous solution is mixed with hydrous iron oxide precursor colloidal sol, stir 0.5 ~ 1h;
(9) solution centrifugal after will stirring separates, and the product that obtains places the vacuum drying oven ageing, promptly gets hydrous iron oxide/graphene oxide matrix material.
2. the preparation method of hydrous iron oxide according to claim 1/graphene oxide matrix material is characterized in that: the mass ratio of powdered graphite, SODIUMNITRATE, the vitriol oil is 1:(0.5 ~ 2 in the step (1)): (75 ~ 100).
3. the preparation method of hydrous iron oxide according to claim 1/graphene oxide matrix material is characterized in that: the mass ratio of powdered graphite and potassium permanganate is 1:(5 ~ 10 in the step (2)).
4. the preparation method of hydrous iron oxide according to claim 1/graphene oxide matrix material is characterized in that: the mass ratio of powdered graphite and deionized water is 1:(75 ~ 90 in the step (3)).
5. the preparation method of hydrous iron oxide according to claim 1/graphene oxide matrix material is characterized in that: the mass ratio of powdered graphite and deionized water is 1:(180 ~ 210 in the step (4)).
6. the preparation method of hydrous iron oxide according to claim 1/graphene oxide matrix material is characterized in that: the molysite in the step (7) in the saturated iron salt solutions is iron protochloride or ferrous sulfate or iron nitrate or ironic oxalate or ferric sulfate.
7. the preparation method of hydrous iron oxide according to claim 1/graphene oxide matrix material is characterized in that: saturated molysite aqueous solution is 1:(10 ~ 20 with the volume ratio of boiling deionized water in the step (7)).
8. the preparation method of hydrous iron oxide according to claim 1/graphene oxide matrix material is characterized in that: the volume ratio of graphite oxide aqueous solution and hydrous iron oxide precursor colloidal sol is 1:(1 ~ 10 in the step (8)).
9. the preparation method of hydrous iron oxide according to claim 1/graphene oxide matrix material is characterized in that: the ageing temperature is 40 ~ 60 ℃ in the step (9), and digestion time is 20 ~ 40h.
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| CN103432973A (en) * | 2013-09-09 | 2013-12-11 | 东南大学 | Method for preparing graphene-ferric oxide nano-particle composite material |
| CN104209534A (en) * | 2014-07-30 | 2014-12-17 | 苏州铉动三维空间科技有限公司 | Preparation method for hybrid structure of iron hydroxide nanorods-gold nanoparticles |
| CN104941576A (en) * | 2014-03-28 | 2015-09-30 | 西南科技大学 | Three dimensional net-shaped hydroxyl iron oxide/bacterial cellulose carbon composite material as well as preparation method and usage thereof |
| CN105597758A (en) * | 2016-02-05 | 2016-05-25 | 武汉理工大学 | Graphene modified iron mud heterogeneous Fenton catalyst and preparation method thereof |
| CN105771880A (en) * | 2015-12-25 | 2016-07-20 | 武汉理工大学 | Iron oxyhydroxide supported montmorillonite adsorption and catalysis double-function material and preparation method thereof |
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| CN106000365A (en) * | 2016-05-17 | 2016-10-12 | 北京化工大学 | Preparation method and application of iron hydroxide-expanded graphite composite material |
| CN106215862A (en) * | 2016-09-13 | 2016-12-14 | 天津大学 | A kind of preparation method and applications of iron oxyhydroxide/graphenoxide oxide composite material |
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| CN109052483A (en) * | 2018-08-29 | 2018-12-21 | 东北师范大学 | A kind of preparation of small size FeOOH nanometer rods |
| CN109449422A (en) * | 2018-11-12 | 2019-03-08 | 东北师范大学 | FeOOH nanometer rods/graphene oxide composite material and the preparation method and application thereof |
| CN110694587A (en) * | 2019-10-25 | 2020-01-17 | 四川大学 | Method for preparing graphene oxide-layered hydroxide loaded iron oxyhydroxide composite material |
| CN110706935A (en) * | 2019-10-12 | 2020-01-17 | 刘沛源 | rGO/FeOOH/rGO composite material, and preparation method and application thereof |
| CN111599600A (en) * | 2020-05-13 | 2020-08-28 | 辽宁科技大学 | Preparation method and application of graphene/iron oxyhydroxide/polyaniline supercapacitor positive electrode material |
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2013
- 2013-04-02 CN CN2013101125194A patent/CN103224255A/en active Pending
Non-Patent Citations (1)
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| FUMIN PENG ET AL.: ""An easy method to synthesize grapheme oxide-FeOOH composites and their potential application in water purification"", 《MATERIALS RESEARCH BULLETIN》 * |
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| CN104941576A (en) * | 2014-03-28 | 2015-09-30 | 西南科技大学 | Three dimensional net-shaped hydroxyl iron oxide/bacterial cellulose carbon composite material as well as preparation method and usage thereof |
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| CN104209534A (en) * | 2014-07-30 | 2014-12-17 | 苏州铉动三维空间科技有限公司 | Preparation method for hybrid structure of iron hydroxide nanorods-gold nanoparticles |
| CN105771880A (en) * | 2015-12-25 | 2016-07-20 | 武汉理工大学 | Iron oxyhydroxide supported montmorillonite adsorption and catalysis double-function material and preparation method thereof |
| CN105597758A (en) * | 2016-02-05 | 2016-05-25 | 武汉理工大学 | Graphene modified iron mud heterogeneous Fenton catalyst and preparation method thereof |
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| CN109449422A (en) * | 2018-11-12 | 2019-03-08 | 东北师范大学 | FeOOH nanometer rods/graphene oxide composite material and the preparation method and application thereof |
| CN110706935A (en) * | 2019-10-12 | 2020-01-17 | 刘沛源 | rGO/FeOOH/rGO composite material, and preparation method and application thereof |
| CN110706935B (en) * | 2019-10-12 | 2021-12-17 | 刘沛源 | rGO/FeOOH/rGO composite material, and preparation method and application thereof |
| CN110694587A (en) * | 2019-10-25 | 2020-01-17 | 四川大学 | Method for preparing graphene oxide-layered hydroxide loaded iron oxyhydroxide composite material |
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Application publication date: 20130731 |