CN107176602A - A kind of graphene oxide composite material with ordered structure and preparation method thereof - Google Patents
A kind of graphene oxide composite material with ordered structure and preparation method thereof Download PDFInfo
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- CN107176602A CN107176602A CN201710352002.0A CN201710352002A CN107176602A CN 107176602 A CN107176602 A CN 107176602A CN 201710352002 A CN201710352002 A CN 201710352002A CN 107176602 A CN107176602 A CN 107176602A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a kind of graphene oxide composite material with ordered structure and preparation method thereof, the present invention builds the lysotropic liquid crystal soft template with different nanostructureds with graphene oxide aqueous dispersions from surfactant first, after the surfactant in solvent removal template, the graphene oxide composite material of ordered structure is obtained.Graphene oxide is configured to the material with long period ordered structure by the present invention by lysotropic liquid crystal soft template, and it protrudes effect and is mainly reflected in the well-regulated stratiform of graphene oxide tool or hexagonal hole road structure, increase accordingly its specific surface area；Preparation method agents useful for same that the present invention is provided is few, step is few, simple to operate, and gained stannic oxide/graphene nano structural order is good.
Description
Technical field
The present invention relates to a kind of graphene oxide composite material with ordered structure and preparation method thereof, belong to pharmaceutical carrier or
Anti-biotic material field.
Background technology
Graphene oxide is the derivative of graphene, is the graphite that bottom surface contains that hydroxyl and epoxy radicals, edge contain carboxyl
Alkene.The presence of oxygen-containing functional group makes it have good hydrophily and biocompatibility, has in biomedical sector extensive
Application prospect.On the one hand, graphene oxide can kill bacterium by mechanical damage or oxidative stress effect, higher as security
Antiseptic；On the other hand, the hydrophily of graphene oxide, biocompatibility, huge specific surface area make it can be as medicine
Carrier loaded high amount of drug, especially some water-insoluble medicines, this is for realizing that it is very heavy that the transmission of medicine in vivo has
The meaning wanted.Either as bactericide or pharmaceutical carrier, the graphene oxide after structuring has higher defect concentration
And specific surface area, there are potential excellent properties and application prospect in antibacterial and load prescription face.
Template is the effective means for obtaining ordered structural material, and these regular nano pore structures can provide bigger
Specific surface area.Wherein, soft template is easy to construct due to it, equipment is simple, form of diverse and be widely adopted.Lysotropic liquid crystal be by
A kind of soft template of water and amphiphilic composition, its various structures is the ideal response of guiding generation nano structural material
Institute.Common Lyotropic Liquid Crystals have layer structure, hexagonal structure etc..
The content of the invention
The present invention is intended to provide a kind of graphene oxide composite material with ordered structure, the material has well-regulated long period
Ordered nano-structure.Present invention also offers the preparation method of the graphene oxide composite material.
The invention provides a kind of preparation method of the graphene oxide composite material with ordered structure, graphite oxide is used first
Alkene aqueous dispersions build the lysotropic liquid crystal soft template with different nanostructureds from surfactant, using in solvent removal template
Surfactant after, obtain ordered structure graphene oxide composite material.
In above-mentioned preparation method, the surfactant is Brij 30, Brij 35, Brij52, Brij 56, Brij
58th, any of Brij72, Brij93, Brij97, Brij S10, Brij O10, Brij S20.
In above-mentioned preparation method, the preparation method of the graphene oxide aqueous dispersions is：Add graphene oxide into
In deionized water, it is configured to suspension and ultrasound is to being uniformly dispersed.
In above-mentioned preparation method, the concentration of the graphene oxide aqueous dispersions is 50 ~ 700 μ g/mL.
Further, above-mentioned preparation method specifically includes following steps：
(1) graphene oxide aqueous dispersions are mixed with surfactant, the two mass ratio is 40-60: 60-40；
(2) by step（1）Gained mixture heating water bath stirs to 40-65 DEG C；
(3) by step（2）In stir after mixture constant temperature stand 2-48h, obtain lysotropic liquid crystal soft template；
(4) by step（3）The lysotropic liquid crystal soft template of gained sloughs the surfactant of organic phase with solvent, is obtained after drying
Replicate the ordered structure graphene oxide composite material of templating nanoparticles structure.
In the above method, step（3）In, mixture thermostat temperature is 40-65 DEG C.
In the above method, step（3）In, the mixture heating of graphene oxide aqueous dispersions and surfactant and constant temperature
During keep closed.
In the above method, step（4）The middle solvent used be ethanol, acetone, ethyl acetate it is any.
In the above method, step（4）During middle removing surfactant, cleaned, filtered 6 ~ 10 times with solvent.
The invention provides the graphene oxide composite material of the ordered structure according to made from above-mentioned preparation method.
Beneficial effects of the present invention：
（1）Graphene oxide is configured to the material with long period ordered structure by the present invention by lysotropic liquid crystal soft template, its
Prominent effect is mainly reflected in graphene oxide and has well-regulated stratiform or hexagonal hole road structure, increase accordingly it and compares surface
Product；
（2）Preparation method agents useful for same that the present invention is provided is few, step is few, simple to operate, gained stannic oxide/graphene nano structure
Order is good.
Brief description of the drawings
Fig. 1 is the petrographic microscope figure of the lyotropic liquid crystal template formed in embodiment 1.
Fig. 2 is the low angle X diffraction patterns of the lyotropic liquid crystal template formed in embodiment 1.
Fig. 3 is the low angle X of the Brij56 rear oxidation graphenes in the lysotropic liquid crystal removing organic phase formed in embodiment 1
Diffraction pattern.
Fig. 4 is the saturating of the Brij56 rear oxidation graphenes in the lyotropic liquid crystal template removing organic phase formed in embodiment 1
Penetrate electron microscope.
Fig. 5 is the petrographic microscope figure of the lyotropic liquid crystal template formed in embodiment 2.
Fig. 6 is the low angle X diffraction patterns of the lyotropic liquid crystal template formed in embodiment 2.
Fig. 7 is the low of the Brij56 rear oxidation graphenes in the lyotropic liquid crystal template removing organic phase formed in embodiment 2
Angle X diffraction patterns.
Fig. 8 is the saturating of the Brij56 rear oxidation graphenes in the lyotropic liquid crystal template removing organic phase formed in embodiment 2
Penetrate electron microscope.
Embodiment
The present invention is further illustrated below by embodiment, but is not limited to following examples.
Embodiment 1
According to graphene oxide aqueous dispersions (300 μ g/mL) and the mass ratioes 40% of Brij 56：60% ratio mixes the two
Close, stirring.By mixture airtight heating to 45 DEG C, and constant temperature stands 12 hours at 45 DEG C, obtains lysotropic liquid crystal phase.Will
Acetone is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 6 times repeatedly, the Brij in removing organic phase
56, obtain replicating the graphene oxide composite material of formwork structure.
In above-mentioned experiment, Fig. 1 is that 40% graphene oxide dispersion (300 μ g/mL) is formed with 60% Brij 56
Lyotropic liquid crystal template petrographic microscope figure, the stripe texture of stratiform is rendered as in Fig. 1.
Fig. 2 is 40% graphene oxide dispersion (300 μ g/mL) and the lyotropic liquid crystal template of 60% Brij 56 formation
Low angle X diffraction patterns.In figure 2 θ be 1.57,3.02,4.63, visible four diffraction maximums at 6.07 °, correspond respectively to this molten
Cause 100,200,300 and 400 crystal faces of liquid crystalline phase.According to bragg's formula, the corresponding interplanar distance d values point of this four diffraction maximums
Not Wei 5.6,2.9,1.9,1.4 nm, ratio close to stratiform phase character 1:1/2:1/3:1/4, show under the composition,
Brij 56 constitutes the layer structure of high-sequential with graphene oxide aqueous dispersions.
Fig. 3 is that 40% graphene oxide dispersion (300 μ g/mL) and the lysotropic liquid crystal of 60% Brij 56 formation are removed
The low angle X diffraction patterns of Brij56 rear oxidation graphenes in organic phase.In figure 2 θ be 5.8 ° place appearance one diffraction maximum, root
According to bragg's formula, its corresponding interplanar distance d value is 1.5nm.Compared with former lyotropic liquid crystal template, 100 peaks are offset to the right, d
Value is reduced to 1.5nm from 5.6.Illustrate during template is removed, although product maintains the feature structure of template stratiform, but
It is that the layer structure of graphene oxide has been shunk, and causes the cycle of its long-range order to reduce during template is removed.
Fig. 4 is that 40% graphene oxide dispersion (300 μ g/mL) and the lysotropic liquid crystal of 60% Brij 56 formation are removed
The transmission electron microscope picture of Brij56 rear oxidation graphenes in organic phase.Obvious layer structure, interlamellar spacing is presented in graphene oxide
About 1.5nm, is consistent with its low angle X diffraction patterns.
Embodiment 2
According to graphene oxide aqueous dispersions (300 μ g/mL) and the mass ratioes 54% of Brij 56：46% ratio mixes the two
Close, stirring.By mixture airtight heating to 50 DEG C, and constant temperature stands 16 hours at 50 DEG C, obtains lysotropic liquid crystal phase.Will
Acetone is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 8 times repeatedly, the Brij in removing organic phase
56, obtain replicating the graphene oxide composite material of formwork structure.
In above-mentioned experiment, Fig. 5 is 54% graphene oxide aqueous dispersions (300 μ g/mL) and the shapes of 46% Brij 56
Into lyotropic liquid crystal template petrographic microscope figure, show the conical texture of hexagonal phase feature.
Fig. 6 is 54% graphene oxide aqueous dispersions (300 μ g/mL) and the lysotropic liquid crystal mould of 46% Brij 56 formation
The low angle X diffraction patterns of plate.In figure 2 θ be 0.92,1.54 and 1.82 ° locate visible three diffraction maximums, correspond respectively to the molten cause
100,110 and 200 liquid crystal templated crystal faces, their corresponding interplanar distance d values are respectively 9.6,5.6 and 4.8 nm, and ratio connects
The 1 of nearly hexagonal phase feature:1/:1/, show under the composition, 54% graphene oxide dispersion (300 μ g/mL) and 46%
Brij 56 constitutes hexagonal structure.
Fig. 7 is 54% graphene oxide aqueous dispersions (300 μ g/mL) and the lysotropic liquid crystal mould of 46% Brij56 formation
The low angle X diffraction patterns of template molecule Brij56 rear oxidation graphenes in plate removing organic phase.In figure 2 θ be 1.02 ° at go out
An existing diffraction maximum, its corresponding interplanar distance d value is 8.6, is more or less the same with the interplanar distance of original template.Illustrate to remove template
Afterwards, graphene oxide maintains the long range ordered structure of template.
Fig. 8 is 54% graphene oxide aqueous dispersions (300 μ g/mL) and the lysotropic liquid crystal mould of 46% Brij56 formation
The transmission electron microscope picture of Brij56 rear oxidation graphenes in plate removing organic phase.The hole of graphene oxide rule can be seen in the figure
Road, hole center is spaced about 9nm, is consistent with its low angle X diffraction patterns.
Embodiment 3
According to graphene oxide aqueous dispersions (600 μ g/mL) and Brij30 mass ratioes 43%：57% ratio mixes the two,
Stirring.By mixture airtight heating to 42 DEG C, and constant temperature stands 2 hours at 42 DEG C, obtains lysotropic liquid crystal phase.By ethanol
It is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 6 times repeatedly, the Brij30 in removing organic phase,
Obtain replicating the graphene oxide composite material of template layer structure.
Embodiment 4
According to graphene oxide aqueous dispersions (100 μ g/mL) and Brij35 mass ratioes 56%：44% ratio mixes the two,
Stirring.By mixture airtight heating to 45 DEG C, and constant temperature stands 8 hours at 45 DEG C, obtains lysotropic liquid crystal phase.By ethanol
It is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 6 times repeatedly, the Brij35 in removing organic phase,
Obtain replicating the graphene oxide composite material of template hexagonal structure.
Embodiment 5
According to graphene oxide aqueous dispersions (350 μ g/mL) and Brij52 mass ratioes 40%：60% ratio mixes the two,
Stirring.By mixture airtight heating to 40 DEG C, and constant temperature stands 10 hours at 40 DEG C, obtains lysotropic liquid crystal phase.By acetic acid
Ethyl ester is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 8 times repeatedly, in removing organic phase
Brij52, obtains replicating the graphene oxide composite material of template layer structure.
Embodiment 6
According to graphene oxide aqueous dispersions (400 μ g/mL) and Brij58 mass ratioes 55.5%：44.5% ratio incite somebody to action the two
Mixing, stirring.By mixture airtight heating to 58 DEG C, and constant temperature stands 12 hours at 58 DEG C, obtains lysotropic liquid crystal phase.
Acetone is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 7 times repeatedly, in removing organic phase
Brij58, obtains replicating the graphene oxide composite material of template hexagonal structure.
Embodiment 7
According to graphene oxide aqueous dispersions (50 μ g/mL) and Brij72 mass ratioes 42.5%：57.5% ratio mixes the two
Close, stirring.By mixture airtight heating to 52 DEG C, and constant temperature stands 18 hours at 52 DEG C, obtains lysotropic liquid crystal phase.By second
Acetoacetic ester is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 8 times repeatedly, in removing organic phase
Brij72, obtains replicating the graphene oxide composite material of template layer structure.
Embodiment 8
According to graphene oxide aqueous dispersions (500 μ g/mL) and Brij93 mass ratioes 56.5%：43.5% ratio incite somebody to action the two
Mixing, stirring.By mixture airtight heating to 50 DEG C, and constant temperature stands 24 hours at 50 DEG C, obtains lysotropic liquid crystal phase.
Acetone is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 9 times repeatedly, in removing organic phase
Brij93, obtains replicating the graphene oxide composite material of template hexagonal structure.
Embodiment 9
According to graphene oxide aqueous dispersions (50 μ g/mL) and Brij97 mass ratioes 44%：56% ratio mixes the two,
Stirring.By mixture airtight heating to 56 DEG C, and constant temperature stands 30 hours at 56 DEG C, obtains lysotropic liquid crystal phase.By acetone
It is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 9 times repeatedly, the Brij97 in removing organic phase,
Obtain replicating the graphene oxide composite material of template layer structure.
Embodiment 10
According to graphene oxide aqueous dispersions (600 μ g/mL) and BrijS10 mass ratioes 57%：43% ratio mixes the two
Close, stirring.By mixture airtight heating to 60 DEG C, and constant temperature stands 36 hours at 55 DEG C, obtains lysotropic liquid crystal phase.Will
Ethanol is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 10 times repeatedly, in removing organic phase
Brij S10, obtain replicating the graphene oxide composite material of template hexagonal structure.
Embodiment 11
According to graphene oxide aqueous dispersions (700 μ g/mL) and BrijO10 mass ratioes 46%：54% ratio mixes the two
Close, stirring.By mixture airtight heating to 55 DEG C, and constant temperature stands 40 hours at 55 DEG C, obtains lysotropic liquid crystal phase.By second
Acetoacetic ester is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 10 times repeatedly, in removing organic phase
BrijO10, obtains replicating the graphene oxide composite material of template layer structure.
Embodiment 12
According to graphene oxide aqueous dispersions (650 μ g/mL) and BrijS20 mass ratioes 56.5%：43.5% ratio incite somebody to action the two
Mixing, stirring.By mixture airtight heating to 65 DEG C, and constant temperature stands 48 hours at 65 DEG C, obtains lysotropic liquid crystal phase.
Acetone is added to cleaning, filtering in the lysotropic liquid crystal after standing.So clean, filter 10 times repeatedly, in removing organic phase
Brij S20, obtain replicating the graphene oxide composite material of template hexagonal structure.
Claims (10)
1. a kind of preparation method of the graphene oxide composite material with ordered structure, it is characterised in that：Graphene oxide is used first
Aqueous dispersions build the lysotropic liquid crystal soft template with different nanostructureds from surfactant, using in solvent removal template
After surfactant, the graphene oxide composite material of ordered structure is obtained.
2. the preparation method of the graphene oxide composite material according to claim 1 with ordered structure, it is characterised in that：Institute
State surfactant for Brij 30, Brij 35, Brij52, Brij 56, Brij 58, Brij72, Brij93, Brij97,
Any of Brij S10, Brij O10, Brij S20.
3. the preparation method of the graphene oxide composite material according to claim 1 with ordered structure, it is characterised in that：Institute
The preparation method for stating graphene oxide aqueous dispersions is：Add graphene oxide into deionized water, be configured to suspension simultaneously
Ultrasound is to being uniformly dispersed.
4. the preparation method of the graphene oxide composite material according to claim 3 with ordered structure, it is characterised in that：Institute
The concentration for stating graphene oxide aqueous dispersions is 50 ~ 700 μ g/mL.
5. the preparation method of the graphene oxide composite material with ordered structure according to any one of claim 1 ~ 4, it is special
Levy and be：Comprise the following steps：
(1) graphene oxide aqueous dispersions are mixed with surfactant, the two mass ratio is 40-60: 60-40；
(2) by step（1）Gained mixture heating water bath stirs to 40-65 DEG C；
(3) by step（2）In stir after mixture constant temperature stand 2-48h, obtain lysotropic liquid crystal soft template；
(4) by step（3）The lysotropic liquid crystal soft template of gained sloughs the surfactant of organic phase with solvent, is obtained after drying
Replicate the ordered structure graphene oxide composite material of templating nanoparticles structure.
6. the preparation method of the graphene oxide composite material according to claim 5 with ordered structure, it is characterised in that：Step
Suddenly（3）In, mixture thermostat temperature is 40-65 DEG C.
7. the preparation method of the graphene oxide composite material according to claim 5 with ordered structure, it is characterised in that：Step
Suddenly（3）In, keep closed in the mixture heating of graphene oxide aqueous dispersions and surfactant and thermostatic process.
8. the preparation method of the graphene oxide composite material according to claim 5 with ordered structure, it is characterised in that：Step
Suddenly（4）The middle solvent used be ethanol, acetone, ethyl acetate it is any.
9. the preparation method of the graphene oxide composite material according to claim 5 with ordered structure, it is characterised in that：Step
Suddenly（4）During middle removing surfactant, cleaned, filtered 6 ~ 10 times with solvent.
10. the graphene oxide composite material of ordered structure made from the preparation method described in a kind of use claim any one of 1-9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108634098A (en) * | 2018-04-27 | 2018-10-12 | 郑州工程技术学院 | A kind of preparation method of pure green broad-spectrum antiseptic feed addictive |
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| CN1654325A (en) * | 2004-12-24 | 2005-08-17 | 武汉理工大学 | Preparation method for optical transparent ordered inter-aperture silica single block |
| WO2015158741A2 (en) * | 2014-04-14 | 2015-10-22 | Imerys Graphite & Carbon Switzerland Ltd. | Amorphous carbon coating of carbonaceous particles from dispersions including amphiphilic organic compounds |
| CN105752971A (en) * | 2016-03-30 | 2016-07-13 | 成都新柯力化工科技有限公司 | Nano-graphene material special for drug carrier and preparing method |
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- 2017-05-18 CN CN201710352002.0A patent/CN107176602B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1654325A (en) * | 2004-12-24 | 2005-08-17 | 武汉理工大学 | Preparation method for optical transparent ordered inter-aperture silica single block |
| WO2015158741A2 (en) * | 2014-04-14 | 2015-10-22 | Imerys Graphite & Carbon Switzerland Ltd. | Amorphous carbon coating of carbonaceous particles from dispersions including amphiphilic organic compounds |
| CN105752971A (en) * | 2016-03-30 | 2016-07-13 | 成都新柯力化工科技有限公司 | Nano-graphene material special for drug carrier and preparing method |
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| 王琳: ""碳材料/表面活性剂分子有序组合体新型复合材料的制备与性质研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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| CN108634098A (en) * | 2018-04-27 | 2018-10-12 | 郑州工程技术学院 | A kind of preparation method of pure green broad-spectrum antiseptic feed addictive |
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