CN106744912A - A kind of preparation method of super-hydrophobic graphene aerogel - Google Patents
A kind of preparation method of super-hydrophobic graphene aerogel Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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Abstract
The present invention relates to a kind of preparation method of super-hydrophobic graphene aerogel, the method utilizes and reducing agent is added in graphene oxide solution, by normal heating redox graphene, it is self-assembled into three-dimensional grapheme hydrogel structure, and the method using freeze-drying is oriented, graphene aerogel material is obtained, after being modified using Long carbon chain alkoxy silane or fluoro Long carbon chain alkoxy silane, super-hydrophobic graphene aerogel material is obtained.The present invention is, using simple efficient, economic and environment-friendly synthetic method, to prepare anti-extrusion and super-hydrophobic graphene aerogel material, is the new method of prepare with scale graphene aerogel material.The super-hydrophobic graphene aerogel material obtained by the method for the invention has density low, and excellent in mechanical performance, heat endurance is good, oil suction multiplying power is high, the advantages of good cycling stability, be a kind of new, efficient water-oil separating material, with good application value and extensive market prospects.
Description
Technical field
The present invention relates to a kind of preparation method of graphene aerogel, more particularly to a kind of super-hydrophobic graphene aerogel
Preparation method, belongs to field of functional materials.
Background technology
With the development of modern industry, oil and various organic solvents taking place frequently for accident of leakage cause calamity to environment
Influence.In addition, oil and most organic solvent are inflammable, the potential safety hazards such as on fire, blast are brought, to environment and human life
The safety of property all causes grave danger.Therefore, oil suction (organic matter) material maintains water quality most to have important meaning for environmental protection
Justice.Although traditional natural oil absorption material low cost, adsorption rate is poor and adsorptive selectivity is low.Artificial synthesized polymeric material
Material, although improve adsorptive selectivity, but adsorption rate is still very low and can cause secondary pollution.Therefore develop in recent years a large amount of
New and effective oil absorption material, such as N doped silica aerogels, nano-cellulose aerogel, ultralight graphene-carbon nano tube aeroge,
Graphene sponge, CNT sponge etc., these material adsorption rates are high, selectivity is strong and can be used for multiple times, but due to being related to
To price and technique, reason, cause these novel oil absorption material large-scales extremely difficult, limit its practical application.In addition
Reclaim method of these oil absorption materials frequently with burning, it is contemplated that oil and organic matter are the important money that can be reused
Source, on the one hand this is a kind of waste, and on the other hand burning can cause secondary environmental pollution.
Graphene aerogel is the gel that decentralized medium is air, and interlocked the three-dimensional communication piled up by graphene sheet layer
Loose structure, the structure are it is possible to prevente effectively from the excessive stacking of ordinary graphite alkene piece, thus graphene aerogel keeps well
The individual layer of Graphene (or a small number of layers) structure and corresponding performance, with high porosity (75-99.9%), extremely low close
Degree (0.001-0.1g cm-3) and big specific surface area (200-1500m2g-1), it is widely used in the fields such as sewage disposal.Graphite
A Major Difficulties prepared by alkene aerogel material are that graphene sheet layer is mutually assembled, and cause its density to be extremely difficult to minimum, after
And it is greatly limited its performance and range of application.Graphene oxide hydrothermal reduction method and templated chemistry vapour deposition process
(CVD) it is to realize the effective ways that graphene aerogel material is prepared on a large scale at present.Although hydro-thermal method can be realized on a large scale
Production graphene aerogel, but the graphene aerogel structure of synthesis is easily caved in, and reduces its application performance；And CVD side
Method growth conditions is harsh, it is difficult to realize the production in enormous quantities of graphene aerogel；
The present invention proposes a kind of preparation method of super-hydrophobic graphene aerogel, can overcome above high cost, frangible
And the problem that difficult large scale is prepared on a large scale, at present, there is not been reported for domestic and international public publication and patent.
The content of the invention
Present invention aim at, it is extremely difficult to solve existing novel graphite alkene oil absorption material large-scale, limit it
The technical problem of practical application, there is provided a kind of with low cost, synthetic method is simple, easy large-scale production it is extrudable, super thin
The preparation method of aquadag alkene aerogel material.The method utilizes and reducing agent is added in graphene oxide solution, by normal pressure
Heating redox graphene, is self-assembled into three-dimensional grapheme hydrogel structure, and the method using freeze-drying is oriented, and obtains
Graphene aerogel material, after being modified using Long carbon chain alkoxy silane or fluoro Long carbon chain alkoxy silane, obtains super thin
Aquadag alkene aerogel material.The super-hydrophobic graphene aerogel material obtained by the method for the invention, with good
Superhydrophobic property, preferable engineering properties and is easy to large-scale production, with good application value and market prospects.
A kind of preparation method of super-hydrophobic graphene aerogel of the present invention, follow these steps to carry out：
A, graphene oxide is scattered in deionized water, ultrasonic disperse forms the oxidation that homogeneous concentration is 2-8mg/mL
Graphene aqueous solution；
B, will to add dopamine 0-1.5mg/mL and reducing agent in step a gained graphene oxide solutions be ascorbic acid 1-
16mg/mL, magnetic agitation is uniform, after being subsequently poured into container and sealing, is put into heating in baking oven, and 60-100 DEG C of temperature is protected
The warm time is 2-12 hours, obtains Graphene hydrogel；
C, the Graphene hydrogel that will be obtained in step b, after being soaked with deionized water, cleaning, in -196 DEG C of temperature
Under conditions of be oriented freezing, obtain frozen samples, then carry out freeze-drying, obtain freeze drying example；
D, the freeze drying example for obtaining step c, be put into containing concentration for 1-5wt% Long carbon chain alkoxy silane or
In the closed container of fluoro Long carbon chain alkoxy silane material-ethanol solution, reacted 3-24 hour at 50-80 DEG C of temperature, it is dry
Super-hydrophobic graphene aerogel is can obtain after dry.
The carbon chain lengths of Long carbon chain alkoxy silane described in step d are 6-30 carbon atom, fluoro Long carbon chain alkoxy
The carbon chain lengths of silane are 6-30 carbon atom.
Application of the super-hydrophobic graphene aerogel material that methods described is obtained in water-oil separating.
Super-hydrophobic graphene aerogel material provided by the present invention has super-hydrophobic in atmosphere (in atmosphere with water
Contact angle is more than 150 °) and super oleophylic (in atmosphere with oily contact angle close to 0 °) property.
A kind of preparation method of super-hydrophobic graphene aerogel of the present invention, the method has easy to operate, cost
The characteristics of low and preparation process is simple, it is expected to realize the big rule of graphene aerogel material and super-hydrophobic graphene aerogel material
It is prepared by mould.The super-hydrophobic graphene aerogel material obtained by the method for the invention, low with density, mechanical property is excellent
Different, heat endurance is good, and oil suction multiplying power is high, and speed of oil absorption is fast, is a kind of new, efficient oil-water the advantages of good cycling stability
Separation material, before the fields such as Organic chemical solvents treatment, oily waste water separation, leakage crude oil recovery have a wide range of applications
Scape.
Brief description of the drawings
Fig. 1 is the super-hydrophobic graphene aerogel optical photograph obtained by the present invention；
Fig. 2 be the present invention measurement water droplet or oil droplets contact angle photo, wherein, Fig. 2 a for measurement water super-hydrophobic
The contact angle photo of graphene aerogel material surface；2b is contact of the measurement oil in super-hydrophobic graphene aerogel material surface
Angle photo figure；
Fig. 3 is adsorption process photo figure of the super-hydrophobic graphene aerogel obtained by the present invention to water float oil.
Specific embodiment
The present embodiment premised on the technical solution of the present invention under implemented, give detailed implementation method and specific
Operating process, but protection scope of the present invention is not limited to following embodiments；
Embodiment 1
A, graphene oxide is scattered in deionized water, ultrasonic disperse forms the oxidation stone that homogeneous concentration is 2mg/mL
Black aqueous solution；
B, will to add reducing agent in step a gained graphene oxide solutions be ascorbic acid 1mg/mL, and magnetic agitation is uniform,
After being subsequently poured into container and sealing, heating in baking oven is put into, temperature 60 C, soaking time is 2 hours, obtains Graphene water
Gel；
C, the Graphene hydrogel that will be obtained in step b, after being soaked with deionized water, cleaning, in -196 DEG C of temperature
Under conditions of be oriented freezing, obtain frozen samples, then carry out freeze-drying, obtain freeze drying example；
D, by freeze drying example, be put into containing concentration as the carbon chain lengths of 1wt% are 6 Long carbon chain alcoxyls of carbon atom
In the closed container of base silane material-ethanol solution, reacted 24 hours under temperature 50 C, super-hydrophobic graphite is obtained after drying
Alkene aeroge.
Embodiment 2
A, graphene oxide is scattered in deionized water, ultrasonic disperse forms the oxidation stone that homogeneous concentration is 4mg/mL
Black aqueous solution；
B, will to add dopamine 0.5mg/mL and reducing agent in step a gained graphene oxide solutions be ascorbic acid 4mg/
ML, magnetic agitation is uniform, after being subsequently poured into container and sealing, is put into heating in baking oven, and temperature 70 C, soaking time is 6
Hour, obtain Graphene hydrogel；
C, the Graphene hydrogel that will be obtained in step b, after being soaked with deionized water, cleaning, in -196 DEG C of temperature
Under conditions of be oriented freezing, obtain frozen samples, then carry out freeze-drying, obtain freeze drying example；
D, by freeze drying example, be put into and contain concentration for fluoro carbon long that the carbon chain lengths of 2wt% are 12 carbon atoms
In the closed container of chain alkoxy silane material-ethanol solution, reacted 16 hours under temperature 60 C, can be surpassed after drying
Hydrophobic graphene aerogel.
Embodiment 3
A, graphene oxide is scattered in deionized water, ultrasonic disperse forms the oxidation stone that homogeneous concentration is 6mg/mL
Black aqueous solution；
B, will to add dopamine 1mg/mL and reducing agent in step a gained graphene oxide solutions be ascorbic acid 8mg/
ML, magnetic agitation is uniform, after being subsequently poured into container and sealing, is put into heating in baking oven, 80 DEG C of temperature, and soaking time is 8
Hour, obtain Graphene hydrogel；
C, the Graphene hydrogel that will be obtained in step b, after being soaked with deionized water, cleaning, in -196 DEG C of temperature
Under conditions of be oriented freezing, obtain frozen samples, then carry out freeze-drying, obtain freeze drying example；
D, by freeze drying example, be put into containing concentration as the carbon chain lengths of 3wt% are 18 Long carbon chain alkane of carbon atom
In the closed container of TMOS material-ethanol solution, reacted 8 hours under temperature 70 C, super-hydrophobic stone is obtained after drying
Black alkene aeroge.
Embodiment 4
A, graphene oxide is scattered in deionized water, ultrasonic disperse forms the oxidation stone that homogeneous concentration is 8mg/mL
Black aqueous solution；
B, it is ascorbic acid to dopamine 1.5mg/mL and reducing agent is added in step a gained graphene oxide solutions
16mg/mL, magnetic agitation is uniform, after being subsequently poured into container and sealing, is put into heating, 100 DEG C of temperature, during insulation in baking oven
Between be 2 hours, obtain Graphene hydrogel；
C, the Graphene hydrogel that will be obtained in step b, after being soaked with deionized water, cleaning, in -196 DEG C of temperature
Under conditions of be oriented freezing, obtain frozen samples, then carry out freeze-drying, obtain freeze drying example；
D, by freeze drying example, be put into and contain concentration for fluoro carbon long that the carbon chain lengths of 5wt% are 24 carbon atoms
In the closed container of chain alkoxy silane material-ethanol solution, reacted 3 hours at 80 DEG C of temperature, obtain super thin after drying
Aquadag alkene aeroge.
Embodiment 5
A, graphene oxide is scattered in deionized water, ultrasonic disperse forms the oxidation stone that homogeneous concentration is 3mg/mL
Black aqueous solution；
B, will to add dopamine 1mg/mL and reducing agent in step a gained graphene oxide solutions be ascorbic acid 1mg/
ML, magnetic agitation is uniform, after being subsequently poured into container and sealing, is put into heating in baking oven, 95 DEG C of temperature, and soaking time is 8
Hour, obtain Graphene hydrogel；
C, the Graphene hydrogel that will be obtained in step b, after being soaked with deionized water, cleaning, in -196 DEG C of temperature
Under conditions of be oriented freezing, obtain frozen samples, then carry out freeze-drying, obtain freeze drying example；
D, by freeze drying example, be put into and contain concentration for fluoro carbon long that the carbon chain lengths of 5wt% are 30 carbon atoms
In the closed container of chain alkoxy silane material-ethanol solution, reacted 8 hours under temperature 60 C, obtain super thin after drying
Aquadag alkene aeroge.
Consider from superhydrophobic property, super-hydrophobic graphene aerogel material prepared by the method for the invention has good
Superhydrophobic property, water contact angle is more than 150 °, with the property that only oil suction does not absorb water, the super-hydrophobic graphene aerogel material one
Denier touches oil water mixture, and oil is inhaled into super-hydrophobic graphene aerogel material internal quickly, and water is not adsorbed, so that real
The quick separating of existing oil water mixture, as shown in Figure 3.
Claims (2)
1. a kind of preparation method of super-hydrophobic graphene aerogel, it is characterised in that follow these steps to carry out：
A, graphene oxide is scattered in deionized water, ultrasonic disperse forms the oxidation stone that homogeneous concentration is 2-8 mg/mL
Black aqueous solution；
B, will to add dopamine 0-1.5 mg/mL and reducing agent in step a gained graphene oxide solutions be ascorbic acid 1-16
Mg/mL, magnetic agitation is uniform, after being subsequently poured into container and sealing, is put into heating in baking oven, 60-100 DEG C of temperature, insulation
Time is 2-12 hours, obtains Graphene hydrogel；
C, the Graphene hydrogel that will be obtained in step b, after being soaked with deionized water, cleaning, in -196 DEG C of bar of temperature
Freezing is oriented under part, frozen samples are obtained, freeze-drying is then carried out, freeze drying example is obtained；
D, the freeze drying example for obtaining step c, are put into Long carbon chain alkoxy silane or fluoro for 1-5 wt% containing concentration
In the closed container of Long carbon chain alkoxy silane material-ethanol solution, reacted 3-24 hour at 50-80 DEG C of temperature, after drying
Can obtain super-hydrophobic graphene aerogel.
2. the preparation method of super-hydrophobic graphene aerogel according to claim 1, it is characterised in that long described in step d
The carbon chain lengths of carbochain alkoxy silane are 6-30 carbon atom, and the carbon chain lengths of fluoro Long carbon chain alkoxy silane are 6-30
Individual carbon atom.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107640760A (en) * | 2017-10-13 | 2018-01-30 | 上海理工大学 | A kind of preparation method of graphene aerogel block, graphene aerogel block and its application |
| CN108439373A (en) * | 2018-02-07 | 2018-08-24 | 山东大学 | A kind of amphiphilic Janus structure graphites alkenyl aeroge and preparation method thereof |
| CN108715444A (en) * | 2018-06-15 | 2018-10-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | The super-hydrophobic oxidation silicon hybridization graphene aerogel micro mist of one kind, preparation method and its application |
| CN108821445A (en) * | 2018-05-31 | 2018-11-16 | 苏州大学 | The graphene aerogel metal organic frame composite material and preparation method of loading microorganisms and the application in azo dyes processing |
| CN109133040A (en) * | 2018-08-07 | 2019-01-04 | 北京科技大学 | A kind of preparation method of the adjustable graphene aerogel of pore-size |
| CN109603748A (en) * | 2018-12-24 | 2019-04-12 | 青岛双瑞海洋环境工程股份有限公司 | For handling the composite material and preparation method of oily waste water |
| CN110255540A (en) * | 2019-06-27 | 2019-09-20 | 中素新科技有限公司 | Oleophilic drainage graphene aerogel and its preparation method and application |
| CN110408074A (en) * | 2019-08-16 | 2019-11-05 | 哈尔滨工业大学 | A kind of preparation method of the graphene oxide based super hydrophobic material of alkylation modification |
| CN110438586A (en) * | 2018-05-04 | 2019-11-12 | 浙江大学 | The preparation method and product of super hydrophobic porous fiber with orientation pore structure and application |
| CN110763377A (en) * | 2019-10-21 | 2020-02-07 | 华南理工大学 | Super-hydrophobic piezoresistive pressure sensor and preparation method and application thereof |
| CN111215029A (en) * | 2020-01-21 | 2020-06-02 | 中国科学院上海硅酸盐研究所 | Graphene sponge capable of being directly baked at high temperature and reused, and preparation method and application thereof |
| CN111346577A (en) * | 2020-03-30 | 2020-06-30 | 浙江晶鑫特种纸业有限公司 | Preparation method and application of high-elasticity layered graphene oxide composite aerogel |
| CN111994901A (en) * | 2020-07-28 | 2020-11-27 | 山西大同大学 | Preparation method and application of hydrophobic graphene aerogel |
| CN112144273A (en) * | 2020-09-30 | 2020-12-29 | 福州大学 | Preparation method of multifunctional fabric surface with super-hydrophobic and conductive functions |
| CN113969433A (en) * | 2021-11-16 | 2022-01-25 | 杭州中尚电子商务有限公司 | Super-hydrophobic antibacterial fabric and preparation method thereof |
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| CN107640760A (en) * | 2017-10-13 | 2018-01-30 | 上海理工大学 | A kind of preparation method of graphene aerogel block, graphene aerogel block and its application |
| CN108439373A (en) * | 2018-02-07 | 2018-08-24 | 山东大学 | A kind of amphiphilic Janus structure graphites alkenyl aeroge and preparation method thereof |
| CN108439373B (en) * | 2018-02-07 | 2019-12-27 | 山东大学 | Amphiphilic Janus structure graphene-based aerogel and preparation method thereof |
| CN110438586B (en) * | 2018-05-04 | 2020-11-17 | 浙江大学 | Preparation method of super-hydrophobic porous fiber with oriented pore structure, product and application |
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| CN109133040A (en) * | 2018-08-07 | 2019-01-04 | 北京科技大学 | A kind of preparation method of the adjustable graphene aerogel of pore-size |
| CN109133040B (en) * | 2018-08-07 | 2020-05-12 | 北京科技大学 | Preparation method of graphene aerogel with adjustable pore size |
| CN109603748A (en) * | 2018-12-24 | 2019-04-12 | 青岛双瑞海洋环境工程股份有限公司 | For handling the composite material and preparation method of oily waste water |
| CN109603748B (en) * | 2018-12-24 | 2022-03-11 | 青岛双瑞海洋环境工程股份有限公司 | Composite material for treating oily wastewater and preparation method thereof |
| CN110255540A (en) * | 2019-06-27 | 2019-09-20 | 中素新科技有限公司 | Oleophilic drainage graphene aerogel and its preparation method and application |
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| CN110408074B (en) * | 2019-08-16 | 2022-05-20 | 哈尔滨工业大学 | Preparation method of alkylation modified graphene oxide-based super-hydrophobic material |
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| CN110763377A (en) * | 2019-10-21 | 2020-02-07 | 华南理工大学 | Super-hydrophobic piezoresistive pressure sensor and preparation method and application thereof |
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| CN111994901B (en) * | 2020-07-28 | 2023-08-01 | 山西大同大学 | Preparation method and application of hydrophobic graphene aerogel |
| CN112144273A (en) * | 2020-09-30 | 2020-12-29 | 福州大学 | Preparation method of multifunctional fabric surface with super-hydrophobic and conductive functions |
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