CN104760950A - Preparation method of graphene hydrogel and application of the graphene hydrogel - Google Patents
Preparation method of graphene hydrogel and application of the graphene hydrogel Download PDFInfo
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- CN104760950A CN104760950A CN201510111293.5A CN201510111293A CN104760950A CN 104760950 A CN104760950 A CN 104760950A CN 201510111293 A CN201510111293 A CN 201510111293A CN 104760950 A CN104760950 A CN 104760950A
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Abstract
The invention discloses a preparation method of graphene hydrogel, which includes following steps: adding a reducing agent to a graphene oxide solution for ultrasonic dispersion; heating the reaction system to carry out a reaction; and washing a reaction product after the reaction finished to obtain the graphene hydrogel. In the invention, a macroscopic form material, graphene hydrogel, in a three-dimensional network structure is assembled and formed with the graphene as a framework, so that problems of nano agglomeration and layer stacking among the layers of the graphene, thereby greatly increasing the specific surface area of the material and enhancing the adsorption effect of the material. The preparation method is easy to perform, is carried out with common reducing agents and under relative mild conditions to prepare the graphene hydrogel in a reduction manner, is decreased in preparation cost, is free of environmental pollution, is free of obviously dangerous raw materials and is suitable for large-scale commercialized production.
Description
Technical field
The invention belongs to chemosynthesis technical field, the chemical preparation relating to a kind of mild condition has the method for the Graphene hydrogel of high-adsorption-capacity to microbiotic.
Background technology
Graphene (GO) is as a kind of popular brand-new material, and have excellent electrical and thermal conductivity performance, superpower mechanical property, high stability and large specific surface area, be subject to worldwide extensive concern.In recent years, along with the continuous progress of scientific technology, the technique of a large amount of production Graphene is ripe all the more, and its cost is also cheap all the more, and high-specific surface area and ripe production technology make Graphene become a kind of potential high-efficiency adsorbent.Because Graphene prepared by ordinary method is all in superfine powdery, in use can there is the problems such as reunion, skewness due to dimensional effect, surface inertness etc., thus cause the excellent properties of material itself to can not get effective performance.Meanwhile, because the Van der Waals force of graphene film interlayer is comparatively large, make that very serious nanometer occurs between layers and reunite and the stacking phenomenon of lamella, greatly reduce the specific surface area of Graphene virtually, strongly limit its application.In water treatment procedure, because Graphene is water dispersion solution, need ultrafiltration or centrifugation after causing absorption, subsequent treatment process is complicated.In addition, there is certain bio-toxicity in the Graphene as nano material, and its secondary pollution object in the environment also result in sizable concern.
Find by literature search, for solving in this type of grapheme material problems such as easily reuniting, not easily separated, be that its self-assembly is formed the macroscopic form material of three-dimensional net structure by skeleton with Graphene, effectively can avoid the reunion between graphene sheet layer, greatly improve the specific surface area of material.Therefore, graphene macroform, because its specific surface area is large, be easy to the feature of separation, makes it in high-efficiency adsorbent and support of the catalyst, all have potential using value.
Along with developing rapidly of China's medicine industry, the pollution of pharmacy waste water to environment increasingly sharpens, and also brings serious threat to human health.Pharmaceutical industry has the features such as product category is many, production process is complicated, industrial scale difference is large.The pharmaceutical industry of current China accounts for 1.7% of national gross industrial output value, and quantity of wastewater effluent accounts for 2% of national quantity of wastewater effluent, one of pharmaceutical industry 12 key industrys being put into environment protection treating, the waste water that pharmaceutical industry produces becomes the most important thing that environmental monitoring is administered, and the antibiotic waste water typical industry waste water of large, the difficult treatment of output in pharmacy waste water especially.Recently, Science Bulletin there is article point out, there are 68 kinds of microbiotic in China's surface water, show urgency and the necessity of microbiotic waste water control.For this reason, need a kind of novel effective sorbent material badly to administer containing microbiotic sewage.
Summary of the invention
For the defect of prior art, the object of the invention is to provide a kind of preparation method of Graphene hydrogel, and reaction conditions is gentle, and products obtained therefrom has high-adsorption-capacity to microbiotic.
Another object of the present invention is to provide the purposes that Graphene hydrogel prepared by a kind of aforesaid method is used as sorbent material.
To achieve these goals, the technical solution used in the present invention is as follows:
The invention provides a kind of preparation method of Graphene hydrogel, comprise the following steps:
In graphene oxide solution, add reductive agent carry out ultrasonic disperse, then heating is reacted, and reaction terminates the washing of rear taking-up product and obtains Graphene hydrogel.
The preparation method of described graphene oxide solution comprises the following steps: graphite oxide is soluble in water, ultrasonic disperse 4 ~ 12h, makes graphite oxide be separated into the graphene oxide solution of stable homogeneous.
The concentration of described graphene oxide solution is 0.5 ~ 8mg/mL.
Ratio >=the 1:1 of described graphene oxide and reductive agent.
Described reductive agent is quadrol, xitix, hydrazine hydrate or gsh.
The time of described ultrasonic disperse is 0.5 ~ 4h.
The time of described heating is 10 ~ 18h.
The temperature of described heating is 70 ~ 100 DEG C.
Described washing adopts distillation washing, repetitive scrubbing.
Present invention also offers the purposes that Graphene hydrogel prepared by a kind of aforesaid method is used as sorbent material.
Present invention also offers Graphene hydrogel prepared by a kind of aforesaid method for purposes antibiotic in absorption effluent.
The present invention compared with the existing technology, has the following advantages and beneficial effect:
The present invention take Graphene as the macroscopic form material Graphene hydrogel that skeleton assembling forms three-dimensional net structure, the nanometer that effectively prevent between graphene sheet layer is reunited and the stacking phenomenon of lamella, drastically increase the specific surface area of material, improve its adsorption effect.
The preparation of powdered graphite alkene is become hydrogel macroscopic body form by the present invention, make it have specific surface area large, be easy to the feature be separated, need the problem of ultrafiltration or centrifugation, subsequent treatment process complexity after the absorption of effective solution powdered graphite alkene, make it in high-efficiency adsorbent and support of the catalyst, all have potential using value.
The Graphene hydrogel that the present invention obtains has higher adsorptive power for antibiotic waste water, is much better than common adsorbents, has widened the range of application of grapheme material.
Of the present invention simple for process, have employed common reductive agent, reduction obtains Graphene hydrogel under relatively mild conditions, reduces preparation cost, and environmentally safe, without obvious hazardous materials, be suitable for large-scale commercial and produce.
Accompanying drawing explanation
Fig. 1 is the optical picture of the Graphene hydrogel that the present invention obtains.
Fig. 2 is the field emission scanning electron microscope figure of the Graphene hydrogel that the present invention obtains.
Fig. 3 is that the Graphene hydrogel that obtains of the present invention is for absorption optical picture antibiotic in sewage.
Fig. 4 is the isothermal map of the Graphene hydrogel that obtains of the present invention for microbiotic absorption in sewage.
Embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the present invention is further detailed explanation.
Embodiment 1
The inventive method adopts chemical reduction method under being used in gentle water-bath condition, and redox graphene makes it that self-assembly phenomenon occur and forms Graphene hydrogel.
Graphite oxide is soluble in water, and ultrasonic 12 hours, the concentration making graphite oxide be separated into stable homogeneous was the graphene oxide solution of 1mg/mL; Be that 1:1 adds reductive agent xitix according to graphene oxide and reductive agent mass ratio in the graphene oxide solution of gained, ultrasonic disperse 2 hours, makes reductive agent mix with graphene oxide solution; Be sub-packed in beaker according to a certain amount of, and seal with sealed membrane, and put into water-bath, controlling water-bath temperature is 70 DEG C, and heat-up time is 10 hours; After reduction reaction end of processing, take out product, gained Graphene hydrogel is soaked in distilled water, constantly change water washing, obtain required product, as shown in Figure 1, Fig. 1 is the optical picture of the Graphene hydrogel that the present invention obtains to its optics picture, graphene oxide solution, through reduction process generation self-assembly, defines hydrophobic three-dimensional macro structure.Through BET test, the specific surface area of this Graphene hydrogel can reach 361m
2/ g.
Embodiment 2
Graphite oxide is soluble in water, and ultrasonic 10 hours, the concentration making graphite oxide be separated into stable homogeneous was the graphene oxide solution of 2mg/mL; Be that 1:1 adds reductive agent xitix according to graphene oxide and reductive agent mass ratio in the graphene oxide solution of gained, ultrasonic disperse 4 hours, makes reductive agent mix with graphene oxide solution; Be sub-packed in beaker according to a certain amount of, and seal with sealed membrane, and put into water-bath, controlling water-bath temperature is 75 DEG C, and heat-up time is 10 hours; After reduction reaction end of processing, take out product, gained Graphene hydrogel is soaked in distilled water, constantly change water washing, obtain required product, as shown in Figure 2, Fig. 2 is the field emission scanning electron microscope figure of the Graphene hydrogel that the present invention obtains to its field emission scanning electron microscope picture, show in figure, between graphene sheet layer, constitute three-dimensional structure through self-assembly is mutually stacking.Through BET test, the specific surface area of this Graphene hydrogel can reach 334m
2/ g
Equivalent Graphene hydrogel is placed in the sample bottle of 25mL, adds the ciprofloxacin solution of 20mL different concns (20mg/L-160mg/L) respectively, sealing mark.The initial concentration of ciprofloxacin solution is determined by preliminary experiment, to ensure about the 20-80% being controlled at initial amount by the Ciprofloxacin adsorbed.Sample bottle is put into vibrator, keeps thermostatic 25 DEG C vibration 120h.Use disposable syringe extracting liquid after reaching the scheduled time, and with filtering with microporous membrane, filtrate is placed in colorimetric cylinder.After dilution certain multiple, under maximum absorption band (λ max=275nm), measure its absorbancy.Each concentration does two Duplicate Samples tests, and equilibrium concentration gets the mean value of twice experimental result.As shown in Figure 3, Fig. 3 be the Graphene hydrogel that obtains of the present invention for absorption optical picture antibiotic in sewage, show in figure, Graphene hydrogel density is greater than solution, has three-dimensional macro structure, is conveniently separated.The Ciprofloxacin blank solution of same concentrations series in contrast.Take equilibrium concentration as X-coordinate, loading capacity is that ordinate zou is mapped, Langmuir and Freundlich model is adopted to carry out matching to result, as shown in Figure 4, Fig. 4 is the isothermal map of the Graphene hydrogel that obtains of the present invention for microbiotic absorption in sewage, and Graphene hydrogel is higher for Langmuir and Freundlich model-fitting degree for antibiotic adsorption isothermal line.Its loading capacity can reach 214mg/g, is in a leading position in allied substances.
Embodiment 3
Graphite oxide is soluble in water, and ultrasonic 4 hours, the concentration making graphite oxide be separated into stable homogeneous was the graphene oxide solution of 4mg/mL; Be that 3:1 adds reductive agent gsh according to graphene oxide and reductive agent mass ratio in the graphene oxide solution of gained, ultrasonic disperse 1.5 hours, makes reductive agent mix with graphene oxide solution; Be sub-packed in beaker according to a certain amount of, and seal with sealed membrane, and put into water-bath, controlling water-bath temperature is 80 DEG C, and heat-up time is 14 hours; After reduction reaction end of processing, take out product, gained Graphene hydrogel is soaked in distilled water, constantly changes water washing, obtain required product.
Embodiment 4
Graphite oxide is soluble in water, and ultrasonic 8 hours, the concentration making graphite oxide be separated into stable homogeneous was the graphene oxide solution of 1mg/mL; Be that 4:1 adds reductive agent quadrol according to graphene oxide and reductive agent mass ratio in the graphene oxide solution of gained, ultrasonic disperse 1 hour, makes reductive agent mix with graphene oxide solution; Be sub-packed in beaker according to a certain amount of, and seal with sealed membrane, and put into water-bath, controlling water-bath temperature is 100 DEG C, and heat-up time is 12 hours; After reduction reaction end of processing, take out product, gained Graphene hydrogel is soaked in distilled water, constantly changes water washing, obtain required product.
Embodiment 5
Graphite oxide is soluble in water, and ultrasonic 6 hours, the concentration making graphite oxide be separated into stable homogeneous was the graphene oxide solution of 8mg/mL; Be that 5:1 adds reductive agent quadrol according to graphene oxide and reductive agent mass ratio in the graphene oxide solution of gained, ultrasonic disperse 0.5 hour, makes reductive agent mix with graphene oxide solution; Be sub-packed in beaker according to a certain amount of, and seal with sealed membrane, and put into water-bath, controlling water-bath temperature is 90 DEG C, and heat-up time is 18 hours; After reduction reaction end of processing, take out product, gained Graphene hydrogel is soaked in distilled water, constantly changes water washing, obtain required product.
Embodiment 6
Graphite oxide is soluble in water, and ultrasonic 9 hours, the concentration making graphite oxide be separated into stable homogeneous was the graphene oxide solution of 6mg/mL; Be that 10:1 adds reductive agent hydrazine hydrate according to graphene oxide and reductive agent mass ratio in the graphene oxide solution of gained, ultrasonic disperse 3 hours, makes reductive agent mix with graphene oxide solution; Be sub-packed in beaker according to a certain amount of, and seal with sealed membrane, and put into water-bath, controlling water-bath temperature is 85 DEG C, and heat-up time is 16 hours; After reduction reaction end of processing, take out product, gained Graphene hydrogel is soaked in distilled water, constantly changes water washing, obtain required product.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. a preparation method for Graphene hydrogel, is characterized in that: comprise the following steps:
In graphene oxide solution, add reductive agent carry out ultrasonic disperse, then heating is reacted, and reaction terminates the washing of rear taking-up product and obtains Graphene hydrogel.
2. the preparation method of Graphene hydrogel according to claim 1, it is characterized in that: the preparation method of described graphene oxide solution comprises the following steps: graphite oxide is soluble in water, ultrasonic disperse 4 ~ 12h, makes graphite oxide be separated into the graphene oxide solution of stable homogeneous.
3. the preparation method of Graphene hydrogel according to claim 2, is characterized in that: the concentration of described graphene oxide solution is 0.5 ~ 8mg/mL.
4. the preparation method of Graphene hydrogel according to claim 1, is characterized in that: the ratio >=1:1 of described graphene oxide and reductive agent.
5. the preparation method of Graphene hydrogel according to claim 1, is characterized in that: described reductive agent is quadrol, xitix, hydrazine hydrate or gsh.
6. the preparation method of Graphene hydrogel according to claim 1, is characterized in that: the time of described ultrasonic disperse is 0.5 ~ 4h.
7. the preparation method of Graphene hydrogel according to claim 1, is characterized in that: the time of described heating is 10 ~ 18h.
8. the preparation method of Graphene hydrogel according to claim 1, is characterized in that: the temperature of described heating is 70 ~ 100 DEG C;
Or described washing adopts distillation washing, repetitive scrubbing.
9. the Graphene hydrogel that prepared by the arbitrary described method of a claim 1 to 8 is used as the purposes of sorbent material.
10. the Graphene hydrogel prepared of the arbitrary described method of a claim 1 to 8 is for purposes antibiotic in absorption effluent.
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Cited By (15)
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|---|---|---|---|---|
| CN105152158A (en) * | 2015-09-23 | 2015-12-16 | 同济大学 | Preparation method for three-dimensional graphene hydrogel electrode material and application thereof to capacitive deionization |
| CN105170085A (en) * | 2015-09-18 | 2015-12-23 | 同济大学 | Method for preparing three-dimensional graphene hydrogel of loaded anatase type titanium dioxide nanotube |
| CN105214607A (en) * | 2015-09-11 | 2016-01-06 | 湖南大学 | The preparation method of redox graphene, redox graphene and application thereof |
| CN105833851A (en) * | 2016-05-18 | 2016-08-10 | 同济大学 | Method for preparing functional group modified alginate-graphene dual-network nano-composite gel beads |
| CN106006616A (en) * | 2016-05-25 | 2016-10-12 | 江苏科技大学 | Preparation method of high-adsorbability graphene aerogel |
| CN106653388A (en) * | 2016-10-08 | 2017-05-10 | 南京师范大学 | Three-dimensional pure graphene hydrogel material with high conductivity and preparation method thereof |
| CN107265434A (en) * | 2017-06-13 | 2017-10-20 | 江苏大学 | A kind of bamboo nano-cellulose/redox graphene is combined the preparation method and applications of carbon aerogels |
| CZ307220B6 (en) * | 2016-12-21 | 2018-04-04 | Vysoké Učení Technické V Brně | A method of preparing graphene hydrogel |
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| CN108275679A (en) * | 2018-02-05 | 2018-07-13 | 山西大学 | A kind of method and its application preparing graphene oxide sponge using glutathione |
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| CN112156753A (en) * | 2020-09-23 | 2021-01-01 | 中国石油大学(华东) | Graphene aerogel and preparation method and application thereof |
| CN115626640A (en) * | 2017-05-05 | 2023-01-20 | 西格马-奥尔德里奇有限责任公司 | Method for manufacturing graphene oxide gel |
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| CN102757040A (en) * | 2012-07-25 | 2012-10-31 | 哈尔滨工业大学 | Graphene-based hydrogel and preparation method thereof as well as preparation method and application of supercapacitor electrode taking graphene-based hydrogel as active material |
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Patent Citations (2)
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| CN101941693A (en) * | 2010-08-25 | 2011-01-12 | 北京理工大学 | Graphene aerogel and preparation method thereof |
| CN102757040A (en) * | 2012-07-25 | 2012-10-31 | 哈尔滨工业大学 | Graphene-based hydrogel and preparation method thereof as well as preparation method and application of supercapacitor electrode taking graphene-based hydrogel as active material |
Cited By (18)
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| CN105214607A (en) * | 2015-09-11 | 2016-01-06 | 湖南大学 | The preparation method of redox graphene, redox graphene and application thereof |
| CN105170085A (en) * | 2015-09-18 | 2015-12-23 | 同济大学 | Method for preparing three-dimensional graphene hydrogel of loaded anatase type titanium dioxide nanotube |
| CN105152158A (en) * | 2015-09-23 | 2015-12-16 | 同济大学 | Preparation method for three-dimensional graphene hydrogel electrode material and application thereof to capacitive deionization |
| CN105833851A (en) * | 2016-05-18 | 2016-08-10 | 同济大学 | Method for preparing functional group modified alginate-graphene dual-network nano-composite gel beads |
| CN106006616A (en) * | 2016-05-25 | 2016-10-12 | 江苏科技大学 | Preparation method of high-adsorbability graphene aerogel |
| CN106653388A (en) * | 2016-10-08 | 2017-05-10 | 南京师范大学 | Three-dimensional pure graphene hydrogel material with high conductivity and preparation method thereof |
| CZ307220B6 (en) * | 2016-12-21 | 2018-04-04 | Vysoké Učení Technické V Brně | A method of preparing graphene hydrogel |
| CN115626640A (en) * | 2017-05-05 | 2023-01-20 | 西格马-奥尔德里奇有限责任公司 | Method for manufacturing graphene oxide gel |
| CN107265434A (en) * | 2017-06-13 | 2017-10-20 | 江苏大学 | A kind of bamboo nano-cellulose/redox graphene is combined the preparation method and applications of carbon aerogels |
| CN108057422A (en) * | 2017-12-14 | 2018-05-22 | 中国科学院生态环境研究中心 | A kind of alcohol bridging enhancing porous hydroxyapatite iron oxide-graphene nano composite hydrogel and preparation method and application |
| CN108057422B (en) * | 2017-12-14 | 2020-03-10 | 中国科学院生态环境研究中心 | Alcohol-bridged reinforced porous iron oxyhydroxide-graphene nano composite hydrogel and preparation method and application thereof |
| CN108275679A (en) * | 2018-02-05 | 2018-07-13 | 山西大学 | A kind of method and its application preparing graphene oxide sponge using glutathione |
| CN109174042A (en) * | 2018-11-09 | 2019-01-11 | 北京交通大学 | A kind of preparation method and applications of poly-dopamine-graphene hydrogel adsorbent |
| CN109622068A (en) * | 2019-01-04 | 2019-04-16 | 河南师范大学 | A kind of preparation method and applications for the load cobalt graphene aerogel composite catalyst that can efficiently activate persulfate |
| CN109622068B (en) * | 2019-01-04 | 2022-03-01 | 河南师范大学 | Preparation method and application of cobalt-loaded graphene aerogel composite catalyst capable of efficiently activating persulfate |
| CN111686688A (en) * | 2020-06-23 | 2020-09-22 | 广东工业大学 | Amino-modified graphene hydrogel and preparation method and application thereof |
| CN111686688B (en) * | 2020-06-23 | 2022-06-24 | 广东工业大学 | Amino-modified graphene hydrogel and preparation method and application thereof |
| CN112156753A (en) * | 2020-09-23 | 2021-01-01 | 中国石油大学(华东) | Graphene aerogel and preparation method and application thereof |
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Application publication date: 20150708 |