CN106006616A - Preparation method of high-adsorbability graphene aerogel - Google Patents
Preparation method of high-adsorbability graphene aerogel Download PDFInfo
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- CN106006616A CN106006616A CN201610353225.4A CN201610353225A CN106006616A CN 106006616 A CN106006616 A CN 106006616A CN 201610353225 A CN201610353225 A CN 201610353225A CN 106006616 A CN106006616 A CN 106006616A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention discloses a preparation method of a high-adsorbability graphene aerogel. The preparation method comprises the following steps: (1) adding graphene oxide into deionized water to obtain a graphene oxide water solution; (2) uniformly mixing an ammonia borane water solution, a ferrous sulfate water solution and the graphene oxide water solution; (3) carrying out constant-temperature hydrothermal reaction on the mixed water solution to obtain a graphene aquagel; and (4) carrying out immersion, prefreezing and freeze-drying on the graphene aquagel to obtain the high-adsorbability graphene aerogel. The ammonia borane and ferrous sulfate are matched to reduce the graphene oxide, thereby increasing the reduction speed of the constant-temperature hydrothermal reaction; and the process is simple to operate and simple in preparation method. The obtained graphene aerogel has efficient adsorption effect on the dye rhodamine B, and can basically finish adsorption within 3 hours.
Description
Technical field
The present invention relates to a kind of grapheme material, be specifically related to the preparation method of a kind of high absorption property graphene aerogel.
Background technology
Along with deepening continuously of Chinese Industrialization and urbanization, the topic that freshwater resources are in short supply is laid out agenda more and more.Freshwater resources deficiency is added water and is polluted two problem superpositions appearance so that the state between supply and demand of water seems and particularly allows of no optimist.In addition to appealing popular using water wisely, another approach effectively solving this difficult problem is exactly the recovery to waste water, processes, recycles.In the middle of this, the process for colored dyes waste water usually uses the means such as absorption, filtration.The material carrying out filtering, adsorbing currently for colored dyes waste water is in the majority with material with carbon element again, and modal adsorptivity material with carbon element is activated carbon, and it has, and plurality of advantages is the most cheap, specific surface area is big.
Since single-layer graphene in 2004 adheres to be found by adhesive tape, as the newcomer of carbon family, it receives the extensive concern of more and more domestic and international scientist.Graphene has the two-dimensional structure of uniqueness, and the thickness of only one of which atom and the highest specific surface area.Therefore some investigators has carried out Graphene and derived material thereof and has polluted the research in this subject under discussion at water, and presents it and have huge application prospect in terms of sewage disposal and further deep-cut space.
After graphenic surface is modified oxygen-containing functional group, graphene oxide is i.e. the classification focus studied as the research of adsorbent.By relatively easy for oxygen-containing for Graphene functionalization operation, it is easy to preparation.But present stage, graphene oxide can not highlight the advantage of graphene product for the absorption of colored dyes, and it is even below activated carbon [Chemical for the absorption of colored dyes sometimes
Engineering Research and Design,91(2013),361-368]。
Graphene aerogel is more and more paid close attention to by all circles as a kind of novel adsorbing material.It is the porous material of a kind of three-dimensional manometer network structure, not only remain the physico-chemical property that Graphene is outstanding, also there is porosity big, the advantage such as pore-size distribution width, make it not only at field of Environment Protection, also applied widely in fields such as mechanics, electricity, optics even medical science.
Summary of the invention
Solve the technical problem that: the deficiency existed for prior art, the invention provides the preparation method of a kind of high absorption property graphene aerogel, simplify preparation technology, reduce energy consumption, improve its adsorption effect to coloured fuel.
Technical scheme: the preparation method of a kind of high absorption property graphene aerogel that the present invention provides, including following preparation process:
(1) adding graphene oxide in deionized water, through ultrasonic disperse or mechanical agitation 30 ~ 60min until mix homogeneously, prepared mass concentration is the graphene oxide water solution of 1～4mg/mL；
(2) ammonia borine aqueous solution and ferrous sulfate aqueous solution it are respectively configured, by ammonia borine aqueous solution, ferrous sulfate aqueous solution with step (1) gained graphene oxide water solution by volume for 1:1:(8～10) mix, and through ultrasonic disperse or mechanical agitation 10 ~ 45min until mix homogeneously, obtain graphene oxide and ammonia borine, the mixed aqueous solution of ferrous sulfate；
(3) mixed aqueous solution step (2) prepared, prepares Graphene hydrogel through incubation water heating reaction, and reaction temperature is 80～160 DEG C, and the response time is 6～12h；
(4) the Graphene hydrogel that step (3) prepares is soaked in aqueous solution 24～72h, under conditions of-20 ~-4 DEG C, then carries out precooling, then through lyophilization, i.e. obtain high absorption property graphene aerogel；Described lyophilization temperature is-50～-80 DEG C, and the time is 24～72h.
The mass concentration of step (2) described ammonia borine aqueous solution is 0.1～1mg/mL, and the molar concentration of described ferrous sulfate aqueous solution is 0.1～1mmol/mL.
The ultrasonic power of step (1) and (2) described ultrasonic disperse is 40～1000W, and supersonic frequency is 20～80KHz, and described churned mechanically rotating speed is 40～4000 revs/min.
The preparation method of step (1) described graphene oxide is: under the conditions of 0-4 DEG C of ice-water bath, and 1g natural flake graphite joins the dense H of 30mL2SO4In, use the speed mechanical agitation of 200～500 revs/min, treat that temperature is cooled to zero degree, add the KNO of 0.5g3KMnO with 3g4, control to react 2h under conditions of reaction temperature is less than 10 DEG C；Reaction system being transferred to stirring reaction 45min again in the water bath with thermostatic control of 35～40 DEG C, then reaction system is transferred in the constant temperature oil bath of 90 DEG C, dropping total amount is the deionized water of 90mL, controls temperature below 110 DEG C；With 20 ~ 50ml 5%H2O2Remove unnecessary KMnO4, now stop mechanical agitation, wash 3-5 time with 5%HCl, more fully wash with deionized water, final product is transferred to be dried in 40 DEG C of baking ovens 24 ~ 72h, obtains graphene oxide.
Beneficial effect: (1) utilizes ammonia borine to coordinate redox graphene with ferrous sulfate, accelerates the reduction rate of incubation water heating reaction, and easy and simple to handle, and preparation method is simple.
(2) graphene aerogel that the present invention prepares, the adsorption effect for dyestuff (rhodamine B) is efficient, within 3 hours, can substantially adsorb complete.Contribute to the further expansion that graphene aerogel is studied at field of Environment Protection.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1 graphene aerogel；
Fig. 2 is the BET De contamination curve chart of embodiment 1 graphene aerogel；
Fig. 3 is macroscopical adsorption effect figure that embodiment 1 adsorbs rhodamine B solution different time sections；
Fig. 4 is the UV-vis absorption spectrum that embodiment 1 adsorbs rhodamine B solution different time sections.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but the most therefore protection scope of the present invention is confined to following embodiment, but is limited by description and claims of this specification.
In embodiment, the preparation of graphene oxide is adopted with the following method: under conditions of the ice-water bath of 0 DEG C, and 1g natural flake graphite joins the dense H of 30mL2SO4(98%), use the speed of 300 revs/min to carry out mechanical agitation, treat that temperature is cooled to zero degree, be slowly added to the KNO of 0.5g3KMnO with 3g4, now control to make reaction carry out 2h under conditions of reaction temperature is less than 10 DEG C.Reaction system is transferred to stirring reaction 45min in the water bath with thermostatic control of 35～40 DEG C again.Then reaction system is transferred in the constant temperature oil bath of 90 DEG C, be slowly added dropwise the deionized water that total amount is 90mL, control temperature below 110 DEG C.5%H by excess2O2Remove unnecessary KMnO4, wash 3 ~ 5 times with 5%HCl after stopping mechanical agitation, more fully wash with deionized water.Transfer to final product the baking oven of 40 DEG C is dried, obtain graphene oxide and retain standby.
Embodiment 1
Weigh 16mg solid oxidation Graphene to be placed in the deionized water of 8mL, ultrasonic 1h, make the aqueous solution of graphene oxide, this aqueous solution is moved in the cylindrical glass bottle of 20mL, mix with volume ratio 8:1:1 with the ammonia Borane solution of 0.3mg/mL and the copperas solution of 0.2mmol/mL and mechanical agitation 20min obtains mixed solution, cylindrical glass bottle is kept 8h in 95 DEG C of reactions, obtains columned product；Columned product is soaked into 48h in deionized water, more described cylindric product is placed in-4 DEG C of precoolings；The material of precooling is put in freezer dryer, lyophilization 48h at-80 DEG C, i.e. can get graphene aerogel, the SEM of graphene aerogel schemes as shown in Figure 1, the nitrogen adsorption curve chart of aeroge is as shown in Figure 2, Graphene synusia in aeroge stacks mutually, forms loose structure, and contributes to its absorption being applied to material.
Embodiment 2
Weigh 30mg solid oxidation Graphene to be placed in the deionized water of 15mL, ultrasonic 1h, make the aqueous solution of graphene oxide, this aqueous solution is moved in the cylindrical glass bottle of 50mL, mix with volume ratio 10:1:1 with the copperas solution of 0.5mmol/mL with the ammonia Borane solution of 0.5mg/mL, ultrasonic disperse 15min obtains mixed solution, in 120 DEG C of reactions, cylindrical glass bottle is kept 6h, obtains columned product；Columned product is soaked into 24h in deionized water, more described cylindric product is placed in-4 DEG C of precoolings；The material of precooling is put in freezer dryer, lyophilization 24h at-80 DEG C, i.e. can get graphene aerogel.
Embodiment 3
Weigh 30mg solid oxidation Graphene to be placed in the deionized water of 10mL, ultrasonic 1h, make the aqueous solution of graphene oxide, this aqueous solution is moved in the cylindrical glass bottle of 50mL, mix with volume ratio 8:1:1 with the copperas solution of 0.5mmol/mL with the ammonia Borane solution of 0.3mg/mL, and mechanical agitation 25min obtains mixed solution, cylindrical glass bottle is kept 7h in 105 DEG C of reactions, obtains columned product；Columned product is soaked into 24h in deionized water, more described cylindric product is placed in-4 DEG C of precoolings；The material of precooling is put in freezer dryer, lyophilization 72h at-80 DEG C, i.e. can get graphene aerogel.
In order to verify the effect of the present invention, we do the absorption experiment of following ultraviolet-visible:
Weigh the graphene aerogel sample 20mg that embodiment 1 prepares, put into (100mL deionized water+9.6mg rhodamine B) in the rhodamine B solution of 10mL, test the absorption spectrum of ultraviolet-visible at regular intervals.
After aeroge absorbs rhodamine B, the macroscopical of color changes as shown in Figure 3.By UV-vis absorption spectrum it can be seen that the graphene aerogel adsorption efficiency prepared of the present invention is high, it can be seen that the adsorption rate of laboratory sample 3h just can reach more than 98% from UV-vis absorption spectrum shown in Fig. 4, absorbability is the quickest.
Claims (5)
1. the preparation method of a high absorption property graphene aerogel, it is characterised in that preparation process is as follows:
(1) adding graphene oxide in deionized water, through ultrasonic disperse or mechanical agitation 30 ~ 60min until mix homogeneously, prepared mass concentration is the graphene oxide water solution of 1～4mg/mL；
(2) ammonia borine aqueous solution and ferrous sulfate aqueous solution it are respectively configured, by ammonia borine aqueous solution, ferrous sulfate aqueous solution with step (1) gained graphene oxide water solution by volume for 1:1:(8～10) mix, and through ultrasonic disperse or mechanical agitation 10 ~ 45min until mix homogeneously, obtain graphene oxide and ammonia borine, the mixed aqueous solution of ferrous sulfate；
(3) mixed aqueous solution step (2) prepared, prepares Graphene hydrogel through incubation water heating reaction, and reaction temperature is 80～160 DEG C, and the response time is 6～12h；
(4) the Graphene hydrogel that step (3) prepares is soaked in aqueous solution 24～72h, under conditions of-20 ~-4 DEG C, then carries out precooling, then through lyophilization, i.e. obtain high absorption property graphene aerogel；Described lyophilization temperature is-50～-80 DEG C, and the time is 24～72h.
The preparation method of a kind of high absorption property graphene aerogel the most according to claim 1, the mass concentration that it is characterized in that step (2) described ammonia borine aqueous solution is 0.1～1mg/mL, and the molar concentration of described ferrous sulfate aqueous solution is 0.1～1mmol/mL.
The preparation method of a kind of high absorption property graphene aerogel the most according to claim 1, it is characterised in that the ultrasonic power of step (1) and (2) described ultrasonic disperse is 40～1000W, supersonic frequency is 20～80KHz.
The preparation method of a kind of high absorption property graphene aerogel the most according to claim 1, it is characterised in that step (1) and (2) described churned mechanically rotating speed are 40～4000 revs/min.
The preparation method of a kind of high absorption property graphene aerogel the most according to claim 1, it is characterised in that the preparation method of step (1) described graphene oxide is: under the conditions of 0-4 DEG C of ice-water bath, and 1g natural flake graphite joins the dense H of 30mL2SO4In, use the speed mechanical agitation of 200～500 revs/min, treat that temperature is cooled to zero degree, add the KNO of 0.5g3KMnO with 3g4, control to react 2h under conditions of reaction temperature is less than 10 DEG C；Reaction system being transferred to stirring reaction 45min again in the water bath with thermostatic control of 35～40 DEG C, then reaction system is transferred in the constant temperature oil bath of 90 DEG C, dropping total amount is the deionized water of 90mL, controls temperature below 110 DEG C；With 20 ~ 50ml 5%H2O2Remove unnecessary KMnO4, now stop mechanical agitation, wash 3-5 time with 5%HCl, more fully wash with deionized water, final product is transferred to be dried in 40 DEG C of baking ovens 24 ~ 72h, obtains graphene oxide.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698398A (en) * | 2016-11-30 | 2017-05-24 | 厦门大学 | Method for preparing graphene aerogel by using activated sludge |
| CN107416800A (en) * | 2017-08-15 | 2017-12-01 | 东南大学 | A kind of method that hydro-thermal method prepares N and S codope three-dimensional grapheme materials |
| 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 |
| CN108285127A (en) * | 2017-01-10 | 2018-07-17 | 空中客车防务和空间有限责任公司 | Ammonia borine limitation in graphene oxide three-dimensional structure |
| CN109553787A (en) * | 2018-12-19 | 2019-04-02 | 北京印刷学院 | A kind of graphene oxide modified polyvinylalcohol film and its preparation and application |
| WO2019149018A1 (en) * | 2018-02-05 | 2019-08-08 | 庄鹏宇 | Preparation method of reduced graphene oxide film |
| CN110817849A (en) * | 2019-11-29 | 2020-02-21 | 无锡市惠山区川大石墨烯应用研究中心 | Sulfhydrylation graphene aerogel and preparation method and application thereof |
| CN111001394A (en) * | 2019-12-26 | 2020-04-14 | 武汉工程大学 | Graphene oxide/sodium alginate composite aerogel efficient adsorbent and preparation method and application thereof |
| CN112934132A (en) * | 2021-03-10 | 2021-06-11 | 瓮福（集团）有限责任公司 | Boron-nitrogen co-doped reduced graphene oxide aerogel and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698398A (en) * | 2016-11-30 | 2017-05-24 | 厦门大学 | Method for preparing graphene aerogel by using activated sludge |
| CN106698398B (en) * | 2016-11-30 | 2018-12-28 | 厦门大学 | A method of graphene aerogel is prepared using activated sludge |
| CN108285127A (en) * | 2017-01-10 | 2018-07-17 | 空中客车防务和空间有限责任公司 | Ammonia borine limitation in graphene oxide three-dimensional structure |
| CN108285127B (en) * | 2017-01-10 | 2023-04-14 | 空中客车防务和空间有限责任公司 | Ammonia borane confinement in graphene oxide three-dimensional structures |
| CN107416800A (en) * | 2017-08-15 | 2017-12-01 | 东南大学 | A kind of method that hydro-thermal method prepares N and S codope three-dimensional grapheme materials |
| 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 |
| WO2019149018A1 (en) * | 2018-02-05 | 2019-08-08 | 庄鹏宇 | Preparation method of reduced graphene oxide film |
| CN109553787A (en) * | 2018-12-19 | 2019-04-02 | 北京印刷学院 | A kind of graphene oxide modified polyvinylalcohol film and its preparation and application |
| CN110817849A (en) * | 2019-11-29 | 2020-02-21 | 无锡市惠山区川大石墨烯应用研究中心 | Sulfhydrylation graphene aerogel and preparation method and application thereof |
| CN111001394A (en) * | 2019-12-26 | 2020-04-14 | 武汉工程大学 | Graphene oxide/sodium alginate composite aerogel efficient adsorbent and preparation method and application thereof |
| CN112934132A (en) * | 2021-03-10 | 2021-06-11 | 瓮福（集团）有限责任公司 | Boron-nitrogen co-doped reduced graphene oxide aerogel and preparation method and application thereof |
| CN112934132B (en) * | 2021-03-10 | 2023-03-03 | 瓮福（集团）有限责任公司 | Boron-nitrogen co-doped reduced graphene oxide aerogel and preparation method and application thereof |
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