CN108423654A - A kind of amination graphene aeroge high-efficiency adsorbent, preparation method and applications - Google Patents
A kind of amination graphene aeroge high-efficiency adsorbent, preparation method and applications 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- 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
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Abstract
The present invention relates to a kind of preparation methods of novel three-dimensional graphene aerogel high-efficiency adsorbent, it is characterized in that graphene oxide water solution and tetraethylenepentamine are placed in high-temperature high-pressure reaction kettle after evenly mixing, amination graphene hydrogel is made after hydro-thermal reaction, amination graphene aeroge is obtained after freeze-dried technology.The present invention prepares aeroge adsorbent using one step hydro thermal method, its is easy to operate, cost it is relatively low and prepare aeroge have three-dimensional porous reticular structure, its density is minimum and has huge specific surface area, use it for the absorption to Cr (IV), excellent adsorption effect is shown, adsorption capacity is up to 361.48mg/g.
Description
Technical field
The present invention relates to graphene aerogel technical field, specifically a kind of amination graphene aeroge efficient absorption
Agent, preparation method and applications.
Background technology
The graphene material that the physics professor Geim of Univ Manchester UK separated monoatomic layer for the first time in 2004
Material, it is this by carbon atom with sp2Hybridized orbit formed hexagon with the new material of cellular periodic arrangement once come out just
Cause the sensation of scientific circles.Graphene with unique mechanical property, excellent electric conductivity and huge compares table because of it
Area and be widely used in the different fields such as ultracapacitor, energy storage material, catalysis material, sensor and water process.
However, the stronger pi-pi accumulation of piece interlayer and Van der Waals after on the one hand being disperseed in aqueous solution due to single-layer graphene
The effect of power causes to cause irreversible agglomeration, and its actual specific surface area is well below theoretical value；On the other hand,
The graphene sorbing material of two-dimentional (2D) exists in water with powdered presence and is difficult to detach and easily cause secondary pollution, this
Largely limit its application in water process.Therefore, in recent years, the research of functionalization three-dimensional grapheme material becomes
Hot spot.
Invention content
In view of the deficienciess of the prior art, the present invention provides a kind of system of amination graphene aeroge high-efficiency adsorbent
Preparation Method, using graphene oxide water solution as presoma, tetraethylenepentamine passes through one as modifying agent, crosslinking agent and reducing agent
The self assembly for walking hydro-thermal reaction experiment graphene has porous structure and the huge three-dimensional grapheme gas of specific surface area to prepare
Gel high-efficiency adsorbent is made by step in detail below：
(1) graphite oxide is dispersed in water, the uniform graphene oxide water solution of a certain concentration is obtained by ultrasound stripping；
(2) it is uniformly mixed after a certain amount of tetraethylenepentamine is added into the graphene oxide water solution obtained by step (1)；
(3) mixed solution obtained in step (2) is placed in high temperature and pressure hydro-thermal reaction kettle, it is anti-under certain temperature and time
Should after obtain amination graphene hydrogel；
(4) certain after being neutrality to cleaning solution with ethanol water dialysis washing by the graphene hydrogel that step (3) obtains
Under the conditions of be dried to obtain the graphene aerogel adsorbent of stable structure.
(5) graphene aerogel for obtaining step (4) is used for the absorption to Cr (IV) aqueous solution under certain condition.
A concentration of 2 ~ 10mg/L of graphene oxide water solution described in above-mentioned steps (1)；
The dosage of tetraethylenepentamine is 0.1 ~ 6mL in above-mentioned steps (2)；
Reaction temperature in above-mentioned steps (3) is 180 DEG C, reaction time 12h；
Dry technology in above-mentioned steps (4) is Freeze Drying Technique, and drying time is 36h or more.
Aeroge adsorbent amount is 0.05 ~ 0.5g, Cr (IV) a concentration of 10 ~ 500mg/L, absorption in above-mentioned steps (5)
Temperature is 20 DEG C ~ 70 DEG C, and adsorption time is 0.1 ~ 6h.
Compared with the prior art, advantages of the present invention is mainly reflected in：
1, the present invention prepares graphene aerogel using one step hydro thermal method, simple for process, easy to operate；
2, tetraethylenepentamine is used as modifying agent, crosslinking agent and reducing agent simultaneously, on the one hand, the covalent friendship that amino is formed with graphene
Connection is so that aerogel structure is stablized；On the other hand, the graphene aerogel that exists for of amino provides more adsorption sites, protonation
Amino and Cr (IV) Electrostatic Absorption, greatly improve adsorption capacity；
3, in the present invention, the reducing degree and amination degree of graphene oxide can be adjusted according to the dosage of tetraethylenepentamine, is
The controllable adjustment of amination graphene aeroge provides possibility；
4, the present invention will make its self assembly obtain having three-dimensional porous cross-linked network after two-dimensional graphene material amination
Graphene adsorbent, not only effectively increases adsorption site, improves absorption property, and avoids secondary caused by nano-powder
Water pollution problems.
Description of the drawings
Fig. 1 is the synthesis mechanism schematic diagram of the present invention；
Fig. 2 is the amination graphene hydrogel photo prepared with various concentration graphene oxide water solution；
Fig. 3 is the photo that the amination graphene that embodiment 2 obtains is stood on dandelion；
Fig. 4 be the obtained amination graphene aeroge of embodiment 2 × 100 times of SEM pictures；
Fig. 5 be the obtained amination graphene aeroge of embodiment 2 × 200 times of SEM pictures；
Fig. 6 be the obtained amination graphene aeroge of embodiment 2 × 500 times of SEM pictures；
Fig. 7 is the amination graphene aeroge (TEPA-GA) and graphene oxide (GO), natural graphite that embodiment 2 obtains
(GN) XRD spectra.
Specific implementation mode
The present invention will be described in detail With reference to embodiment.
A kind of preparation method of amination graphene aeroge high-efficiency adsorbent of the present invention, simple for process, operation
Simplicity, synthesis mechanism schematic diagram are as shown in Figure 1.
Using specific embodiment below, the present invention will be described in detail, and the present embodiment is being with technical solution of the present invention
Under the premise of implemented, provide detailed embodiment and process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1
(1) 0.06g graphite oxides are dissolved in 20mL distilled water, are put it into ultrasonic machine, surpassed in the case where supersonic frequency is 100Hz
Sound 1h obtains finely dispersed a concentration of 3mg/mL graphene oxide water solutions.
(2) 0.3mL tetraethylenepentamine is added in the graphene oxide water solution into step (1), is stirred with magnetic force under room temperature
It mixes device stirring 5min and obtains uniform mixed solution；
(3) mixed solution obtained in above-mentioned steps (2) is moved into the high temperature and pressure hydro-thermal that 100mL carries polytetrafluoroethyllining lining
In reaction kettle, 12h is reacted at 180 DEG C；
(4) the product dialysis washing obtained by step (3) is in neutrality with 10% ethanol water to dialyzate, obtains hydrogel, it is cold
Dry 36h aeroges derived above are lyophilized.
Embodiment 2
(1) 0.06g graphite oxides are dissolved in 20mL distilled water, are put it into ultrasonic machine, surpassed in the case where supersonic frequency is 100Hz
Sound 1h obtains finely dispersed a concentration of 3mg/mL graphene oxide water solutions.
(2) 0.5mL tetraethylenepentamine is added in the graphene oxide water solution into step (1), is stirred with magnetic force under room temperature
It mixes device stirring 5min and obtains uniform mixed solution；
(3) mixed solution obtained in above-mentioned steps (2) is moved into the high temperature and pressure hydro-thermal that 100mL carries polytetrafluoroethyllining lining
In reaction kettle, 12h is reacted at 180 DEG C；
(4) the product dialysis washing obtained by step (3) is in neutrality with 10% ethanol water to dialyzate, obtains hydrogel, it is cold
Dry 36h aeroges derived above are lyophilized.
Fig. 3 is the photo that the amination graphene that the present embodiment obtains is stood on dandelion, illustrates ammonia prepared by this patent
Base graphite alkene aeroge is ultralight aerogel material.
Fig. 4 ~ Fig. 6 is the SEM pictures for the amination graphene aeroge that the present embodiment obtains, it can be seen that prepared by this patent
Amination graphene aeroge stacked by amination graphene lamella self assembly, have three-dimensional network-like structure.
Fig. 7 is the amination graphene aeroge (TEPA-GA) and graphene oxide (GO), natural stone that the present embodiment obtains
The XRD spectra of black (GN), it will be apparent that it can be seen that natural flake graphite and GO crystallinity are preferable, the two respectively 2 θ=
There is strong diffraction maximum in 26.41 ° and 2 θ=10.92 °, and place can calculate natural flake graphite according to Bragg equation 2dsin θ=n λ
Interlamellar spacing with GO is respectively 0.33nm and 0.81nm, this phenomenon illustrates that oxygen-containing functional group successfully carries out natural flake graphite
Intercalation makes its interlamellar spacing expand.Graphene aerogel does not have apparent diffraction maximum, the weaker disperse peak in several places only occurs.
Embodiment 3
(1) 0.06g graphite oxides are dissolved in 20mL distilled water, are put it into ultrasonic machine, surpassed in the case where supersonic frequency is 100Hz
Sound 1h obtains finely dispersed a concentration of 3mg/mL graphene oxide water solutions.
(2) 1mL tetraethylenepentamine is added in the graphene oxide water solution into step (1), magnetic agitation is used under room temperature
Device stirs 5min and obtains uniform mixed solution；
(3) mixed solution obtained in above-mentioned steps (2) is moved into the high temperature and pressure hydro-thermal that 100mL carries polytetrafluoroethyllining lining
In reaction kettle, 12h is reacted at 180 DEG C；
(4) the product dialysis washing obtained by step (3) is in neutrality with 10% ethanol water to dialyzate, obtains hydrogel, it is cold
Dry 36h aeroges derived above are lyophilized.
Embodiment 4
(1) 0.02g graphite oxides are dissolved in 20mL distilled water, are put it into ultrasonic machine, surpassed in the case where supersonic frequency is 100Hz
Sound 1h obtains finely dispersed a concentration of 1mg/mL graphene oxide water solutions.
(2) 0.1mL tetraethylenepentamine is added in the graphene oxide water solution into step (1), is stirred with magnetic force under room temperature
It mixes device stirring 5min and obtains uniform mixed solution；
(3) mixed solution obtained in above-mentioned steps (2) is moved into the high temperature and pressure hydro-thermal that 100mL carries polytetrafluoroethyllining lining
In reaction kettle, 12h is reacted at 180 DEG C；
(4) the product dialysis washing obtained by step (3) is in neutrality with 10% ethanol water to dialyzate, obtains hydrogel, it is cold
Dry 36h aeroges derived above are lyophilized.
Embodiment 5
(1) 0.12g graphite oxides are dissolved in 20mL distilled water, are put it into ultrasonic machine, surpassed in the case where supersonic frequency is 100Hz
Sound 1h obtains finely dispersed a concentration of 6mg/mL graphene oxide water solutions.
(2) 6mL tetraethylenepentamine is added in the graphene oxide water solution into step (1), magnetic agitation is used under room temperature
Device stirs 5min and obtains uniform mixed solution；
(3) mixed solution obtained in above-mentioned steps (2) is moved into the high temperature and pressure hydro-thermal that 100mL carries polytetrafluoroethyllining lining
In reaction kettle, 12h is reacted at 180 DEG C；
(4) the product dialysis washing obtained by step (3) is in neutrality with 10% ethanol water to dialyzate, obtains hydrogel, it is cold
Dry 36h aeroges derived above are lyophilized.
Embodiment 6
The heavy chromium for aeroge adsorbent 0.05g inputs 30mLCr (IV) a concentration of 100mg/mL that Example 1 ~ 3 is prepared
In sour potassium standard solution, 3h is reacted in thermostatic control oscillator vibration at 40 DEG C.After adsorption reaction, 1mL is pipetted after filtering
Filtrate is separately added into 2.5mL sulfuric acid solutions and 2.5mL diphenylcarbazide color developing agents, passes through hexichol carbon in 50mL colorimetric cylinders
Two hydrazine spectrophotometry of acyl calculates adsorption capacity after measuring its absorbance, carries out 3 groups of parallel laboratory tests, is averaged.
The experimental data of above 3 embodiments：
Data above shows that amination graphene aeroge density prepared by the present invention is minimum and has huge specific surface area,
Excellent adsorption effect is shown to the absorption of Cr (IV).
Claims (6)
1. a kind of amination graphene aeroge adsorbent, which is characterized in that including being self-assembled by amination graphene lamella
Three-dimensional porous network shape structure；There is amination graphene piece interlayer amino to react shape by hydrothermal reduction with graphene oxide
At covalent bond；Further include the amino not with graphite oxide alkene reaction, the graphene aerogel that exists for of amino provides additionally
Adsorption site.
2. a kind of preparation method of amination graphene aeroge high-efficiency adsorbent, which is characterized in that include the following steps：
Mixture comprising single-layer graphene oxide, tetraethylenepentamine and water is uniformly dispersed, be placed under hydro-thermal reaction environment into
Row hydro-thermal reaction, obtains intermediate product；The intermediate product of hydro-thermal reaction is dialysed to dialyzate and is in neutrality, amino graphite is obtained
Alkene hydrogel；It is freeze-dried amination graphene hydrogel, obtains amination graphene aeroge.
3. the preparation method of amination graphene aeroge high-efficiency adsorbent according to claim 2, which is characterized in that tool
Body step includes：
1) finely dispersed graphene oxide water solution is prepared；
2) it is stirred evenly after tetraethylenepentamine being added in the graphene oxide water solution of gained into step 1)；
3) mixed solution in step 2) is moved into progress hydro-thermal reaction in high-temperature high-pressure reaction kettle and obtains hydrogel；
4) product after reacting is dialysed with ethanol water repeatedly after washing, and aeroge is obtained after freeze-drying.
4. the preparation method of amination graphene aeroge according to claim 2 or 3, specifically, it is characterized in that, tool
Body step includes：
1) a certain amount of graphite oxide is dissolved in 20mL distilled water, is put it into ultrasonic machine, in the case where supersonic frequency is 100Hz
Ultrasonic 1h obtains finely dispersed a concentration of 1 ~ 6mg/mL graphene oxide water solutions；
2) 0.1 ~ 6mL tetraethylenepentamine is added into the graphene oxide water solution in step 1), magnetic stirring apparatus is used under room temperature
It stirs 5min and obtains uniform mixed solution；
3) by above-mentioned steps 2) in obtained mixed solution to move into high temperature and pressure hydro-thermals of the 100mL with polytetrafluoroethyllining lining anti-
It answers in kettle, reacts 12h at 180 DEG C；
4) the product dialysis washing obtained by step 3) is in neutrality with 10% ethanol water to dialyzate, obtains hydrogel, freezes
Dry 36h aeroges derived above.
5. application of the amination graphene aeroge adsorbent in terms of the absorption of Cr (IV) described in claim 1.
6. application of the amination graphene aeroge adsorbent according to claim 5 in terms of the absorption of Cr (IV),
It is characterized in that, includes the following steps：
It takes amination graphene aeroge adsorbent to put into pending liquid, 0.1 ~ 6h is reacted at 20 DEG C ~ 70 DEG C；Absorption
After reaction, amino graphite, the Cr (IV) in liquid of the detection by the absorption of amination graphene aeroge are separated by filtration
Content.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110282620A (en) * | 2019-07-30 | 2019-09-27 | 南京林业大学 | A kind of graphite oxide aerogel and its preparation method and application |
| CN110404519A (en) * | 2019-09-04 | 2019-11-05 | 安徽省聚科石墨烯科技股份公司 | A kind of graphene aerogel adsorbent detected for phenylurea analog herbicide in water |
| CN110713181A (en) * | 2019-09-30 | 2020-01-21 | 北京石墨烯技术研究院有限公司 | Modified graphene for removing metal ions in water, preparation method thereof, product containing modified graphene and application of modified graphene |
| 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 |
| CN111137985A (en) * | 2020-01-08 | 2020-05-12 | 西南科技大学 | Preparation method of microbial degradation material for treating ammonia nitrogen in sewage |
| CN111554901A (en) * | 2020-05-11 | 2020-08-18 | 赵东伟 | Nano hollow SnO2-graphene lithium ion battery cathode material and preparation method thereof |
| CN113600135A (en) * | 2021-07-27 | 2021-11-05 | 中山大学 | Three-dimensional porous graphene aerogel material and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110282620A (en) * | 2019-07-30 | 2019-09-27 | 南京林业大学 | A kind of graphite oxide aerogel and its preparation method and application |
| CN110282620B (en) * | 2019-07-30 | 2022-11-18 | 南京林业大学 | Graphene oxide aerogel and preparation method and application thereof |
| CN110404519A (en) * | 2019-09-04 | 2019-11-05 | 安徽省聚科石墨烯科技股份公司 | A kind of graphene aerogel adsorbent detected for phenylurea analog herbicide in water |
| CN110713181A (en) * | 2019-09-30 | 2020-01-21 | 北京石墨烯技术研究院有限公司 | Modified graphene for removing metal ions in water, preparation method thereof, product containing modified graphene and application of modified graphene |
| 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 |
| CN111137985A (en) * | 2020-01-08 | 2020-05-12 | 西南科技大学 | Preparation method of microbial degradation material for treating ammonia nitrogen in sewage |
| CN111554901A (en) * | 2020-05-11 | 2020-08-18 | 赵东伟 | Nano hollow SnO2-graphene lithium ion battery cathode material and preparation method thereof |
| CN111554901B (en) * | 2020-05-11 | 2021-08-24 | 吉林中溢炭素科技有限公司 | Nano hollow SnO2-graphene lithium ion battery cathode material and preparation method thereof |
| CN113600135A (en) * | 2021-07-27 | 2021-11-05 | 中山大学 | Three-dimensional porous graphene aerogel material and preparation method and application thereof |
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