CN109692669A - A kind of preparation method of graphene metal ion adsorbent - Google Patents
A kind of preparation method of graphene metal ion adsorbent Download PDFInfo
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- CN109692669A CN109692669A CN201811337328.7A CN201811337328A CN109692669A CN 109692669 A CN109692669 A CN 109692669A CN 201811337328 A CN201811337328 A CN 201811337328A CN 109692669 A CN109692669 A CN 109692669A
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- graphene
- dopamine
- metal ion
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- ion adsorbent
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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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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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
Abstract
The invention belongs to technical field of function materials more particularly to a kind of preparation methods of graphene metal ion adsorbent.The preparation method of a kind of graphene metal ion adsorbent disclosed by the invention, comprising the following steps: (1) graphene is added in dopamine solution, it is grapheme modified that poly-dopamine is made；(2) it is added to poly-dopamine is grapheme modified in 3- mercaptopropionic acid, graphene metal ion adsorbent is made after separating, washing.Graphene metal ion adsorption material preparation method made from preparation method of the present invention is simple, and water dispersible is good, can quickly, high capacity adsorbing metal ions, therefore metal ion remove and detect in have broad application prospects.
Description
Technical field
The invention belongs to technical field of function materials more particularly to a kind of preparation sides of graphene metal ion adsorbent
Method.
Background technique
Graphene is a kind of New Two Dimensional carbon nanomaterial being made of single layer of carbon atom.Since graphene has specific surface
The features such as product is high, and electric conductivity is strong, mechanical performance is high, thermal conductivity is high nanoelectronics, energy storage and conversion, chemistry and
The fields such as biosensor, composite material and biotechnology show application value, the extensive concern by scientist.Meanwhile
Graphene has the features such as high-specific surface area, chemical stability be good, this makes grapheme material be expected to become in processing water pollution
Fabulous adsorbent material.However, the hydrophobicity of graphene itself and easy aggregation limit its application in water process, therefore
The composite material for developing hydrophily, biocompatibility, is the research direction of novel graphene adsorbent material.
Dopamine (DA) can under alkaline aerobic conditions autohemagglutination formed poly-dopamine (pDA), pDA contain on surface easily by
The catechol group of oxidation not only can effectively enhance the hydrophilicity of graphene, and the catechol group in its structure
Secondary response can occur by Schiff reaction or Michael addition reaction and-NH2 and-SH group, generating has well
Biocompatibility and the composite material for being easy to derivatization.Tri-thiol propionic acid is due to that can occur secondary response with pDA containing-SH and draw
Enter metal complexing groups-COOH, and then realizes the absorption to metal ion.Therefore, by graphene, compound and derivatization is obtained with pDA
To composite material be expected to become good adsorbent.
Summary of the invention
In order to overcome defect present in background technique, the technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of graphene metal ion adsorbent, it is characterised in that the steps include:
(1), graphene is added in dopamine solution, it is grapheme modified that poly-dopamine is made；
(2), it is added to poly-dopamine is grapheme modified in 3- mercaptopropionic acid, graphene metal is made after separating, washing
Ion adsorbent.
The preferred dopamine solution concentration is 0.1~5mg/mL.
The preferred dopamine solution is made by the phosphate buffer that dopamine is dissolved in 0.02~0.2mol/L, and phosphoric acid is slow
PH > 7.5 of fliud flushing.
The action time of the preferred graphene and dopamine solution is 0.5~2h.
Under weak basic condition, the specific reactional equation that dopamine gathers and generate poly-dopamine (pDA) is as follows:
The poly-dopamine (pDA) and graphene by π-π act on direct combination, and that poly-dopamine is prepared is grapheme modified.
The concentration of the preferred 3- mercaptopropionic acid is 5 ~ 25 mmol/L.
The preferred 3- mercaptopropionic acid and the grapheme modified reaction medium of dopamine are the alkaline medium of pH > 8.0.
The preferred 3- mercaptopropionic acid and dopamine grapheme modified reaction time are 1-12h.
The poly-dopamine (pDA) can react with the molecule generation Schiff containing sulfydryl (- SH) or Michael addition
Reaction.By sulfydryl (- SH) and the poly-dopamine (pDA) secondary response occurs for 3- mercaptopropionic acid.Since 3- mercaptopropionic acid has
There is significant metallic ion coordination ability, therefore the grapheme material being prepared can be metal ion with adsorbing metal ions
Adsorbent.
The present invention is based on the grapheme materials with high-specific surface area, using poly-dopamine as bridging agent, are acted on by π-π
It is compound with graphene, the hydrophilicity of graphene is enhanced, and further introduce 3- mercaptopropionic acid and adsorption of metal ions is made
Material.The graphene metal ion adsorbent, specific surface area is high, and water dispersible is good, and adsorption of metal ions performance is high, in metal
The fields such as ion remaval, detection have potential application, can be used for adsorbing heavy metal ion.
Compared with the existing technology, the invention has the benefit that
(1) graphene adsorbent prepared by the present invention, preparation method are simple.
(2) graphene adsorbent prepared by the present invention has good water dispersible, does not reunite in salt-containing solution.
(3) graphene adsorbent material prepared by the present invention has excellent adsorption of metal ions performance, and adsorption capacity is high, inhales
Attached rate is fast.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is photo of the graphene in the NaCl and phosphate buffer solution (PBS) of 0.1M in the embodiment of the present invention 1；
Fig. 2 is photo of the graphene adsorbent in the NaCl and phosphate buffer solution (PBS) of 0.1M in the embodiment of the present invention 1；
Fig. 3 is photo of the graphene adsorbent in pH3-13 solution in the embodiment of the present invention 1；
Fig. 4 is in the embodiment of the present invention 1, and graphene adsorbent adsorbs the kinetic curve of copper ion；
Fig. 5 is in the embodiment of the present invention 1, and graphene adsorbent adsorbs the adsorption isotherm of copper ion.
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.Attached drawing is simplified schematic diagram, only with signal side
Formula illustrates basic structure of the invention, therefore it only shows the composition relevant to the invention.
A kind of specific embodiment one, preparation method of graphene metal ion adsorbent, the steps include:
(1) graphene is added in dopamine solution, it is grapheme modified that poly-dopamine is made.
(2) it is added to poly-dopamine is grapheme modified in 3- mercaptopropionic acid, graphene is made after separating, washing
Metal ion adsorbent.
The dopamine solution concentration is 0.5mg/mL, and dopamine solution is dissolved in the phosphoric acid buffer of 0.1mol/L by dopamine
Liquid is made, and the pH of phosphate buffer is 8.0.The action time of graphene and dopamine solution is 2h.The 3- mercaptopropionic acid
Concentration is 20 mmol/L, and reaction medium is the alkaline medium of pH 8.5, reaction time 6h.
Then, the dispersibility to graphene in saline solns, and the graphene adsorbent prepared through step (1) ~ (2) exist
Dispersibility in saline solns, the dispersibility in different pH solution, adsorb the kinetic curve of copper ion, adsorption isotherm into
Row test, obtained Measurement results are as shown in Fig. 1 ~ 5.
Fig. 1 show photo of the graphene in the NaCl and phosphate buffer solution (PBS) of 0.1M.As can be seen that working as stone
When NaCl and PBS of 0.1M is added in black alkene, graphene can reunite, and can not disperse.This prove graphene, hydrophilicity compared with
Difference, dispersibility is poor in saline solns.Fig. 2 is graphene adsorbent in the NaCl and phosphate buffer solution (PBS) of 0.1M
Photo.As shown, graphene adsorbent will not occur when the NaCl and PBS solution of 0.1M is added in graphene adsorbent
Reunite.This is mainly after DA autohemagglutination under alkaline aerobic conditions is pDA, and it is hydrophilic that pDA contains on surface a large amount of catechol etc.
Property group.Graphene is combined with pDA by π-π, and pDA effectively performs the derivatization graphene surface, introduces hydrophilic radical,
The hydrophilicity of graphene is enhanced, water dispersion ability is improved.The mercaptopropionic acid being further introduced into also contains hydrophilic radical,
Therefore graphene adsorbent has good dispersibility in salt-containing solution.
Fig. 3 is photo of the graphene adsorbent in pH3-13 solution.When the pH of graphene adsorbent solution is adjusted to
When 3.0-13.0, graphene adsorbent is not reunited.This further prove pDA and 3- mercaptopropionic acid to graphene surface into
Row derivatization introduces hydrophilic radical, effectively enhances the hydrophilicity of graphene adsorbent, improve water dispersion ability.
By taking copper ion as an example, the performance of graphene adsorbent absorption copper ion is had studied.Fig. 4 is the absorption of graphene adsorbent
The kinetic curve of copper ion.The adsorption time of investigation is respectively 5 min, 10 min, 15 min, 30 min, 60 min, 90
min.As can be seen from the figure in 30 min composite material to Cu2+Adsorbance steeply rises, and then adsorbance gradually tends to flat
Weighing apparatus, therefore saturated adsorption time is 30 min.Illustrate that graphene adsorbent can be with quick adsorption copper ion.Fig. 5 is graphene suction
The adsorption isotherm of attached dose of absorption copper ion.It can be seen from the figure that with Cu2+Concentration gradually increases, and adsorbance steeply rises
It tends to balance later.Adsorption capacity is that every gram of graphene adsorbent adsorbs 1300mg copper ion.
A kind of specific embodiment two, preparation method of graphene metal ion adsorbent, the steps include:
(1) graphene is added in dopamine solution, it is grapheme modified that poly-dopamine is made.
(2) it is added to poly-dopamine is grapheme modified in 3- mercaptopropionic acid, graphene is made after separating, washing
Metal ion adsorbent.
The dopamine solution concentration is 0.8mg/mL, and dopamine solution is delayed by the phosphoric acid that dopamine is dissolved in 0.15mol/L
Fliud flushing is made, and the pH of phosphate buffer is 8.5.The action time of graphene and dopamine solution is 1h.The 3- mercaptopropionic acid
Concentration be 15 mmol/L, reaction medium be pH 8.0 alkaline medium, reaction time 4h.
It proves after tested, graphene adsorbent prepared by embodiment 2 equally has good water dispersible, quick, Gao Rong
The adsorption of cupper ions of amount.
The present invention devises a kind of preparation method of graphene metal ion adsorbent, the graphene metal ion adsorbent
Have the beneficial effect that
(1) graphene adsorbent prepared by the present invention, preparation method are simple.
(2) graphene adsorbent prepared by the present invention has good water dispersible, does not reunite in salt-containing solution.
(3) graphene adsorbent material prepared by the present invention has excellent adsorption of metal ions performance, and adsorption capacity is high, inhales
Attached rate is fast.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (7)
1. a kind of preparation method of graphene metal ion adsorbent, it is characterised in that the steps include:
(1), graphene is added in dopamine solution, it is grapheme modified that poly-dopamine is made；
(2), it is added to poly-dopamine is grapheme modified in 3- mercaptopropionic acid, graphene metal is made after separating, washing
Ion adsorbent.
2. a kind of preparation method of graphene metal ion adsorbent according to claim 1, which is characterized in that described more
Bar amine aqueous solution concentration is 0.1~5mg/mL.
3. a kind of preparation method of graphene metal ion adsorbent according to claim 1, which is characterized in that described more
Bar amine aqueous solution is made by the phosphate buffer that dopamine is dissolved in 0.02~0.2mol/L, pH > 7.5 of phosphate buffer.
4. a kind of preparation method of graphene metal ion adsorbent according to claim 1, which is characterized in that the stone
The action time of black alkene and dopamine solution is 0.5~2h.
5. a kind of preparation method of graphene metal ion adsorbent according to claim 1, which is characterized in that the 3-
The concentration of mercaptopropionic acid is 5 ~ 25 mmol/L.
6. a kind of preparation method of graphene metal ion adsorbent according to claim 1, which is characterized in that the 3-
Mercaptopropionic acid and the grapheme modified reaction medium of dopamine are the alkaline medium of pH > 8.0.
7. a kind of preparation method of graphene metal ion adsorbent according to claim 1, which is characterized in that the 3-
Mercaptopropionic acid and dopamine grapheme modified reaction time are 1-12h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110801818A (en) * | 2019-10-25 | 2020-02-18 | 南昌大学 | Composite functional material for removing radioactive iodine and application thereof |
| CN111534243A (en) * | 2020-05-08 | 2020-08-14 | 安徽格林开思茂光电科技股份有限公司 | Carbon-coated aluminum foil conductive adhesive tape for lithium battery and preparation method thereof |
| CN112624096A (en) * | 2020-12-23 | 2021-04-09 | 西安交通大学 | Graphene surface dispersibility modification method |
| CN113390816A (en) * | 2021-06-16 | 2021-09-14 | 西北大学 | Method for detecting heavy metal ions of polydopamine-graphene oxide coated fiber bragg grating |
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| CN104399090A (en) * | 2014-11-12 | 2015-03-11 | 深圳先进技术研究院 | Poly dopamine-modified reduced graphene oxide and preparation method and application thereof |
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| CN104399090A (en) * | 2014-11-12 | 2015-03-11 | 深圳先进技术研究院 | Poly dopamine-modified reduced graphene oxide and preparation method and application thereof |
| CN105254916A (en) * | 2015-09-30 | 2016-01-20 | 西南交通大学 | Preparation method for oxidized graphene-poly-dopamine composite aerogel |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110801818A (en) * | 2019-10-25 | 2020-02-18 | 南昌大学 | Composite functional material for removing radioactive iodine and application thereof |
| CN111534243A (en) * | 2020-05-08 | 2020-08-14 | 安徽格林开思茂光电科技股份有限公司 | Carbon-coated aluminum foil conductive adhesive tape for lithium battery and preparation method thereof |
| CN112624096A (en) * | 2020-12-23 | 2021-04-09 | 西安交通大学 | Graphene surface dispersibility modification method |
| CN113390816A (en) * | 2021-06-16 | 2021-09-14 | 西北大学 | Method for detecting heavy metal ions of polydopamine-graphene oxide coated fiber bragg grating |
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Application publication date: 20190430 |