CN105749876B - A kind of preparation method of chitosan-modified graphene oxide quantum dot sorbing material - Google Patents
A kind of preparation method of chitosan-modified graphene oxide quantum dot sorbing material Download PDFInfo
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- CN105749876B CN105749876B CN201610260866.5A CN201610260866A CN105749876B CN 105749876 B CN105749876 B CN 105749876B CN 201610260866 A CN201610260866 A CN 201610260866A CN 105749876 B CN105749876 B CN 105749876B
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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
- 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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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention discloses a kind of preparation methods of chitosan-modified graphene oxide quantum dot sorbing material, it is that crosslinking agent and graphene oxide quantum dot are added in the acetic acid solution of chitosan, magnetic agitation mixes under certain pH, certain temperature, it is lyophilized after deionized water and ethyl alcohol clean repeatedly again, obtains chitosan-modified graphene oxide quantum dot sorbing material.Preparation method of the present invention is easy to operate, raw material is easy to get, mild condition, and gained sorbing material has good adsorption properties, can be used for the fields such as water pollution processing, biological medicine.
Description
Technical field
The invention belongs to graphene oxide quantum dot technical field of composite materials, and in particular to a kind of chitosan-modified oxygen
The preparation method of graphite alkene quantum dot sorbing material.
Background technology
Graphene oxide（GO）It is product of the powdered graphite after chemical stripping, is a kind of emerging in recent years two-dimentional carbon materials
Material has single atomic layer, and its surface has more hydroxyl, carboxyl and epoxy-functional；Meanwhile GO itself also has
There are preferable chemical stability, hydrophily, antifouling property, biocompatibility and mechanical performance, in ultracapacitor, transparent
Electrode, sea water desalination, light emitting diode, sensor, hydrogen storage, solar cell, catalyst carrier, composite material, biological support
The fields such as material, bio-imaging, drug conveying, weaving, printing and dyeing are widely used.Graphene oxide quantum dot is as oxidation stone
The derived material of black alkene is the nano material of quasi-zero dimension.As a kind of novel quantum dot, graphene oxide quantum dot is notable because of it
Quantum confinement and edge effect, a large amount of novel physics, chemical property are showed, including hypotoxicity, dissolubility, chemistry
Stability, photostability etc. make it have prodigious application potential in bio-imaging, medicine, material etc..
Chitosan（Chitosan）It is chitin（chitin）The product after the acetyl group of part is sloughed, is a kind of common day
The copolymer of right macromolecule and a kind of aminoglucose and N-acetyl-glucosamine.In chitosan molecule containing a large amount of amino and
Hydroxyl, therefore its chemical property is very active, can carry out a variety of chemistry such as acylation, carboxylated, etherificate, alkylation, esterification and halogenation
Reaction, can prepare a variety of chitosan derivatives, to assign its more specific function accordingly.Chitosan has good life
Object compatibility, degradability and antibacterial, hemostasis and promote the functions such as wound healing, and with good film forming, adsorptivity,
Gas permeability and permeability.These excellent performances make it in water process and papermaking, food fresh keeping membrane, hard tissue repair, medicament slow release
Numerous aspects such as material are detected with biological diagnosis to be widely used.
Invention content
The purpose of the present invention is to provide a kind of preparation sides of chitosan-modified graphene oxide quantum dot sorbing material
Method, the method for the present invention process is simple, mild condition, easy to operate, and gained sorbing material can be used for water pollution processing, biological medicine etc.
Field.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of chitosan-modified graphene oxide quantum dot sorbing material, includes the following steps：
1）0.5-2.0g chitosans are dissolved in the acetic acid solution that 100mL mass fractions are 4%, 100W is ultrasonically treated
30min；
2）In step 1）Chitosan acetic acid solution in 10-20mL crosslinking agents glutaraldehyde and 0.4-0.6g graphite oxides is added
Alkene quantum dot, room temperature magnetic agitation handle 60-90min；
3）Set-up procedure 2）The pH value of mixed solution is 9-10, then continues magnetic agitation 1h at 60-80 DEG C；
4）Gained mixture water, ethyl alcohol are washed till neutrality repeatedly, are lyophilized to get chitosan-modified graphene oxide quantum
Point sorbing material.
The beneficial effects of the present invention are：
（1）Raw material sources of the present invention are extensive, are easy to get, are of low cost, and preparation process is simple, mild condition.
（2）The present invention uses chitosan-modified graphene oxide quantum dot, further improves graphene oxide quantum dot
The performances such as biocompatibility, and there is stronger adsorption capacity to heavy metal, organic dyestuff etc..
（3）Chitosan-modified graphene oxide quantum dot quantum confinement effect prepared by the present invention is notable, biology,
The fields such as material have important potential application.
（4）Chitosan-modified graphene oxide quantum dot sorbing material prepared by the present invention has good dispersiveness
Can, it can be used for water pollution processing, biological medicine etc..
Description of the drawings
Fig. 1 is the chitosan-modified graphene oxide quantum dot sorbing material of the preparation of embodiment 1 to organic dyestuff methylene
The Adsorption experimental results figure of base indigo plant.
Specific implementation mode
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
A kind of preparation method of chitosan-modified graphene oxide quantum dot sorbing material, includes the following steps：
1）0.5g chitosans are dissolved in the acetic acid solution that 100mL mass fractions are 4%, 100W is ultrasonically treated 30min；
2）In step 1）Chitosan acetic acid solution in 10mL glutaraldehydes and 0.4g graphene oxide quantum dots, room temperature is added
Magnetic agitation handles 60min；
3）The pH value for adjusting mixed solution is 9, then continues magnetic agitation 1h at 60 DEG C；
4）Gained mixture water, ethyl alcohol are washed till neutrality repeatedly, are lyophilized to get chitosan-modified graphite oxide quantum dot
Alkene sorbing material.
Embodiment 2
A kind of preparation method of chitosan-modified graphene oxide quantum dot sorbing material, includes the following steps：
1）1.0g chitosans are dissolved in the acetic acid solution that 100mL mass fractions are 4%, 100W is ultrasonically treated 30min；
2）In step 1）Chitosan acetic acid solution in 12mL glutaraldehydes and 0.5g graphene oxide quantum dots, room temperature is added
Magnetic agitation handles 70min；
3）The pH value for adjusting mixed solution is 9, then continues magnetic agitation 1h at 65 DEG C；
4）Gained mixture water, ethyl alcohol are washed till neutrality repeatedly, are lyophilized to get chitosan-modified graphene oxide quantum
Point sorbing material.
Embodiment 3
A kind of preparation method of chitosan-modified graphene oxide quantum dot sorbing material, includes the following steps：
1）1.5g chitosans are dissolved in the acetic acid solution that 100mL mass fractions are 4%, 100W is ultrasonically treated 30min；
2）In step 1）Chitosan acetic acid solution in 16mL glutaraldehydes and 0.5g graphene oxide quantum dots, room temperature is added
Magnetic agitation handles 80min；
3）The pH value for adjusting mixed solution is 9, then continues magnetic agitation 1h at 70 DEG C；
4）Gained mixture water, ethyl alcohol are washed till neutrality repeatedly, are lyophilized to get chitosan-modified graphene oxide quantum
Point sorbing material.
Embodiment 4
A kind of preparation method of chitosan-modified graphene oxide quantum dot sorbing material, includes the following steps：
1）2.0g chitosans are dissolved in the acetic acid solution that 100mL mass fractions are 4%, 100W is ultrasonically treated 30min；
2）In step 1）Chitosan acetic acid solution in 20mL glutaraldehydes and 0.6g graphene oxide quantum dots, room temperature is added
Magnetic agitation handles 90min；
3）The pH value for adjusting mixed solution is 10, then continues magnetic agitation 1h at 80 DEG C；
4）Gained mixture water, ethyl alcohol are washed till neutrality repeatedly, are lyophilized to get chitosan-modified graphene oxide quantum
Point sorbing material.
Methylene blue adsorption number is tested：
The ylidene methyl indigo plant solution for standby for preparing 500 mg/L first, then it is diluted to respectively a concentration of 0.5 mg/L,
The serial solution of 1.25 mg/L, 2.5 mg/L, 5 mg/L, 10 mg/L, using ultraviolet specrophotometer in its 670 nm feature
Its absorbance is surveyed under absorbing wavelength, and draws absorbance-concentration standard curve.
5 parts of chitosan-modified graphene oxide quantum dot sorbing material for weighing the preparation of equivalent embodiment 1, is distinguished
It is added in the methylene blue solution of equivalent same concentrations, in 30 DEG C of thermostat water baths that then earthquake speed is 120 rpm
It shakes 1,2,3,4,5 day, after the completion of concussion, sample solution is taken out respectively, measured using ultraviolet specrophotometer sub- after shaking
Then the absorbance of methyl blue solution calculates the concentration of Methylene Blue in Solution according to gained standard curve, and according to methylene
The variation of blue solution concentration calculates adsorption capacity of the chitosan-modified graphene oxide quantum dot sorbing material to methylene blue.
Fig. 1 is adsorption experiment of the chitosan-modified graphene oxide quantum dot sorbing material to organic dyestuff methylene blue
Result figure.It will be seen from figure 1 that chitosan-modified graphene oxide quantum dot sorbing material has preferably methylene blue
Adsorption capacity.With the extension of concussion time, the adsorbance of methylene blue is gradually increased；When it is 5 days to shake the time, inhale
Attached amount reaches 22 mg/g.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (1)
1. a kind of preparation method of chitosan-modified graphene oxide quantum dot sorbing material, it is characterised in that：Including following
Step：
1）It dissolves the chitosan in the acetic acid solution that mass fraction is 4%, 100W is ultrasonically treated 30min；
2）In step 1）Chitosan acetic acid solution in crosslinking agent and graphene oxide quantum dot, the processing of room temperature magnetic agitation is added
60-90min；
3）Set-up procedure 2）After the pH of mixed solution, continue magnetic agitation 1h；
4）Gained mixture water, ethyl alcohol are washed till neutrality repeatedly, up to chitosan-modified graphene oxide quantum dot after freeze-drying
Sorbing material；
The crosslinking agent is glutaraldehyde；
Step 3）The ranging from 9-10 of middle pH value, magnetic agitation temperature are 60-80 DEG C.
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| CN201610260866.5A CN105749876B (en) | 2016-04-26 | 2016-04-26 | A kind of preparation method of chitosan-modified graphene oxide quantum dot sorbing material |
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| CN105749876B true CN105749876B (en) | 2018-07-17 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880880B (en) * | 2017-10-24 | 2020-05-22 | 温州医科大学 | Chitosan Schiff base modified graphene quantum dot and preparation method and application thereof |
| CN109289779B (en) * | 2018-10-16 | 2021-09-14 | 西南石油大学 | Modified adsorbent based on graphene oxide dynamic covalent bond and preparation method thereof |
| CN109607943B (en) * | 2018-12-18 | 2021-09-24 | 曲阜师范大学 | Sewage treatment method for composite treatment of high-phosphorus wastewater and high-ammonia-nitrogen wastewater |
| CN110013833B (en) * | 2019-04-22 | 2021-08-24 | 曲阜师范大学 | Preparation method of MgO/GQD/chitosan oligosaccharide/PVA composite adsorption film |
| CN112916045A (en) * | 2021-01-31 | 2021-06-08 | 胡国强 | Load ZnO-TiO2Preparation method of magnetic graphene oxide/chitosan composite material |
| CN113214828B (en) * | 2021-04-29 | 2023-03-10 | 西安建筑科技大学 | Graphene quantum dot loaded fluorescent adsorption material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103447013A (en) * | 2013-09-23 | 2013-12-18 | 青岛大学 | Method for preparing graphene/chitosan adsorbent and application method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103447013A (en) * | 2013-09-23 | 2013-12-18 | 青岛大学 | Method for preparing graphene/chitosan adsorbent and application method thereof |
Non-Patent Citations (2)
| Title |
|---|
| "Adsorption of graphene oxide/chitosan porous materials for metal ions";Yong Qiang He等;《Chinese Chemical Letters》;20110417;第22卷;第859-862页 * |
| "石墨烯量子点的制备";王娇娇等;《化学进展》;20130131;第25卷(第1期);第87页第1段 * |
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