CN105749876A - Method for preparing graphene oxide quantum dot adsorption material modified through chitosan - Google Patents
Method for preparing graphene oxide quantum dot adsorption material modified through chitosan Download PDFInfo
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- CN105749876A CN105749876A CN201610260866.5A CN201610260866A CN105749876A CN 105749876 A CN105749876 A CN 105749876A CN 201610260866 A CN201610260866 A CN 201610260866A CN 105749876 A CN105749876 A CN 105749876A
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- 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
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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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- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a method for preparing a graphene oxide quantum dot adsorption material modified through chitosan.The method comprises the steps of adding a cross-linking agent and graphene oxide quantum dots to a chitosan acetic acid solution, conducting magnetic stirring and mixing at a certain pH value and a certain temperature, then conducting repeated cleaning with deionized water and ethanol, and then conducting freeze-drying, so that the graphene oxide quantum dot adsorption material modified through chitosan is obtained.The method for preparing the graphene oxide quantum dot adsorption material modified through chitosan is simple in operation, raw materials are easy to obtain, the condition is mild, and the obtained adsorption material has good adsorption performance and can be applied to such fields as water pollution treatment ad biological medicine.
Description
Technical field
The invention belongs to graphene oxide quantum dot technical field of composite materials, the preparation method being specifically related to a kind of chitosan-modified graphene oxide quantum dot adsorbing material.
Background technology
Graphene oxide (GO) is powdered graphite product after chemical stripping, is a kind of Two-dimensional Carbon material emerging in recent years, has a single atomic layer, and its surface has more hydroxyl, carboxyl and epoxy-functional；Simultaneously, GO itself also has good chemical stability, hydrophilic, antifouling property, biocompatibility and mechanical performance, is widely used in fields such as ultracapacitor, transparency electrode, desalinization, light emitting diode, sensor, hydrogen storage, solaode, catalyst carrier, composite, biologic bracket material, bio-imaging, medicine conveying, weaving, printing and dyeing.Graphene oxide quantum dot, as the derived material of graphene oxide, is the nano material of quasi-zero dimension.As a kind of novel quantum dot, graphene oxide quantum dot is because of its significant quantum confinement and edge effect, present a large amount of novel physics, chemical property, including hypotoxicity, dissolubility, chemical stability, light stability etc. so that it is have very big application potential in bio-imaging, medical science, material etc..
Chitosan (Chitosan) is the product after chitin (chitin) sloughs part acetyl group, is a kind of common natural polymer, is also the copolymer of a kind of aminoglucose and N-acetyl-glucosamine.Containing substantial amounts of amino and hydroxyl in chitosan molecule; therefore its chemical property is very active; acidylate, carboxylated, etherificate, the multiple chemical reaction such as alkylation, esterification and halogenation can being carried out, multiple chitosan derivatives can being prepared accordingly, thus giving its more specific function.Chitosan has good biocompatibility, degradability and antibacterial, hemostasis and promotes the functions such as wound healing, and has good film property, adsorptivity, breathability and permeability.These premium properties so that it is be widely used in water processes and papermaking, food fresh keeping membrane, hard tissue repair, medicament slow release and biological diagnosis test material etc. are numerous.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of chitosan-modified graphene oxide quantum dot adsorbing material, the inventive method process is simple, mild condition, easily operate, and gained adsorbing material can be used for the fields such as water pollution process, biological medicine.
For achieving the above object, the present invention adopts the following technical scheme that
The preparation method of a kind of chitosan-modified graphene oxide quantum dot adsorbing material, comprises the following steps:
1) 0.5-2.0g chitosan is dissolved in the acetic acid solution that 100mL mass fraction is 4%, 100W supersound process 30min；
2) adding 10-20mL cross-linking agent glutaraldehyde and 0.4-0.6g graphene oxide quantum dot in the chitosan acetic acid solution of step 1), room temperature magnetic agitation processes 60-90min；
3) set-up procedure 2) pH value of mixed solution is 9-10, then continues magnetic agitation 1h at 60-80 DEG C；
4) gained mixture water, ethanol are washed till neutrality, lyophilizing repeatedly, obtain chitosan-modified graphene oxide quantum dot adsorbing material.
The beneficial effects of the present invention is:
(1) raw material sources of the present invention extensively, be easy to get, with low cost, preparation technology is simple, mild condition.
(2) present invention adopts chitosan-modified graphene oxide quantum dot, the performance such as biocompatibility further increasing graphene oxide quantum dot, and heavy metal, organic dyestuff etc. have stronger absorbability.
(3) the chitosan-modified graphene oxide quantum dot quantum confinement effect prepared by the present invention is notable, has important potential application in fields such as biology, materials.
(4) the chitosan-modified graphene oxide quantum dot adsorbing material prepared by the present invention has good adsorption properties, can be used for the aspects such as water pollution process, biological medicine.
Accompanying drawing explanation
Fig. 1 is the chitosan-modified graphene oxide quantum dot adsorbing material of the embodiment 1 preparation Adsorption experimental results figure to organic dyestuff methylene blue.
Detailed description of the invention
In order to make content of the present invention easily facilitate understanding, below in conjunction with detailed description of the invention, technical solutions according to the invention are described further, but the present invention is not limited only to this.
Embodiment 1
The preparation method of a kind of chitosan-modified graphene oxide quantum dot adsorbing material, comprises the following steps:
1) 0.5g chitosan is dissolved in the acetic acid solution that 100mL mass fraction is 4%, 100W supersound process 30min；
2) adding 10mL glutaraldehyde and 0.4g graphene oxide quantum dot in the chitosan acetic acid solution of step 1), room temperature magnetic agitation processes 60min；
3) pH value adjusting mixed solution is 9, then continues magnetic agitation 1h at 60 DEG C；
4) gained mixture water, ethanol are washed till neutrality, lyophilizing repeatedly, obtain chitosan-modified graphite oxide quantum dot alkene adsorbing material.
Embodiment 2
The preparation method of a kind of chitosan-modified graphene oxide quantum dot adsorbing material, comprises the following steps:
1) 1.0g chitosan is dissolved in the acetic acid solution that 100mL mass fraction is 4%, 100W supersound process 30min；
2) adding 12mL glutaraldehyde and 0.5g graphene oxide quantum dot in the chitosan acetic acid solution of step 1), room temperature magnetic agitation processes 70min；
3) pH value adjusting mixed solution is 9, then continues magnetic agitation 1h at 65 DEG C；
4) gained mixture water, ethanol are washed till neutrality, lyophilizing repeatedly, obtain chitosan-modified graphene oxide quantum dot adsorbing material.
Embodiment 3
The preparation method of a kind of chitosan-modified graphene oxide quantum dot adsorbing material, comprises the following steps:
1) 1.5g chitosan is dissolved in the acetic acid solution that 100mL mass fraction is 4%, 100W supersound process 30min；
2) adding 16mL glutaraldehyde and 0.5g graphene oxide quantum dot in the chitosan acetic acid solution of step 1), room temperature magnetic agitation processes 80min；
3) pH value adjusting mixed solution is 9, then continues magnetic agitation 1h at 70 DEG C；
4) gained mixture water, ethanol are washed till neutrality, lyophilizing repeatedly, obtain chitosan-modified graphene oxide quantum dot adsorbing material.
Embodiment 4
The preparation method of a kind of chitosan-modified graphene oxide quantum dot adsorbing material, comprises the following steps:
1) 2.0g chitosan is dissolved in the acetic acid solution that 100mL mass fraction is 4%, 100W supersound process 30min；
2) adding 20mL glutaraldehyde and 0.6g graphene oxide quantum dot in the chitosan acetic acid solution of step 1), room temperature magnetic agitation processes 90min；
3) pH value adjusting mixed solution is 10, then continues magnetic agitation 1h at 80 DEG C；
4) gained mixture water, ethanol are washed till neutrality, lyophilizing repeatedly, obtain chitosan-modified graphene oxide quantum dot adsorbing material.
Methylene blue adsorption number is tested:
First the ylidene methyl indigo plant solution for standby of 500mg/L is prepared, then it is diluted to respectively the serial solution that concentration is 0.5mg/L, 1.25mg/L, 2.5mg/L, 5mg/L, 10mg/L, utilize ultraviolet spectrophotometer to survey its absorbance under its 670nm characteristic absorption wavelength, and draw absorbance-concentration standard curve.
Weigh the chitosan-modified graphene oxide quantum dot adsorbing material 5 parts of equivalent embodiment 1 preparation, it is added separately in the methylene blue solution of equivalent same concentrations, then earthquake speed be 120rpm 30 DEG C of thermostat water baths in shake 1 respectively, 2, 3, 4, 5 days, after having shaken, sample solution is taken out, the absorbance of methylene blue solution after utilizing ultraviolet spectrophotometer measurement to shake, then the concentration of Methylene Blue in Solution is calculated according to gained standard curve, and according to the change calculations of the methylene blue solution concentration chitosan-modified graphene oxide quantum dot adsorbing material absorbability to methylene blue.
Fig. 1 is the chitosan-modified graphene oxide quantum dot adsorbing material Adsorption experimental results figure to organic dyestuff methylene blue.It will be seen from figure 1 that methylene blue is had good absorbability by chitosan-modified graphene oxide quantum dot adsorbing material.Along with the prolongation of concussion time, the adsorbance of methylene blue is increased by gradually；When the concussion time is 5 days, adsorbance reaches 22mg/g.
The foregoing is only presently preferred embodiments of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to the covering scope of the present invention.
Claims (3)
1. the preparation method of graphene oxide quantum dot adsorbing material one kind chitosan-modified, it is characterised in that: comprise the following steps:
1) dissolve the chitosan in the acetic acid solution that mass fraction is 4%, 100W supersound process 30min；
2) adding cross-linking agent and graphene oxide quantum dot in the chitosan acetic acid solution of step 1), room temperature magnetic agitation processes 60-90min；
3) set-up procedure 2) mixed solution pH after, continue magnetic agitation 1h；
4) gained mixture water, ethanol are washed till neutrality repeatedly, namely obtain chitosan-modified graphene oxide quantum dot adsorbing material after lyophilizing.
2. the preparation method of graphene oxide quantum dot adsorbing material chitosan-modified according to claim 1, it is characterised in that: described cross-linking agent is glutaraldehyde.
3. the preparation method of graphene oxide quantum dot adsorbing material chitosan-modified according to claim 1, it is characterised in that: in step 3) pH value range for 9-10, magnetic agitation temperature is 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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| 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880880A (en) * | 2017-10-24 | 2018-04-06 | 温州医科大学 | Graphene quantum dot that a kind of chitosan schiff-base is modified and preparation method and application |
| CN109289779A (en) * | 2018-10-16 | 2019-02-01 | 西南石油大学 | A kind of modified adsorbent and preparation method thereof based on graphene oxide dynamic covalent bond |
| CN109607943A (en) * | 2018-12-18 | 2019-04-12 | 曲阜师范大学 | A kind of sewage water treatment method of high phosphorus waste water and high ammonia-nitrogen wastewater combined processing |
| CN110013833A (en) * | 2019-04-22 | 2019-07-16 | 曲阜师范大学 | A kind of 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 |
| CN113214828A (en) * | 2021-04-29 | 2021-08-06 | 西安建筑科技大学 | Graphene quantum dot loaded fluorescent adsorption material and preparation method thereof |
Citations (1)
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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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2016
- 2016-04-26 CN CN201610260866.5A patent/CN105749876B/en not_active Expired - Fee Related
Patent Citations (1)
| 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)
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| YONG QIANG HE等: ""Adsorption of graphene oxide/chitosan porous materials for metal ions"", 《CHINESE CHEMICAL LETTERS》 * |
| 王娇娇等: ""石墨烯量子点的制备"", 《化学进展》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880880A (en) * | 2017-10-24 | 2018-04-06 | 温州医科大学 | Graphene quantum dot that a kind of chitosan schiff-base is modified and preparation method and application |
| 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 |
| CN109289779A (en) * | 2018-10-16 | 2019-02-01 | 西南石油大学 | A kind of modified adsorbent and preparation method thereof based on graphene oxide dynamic covalent bond |
| 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 |
| CN109607943A (en) * | 2018-12-18 | 2019-04-12 | 曲阜师范大学 | A kind of sewage water treatment method of high phosphorus waste water and high ammonia-nitrogen wastewater combined processing |
| 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 |
| CN110013833A (en) * | 2019-04-22 | 2019-07-16 | 曲阜师范大学 | A kind of 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 |
| CN113214828A (en) * | 2021-04-29 | 2021-08-06 | 西安建筑科技大学 | Graphene quantum dot loaded fluorescent adsorption material and preparation method thereof |
| 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 |
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