CN108236919A - A kind of graphene oxide of surface modification and its application in pharmaceutical wastewater processing - Google Patents
A kind of graphene oxide of surface modification and its application in pharmaceutical wastewater processing Download PDFInfo
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- CN108236919A CN108236919A CN201611212330.2A CN201611212330A CN108236919A CN 108236919 A CN108236919 A CN 108236919A CN 201611212330 A CN201611212330 A CN 201611212330A CN 108236919 A CN108236919 A CN 108236919A
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- graphene oxide
- surface modification
- mixed solution
- ethylene glycol
- acetic acid
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
- C02F2103/026—Treating water for medical or cosmetic purposes
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- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Graphene oxide and its application in pharmaceutical wastewater processing, the graphene oxide of surface modification the invention discloses a kind of surface modification are prepared by the following method：It adds graphene oxide into the mixed solution of ethylene glycol and acetone, ultrasonic disperse, it is uniform to add in nanometer iron chloride ultrasonic disperse, sodium acetate is added to above-mentioned solution again to be vigorously stirred, then the chitosan for being dissolved in acetic acid aqueous solution is added in, the mixed solution of formation is put into hydrothermal reaction kettle and carries out hydro-thermal reaction after stirring evenly, washed, be dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.The graphene oxide of surface modification provided by the invention can be used for adsorbing the sulfa drugs in pharmaceutical wastewater.
Description
Technical field
The invention belongs to pollution control fields, and in particular to the graphene oxide of a kind of surface modification and its in pharmaceutical wastewater
Application in processing.
Background technology
Sulfa drugs is using the artificial synthesized antibacterials of earliest one kind, belongs to extensive pedigree antibiotic, because it is anti-
The advantages that bacterium spectrum is wide, curative effect is strong, convenient and safe is widely used in human body and animal, and sulfanilamide (SN) antibiotic is taken by human or animal
Afterwards, only 20%-40% can be absorbed and play drug effect, remaining most of drug is in 1-2d with parent or metabolite form with row
It lets out object to be expelled directly out, the excreta containing sulfa drugs is entered in natural environment or sewage treatment plant.Since sulfamido exists
Removal efficiency is limited in sewage treatment plant, can not remove completely, and the antibiotic without removal is finally diffused into surface water, underground
Water or deposit, finally damage to human health and Environment-Ecosystem.How it effectively to be removed into from environment
For the research topic for being badly in need of solving, the removal for sulphadiazine, at present other than biochemical process and advanced oxidation processes, non-demolition
The absorption method of property is due at low cost, easy to operate and do not generate high toxicity catabolite and favored.
Graphene oxide, as the new carbon of the two-dimensional structure with monoatomic layer thickness, since it is with huge
Specific surface area, the heteroaryl structure of graphene oxide is also beneficial to generate phase interaction to hydrophobic class substance by the effect of π-π stackings
With;Therefore, numerous studies carry out the absorption property of graphene oxide or graphene oxide based composites in recent years
Research.
Invention content
A kind of graphene oxide the object of the present invention is to provide surface modification and its application in pharmaceutical wastewater processing.
Above-mentioned purpose is achieved by the following technical solution：
A kind of graphene oxide of surface modification, is prepared by the following method：Add graphene oxide into ethylene glycol and third
In the mixed solution of ketone, ultrasonic disperse, addition nanometer iron chloride ultrasonic disperse is uniform, then sodium acetate is added to above-mentioned solution play
Strong stirring, then adds in the chitosan for being dissolved in acetic acid aqueous solution, and the mixed solution of formation is put into hydro-thermal after stirring evenly
Reaction kettle carries out hydro-thermal reaction, is washed, is dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.
Preferably, the volume ratio of the ethylene glycol and acetone is 2-3:1.
Preferably, the mass ratio of graphene oxide quality and ethylene glycol acetone mixed solution is 1:7-9.
Preferably, nanometer chlorination weight of iron and the mass ratio of ethylene glycol acetone mixed solution are 1:12-14.
Preferably, the mass ratio of sodium acetate quality and ethylene glycol acetone mixed solution is 1:65-85.
Preferably, the mass fraction of acetic acid aqueous solution is 1-3%, and mass concentration of the chitosan in acetic acid aqueous solution is 25-
35%。
Preferably, hydrothermal temperature is 180-240 DEG C, and the hydro-thermal reaction time is 1-3 hours.
The application of the graphene oxide of above-mentioned surface modification sulfonamide in pharmaceutical wastewater is adsorbed.
Beneficial effects of the present invention：
The graphene oxide of surface modification provided by the invention can be used for adsorbing the sulfa drugs in pharmaceutical wastewater.
Specific embodiment
Intend specifically introducing the technical solution of the invention below by specific embodiment.
Embodiment 1：
A kind of graphene oxide of surface modification, is prepared by the following method：Add graphene oxide into ethylene glycol and third
In the mixed solution of ketone, ultrasonic disperse, addition nanometer iron chloride ultrasonic disperse is uniform, then sodium acetate is added to above-mentioned solution play
Strong stirring, then adds in the chitosan for being dissolved in acetic acid aqueous solution, and the mixed solution of formation is put into hydro-thermal after stirring evenly
Reaction kettle carries out hydro-thermal reaction, is washed, is dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.
Wherein, the volume ratio of the ethylene glycol and acetone is 2.5:1；Graphene oxide quality and the mixing of ethylene glycol acetone are molten
The mass ratio of liquid is 1:8；Nanometer chlorination weight of iron and the mass ratio of ethylene glycol acetone mixed solution are 1:13.
Wherein, the mass ratio of sodium acetate quality and ethylene glycol acetone mixed solution is 1:75.
Wherein, the mass fraction of acetic acid aqueous solution is 2%, and mass concentration of the chitosan in acetic acid aqueous solution is 30%.
Wherein, hydrothermal temperature is 210 DEG C, and the hydro-thermal reaction time is 2 hours.
Embodiment 2：
A kind of graphene oxide of surface modification, is prepared by the following method：Add graphene oxide into ethylene glycol and third
In the mixed solution of ketone, ultrasonic disperse, addition nanometer iron chloride ultrasonic disperse is uniform, then sodium acetate is added to above-mentioned solution play
Strong stirring, then adds in the chitosan for being dissolved in acetic acid aqueous solution, and the mixed solution of formation is put into hydro-thermal after stirring evenly
Reaction kettle carries out hydro-thermal reaction, is washed, is dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.
Wherein, the volume ratio of the ethylene glycol and acetone is 2:1；Graphene oxide quality and ethylene glycol acetone mixed solution
Mass ratio be 1:7；Nanometer chlorination weight of iron and the mass ratio of ethylene glycol acetone mixed solution are 1:12.
Wherein, the mass ratio of sodium acetate quality and ethylene glycol acetone mixed solution is 1:65.
Wherein, the mass fraction of acetic acid aqueous solution is 1%, and mass concentration of the chitosan in acetic acid aqueous solution is 25%.
Wherein, hydrothermal temperature is 180 DEG C, and the hydro-thermal reaction time is 3 hours.
Embodiment 3：
A kind of graphene oxide of surface modification, is prepared by the following method：Add graphene oxide into ethylene glycol and third
In the mixed solution of ketone, ultrasonic disperse, addition nanometer iron chloride ultrasonic disperse is uniform, then sodium acetate is added to above-mentioned solution play
Strong stirring, then adds in the chitosan for being dissolved in acetic acid aqueous solution, and the mixed solution of formation is put into hydro-thermal after stirring evenly
Reaction kettle carries out hydro-thermal reaction, is washed, is dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.
Wherein, the volume ratio of the ethylene glycol and acetone is 3:1；Graphene oxide quality and ethylene glycol acetone mixed solution
Mass ratio be 1:9；Nanometer chlorination weight of iron and the mass ratio of ethylene glycol acetone mixed solution are 1:14.
Wherein, the mass ratio of sodium acetate quality and ethylene glycol acetone mixed solution is 1:85.
Wherein, the mass fraction of acetic acid aqueous solution is 3%, and mass concentration of the chitosan in acetic acid aqueous solution is 35%.
Wherein, hydrothermal temperature is 240 DEG C, and the hydro-thermal reaction time is 1 hour.
Embodiment 4：
A kind of graphene oxide of surface modification, is prepared by the following method：Add graphene oxide into ethylene glycol and third
In the mixed solution of ketone, ultrasonic disperse, addition nanometer iron chloride ultrasonic disperse is uniform, then sodium acetate is added to above-mentioned solution play
Strong stirring, then adds in the chitosan for being dissolved in acetic acid aqueous solution, and the mixed solution of formation is put into hydro-thermal after stirring evenly
Reaction kettle carries out hydro-thermal reaction, is washed, is dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.
Wherein, the volume ratio of the ethylene glycol and acetone is 2.5:1；Graphene oxide quality and the mixing of ethylene glycol acetone are molten
The mass ratio of liquid is 1:8；Nanometer chlorination weight of iron and the mass ratio of ethylene glycol acetone mixed solution are 1:13.
Wherein, the mass ratio of sodium acetate quality and ethylene glycol acetone mixed solution is 1:70.
Wherein, the mass fraction of acetic acid aqueous solution is 2%, and mass concentration of the chitosan in acetic acid aqueous solution is 30%.
Wherein, hydrothermal temperature is 210 DEG C, and the hydro-thermal reaction time is 2 hours.
Embodiment 5：
A kind of graphene oxide of surface modification, is prepared by the following method：Add graphene oxide into ethylene glycol and third
In the mixed solution of ketone, ultrasonic disperse, addition nanometer iron chloride ultrasonic disperse is uniform, then sodium acetate is added to above-mentioned solution play
Strong stirring, then adds in the chitosan for being dissolved in acetic acid aqueous solution, and the mixed solution of formation is put into hydro-thermal after stirring evenly
Reaction kettle carries out hydro-thermal reaction, is washed, is dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.
Wherein, the volume ratio of the ethylene glycol and acetone is 2.5:1；Graphene oxide quality and the mixing of ethylene glycol acetone are molten
The mass ratio of liquid is 1:8；Nanometer chlorination weight of iron and the mass ratio of ethylene glycol acetone mixed solution are 1:13.
Wherein, the mass ratio of sodium acetate quality and ethylene glycol acetone mixed solution is 1:80.
Wherein, the mass fraction of acetic acid aqueous solution is 2%, and mass concentration of the chitosan in acetic acid aqueous solution is 30%.
Wherein, hydrothermal temperature is 210 DEG C, and the hydro-thermal reaction time is 2 hours.
Embodiment 6：
A kind of graphene oxide of surface modification, is prepared by the following method：Add graphene oxide into ethylene glycol and third
In the mixed solution of ketone, ultrasonic disperse, addition nanometer iron chloride ultrasonic disperse is uniform, then sodium acetate is added to above-mentioned solution play
Strong stirring, then adds in the chitosan for being dissolved in acetic acid aqueous solution, and the mixed solution of formation is put into hydro-thermal after stirring evenly
Reaction kettle carries out hydro-thermal reaction, is washed, is dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.
Wherein, the volume ratio of the ethylene glycol and acetone is 2.5:1；Graphene oxide quality and the mixing of ethylene glycol acetone are molten
The mass ratio of liquid is 1:8；Nanometer chlorination weight of iron and the mass ratio of ethylene glycol acetone mixed solution are 1:13.
Wherein, the mass ratio of sodium acetate quality and ethylene glycol acetone mixed solution is 1:75.
Wherein, the mass fraction of acetic acid aqueous solution is 2%, and mass concentration of the chitosan in acetic acid aqueous solution is 30%.
Wherein, hydrothermal temperature is 200 DEG C, and the hydro-thermal reaction time is 2 hours.
Embodiment 7：
A kind of graphene oxide of surface modification, is prepared by the following method：Add graphene oxide into ethylene glycol and third
In the mixed solution of ketone, ultrasonic disperse, addition nanometer iron chloride ultrasonic disperse is uniform, then sodium acetate is added to above-mentioned solution play
Strong stirring, then adds in the chitosan for being dissolved in acetic acid aqueous solution, and the mixed solution of formation is put into hydro-thermal after stirring evenly
Reaction kettle carries out hydro-thermal reaction, is washed, is dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.
Wherein, the volume ratio of the ethylene glycol and acetone is 2.5:1；Graphene oxide quality and the mixing of ethylene glycol acetone are molten
The mass ratio of liquid is 1:8；Nanometer chlorination weight of iron and the mass ratio of ethylene glycol acetone mixed solution are 1:13.
Wherein, the mass ratio of sodium acetate quality and ethylene glycol acetone mixed solution is 1:75.
Wherein, the mass fraction of acetic acid aqueous solution is 2%, and mass concentration of the chitosan in acetic acid aqueous solution is 30%.
Wherein, hydrothermal temperature is 220 DEG C, and the hydro-thermal reaction time is 2 hours.
The graphene oxide of surface modification provided by the invention can be used for adsorbing the sulfa drugs in pharmaceutical wastewater.
The effect of above-mentioned specific embodiment indicates that the essentiality content of the invention, but do not limit this hair with this
The protection domain of bright creation.Simply modification or equivalent replacement are carried out to the technical solution of the invention, without departing from this hair
It is bright to create the essence of technical solution, thus necessarily fall into the protection domain of the invention.
Claims (8)
1. a kind of graphene oxide of surface modification, which is characterized in that be prepared by the following method：It adds graphene oxide into
Into the mixed solution of ethylene glycol and acetone, ultrasonic disperse, addition nanometer iron chloride ultrasonic disperse is uniform, then sodium acetate is added in
It is vigorously stirred to above-mentioned solution, then adds in the chitosan for being dissolved in acetic acid aqueous solution, the mixed solution stirring of formation is equal
Hydrothermal reaction kettle is put into after even and carries out hydro-thermal reaction, is washed, is dried in vacuo with ethyl alcohol and deionized water after being cooled to room temperature to obtain the final product.
2. the graphene oxide of surface modification according to claim 1, it is characterised in that：The body of the ethylene glycol and acetone
Product is than being 2-3:1.
3. the graphene oxide of surface modification according to claim 1, it is characterised in that：Graphene oxide quality and second two
The mass ratio of alcohol acetone mixed solution is 1:7-9.
4. the graphene oxide of surface modification according to claim 1, it is characterised in that：Nanometer chlorination weight of iron and second two
The mass ratio of alcohol acetone mixed solution is 1:12-14.
5. the graphene oxide of surface modification according to claim 1, it is characterised in that：Sodium acetate quality and ethylene glycol third
The mass ratio of ketone mixed solution is 1:65-85.
6. the graphene oxide of surface modification according to claim 1, it is characterised in that：The mass fraction of acetic acid aqueous solution
For 1-3%, mass concentration of the chitosan in acetic acid aqueous solution is 25-35%.
7. the graphene oxide of surface modification according to claim 1, it is characterised in that：Hydrothermal temperature is 180-
240 DEG C, the hydro-thermal reaction time is 1-3 hours.
8. the application of graphene oxide sulfonamide in pharmaceutical wastewater is adsorbed of any surface modifications of claim 1-7.
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| CN201611212330.2A CN108236919A (en) | 2016-12-27 | 2016-12-27 | A kind of graphene oxide of surface modification and its application in pharmaceutical wastewater processing |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824130A (en) * | 2017-02-22 | 2017-06-13 | 李峰 | A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil |
| CN110280224A (en) * | 2019-08-08 | 2019-09-27 | 西南科技大学 | The preparation method and application of functionalization graphene base aeroge |
| CN114682217A (en) * | 2022-04-07 | 2022-07-01 | 华北电力大学 | Metal monatomic doped biomass carbon adsorption material, preparation method and application |
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| CN103693639A (en) * | 2013-12-13 | 2014-04-02 | 天津工业大学 | Preparation method of iron/manganese oxide doped graphene composite material |
| CN104096536A (en) * | 2013-04-01 | 2014-10-15 | 同济大学 | Preparation of magnetic reduced graphene oxide composite material and method for removing quinolone antibiotics from water by the same |
| CN105056897A (en) * | 2015-07-16 | 2015-11-18 | 湖南大学 | Graphene oxide modified biochar composite as well as preparation method and application thereof |
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2016
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Patent Citations (4)
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| CN101417822A (en) * | 2008-11-24 | 2009-04-29 | 中国科学院长春应用化学研究所 | Method for preparing super paramagnetic mesoporous ferriferrous oxide nano particle |
| CN104096536A (en) * | 2013-04-01 | 2014-10-15 | 同济大学 | Preparation of magnetic reduced graphene oxide composite material and method for removing quinolone antibiotics from water by the same |
| CN103693639A (en) * | 2013-12-13 | 2014-04-02 | 天津工业大学 | Preparation method of iron/manganese oxide doped graphene composite material |
| CN105056897A (en) * | 2015-07-16 | 2015-11-18 | 湖南大学 | Graphene oxide modified biochar composite as well as preparation method and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824130A (en) * | 2017-02-22 | 2017-06-13 | 李峰 | A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil |
| CN110280224A (en) * | 2019-08-08 | 2019-09-27 | 西南科技大学 | The preparation method and application of functionalization graphene base aeroge |
| CN114682217A (en) * | 2022-04-07 | 2022-07-01 | 华北电力大学 | Metal monatomic doped biomass carbon adsorption material, preparation method and application |
| CN114682217B (en) * | 2022-04-07 | 2023-10-27 | 华北电力大学 | Metal monoatomic doped biomass charcoal adsorption material, preparation method and application |
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