CN110339733A - A kind of graphene oxide/polyaniline composite film and its application - Google Patents
A kind of graphene oxide/polyaniline composite film and its application Download PDFInfo
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- CN110339733A CN110339733A CN201910547558.4A CN201910547558A CN110339733A CN 110339733 A CN110339733 A CN 110339733A CN 201910547558 A CN201910547558 A CN 201910547558A CN 110339733 A CN110339733 A CN 110339733A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/60—Polyamines
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/82—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74 characterised by the presence of specified groups, e.g. introduced by chemical after-treatment
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic 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
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/12—Adsorbents being present on the surface of the membranes or in the pores
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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
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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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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- Organic Chemistry (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to water process and field of membrane material, it discloses a kind of graphene oxide/polyaniline composite film and its application, the graphene oxide/polyaniline composite film is, on matrix prepared by graphene oxide and formed a film, then aniline and ammonium persulfate are dissolved in acid solution respectively, it is sufficiently mixed, graphene oxide membrane is immersed in mixed solution, reacted under condition of ice bath, after graphene oxide film surface grafting polyaniline, it takes out, clean the surface is dried at room temperature for being made.Graphene oxide/polyaniline composite film in the present invention, preparation process is simple, at low cost, and clean-up effect is good.Composite membrane of the invention can be in the application in sewage treatment field, the especially industrial wastewater containing one or more of methylene blue dye, copper, zinc or nickel ion.
Description
Technical field
The invention belongs to water process and field of membrane material, more particularly, to a kind of graphene oxide/polyaniline composite film
And its application.
Background technique
Water resource is material base for the survival of mankind, but as world population increases and industrialized continuous hair
Exhibition, the water resources crisis that the mankind are faced is increasingly severe, and especially China human mortality is numerous, and distribution of water resources is uneven, water shortage day
It is beneficial serious.Further, since China is in Rapid development stage, environmental consciousness is not strong, and every pollutant is unprocessed just direct
Discharge causes the serious pollution of rivers and lakes large area, has directly aggravated the water resources crisis in China.Therefore, how efficiently sharp
The emphasis and hot spot for current research are become with water resource.
A few days ago, for the method for sewage treatment, most widely used is membrane technology, and graphene film utilizes its interlayer
Concern away from the fast and effective purification that can be realized to pollutant by science and industrial circle, but graphene oxide is due to its surface
The hydrophilic interaction of functional group, cause in water interlamellar spacing become larger, the rejection of pollutant is reduced, its height to sewage is unfavorable for
Effect processing.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art, primary and foremost purpose of the present invention is to provide a kind of oxidation stone
Black alkene/polyaniline composite film, the graphene oxide/polyaniline composite film clean-up effect are good.
Another object of the present invention is to provide the preparation methods of above-mentioned graphene oxide/polyaniline composite film.This method
Preparation process is simple, at low cost, environmental-friendly.
A further object of the present invention is to provide the applications of above-mentioned graphene oxide/polyaniline composite film.
The purpose of the present invention is realized by following technical proposals:
A kind of graphene oxide/polyaniline composite film, the graphene oxide/polyaniline composite film is first will on matrix
Graphene oxide membrane, is immersed in the acid solution of aniline and ammonium persulfate instead by graphene oxide preparation film forming under condition of ice bath
It answers, after making graphene oxide film surface grafting polyaniline, takes out, clean the surface is dried at room temperature for being made.
Preferably, the matrix is microfiltration membranes, ultrafiltration membrane, nanofiltration membrane or reverse osmosis membrane.
Preferably, load capacity of the graphene oxide on matrix is 50~1000mg/m2。
Preferably, the method for graphene oxide film forming is spray coating method, rubbing method, filter press technique or suction method.
Preferably, in the acid solution of the aniline and ammonium persulfate aniline or ammonium persulfate mole and acid solution body
Product is than being 0.1mol:(0.5~10) L, the molar ratio of the aniline and ammonium persulfate is 1:(0.5~2).
Preferably, the acid solution is hydrochloric acid, sulfuric acid or perchloric acid；The concentration of the acid solution is 0.5~2mol/
L。
Preferably, the time of the reaction is 3~12h.
Application of the graphene oxide/polyaniline composite film in sewage treatment field.
Preferably, the sewage is the Industry Waste containing one or more of methylene blue dye, copper, zinc or nickel ion
Water.
Compared with prior art, the invention has the following advantages:
1. the present invention provides a kind of graphene oxide/polyaniline composite film for water process, due to graphene oxide table
A large amount of functional groups are contained in face, can be effectively combined together in a manner of covalent bond with polyaniline, its stabilization is made to be attached to oxidation
The surface of graphene film, composite membrane is positively charged in water, has repulsive interaction to heavy metal ion positively charged in water, to band
The pollutant of negative electrical charge has suction-operated, can effectively improve graphene oxide membrane to methylene blue dye and heavy metal ion
(for example, Cu2+、Zn2+Or Ni2+) rejection.
2. preparation process of the present invention is simple, the either synthesis of graphene oxide or polyaniline and the preparation of composite membrane
It is in water-soluble middle progress, no toxic solvent is environmentally protective, and the graphene and polyaniline dosage of every square metre of composite membrane needs
Seldom, production cost and processing cost are reduced.
Detailed description of the invention
Fig. 1 is the film SEM photograph of the resulting graphene being supported on ultrafiltration membrane of embodiment 1.
Fig. 2 is the composite film material SEM photograph that embodiment 1 has been grafted polyaniline.
Specific embodiment
For the present invention is further explained, embodiment is given below to illustrate, in subordinate's example, it is several to provide the present invention
Embodiment and composition, however the invention is not limited to using following manner implementation, those skilled in the art are understanding this hair
Change, replacement, the improvement carried out on the basis of bright to the present invention still belongs to the scope of protection of the present invention.
Embodiment 1
By the graphene oxide graphene oxide solution soluble in water for being configured to 10mg/L, 18.8ml, ultrasonic 30min are taken,
Graphene oxide is prepared to film forming on ultrafiltration membrane by the method for suction filtration, the effective area of ultrafiltration membrane is 12.56cm2, preparation
Load capacity is 150mg/m out2Graphene oxide membrane, after 0.1mol aniline and 0.1mol ammonium persulfate are added to 1L's respectively
It in the perchloric acid of 1mol/L, is sufficiently mixed, under condition of ice bath, graphene oxide membrane is impregnated in mixed solution, condition of ice bath
Lower reaction 6h removes surface impurity, is dried at room temperature for get graphene oxide/polyaniline composite film is arrived.
Gained graphene oxide/polyaniline composite film water flux is 19L/ (m2Hbar), to 0.0025mol/L's
The permeation flux of copper ion is 18L/ (m2Hbar), for rejection up to 93%, the permeation flux to methylene blue is 15L/
(m2Hbar) rejection is 98%.
Fig. 1 is the film SEM photograph of the resulting graphene being supported on ultrafiltration membrane of the present embodiment.Wherein, the left side is porous
Material is ultrafiltration membrane, and the right is graphene oxide membrane in the film of accordion, and graphene oxide membrane is successfully supported on matrix.Fig. 2
The SEM photograph of the composite film material of polyaniline has been grafted for the present embodiment.As can be seen from Figure 2, polyaniline grafted to arrive graphene oxide
On film, polyaniline size and distribution are relatively uniform, and graft effect is good.
Embodiment 2
By the graphene oxide graphene oxide solution soluble in water for being configured to 10mg/L, 37.6ml, ultrasonic 30min are taken,
Graphene oxide is prepared to film forming on ultrafiltration membrane by the method for filters pressing, the effective area of ultrafiltration membrane is 12.56cm2, preparation
Load capacity is 300mg/m out2Graphene oxide membrane, after 0.1mol aniline and 0.1mol ammonium persulfate are added to 1L's respectively
It in the hydrochloric acid of 0.5mol/L, is sufficiently mixed, graphene oxide membrane is impregnated in mixed solution, reacts 3h under condition of ice bath,
It dries at room temperature, removes surface impurity to get graphene oxide/polyaniline composite film is arrived.
Gained graphene oxide/polyaniline composite film water flux is 15L/ (m2Hbar), to 0.0025mol/L's
The permeation flux of copper ion is 15L/ (m2Hbar), for rejection up to 95%, the permeation flux to methylene blue is 11L/
(m2Hbar) rejection is 99%.
Embodiment 3
Graphene oxide is soluble in water, it is configured to the graphene oxide solution of 10mg/L, takes 125.6ml, ultrasound
Graphene oxide is prepared film forming by the method for filters pressing by 30min on ultrafiltration membrane, and the effective area of ultrafiltration membrane is
12.56cm2, preparing load capacity is 1000mg/m2Graphene oxide membrane, after respectively by 0.1mol aniline and 0.1mol over cure
Sour ammonium is added in the perchloric acid of the 1mol/L of 1L, is sufficiently mixed, and graphene oxide membrane is impregnated in mixed solution, ice bath item
9h is reacted under part, is dried at room temperature for, removes surface impurity to get graphene oxide/polyaniline composite film is arrived.
Gained graphene oxide/polyaniline composite film water flux is 10L/ (m2Hbar), to 0.0025mol/L's
The permeation flux of copper ion is 10L/ (m2Hbar), for rejection up to 95%, the permeation flux to methylene blue is 7L/
(m2Hbar) rejection is 99%.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of graphene oxide/polyaniline composite film, which is characterized in that the graphene oxide/polyaniline composite film is first
It on matrix prepared by graphene oxide and is formed a film, graphene oxide membrane is immersed in aniline and ammonium persulfate under condition of ice bath
It reacts, after making graphene oxide film surface grafting polyaniline, takes out, clean the surface is dried at room temperature for being made in acid solution.
2. graphene oxide/polyaniline composite film according to claim 1, which is characterized in that the matrix is micro-filtration
Film, ultrafiltration membrane, nanofiltration membrane or reverse osmosis membrane.
3. graphene oxide/polyaniline composite film according to claim 1, which is characterized in that the graphene oxide
Load capacity on matrix is 50~1000mg/m2。
4. graphene oxide/polyaniline composite film according to claim 1, which is characterized in that the graphene oxide
The method of film forming is spray coating method, rubbing method, filter press technique or suction method.
5. graphene oxide/polyaniline composite film according to claim 1, which is characterized in that the aniline and over cure
In the acid solution of sour ammonium aniline or ammonium persulfate mole and the volume ratio of acid solution be 0.1mol:(0.5~10) L, it is described
The molar ratio of aniline and ammonium persulfate is 1:(0.5~2).
6. graphene oxide/polyaniline composite film according to claim 5, which is characterized in that the acid solution is salt
Acid, sulfuric acid or perchloric acid；The concentration of the acid solution is 0.5~2mol/L.
7. graphene oxide/polyaniline composite film according to claim 1, which is characterized in that the time of the reaction
For 3~12h.
8. application of the described in any item graphene oxide/polyaniline composite films of claim 1-7 in sewage treatment field.
9. application of the graphene oxide/polyaniline composite film according to claim 8 in water treatment field, feature exist
In the sewage is the industrial wastewater containing one or more of methylene blue dye, copper, zinc or nickel ion.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110975828A (en) * | 2019-11-20 | 2020-04-10 | 广东工业大学 | Adsorbing material for purifying sludge incineration flue gas and preparation method thereof |
| CN111252759A (en) * | 2019-11-20 | 2020-06-09 | 厦门大学 | Method for preparing graphene oxide by illumination and product |
| WO2021098165A1 (en) * | 2019-11-20 | 2021-05-27 | 厦门大学 | Graphene oxide material, halogenated graphene material, preparation methods therefor, and electrolysis system |
| CN114307674A (en) * | 2021-12-28 | 2022-04-12 | 北京林业大学 | Preparation method of special hydrophilic and hydrophobic membrane based on electric gradient morphology regulation |
| CN115193275A (en) * | 2022-07-08 | 2022-10-18 | 中国科学院生态环境研究中心 | Electric response film and preparation method and application thereof |
| CN116585916A (en) * | 2023-07-18 | 2023-08-15 | 西安金沃泰环保科技有限公司 | Selective polymer filter material for copper removal of waste acid and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110975828A (en) * | 2019-11-20 | 2020-04-10 | 广东工业大学 | Adsorbing material for purifying sludge incineration flue gas and preparation method thereof |
| CN111252759A (en) * | 2019-11-20 | 2020-06-09 | 厦门大学 | Method for preparing graphene oxide by illumination and product |
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| WO2021098165A1 (en) * | 2019-11-20 | 2021-05-27 | 厦门大学 | Graphene oxide material, halogenated graphene material, preparation methods therefor, and electrolysis system |
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| CN114307674A (en) * | 2021-12-28 | 2022-04-12 | 北京林业大学 | Preparation method of special hydrophilic and hydrophobic membrane based on electric gradient morphology regulation |
| CN114307674B (en) * | 2021-12-28 | 2022-12-09 | 北京林业大学 | Preparation method of special hydrophilic and hydrophobic membrane based on electric gradient morphology regulation |
| CN115193275A (en) * | 2022-07-08 | 2022-10-18 | 中国科学院生态环境研究中心 | Electric response film and preparation method and application thereof |
| CN116585916A (en) * | 2023-07-18 | 2023-08-15 | 西安金沃泰环保科技有限公司 | Selective polymer filter material for copper removal of waste acid and preparation method thereof |
| CN116585916B (en) * | 2023-07-18 | 2023-09-22 | 西安金沃泰环保科技有限公司 | Selective polymer filter material for copper removal of waste acid and preparation method thereof |
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