CN103418340A - Reduction-oxidation graphene-Fe3O4 nano composite, preparation method thereof, and application of reduction-oxidation graphene-Fe3O4 nano composite in absorbing bisphenol A - Google Patents
Reduction-oxidation graphene-Fe3O4 nano composite, preparation method thereof, and application of reduction-oxidation graphene-Fe3O4 nano composite in absorbing bisphenol A Download PDFInfo
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- CN103418340A CN103418340A CN2013102875319A CN201310287531A CN103418340A CN 103418340 A CN103418340 A CN 103418340A CN 2013102875319 A CN2013102875319 A CN 2013102875319A CN 201310287531 A CN201310287531 A CN 201310287531A CN 103418340 A CN103418340 A CN 103418340A
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Abstract
The invention discloses a reduction-oxidation graphene-Fe3O4 nano composite, a preparation method thereof, and an application of the reduction-oxidation graphene-Fe3O4 nano composite in absorbing bisphenol A. The reduction-oxidation graphene-Fe3O4 nano composite comprises Fe3O4 nano particles and reduction-oxidation graphene. The reduction-oxidation graphene-Fe3O4 nano composite and a solution containing the bisphenol A are in full contact in an ambient temperature, the bisphenol A is absorbed and removed. Compared with the prior art, the advantages of small material dose, simplicity in operation, mild processing condition, fast processing speed, and no harm for the environment, and recycling nano-composite materials, and the like are achieved.
Description
Technical field
The invention belongs to nanometer technology and water-treatment technology field, relate to a kind of redox graphene (rGO)-Fe
3O
4Nano composite material and preparation method thereof, with and the application in bisphenol-A in absorption.
Background technology
Bisphenol-A ((CH
3)
2C(C
6H
4OH)
2, BPA) be used as raw material and the additive of industrial production Merlon, epoxy resin and other plastics.Recent years, BPA can imitate estrogen as a kind of endocrine interferon (EDCs), and human and animal's health is caused negative impact and caused both at home and abroad very large concern and report.Even report points out that, under the low dosage of part per trillion, BPA also may cause tumour, inborn defect, maldevelopment.BPA in environment water is mainly from the discharge of municipal sewage and trade effluent, closely bound up with our daily life.Because BPA can't carry out biodegradation and chemical degradation, also difficulty is larger
[, in the urgent need to developing fast, effectively, processing method cheaply, prevent its contaminated environment.
The processing method that BPA is traditional mainly comprises the technology such as absorption, solvent extraction, film separation and light degradation.Wherein, adsorption technology is processed means because the advantages such as it is simple to operate, efficiency is high, applicability is strong are considered to effective BPA.Carbonaceous material has very large specific area, and BPA is had to very strong adsorption capacity, as activated carbon, CNT all have been reported, is applied to the BPA adsorption treatment.
Graphene is a kind of emerging Two-dimensional Carbon material, has the specific area of excellent electric conductivity, mechanical strength, toughness and superelevation.The derivative of Graphene, as redox graphene (rGO) and functionalization graphene show good performance in fields such as catalysis, capacitor, photoelectric material, adsorbents.Owing between the local π on Graphene surface-electron system energy and phenyl ring, forming pi-pi accumulation, so Graphene has more advantage as adsorbent in the processing of organic dyestuff, agricultural chemicals, aldehydes matter.Recently, have been reported and adopt Graphene absorption BPA absorption, pi-pi accumulation effect and hydrogen bond action section are conducive to BPA and are adsorbed by Graphene.Yet, use on a large scale Graphene can have the difficult problem of separating and regenerating as adsorbent, therefore need exploitation efficiently cheap, be easy to regeneration and the graphene composite material separated.
Summary of the invention
For overcoming the above-mentioned existing problems of prior art, the present invention innovates and proposes a kind of redox graphene (rGO)-Fe
3O
4Nano composite material and preparation method thereof, and this redox graphene (rGO)-Fe
3O
4The application of nano composite material in the absorption bisphenol-A.
The present invention proposes a kind of redox graphene-Fe
3O
4Nano composite material, described redox graphene-Fe
3O
4Nano composite material comprises Fe
3O
4Nano particle and redox graphene; Wherein, described Fe
3O
4Nano particle is evenly dispersed in described redox graphene surface, and described graphene-structured is scraps of paper shape.
Redox graphene-Fe of the present invention
3O
4The saturation magnetization of nano composite material is 36-51emug
-1.Preferably, saturation magnetization is 36emug
-1Left and right.
Redox graphene-Fe of the present invention
3O
4In nano composite material, described Fe
3O
4The average diameter of nano particle is 8-15nm.Preferably, Fe
3O
4The average diameter of nano particle is the 10nm left and right.
Redox graphene-Fe of the present invention
3O
4Nano composite material, introduce Fe on the redox graphene surface
3O
4Nano particle can bring into play the easy advantage of separating of the high absorption capacity of redox graphene and magnetic material, and the existence of redox graphene can reduce Fe effectively simultaneously
3O
4The reunion of nano particle.Compared with prior art, redox graphene-Fe of the present invention
3O
4Nano composite material has high-specific surface area and magnetic responsiveness, and bisphenol-A (BPA) is had to good absorption property.Adsorbent based on magnetic Nano material just can be separated simply and be regenerated by externally-applied magnetic field, and without centrifugal or filtration, therefore, by externally-applied magnetic field, composite of the present invention can carry out Magnetic Isolation and cycling and reutilization easily.
The invention allows for a kind of redox graphene-Fe
3O
4The preparation method of nano composite material, be scattered in the redox Graphene in redistilled water through ultrasonic, adds hydrazine hydrate and ammonia spirit, obtain finely dispersed solution after stirring, reflux in 50-100 ℃ of oil bath, through centrifugal, vacuum drying, make redox graphene; By aforementioned redox graphene, FeCl
24H
2O, FeCl
3Be dispersed in redistilled water, add sodium hydrate regulator solution pH value to 11-12, be heated to 80 ℃ and stirring, through the distilled water washing, obtain purpose product redox graphene-Fe
3O
4Nano composite material.
In preparation method of the present invention, described redox graphene, FeCl
24H
2O, FeCl
3With ratio 1: 0.5～1.5: 1.5～3.0, be scattered in redistilled water.Preferably, described redox graphene, FeCl
24H
2O, FeCl
3Ratio be 200: 172: 281.
The invention allows for redox graphene-Fe
3O
4The application of nano composite material in the absorption bisphenol-A.Particularly, redox graphene-Fe of the present invention
3O
4Nano composite material can be used for bisphenol-A contained in adsorbent solution (BPA), for example, and for the bisphenol-A of the solution such as adsorbed water, milk, beverage.The present invention has proposed redox graphene-Fe with innovating first
3O
4Nanocomposite applications is in the absorption bisphenol-A.
In the present invention's application, utilize redox graphene-Fe
3O
4The method of nano composite material absorption bisphenol-A, for example, for the BPA of adsorbed water body.By redox graphene-Fe of the present invention
3O
4Nano composite material is positioned in the solution containing bisphenol-A, at room temperature stirs 2-6 hour, makes redox graphene-Fe
3O
4Nano composite material fully contacts with this solution, for example, fully stirs contact 2 hours or 6 hours, fully to adsorb bisphenol-A.This composite has high-specific surface area and magnetic responsiveness, and bisphenol-A in water body (BPA) is had to good absorption property.Then, the redox graphene-Fe of bisphenol-A will fully have been adsorbed by the magnetic separate mode
3O
4Nano composite material is separated from solution, for example, adopts externally-applied magnetic field to be separated nano composite material.After absorption, the content of bisphenol A in solution greatly reduces.Fully, after absorption, can realize removing the effect of bisphenol-A in solution.Redox graphene-Fe of the present invention
3O
4BPA in the effective adsorption aqueous solution of nano composite material energy-absorbing and the mode that can separate by magnetic are carried out cycling and reutilization.
In the present invention's application, the pH of the described solution containing bisphenol-A is adjusted to 2-8.Utilizing redox graphene-Fe
3O
4In the method for nano composite material absorption bisphenol-A, reaction is carried out at normal temperatures and pressures.Solution can be the various solution such as water, milk, beverage, unrestricted.
In the present invention's application, further, can utilize methyl alcohol, acetone equal solvent, the redox graphene-Fe that has adsorbed bisphenol-A obtained after separating by magnetic field
3O
4Nano composite material is carried out desorption and regeneration, then be positioned over containing in the solution of bisphenol-A with absorption bisphenol-A.Redox graphene-Fe of the present invention
3O
4Nano composite material can be repeated multiple times for adsorbing bisphenol-A, thereby realize the cycling and reutilization effect.
The present invention has that material usage is few, simple to operate, treatment conditions are gentle, it is quick to process, environmentally safe harmless, the advantage such as nano material can be recycled.Beneficial effect of the present invention comprises: redox graphene-Fe of the present invention
3O
4Nano composite material is to the bisphenol-A advantages of good adsorption effect, and sorbing material has high-specific surface area, and BPA is had to very strong adsorption capacity, and time of equilibrium adsorption is short.The preparation of nano material of the present invention is simple, is easy to control and operation.Nano material has high magnetic responsiveness, and the magnetic nanometer composite material after the present invention's absorption carries out Separation of Solid and Liquid by externally-applied magnetic field, and whole process rapidly and efficiently.The present invention can realize the recycling of resource, and the magnetic nanometer composite material after absorption can be recycled after regeneration.
The accompanying drawing explanation
Redox graphene-Fe that Fig. 1 is embodiment 1
3O
4The hysteresis graph of nano composite material.
Redox graphene-Fe that Fig. 2 is embodiment 1
3O
4The transmission electron microscope figure of nano composite material.
Redox graphene-Fe that Fig. 3 is embodiment 1
3O
4The scanning electron microscope diagram of nano composite material.
The sorption reaction time that Fig. 4 is embodiment 2 and bisphenol-A clearance change curve.
Fig. 5 is redox graphene-Fe of the present invention
3O
4Nano composite material recycles number of times and adsorption capacity changes schematic diagram.
Concrete embodiment
In conjunction with following specific embodiments and the drawings, the present invention is described in further detail, and protection content of the present invention is not limited to following examples.Under the spirit and scope that do not deviate from inventive concept, variation and advantage that those skilled in the art can expect all are included in the present invention, and take appending claims as protection domain.Implement process of the present invention, condition, reagent, experimental technique etc., except the following content of mentioning specially, be universal knowledege and the common practise of this area, the present invention is not particularly limited content.
Redox graphene-Fe of the present invention
3O
4The preparation method of nano composite material comprises: graphene oxide is scattered in redistilled water through ultrasonic, adds hydrazine hydrate and ammonia spirit, obtain finely dispersed solution after stirring, reflux in 50-100 ℃ of oil bath, through centrifugal, vacuum drying, make redox graphene; By 200mg redox graphene, 172.2mg FeCl
24H
2O and 280.95mg FeCl
3Be dissolved in the 200ml deionized water, then add 1.5mLNaOH (10molL
-1), the final pH of system is controlled at 11-12, then mechanical agitation 1 hour under the condition of 80 ℃.The gained sediment carries out Magnetic Isolation, and vacuum drying again after washing obtains redox graphene-Fe
3O
4Nano composite material.
Utilize redox graphene-Fe of the present invention
3O
4The waste water that nano composite material is processed containing bisphenol-A adsorbs bisphenol-A, particularly, with distilled water configuration 20mg/L bisphenol-A solutions simulate waste water solution, gets 10mg Graphene-Fe
3O
4Nano composite material (rGO-MNPs) is dispersed in as adsorbent in the BPA solution of 20mg/L of 50mL, after stirring at room 2-6 hour, with magnet by this nano material absorption migration out, calculates the clearance of bisphenol-A in solution and reaches 95% left and right.
Utilize redox graphene-Fe
3O
4Nano composite material absorption, containing bisphenol-A, further, is carried out redox graphene-Fe
3O
4Nano composite material regeneration: the redox graphene-Fe that will adsorb bisphenol-A
3O
4Nano composite material, with after deionized water washing one time, adds 10mL methyl alcohol, and concussion 30min finally, with deionized water washing 2-3 time, can come into operation in oven for drying again.Redox graphene-Fe
3O
4After nano composite material again drops into and recycles 5 times, its adsorption capacity still can keep 95% original left and right.
Embodiment 1:
Redox graphene is scattered in redistilled water through ultrasonic, adds hydrazine hydrate and ammonia spirit, obtains finely dispersed solution after stirring, in 50-100 ℃ of oil bath, refluxes, and through centrifugal, vacuum drying, makes redox graphene; By the 200mg redox graphene, 172.2mg FeCl
24H
2O and 280.95mg FeCl
3Be dissolved in the 200ml deionized water, then add 1.5mL NaOH (10molL
-1), the final pH of reaction system is controlled at 11-12, and then mechanical agitation 1 hour under the condition of 80 ℃, be precipitated thing.The gained sediment carries out Magnetic Isolation, and vacuum drying again after washing obtains redox graphene-Fe
3O
4Nano composite material, its saturation magnetization is 36emu g
-1, as shown in Figure 1.The redox graphene structure is scraps of paper shape, Fe
3O
4Nano particle is evenly dispersed in Graphene surface, Fe
3O
4The average diameter of nano particle is the 10nm left and right, and as shown in Figure 2, transmission electron microscope picture as shown in Figure 3 for its scanning electron microscope (SEM) photograph.
Embodiment 2:
Get the waste water solution of 50mL containing 20mg/L BPA, pH=2-8, add 10mg redox graphene-Fe therein
3O
4Nano composite material, at stirring at room absorption certain hour, as 6 hours.With magnet, nano composite material is removed, detect the content of bisphenol A in the rear solution of absorption, calculate bisphenol-A clearance in solution.As shown in Figure 4, along with the increase in processing time, in solution, the clearance of bisphenol-A raises gradually for bisphenol-A clearance and processing time change curve, and in the 2h left and right, its absorption reaches balance, and the clearance of bisphenol-A reaches 96% left and right.
Embodiment 3:
Redox graphene-the Fe of bisphenol-A will have been adsorbed
3O
4Nano composite material, with after deionized water washing one time, adds 10mL methyl alcohol, and concussion 30min finally, with deionized water washing 2-3 time, can come into operation in the absorption of bisphenol-A in oven for drying, with reference to the application process of embodiment 2 again.Redox graphene-Fe after regeneration
3O
4After nano composite material recycles 5 times, it is original 95% that its adsorption capacity still can keep, and recycles number of times on the impact of BPA adsorption capacity as shown in Figure 5.
Claims (9)
1. a redox graphene-Fe
3O
4Nano composite material, is characterized in that, described redox graphene-Fe
3O
4Nano composite material comprises Fe
3O
4Nano particle and redox graphene, wherein, described Fe
3O
4Nano particle is evenly dispersed in described redox graphene surface, and described redox graphene structure is scraps of paper shape, described Fe
3O
4The average diameter of nano particle is 8-15nm; Described redox graphene-Fe
3O
4The saturation magnetization of nano composite material is 36-51emug
-1.
2. redox graphene-Fe as claimed in claim 1
3O
4Nano composite material, is characterized in that, described Fe
3O
4The average diameter of nano particle is 10nm.
3. redox graphene-Fe as claimed in claim 1
3O
4Nano composite material, is characterized in that, described redox graphene-Fe
3O
4The saturation magnetization of nano composite material is 36emug
-1.
4. a redox graphene-Fe
3O
4The preparation method of nano composite material, is characterized in that, graphene oxide is scattered in redistilled water through ultrasonic, add hydrazine hydrate and ammonia spirit, obtain finely dispersed solution after stirring, reflux in 50-100 ℃ of oil bath, through centrifugal, vacuum drying, make redox graphene; By aforementioned redox graphene, FeCl
24H
2O, FeCl
3Be dispersed in redistilled water, add sodium hydrate regulator solution pH value to 11-12, be heated to 80 ℃ and stirring, through the distilled water washing, obtain redox graphene-Fe as claimed in claim 1
3O
4Nano composite material.
5. preparation method as claimed in claim 4, is characterized in that, described redox graphene, FeCl
24H
2O, FeCl
3Ratio be 1: 0.5～1.5: 1.5～3.0.
6. redox graphene-Fe as claimed in claim 1
3O
4The application of nano composite material in the absorption bisphenol-A.
7. application as claimed in claim 6, utilize the bisphenol-A in redox graphene-Fe3O4 nano composite material adsorbent solution, it is characterized in that, described redox graphene-Fe3O4 nano composite material is positioned in the solution containing bisphenol-A, at room temperature stir 2-6 hour, by described redox graphene-Fe3O4 nano composite material absorption bisphenol-A; Separate from solution and separate by magnetic having adsorbed the redox graphene of bisphenol-A-Fe3O4 nano composite material.
8. application as claimed in claim 6, is characterized in that, the pH of the described solution containing bisphenol-A is 2-8.
9. application as claimed in claim 6, is characterized in that, further comprises, utilizes methyl alcohol, acetone solvent, by the redox graphene of absorption bisphenol-A-Fe3O4 nano composite material desorption and regeneration, then is positioned in the solution containing bisphenol-A, with the absorption bisphenol-A.
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