CN106587326B - A kind of preparation method of the graphene oxide of carried magnetic nano particle and conducting polymer Fenton gel - Google Patents
A kind of preparation method of the graphene oxide of carried magnetic nano particle and conducting polymer Fenton gel Download PDFInfo
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
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Abstract
A kind of preparation method of the graphene oxide of carried magnetic nano particle/conducting polymer Fenton gel, belongs to the synthesis and application field of nano material.The method comprises the following steps: step 1: in graphene oxide solution, conductive high polymer monomer is added, stirring is allowed to form homogeneous solution A;Step 2: molysite is added in solution A, and is continued stirring and formed solution B;Step 3: after alkaline solution is added dropwise into solution B, continue to stir to get product C;Step 4: product C is washed, the compound Fenton gel of graphene oxide/conducting polymer after freeze-drying to get carried magnetic nano particle.The invention proposes a kind of graphene oxide of carried magnetic nano particle/conducting polymer Fenton gel preparation method, the nanogel of preparation has higher absorption property, is conducive to the enrichment of dirty Organic substance in water；With faster degradation rate；Magnetic nano-particle loss can be reduced；Efficiency is recycled with higher, can be repeatedly used.
Description
Technical field
The present invention relates to the preparation methods of a kind of graphene oxide and conducting polymer Fenton gel, belong to nano material
Synthesis and application field.
Background technique
The world today, because water pollution caused by organic matter is on the rise.This pollutant have mobility is big, concentration is low,
The features such as toxicity height and strong characteristic of concentration, is difficult to be effectively treated with the prior art.Fenton degradation is in recent years based on nanotechnology
And a kind of means of the emerging processing organic pollutant to grow up.In the method, Fenton reagent is by H2O2It is decomposed into hyperoxia
The OH for the property changed, OH can be inorganic molecules without simultaneously mineralising is selectively decomposed all kinds of organic pollutants.
Traditional heterophase Fenton reagent is mainly based on iron-containing magnetic nano-particle.Such material in application process,
It has the following deficiencies: (1) magnetic attachment each other, is easy to appear aggregation, specific surface area is caused to reduce, degradation effect weakens；(2)
Magnetic nano-particle stability is poor, easily by solution corrosion, ferro element is caused to be lost, recycling property is bad；(3) organic contamination
Object concentration is lower, causes Fenton degradation rate slower.
And graphene oxide and conducting polymer surface have functional group abundant, pass through electrostatic force, hydrogen bond, Van der Waals force
It interacts with π-π, can realize organic pollutant enrichment by Adsorption of Organic on surface, improve absorption property.This
Outside, it is coexisted in graphene oxide and macropore in conductive polymer gel and meso-hole structure, this graded porous structure is conducive to increase
Big gel specific surface area, comes into full contact with magnetic nano-particle with organic pollutant, improves degradation rate.Importantly, by
In the protective effect of microenvironment in gel, can effective magnetic nano-particle stability, reduce the appearance of leakage, thus
Improve the recycling property of Fenton reagent.
Summary of the invention
Present invention aims at propose that a kind of graphene oxide/conducting polymer Fenton of carried magnetic nano particle is solidifying
The preparation method of glue, to solve, previous heterophase Fenton reagent absorption property is weak, degradation rate is slow, stability is low and recycles
The problems such as property is poor.
Realize above-mentioned purpose, the technical solution adopted by the present invention is as follows:
A kind of preparation method of the graphene oxide of carried magnetic nano particle and the compound Fenton gel of conducting polymer,
The method and step is as follows:
Step 1: in graphene oxide solution, conductive high polymer monomer is added, stirring is allowed to form homogeneous solution A；Institute
The conductive high polymer monomer stated is pyrrole monomer or aniline monomer；
Step 2: molysite is added in the solution A, and continues to stir, molysite is made to react to form solution B with solution A；
Step 3: after alkaline solution is added dropwise in the solution B of Xiang Suoshu, continues to stir, react alkaline solution with solution B
To product C；
Step 4: the product C is washed, to get carried magnetic nano particle and graphene oxide after freeze-drying
And the compound Fenton gel of conducting polymer.
The beneficial effect of the present invention compared with the existing technology is:
1, nanogel prepared by the present invention has higher absorption property, is conducive to the enrichment of dirty Organic substance in water；
2, nanogel prepared by the present invention has faster degradation rate, and degradation rate is common Fe3O4Nanoparticle
7.8 times；
3, nanogel prepared by the present invention has better stability, can reduce magnetic nano-particle loss；
4, the present invention prepares nanogel and recycles efficiency with higher, can repeatedly use.
It is also an advantage of the present invention that: since graphene oxide and conducting polymer surface contain a large amount of functional groups, favorably
In the enrichment of dirty Organic substance in water, to improve the absorption property of material；Due to gel macropore and the mesoporous hierarchical structure coexisted,
Make material that there is higher specific surface area, is conducive to coming into full contact with for magnetic nano-particle and organic matter, to improve Fenton
Degradation rate；Due to the special microenvironment of gel, protection can be provided for magnetic nano-particle, to reduce magnetic nano-particle
Loss, improve stability, improve recycling property.
Detailed description of the invention
Fig. 1 is the graphene oxide and conducting polymer Fenton gel of a kind of carried magnetic nano particle of the invention
In the embodiment one of preparation method, the inverted photo of gel；
Fig. 2 is the graphene oxide and conducting polymer Fenton gel of a kind of carried magnetic nano particle of the invention
In the embodiment one of preparation method, the SEM photograph of gained gel；
Fig. 3 is the graphene oxide and conducting polymer Fenton gel of a kind of carried magnetic nano particle of the invention
In the embodiment one of preparation method, the TEM photo of gained gel；
Fig. 4 is the graphene oxide and conducting polymer Fenton gel of a kind of carried magnetic nano particle of the invention
In the embodiment one of preparation method, Fenton gel and tradition Fe3O4The comparison of nanoparticle degradable organic pollutant methylene blue
Figure；
Fig. 5 is the graphene oxide and conducting polymer Fenton gel of a kind of carried magnetic nano particle of the invention
In the embodiment one of preparation method, Fenton gel recycles the degradation rate figure of degradation of methylene blue；
Fig. 6 is the graphene oxide and conducting polymer Fenton gel of a kind of carried magnetic nano particle of the invention
TEM photo in the embodiment one of preparation method, after gained gel circulation degradation of methylene blue 10 times；
Fig. 7 is the graphene oxide and conducting polymer Fenton gel of a kind of carried magnetic nano particle of the invention
In the embodiment two of preparation method, the TEM photo of gained gel.
Further description of the technical solution of the present invention with reference to the accompanying drawing, and however, it is not limited to this, all to this
Inventive technique scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered
Within the protection scope of the present invention.
Specific embodiment
Specific embodiment 1: a kind of graphene oxide of carried magnetic nano particle and the compound Fenton of conducting polymer
The preparation method of gel, the method and step are as follows:
Step 1: in graphene oxide solution, being added conductive high polymer monomer, stirring be allowed to be formed homogeneous solution A(this
The mixed solution of kind conductive high polymer monomer and graphene oxide, we term it solution As)；
Step 2: molysite being added in the solution A, and continue to stir, and reacting molysite with solution A, (molysite causes
Polymerization reaction) forming solution B, (there are graphene oxide, conducting polymer, iron ion and ferrous ions in solution at this time.I
This complicated system is called solution B)；
Step 3: after alkaline solution is added dropwise in the solution B of Xiang Suoshu, continues to stir, react alkaline solution with solution B
The graphene oxide of carried magnetic nano particle and the presoma of conductive polymer gel are obtained to product C(, we term it productions
Object C)；
Step 4: the product C is washed, to get carried magnetic nano particle and graphene oxide after freeze-drying
And the compound Fenton gel of conducting polymer.
Specific embodiment 2: a kind of graphene oxide of carried magnetic nano particle described in specific embodiment one with
The preparation method of the compound Fenton gel of conducting polymer, in step 1, the concentration of the graphene oxide solution is 0.1 ~
50 mg/mL, the dosage of the conductive high polymer monomer are 10 ~ 1000 μ L, graphene oxide and conductive high polymer monomer
Mass ratio is 0.1 ~ 10, and the mixing time is 1.0 min ~ 60min.
Specific embodiment 3: a kind of graphite oxide of carried magnetic nano particle described in specific embodiment one or two
The preparation method of alkene and the compound Fenton gel of conducting polymer, in step 1, the conductive high polymer monomer is aniline, pyrrole
Cough up, one of thiophene, acetylene, 3- hexyl thiophene and 3,4- ethene dioxythiophene or at least two combination.
Specific embodiment 4: a kind of graphene oxide of carried magnetic nano particle described in specific embodiment one with
The preparation method of the compound Fenton gel of conducting polymer, in step 2, the molysite is FeCl3、Fe(NO3)3、Fe2
(SO4)3Or K3Fe(CN)6。
Specific embodiment 5: a kind of graphite oxide of carried magnetic nano particle described in specific embodiment one or four
The preparation method of alkene and the compound Fenton gel of conducting polymer, in step 2, the iron salt concentration is 10 ~ 100 mg/mL,
The mass ratio of molysite and conductive high polymer monomer is 1 ~ 100.
Specific embodiment 6: a kind of graphene oxide of carried magnetic nano particle described in specific embodiment five with
The preparation method of the compound Fenton gel of conducting polymer, in step 2, the molysite and solution A reaction time is 6.0 ~
24.0 h。
Specific embodiment 7: a kind of graphene oxide of carried magnetic nano particle described in specific embodiment one with
The preparation method of the compound Fenton gel of conducting polymer, in step 3, the alkaline solution is ammonium hydroxide, sodium hydroxide, hydrogen
Potassium oxide or calcium hydroxide, the alkaline solution concentration are 0.01 ~ 50 mg/mL, and alkaline solution is with the solution B reaction time
10 min~3.0 h。
Specific embodiment 8: a kind of graphene oxide of carried magnetic nano particle described in specific embodiment one with
In step 3, the speed of alkaline solution drop is added dropwise in the preparation method of the compound Fenton gel of conducting polymer in the solution B of Xiang Suoshu
Rate is 0.1 ~ 2.0 mL/min, and time for adding is 1.0 ~ 10.0 min.
Specific embodiment 9: a kind of graphene oxide of carried magnetic nano particle described in specific embodiment one with
The preparation method of the compound Fenton gel of conducting polymer, in step 4, the product C sublimation drying is 1 ~ 20 day.
Embodiment one:
What embodiment one was recorded be a kind of carried magnetic nano particle graphene oxide and conducting polymer it is compound
The preparation method of Fenton gel adds into the graphene oxide solution that 100 mL concentration are 2.0 mg/mL during the preparation process
Enter the solution that 100 μ L contain pyrrole monomer, stir 30 min, forms homogeneous solution A.Then, 20 mg/ are added into solution A
mL FeCl3, 7h is reacted, solution B is formed.Next, 10mg/mL hydroxide is added dropwise with the rate of 2.0 mL/min into solution B
Sodium obtains product C after reacting 2h.By product C centrifuge washing, to get the oxygen of carried magnetic nano particle after freeze-drying 10 days
Graphite alkene and conducting polymer Fenton gel.
As shown in Figure 1, the left side is to start reaction solution A, the right is the digital camera photo of one gained gel of the present embodiment
Inverted Gel Precursor C, it can be seen that gel has been formed from inversion experiment.Fig. 2 is the SEM photograph of gel, in figure
Graphene oxide be in sheet, be connected between lamella and lamella by conducting high polymers object, thus will form macropore with
Structure that is mesoporous and depositing, this is the feature structure of gel.Fig. 3 is TEM photo, and sheet is presented in graphene oxide in photo,
In sheet surfaces it can be seen that evenly dispersed magnetic nano-particle of the partial size in 10 ~ 20 rans.Fig. 4 is organic dirt of degrading
Contaminate the Fenton gel and Fe of object3O4The comparison diagram of nanoparticle.In this experiment, the concentration of initial methylene blue is identical.It uses
The rate that gel carries out Fenton degradation is significantly faster than that traditional Fe3O4Nanoparticle, the former degradation rate are 7.8 times of the latter.
Fig. 5 is the result that gel carries out repeatedly circulation Fenton experiment.Therefrom it can be seen that, even if being recycled 10 times, activity remains unchanged
It is maintained at 90% or more.Fig. 6 is the gel TEM photo being recycled by 10 times, and graphene oxide still keeps sheet, table
The magnetic nano-particle of face load still maintains good dispersibility, occurs without any clustering phenomena.Complex chart 5 and Fig. 6, can
To find out that Fenton gel is with good stability and recycling property.
Embodiment two:
What embodiment two was recorded be a kind of carried magnetic nano particle graphene oxide and conducting polymer it is compound
The preparation method of Fenton gel, during preparation, into the graphene oxide solution that 10 mL concentration are 0.5 mg/mL
20 μ L are added and contain aniline monomer solution, stir 60 min, form homogeneous solution A.Then, 5 mg/mL are added into solution A
Fe(NO3)3, 6h is reacted, solution B is formed.Next, 2 mg/mL hydroxides are added dropwise with the rate of 1.0 mL/min into solution B
Sodium reacts 3h, obtains product C.By product C centrifuge washing, to get the oxidation of carried magnetic nano particle after freeze-drying 5 days
Graphene and conducting polymer Fenton gel, as shown in Figure 7.
Claims (8)
1. the preparation method of a kind of graphene oxide of carried magnetic nano particle and the compound Fenton gel of conducting polymer,
Be characterized in that: the method and step is as follows:
Step 1: in graphene oxide solution, conductive high polymer monomer is added, stirring is allowed to form homogeneous solution A；Described
Conductive high polymer monomer is pyrrole monomer or aniline monomer；
Step 2: molysite is added in the solution A, and continues to stir, molysite is made to react to form solution B with solution A；
Step 3: after alkaline solution is added dropwise in the solution B of Xiang Suoshu, continues to stir, react alkaline solution with solution B and produced
Object C；
Step 4: the product C is washed, and to get carried magnetic nano particle and graphene oxide and is led after freeze-drying
The electric compound Fenton gel of macromolecule.
2. the graphene oxide and conducting polymer of a kind of carried magnetic nano particle according to claim 1 are compound
The preparation method of Fenton gel, it is characterised in that: in step 1, the concentration of the graphene oxide solution is 0.1 ~ 50
Mg/mL, the dosage of the conductive high polymer monomer are 10 ~ 1000 μ L, the quality of graphene oxide and conductive high polymer monomer
Than being 0.1 ~ 10, the mixing time is 1.0 min ~ 60min.
3. the graphene oxide and conducting polymer of a kind of carried magnetic nano particle according to claim 1 are compound
The preparation method of Fenton gel, it is characterised in that: in step 2, the molysite is FeCl3、Fe(NO3)3、Fe2(SO4)3Or
K3Fe(CN)6。
4. the graphene oxide and conducting polymer of a kind of carried magnetic nano particle according to claim 1 or 3 are compound
The preparation method of Fenton gel, it is characterised in that: in step 2, the iron salt concentration be 10 ~ 100 mg/mL, molysite with
The mass ratio of conductive high polymer monomer is 1 ~ 100.
5. the graphene oxide and conducting polymer of a kind of carried magnetic nano particle according to claim 4 are compound
The preparation method of Fenton gel, it is characterised in that: in step 2, the molysite and solution A reaction time are 6.0 ~ 24.0
h。
6. the graphene oxide and conducting polymer of a kind of carried magnetic nano particle according to claim 1 are compound
The preparation method of Fenton gel, it is characterised in that: in step 3, the alkaline solution is ammonium hydroxide, sodium hydroxide, hydroxide
Potassium or calcium hydroxide, the alkaline solution concentration are 0.01 ~ 50 mg/mL, and alkaline solution and solution B reaction time are 10
min~3.0 h。
7. the graphene oxide and conducting polymer of a kind of carried magnetic nano particle according to claim 1 are compound
The preparation method of Fenton gel, it is characterised in that: in step 3, the rate of alkaline solution drop is added dropwise in the solution B of Xiang Suoshu
For 0.1 ~ 2.0 mL/min, time for adding is 1.0 ~ 10.0 min.
8. the graphene oxide and conducting polymer of a kind of carried magnetic nano particle according to claim 1 are compound
The preparation method of Fenton gel, it is characterised in that: in step 4, the product C sublimation drying is 1 ~ 20 day.
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