CN106587326A - Preparation method of oxidized graphene and conducting polymer Fenton gel loaded with magnetic nanoparticles - Google Patents
Preparation method of oxidized graphene and conducting polymer Fenton gel loaded with magnetic nanoparticles Download PDFInfo
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- CN106587326A CN106587326A CN201611224040.XA CN201611224040A CN106587326A CN 106587326 A CN106587326 A CN 106587326A CN 201611224040 A CN201611224040 A CN 201611224040A CN 106587326 A CN106587326 A CN 106587326A
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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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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- 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
- B01J20/28047—Gels
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The invention relates to a preparation method of oxidized graphene/conducting polymer Fenton gel loaded with magnetic nanoparticles, and belongs to the fields of synthesis and application of nanometer materials. The method comprises the following steps of step I, adding conducting polymer monomers to an oxidized graphene solution, and performing stirring so that a uniform solution A is obtained; step II, adding iron salt to the solution A, and continuing stirring so as to obtain a solution B; step III, dropwise adding an alkaline solution to the solution B, and continuing stirring so as to obtain a product C; and step IV, washing the product C, and performing freeze drying so as to obtain the oxidized graphene/conducting polymer Fenton gel loaded with magnetic nanoparticles. The invention provides the preparation method of the oxidized graphene/conducting polymer Fenton gel loaded with magnetic nanoparticles, and the prepared nano gel has high adsorbability. Enrichment of organics in wastewater is facilitated, and the preparation method has high degradation rate. According to the preparation method disclosed by the invention, running off of the magnetic nanoparticles can be reduced, high cyclic utilization efficiencies can be obtained, and the oxidized graphene/conducting polymer Fenton gel can be repeatedly used.
Description
Technical field
The present invention relates to a kind of graphene oxide and the preparation method of conducting polymer Fenton gels, belong to nano material
Synthesis and application.
Background technology
The world today, because water pollution is on the rise caused by Organic substance.This pollutant has that mobility is big, concentration is low,
The features such as toxicity is high strong with characteristic of concentration, with prior art it is difficult to effective process.Fenton degradeds are to be based on nanotechnology in recent years
And the means of a kind of emerging process organic pollution for growing up.In the method, Fenton reagent is by H2O2It is decomposed into hyperoxia
The OH of the property changed, OH can be all kinds of organic pollutions are without selectively decomposition and mineralising is inorganic molecules.
Traditional heterophase Fenton reagent is mainly based on the magnetic nano-particle of iron content.Such material in application process,
There is following defect:(1), easily there is aggregation in magnetic attraction each other, causes specific surface area to reduce, and degradation effect weakens;(2)
Magnetic nano-particle less stable, easily by solution corrosion, causes ferrum element to be lost in, and recycling property is bad;(3)Organic contamination
Thing concentration is relatively low, causes Fenton degradation rates slower.
And graphene oxide and conducting polymer surface have abundant functional group, by electrostatic force, hydrogen bond, Van der Waals force
Interact with π-π, organic pollutant enrichment can be realized by Adsorption of Organic on surface, improve absorption property.This
Outward, macropore and meso-hole structure coexist in graphene oxide with conductive polymer gel, and this graded porous structure is conducive to increasing
Big gel specific surface area, makes magnetic nano-particle be fully contacted with organic pollution, improves degradation rate.Importantly, by
The protective effect of microenvironment in gel, can effective magnetic nano-particle stability, reduce the appearance of leakage, so as to
Improve the recycling property of Fenton reagent.
The content of the invention
Present invention aim at proposing that a kind of graphene oxide of carried magnetic nano particle/conducting polymer Fenton coagulates
The preparation method of glue, to solve, conventional heterophase Fenton reagent absorption property is weak, degradation rate is slow, stability is low and recycles
Property difference the problems such as.
Above-mentioned purpose is realized, the technical scheme that the present invention takes is as follows:
The present invention is relative to the beneficial effect of prior art:
1st, nanogel prepared by the present invention has higher absorption property, is conducive to the enrichment of dirty Organic substance in water;
2nd, nanogel prepared by the present invention has faster degradation rate, and its degradation rate is common Fe3O4Nanoparticle
7.8 again;
3rd, nanogel prepared by the present invention has more preferable stability, can reduce magnetic nano-particle loss;
4th, the present invention prepares nanogel and recycles efficiency with higher, can repeatedly use.
It is also an advantage of the present invention that:Because a large amount of functional groups are contained on graphene oxide and conducting polymer surface, favorably
In the enrichment of dirty Organic substance in water, so as to improve the absorption property of material;Due to gel macropore and the mesoporous hierarchy for coexisting,
Make material that there is higher specific surface area, be conducive to being fully contacted for magnetic nano-particle and Organic substance, so as to improve Fenton
Degradation rate;Due to the special microenvironment of gel, protection can be provided for magnetic nano-particle, so as to reduce magnetic nano-particle
Loss, improve stability, improve recycling property.
Description of the drawings
Fig. 1 is a kind of graphene oxide and conducting polymer Fenton gels of carried magnetic nano particle of the present invention
In the embodiment one of preparation method, the inverted photo of gel;
Fig. 2 is a kind of preparation of the graphene oxide with conducting polymer Fenton gels of carried magnetic nano particle of the present invention
In the embodiment one of method, the SEM photograph of gained gel;
Fig. 3 is a kind of preparation of the graphene oxide with conducting polymer Fenton gels of carried magnetic nano particle of the present invention
In the embodiment one of method, the TEM photos of gained gel;
Fig. 4 is a kind of preparation of the graphene oxide with conducting polymer Fenton gels of carried magnetic nano particle of the present invention
In the embodiment one of method, Fenton gels and tradition Fe3O4The comparison diagram of nanoparticle degradable organic pollutant methylene blue;
Fig. 5 is a kind of preparation of the graphene oxide with conducting polymer Fenton gels of carried magnetic nano particle of the present invention
In the embodiment one of method, Fenton gels circulate the degradation rate figure of degradation of methylene blue;
Fig. 6 is a kind of preparation of the graphene oxide with conducting polymer Fenton gels of carried magnetic nano particle of the present invention
TEM photos in the embodiment one of method, after gained gel circulation degradation of methylene blue 10 times;
Fig. 7 is a kind of preparation of the graphene oxide with conducting polymer Fenton gels of carried magnetic nano particle of the present invention
In the embodiment two of method, the TEM photos of gained gel.
Technical scheme is further described below in conjunction with the accompanying drawings, but is not limited thereto, it is every to this
Inventive technique scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should be covered
In protection scope of the present invention.
Specific embodiment
Specific embodiment one:A kind of graphene oxide of carried magnetic nano particle Fenton compound with conducting polymer
The preparation method of gel, methods described step is as follows:
Step one:In graphene oxide solution, conductive high polymer monomer, stirring is added to be allowed to form homogeneous solution A(It is this to lead
The mixed solution of electric high polymer monomer and graphene oxide, we term it solution A);
Step 2:Iron salt is added in described solution A, and continues stirring, iron salt is reacted with solution A(Iron salt causes polymerization
Reaction)Form solution B(There is graphene oxide, conducting polymer, iron ion and ferrous ion in solution now.We
This complicated system is referred to as solution B);
Step 3:To in described solution B after Deca alkaline solution, continue to stir, alkaline solution is produced with solution B reaction
Thing C(The graphene oxide of carried magnetic nano particle and the presoma of conductive polymer gel are obtained, we term it product
C);
Step 4:Described product C is washed, after lyophilization, carried magnetic nano particle and graphene oxide is obtained final product and is led
The compound Fenton gels of electric macromolecule.
Specific embodiment two:A kind of graphene oxide of the carried magnetic nano particle described in specific embodiment one with
The preparation method of the compound Fenton gels of conducting polymer, in step one, the concentration of described graphene oxide solution is 0.1 ~
50 mg/mL, the consumption of described conductive high polymer monomer is 10 ~ 1000 μ L, graphene oxide and conductive high polymer monomer
Mass ratio is 0.1 ~ 10, and described mixing time is 1.0 min ~ 60min.
Specific embodiment three:A kind of graphite oxide of the carried magnetic nano particle described in specific embodiment one or two
Alkene is combined the preparation method of Fenton gels with conducting polymer, and in step one, described conductive high polymer monomer is aniline, pyrrole
Cough up, the one kind in thiophene, acetylene, 3- hexyl thiophenes and 3,4- ethene dioxythiophenes or at least two combination.
Specific embodiment four:A kind of graphene oxide of the carried magnetic nano particle described in specific embodiment one with
The preparation method of the compound Fenton gels of conducting polymer, in step 2, described iron salt is FeCl3、Fe(NO3)3、Fe2
(SO4)3Or K3Fe(CN)6。
Specific embodiment five:A kind of graphite oxide of the carried magnetic nano particle described in specific embodiment one or four
Alkene is combined the preparation method of Fenton gels with conducting polymer, and in step 2, described iron salt concentration is 10 ~ 100 mg/mL,
Iron salt is 1 ~ 100 with the mass ratio of conductive high polymer monomer.
Specific embodiment six:A kind of graphene oxide of the carried magnetic nano particle described in specific embodiment five with
The preparation method of the compound Fenton gels of conducting polymer, in step 2, described iron salt and solution A response time is 6.0 ~
24.0 h。
Specific embodiment seven:A kind of graphene oxide of the carried magnetic nano particle described in specific embodiment one with
The preparation method of the compound Fenton gels of conducting polymer, in step 3, described alkaline solution is ammonia, sodium hydroxide, hydrogen
Potassium oxide or calcium hydroxide, described alkaline solution concentration is 0.01 ~ 50 mg/mL, and alkaline solution is with the solution B response time
10 min~3.0 h。
Specific embodiment eight:A kind of graphene oxide of the carried magnetic nano particle described in specific embodiment one with
The preparation method of the compound Fenton gels of conducting polymer, in step 3, the speed of Deca alkaline solution drop in described solution B
Rate is 0.1 ~ 2.0 mL/min, and time for adding is 1.0 ~ 10.0 min.
Specific embodiment nine:A kind of graphene oxide of the carried magnetic nano particle described in specific embodiment one with
The preparation method of the compound Fenton gels of conducting polymer, in step 4, described product C sublimation dryings are 1 ~ 20 day.
Embodiment one:
What embodiment one was recorded is that a kind of graphene oxide of carried magnetic nano particle Fenton compound with conducting polymer coagulates
The preparation method of glue, in preparation process, toward the graphene oxide solution that 100 mL concentration are 2.0 mg/mL 100 μ L is added
Solution containing pyrrole monomer, stirs 30 min, forms homogeneous solution A.Then, 20 mg/mL FeCl are added in solution A3,
Reaction 7h, forms solution B.Next, in solution B with the speed Deca 10mg/mL sodium hydroxide of 2.0 mL/min, reacting 2h
Afterwards, product C is obtained.By product C centrifuge washings, after lyophilization 10 days, the graphene oxide of carried magnetic nano particle is obtained final product
With conducting polymer Fenton gels.
As shown in figure 1, the left side is to start reaction solution A, the right is for the digital camera photo of the gained gel of the present embodiment one
Inverted Gel Precursor C, it can be seen that gel has been formed from the inversion experiment.Fig. 2 is the SEM photograph of gel, in figure
Graphene oxide be in sheet, be connected by conducting high polymers thing between lamella and lamella, thus can be formed macropore with
Structure that is mesoporous and depositing, this is the feature structure of gel.Fig. 3 is TEM photos, and graphene oxide is presented sheet in photo,
Can see dispersed magnetic nano-particle of the particle diameter in 10 ~ 20 rans in sheet surfaces.Fig. 4 is the organic dirt of degraded
The Fenton gels and Fe of dye thing3O4The comparison diagram of nanoparticle.In this experiment, the concentration of initial methylene blue is identical.Use
Gel carries out the speed of Fenton degradeds and is significantly faster than that traditional Fe3O4Nanoparticle, the former degradation rate is 7.8 times of the latter.
Fig. 5 is repeatedly circulated the result of Fenton experiments for gel.Therefrom can see, even if recycling 10 times, activity remains unchanged
It is maintained at more than 90%.Fig. 6 is the gel TEM photos through 10 recyclings, and graphene oxide still keeps sheet, table
The magnetic nano-particle of face load still maintains good dispersibility, occurs without any clustering phenomena.Comprehensive Fig. 5 and Fig. 6, can
To find out that Fenton gels have good stability and recycling property.
Embodiment two:
What embodiment two was recorded is that a kind of graphene oxide of carried magnetic nano particle Fenton compound with conducting polymer coagulates
The preparation method of glue, during preparation, toward the graphene oxide solution that 10 mL concentration are 0.5 mg/mL 20 μ L is added
Containing aniline monomer solution, 60 min are stirred, form homogeneous solution A.Then, 5 mg/mL Fe (NO are added in solution A3)3,
Reaction 6h, forms solution B.Next, in solution B with the mg/mL sodium hydroxide of speed Deca 2 of 1.0 mL/min, reaction
3h, obtains product C.By product C centrifuge washings, after lyophilization 5 days, obtain final product the graphene oxide of carried magnetic nano particle with
Conducting polymer Fenton gels, as shown in Figure 7.
Claims (9)
1. a kind of graphene oxide of carried magnetic nano particle and conducting polymer are combined the preparation method of Fenton gels, its
It is characterised by:Methods described step is as follows:
Step one:In graphene oxide solution, conductive high polymer monomer, stirring is added to be allowed to form homogeneous solution A;
Step 2:Iron salt is added in described solution A, and continues stirring, make iron salt react to form solution B with solution A;
Step 3:To in described solution B after Deca alkaline solution, continue to stir, alkaline solution is produced with solution B reaction
Thing C;
Step 4:Described product C is washed, after lyophilization, carried magnetic nano particle and graphene oxide is obtained final product and is led
The compound Fenton gels of electric macromolecule.
2. a kind of graphene oxide of carried magnetic nano particle according to claim 1 is combined with conducting polymer
The preparation method of Fenton gels, it is characterised in that:In step one, the concentration of described graphene oxide solution is 0.1 ~ 50
Mg/mL, the consumption of described conductive high polymer monomer is the quality of 10 ~ 1000 μ L, graphene oxide and conductive high polymer monomer
Than for 0.1 ~ 10, described mixing time is 1.0 min ~ 60min.
3. a kind of graphene oxide of carried magnetic nano particle according to claim 1 and 2 is combined with conducting polymer
The preparation method of Fenton gels, it is characterised in that:In step one, described conductive high polymer monomer is aniline, pyrroles, thiophene
One kind or at least two combination in fen, acetylene, 3- hexyl thiophenes and 3,4- ethene dioxythiophenes.
4. a kind of graphene oxide of carried magnetic nano particle according to claim 1 is combined with conducting polymer
The preparation method of Fenton gels, it is characterised in that:In step 2, described iron salt is FeCl3、Fe(NO3)3、Fe2(SO4)3Or
K3Fe(CN)6。
5. a kind of graphene oxide of the carried magnetic nano particle according to claim 1 or 4 is combined with conducting polymer
The preparation method of Fenton gels, it is characterised in that:In step 2, described iron salt concentration is 10 ~ 100 mg/mL, iron salt with
The mass ratio of conductive high polymer monomer is 1 ~ 100.
6. a kind of graphene oxide of carried magnetic nano particle according to claim 5 is combined with conducting polymer
The preparation method of Fenton gels, it is characterised in that:In step 2, described iron salt and solution A response time is 6.0 ~ 24.0
h。
7. a kind of graphene oxide of carried magnetic nano particle according to claim 1 is combined with conducting polymer
The preparation method of Fenton gels, it is characterised in that:In step 3, described alkaline solution is ammonia, sodium hydroxide, hydroxide
Potassium or calcium hydroxide, described alkaline solution concentration is 0.01 ~ 50 mg/mL, and alkaline solution is 10 with the solution B response time
min~3.0 h。
8. a kind of graphene oxide of carried magnetic nano particle according to claim 1 is combined with conducting polymer
The preparation method of Fenton gels, it is characterised in that:In step 3, the speed of Deca alkaline solution drop in described solution B
For 0.1 ~ 2.0 mL/min, time for adding is 1.0 ~ 10.0 min.
9. a kind of graphene oxide of carried magnetic nano particle according to claim 1 is combined with conducting polymer
The preparation method of Fenton gels, it is characterised in that:In step 4, described product C sublimation dryings are 1 ~ 20 day.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107670691A (en) * | 2017-09-21 | 2018-02-09 | 广州大学 | One kind is without heterogeneous class Fenton type catalyst of metal and preparation method and application |
CN109369911A (en) * | 2018-09-20 | 2019-02-22 | 哈尔滨工业大学 | A kind of preparation method of the Prussian blue@ferroso-ferric oxide@polypyrrole gel of raspberry structure |
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CN103341346A (en) * | 2013-06-26 | 2013-10-09 | 江苏省环境科学研究院 | Preparation method of manganese ferrite nanoparticle-graphene compound |
CN104190422A (en) * | 2014-09-22 | 2014-12-10 | 北京师范大学 | Heterogeneous light fenton catalyst and application thereof |
CN104998266A (en) * | 2015-06-30 | 2015-10-28 | 浙江师范大学 | Preparation and application of magnetic graphene oxide compound |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103341346A (en) * | 2013-06-26 | 2013-10-09 | 江苏省环境科学研究院 | Preparation method of manganese ferrite nanoparticle-graphene compound |
CN104190422A (en) * | 2014-09-22 | 2014-12-10 | 北京师范大学 | Heterogeneous light fenton catalyst and application thereof |
CN104998266A (en) * | 2015-06-30 | 2015-10-28 | 浙江师范大学 | Preparation and application of magnetic graphene oxide compound |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107670691A (en) * | 2017-09-21 | 2018-02-09 | 广州大学 | One kind is without heterogeneous class Fenton type catalyst of metal and preparation method and application |
CN107670691B (en) * | 2017-09-21 | 2020-04-14 | 广州大学 | Metal-free heterogeneous Fenton-like catalyst and preparation method and application thereof |
CN109369911A (en) * | 2018-09-20 | 2019-02-22 | 哈尔滨工业大学 | A kind of preparation method of the Prussian blue@ferroso-ferric oxide@polypyrrole gel of raspberry structure |
CN109369911B (en) * | 2018-09-20 | 2020-12-29 | 哈尔滨工业大学 | Preparation method of prussian blue @ ferroferric oxide @ polypyrrole gel with raspberry structure |
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