CN106215862A - A kind of preparation method and applications of iron oxyhydroxide/graphenoxide oxide composite material - Google Patents
A kind of preparation method and applications of iron oxyhydroxide/graphenoxide oxide composite material Download PDFInfo
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- CN106215862A CN106215862A CN201610821003.0A CN201610821003A CN106215862A CN 106215862 A CN106215862 A CN 106215862A CN 201610821003 A CN201610821003 A CN 201610821003A CN 106215862 A CN106215862 A CN 106215862A
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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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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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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
- C02F2101/36—Organic compounds containing halogen
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Abstract
The present invention relates to the preparation method and applications of a kind of iron oxyhydroxide/graphenoxide oxide composite material.Iron oxyhydroxide/graphenoxide oxide composite material is that the suspension of the suspension by graphene oxide and FeOOH is composited by hydro-thermal method after according to volume ratio 1:1～2 mixing, dispersion.Prepared iron oxyhydroxide/graphenoxide oxide composite material is used for the process of phenol wastewater, take FeOOH/graphene oxide composite adsorption material 0.5～5g put into 1000ml containing in the waste water that parachlorophenol concentration is 10～60mg/l, constant-temperature table fully shakes, control water temperature at 25 DEG C, by waste water filtering after reaction 3h, detection parachlorophenol clearance is 87～93.2%, and water outlet chlorophenol concentration is 1.3～5.2mg/l, and adsorbance is 11～17.4mg/l.
Description
Technical field
The present invention relates to technical field of water pollution control, be specifically related to a kind of FeOOH/graphene oxide composite wood
The preparation method of material and the application in water processes thereof.
Background technology
Along with developing rapidly of chemical industry, organochlorine compound medicine, agricultural supplie, textile, household chemicals and
The fields such as public health also result in serious environmental pollution while being widely applied.Many organochlorine compound toxicity
Greatly, difficult for biological degradation, long half time, having " three cause effect " and genetoxic, these organochlorine compounds are the most long-term
Residual can impact and then endanger the health of various biology and human body to environment.
Chlorophenols aromatic compound is a quasi-representative organochlorine compound, can be to various biological generations after entering in environment
Toxic action, can cause the destruction of whole ecosystem time serious.Research the most in recent years shows, most of chlorophenols compounds
It is incretion interferent or potential incretion interferent, when they long-term existence are in organism, biology can be caused
Various biologies and human reproductive system can be caused murder by poisoning impact, even if also can be to life at low concentration by the endocrine regulation of body
Object works the mischief.Research shows that chlorophenol can produce toxic action to aquatile.When the concentration in fresh water or ocean reaches 1～10
Aquatile will be produced acute virus action during μ g/L.
In environment, chlorophenols is essentially from the most synthetically produced in environment, the degraded of chlorinated organics, processing or clean
Side-product in metallization processes and the chlorine-containing compound of synthetic.
The control major control of China's parachlorophenol is in field of water pollution control at present.According to China's " surface water environment quality
Standard " regulation of (GB 3,838 2002), the maximum permissible concentration of surface water V class volatile phenol in water is 0.1mg/L；China
In " Drinking Water water standard " (GB5749 2006), in regulation Drinking Water, volatile phenol concentration is less than 0.002mg/
L；China " urban water supply water standard " (CJ/T206 2005) regulation chlorophenol total amount (include 2 monochlorphenols, 2,4 one Dichlorophenols, 2,
4,6 one trichlorophenols) must not exceed 0.01mg/L.
At present conventional control chlorophenol pollutant method have chemical oxidization method, photocatalysis, membrane separation process, biological degradation method,
Absorption method etc..Chemical oxidization method uses strong oxidizer such as O3, Fenton reagent etc. carry out oxidation processes, Phenol-Containing Wastewater Treatment effect
The most still oxidant cost is high and technical equipment requires height；Photocatalytic oxidation produces hydroxyl radical free radical by catalysis and aoxidizes
Chlorophenol, although this method high treating effect and response time are short, but may produce in some processing procedure toxicity bigger in
Between product so that chemical Treatment chlorinated phenol is difficult to be used widely；Membrane separation process is to be processed containing phenol by synthesis membrane filtration
Waste water, but film is the most blocked after long-play, causes the penetrating amount of film to decline, and membrane module often to be changed, and causes fortune
Row cost is high, and these problems make membrane separation technique have certain limitation in actual applications；Biochemical method phenol wastewater
Though low cost, non-secondary pollution, biosystem treatment effeciency is low, and the poor stability of operation limits Biochemical method and contains
The application of phenol waste water.Absorption method Phenol-Containing Wastewater Treatment will not be affected by the water yield, impact, has operating cost low, without middle
Product produces, efficient advantage, uses absorption method Phenol-Containing Wastewater Treatment can overcome above numerous shortcoming.
Absorption method processes the material category of chlorophenol much at present, if carbon matrix is the activated carbon of master, carbon fiber etc., organic
Thing/high polymer is main resin, chitosan microball etc. and based on the montmorillonite of inorganic mineral substrate, brucite etc..
This law provides a kind of method being carried out Phenol-Containing Wastewater Treatment by FeOOH and graphene oxide composite material, oxidation
Graphene is a kind of Graphene derivative, is a kind of novel two-dimension nano materials, huge specific surface area and substantial amounts of oxygen-containing
Functional group becomes adsorbent of good performance.The nano material of two dimension is susceptible to irreversible stacking in actual applications
And there is agglomerate, graphene oxide is modified by this law by FeOOH so that it is become the excellent of stable performance
Water treatment absorbent, effective Phenol-Containing Wastewater Treatment.
Summary of the invention:
It is an object of the invention to provide the preparation method of a kind of iron oxyhydroxide/graphenoxide oxide composite material and answered
For Phenol-Containing Wastewater Treatment.
The technical scheme that the present invention takes is realized by following steps:
A kind of iron oxyhydroxide/graphenoxide oxide composite material is the suspension by graphene oxide and FeOOH
Suspension is composited by hydro-thermal method after according to volume ratio 1:1～2 mixing, dispersion.
FeOOH component in a kind of iron oxyhydroxide/graphenoxide oxide composite material is to utilize hydro-thermal method by Fe
(NO3)3`2H2O with NaOH adds in 100ml deionized water according to mass ratio 0.5～1.2:1 and mixes 30min, at 120～150 DEG C
Baking oven in keep 24 hours, after centrifugal drying prepare.
Graphite oxide in a kind of iron oxyhydroxide/graphenoxide oxide composite material is graphite powder with potassium permanganate according to matter
Amount ratio 1:1～3, adds concentrated sulphuric acid and the nitration mixture that strong phosphoric acid volume ratio is 6～8:1,50 DEG C of heating in water bath 2h, prepares.
A kind of composite steps of iron oxyhydroxide/graphenoxide oxide composite material:
(1) take the oxidation graphite solid of 1g, add 50ml deionized water, disperse 5～10min, i.e. prepare mass body integration
Number is about the graphene oxide suspension of 0.02g/ml；
(2) by taking the FeOOH of 0.5～1g in 50ml deionized water, disperse 5min, i.e. prepare mass body integration
Several 0.1～the suspension of 0.2g/ml FeOOH；
(3) finely dispersed FeOOH suspension is joined in the most scattered graphene oxide suspension, and
Mixed liquor is disperseed 5～10min, the baking oven of 120 DEG C keeps 12～24h, after centrifugal drying, i.e. prepares described composite.
Above-mentioned graphene oxide is combined with the electrostatic force between FeOOH group by group on Graphene and forms hydroxyl
Base ferrum oxide/graphene oxide composite material.
Prepared iron oxyhydroxide/graphenoxide oxide composite material is used for the process of phenol wastewater, specifically comprises the following steps that
Take FeOOH/graphene oxide composite adsorption material 0.5～5g put into 1000ml containing parachlorophenol concentration be 10～
In the waste water of 60mg/l, fully shaking on constant-temperature table, control water temperature is at 25 DEG C, and by waste water filtering after reaction 3h, it is right to detect
Chlorophenol clearance is 87～93.2%, and water outlet chlorophenol concentration is 1.3～5.2mg/l, and adsorbance is 11～17.4mg/l.
Iron oxyhydroxide/graphenoxide oxide composite material prepared by the present invention has the advantage that
1, graphene oxide and the recombination energy of FeOOH in iron oxyhydroxide/graphenoxide oxide composite material of the present invention
Being prevented effectively from the agglomerate of graphene oxide, graphene oxide can effectively keep two-dimensional structure；
2, the graphene oxide that the present invention uses is the Graphene of moderate oxidation, has abundant oxy radical and bigger
Specific surface area, can efficient absorption chlorophenol；
3, in iron oxyhydroxide/graphenoxide oxide composite material, FeOOH, as substrate, has certain absorption and oxygen
Change effect, can adsorb and oxidized portion chlorophenol.
Detailed description of the invention
Embodiment 1
Graphite powder and potassium permanganate are according to mass ratio 1:1, and adding sulphuric acid with phosphoric acid volume ratio is the nitration mixture of 8:1,50 DEG C of water
Bath heating 2h.Will oxidation after graphite filter, dry, pulverize standby.
Graphite oxide quality and deionized water volume are pressed 1g:50ml, mixes, disperse 5～10min to prepare 0.02g/ml's
The suspension of graphene oxide.
By Fe (NO3)3`2H2O with NaOH adds in 100ml deionized water according to thing mass ratio 1.2:1 and mixes 30min,
The baking oven of 150 DEG C keeps 24 hours preparing.
Being mixed according to 0.5g:50ml with deionized water volume by prepared hydroxyl oxidize weight of iron, dispersion 5min prepares 0.1g/
The FeOOH suspension of ml.Finely dispersed FeOOH suspension is joined the most scattered graphene oxide hang
In turbid liquid, and mixed liquor is disperseed 5～10min, the baking oven of 120 DEG C keeps 24h.
Prepared iron oxyhydroxide/graphenoxide oxide composite material is used for the process of phenol wastewater, specifically comprises the following steps that
Take FeOOH/graphene oxide composite adsorption material 0.5g input 1000ml is the useless of 10mg/l containing parachlorophenol concentration
In water, fully shaking on constant-temperature table, waste water filtering, at 25 DEG C, is filtered after reaction 3h by control water temperature, water outlet chlorophenol concentration
At 1.3mg/l, adsorbance is 17.4mg/g.Detection parachlorophenol clearance is 87%
Embodiment 2
Graphite powder and potassium permanganate are according to mass ratio 1:2, and adding sulphuric acid with phosphoric acid volume ratio is the nitration mixture of 7:1,50 DEG C of water
Bath heating 2h.Will oxidation after graphite filter, dry, pulverize standby.
Graphite oxide quality is mixed by 1g:50ml with deionized water volume, disperses 5～10min to prepare 0.02g/ml's
The suspension of graphene oxide.
By Fe (NO3)3`2H2O with NaOH adds in 100ml deionized water according to thing mass ratio 1:1 and mixes 30min, 120
DEG C baking oven in keep 24 hours prepare.
Being mixed according to 1g:50ml with deionized water volume by prepared hydroxyl oxidize weight of iron, dispersion 5min prepares 0.2g/ml
FeOOH suspension.Finely dispersed FeOOH suspension is joined the most scattered graphene oxide suspended
In liquid, and mixed liquor is disperseed 5～10min, the baking oven of 120 DEG C keeps 24h.
Prepared iron oxyhydroxide/graphenoxide oxide composite material is used for the process of phenol wastewater, specifically comprises the following steps that
Take FeOOH/graphene oxide composite adsorption material 3g input 1000ml is the waste water of 50mg/l containing parachlorophenol concentration
In, constant-temperature table fully shakes, waste water filtering, at 25 DEG C, is filtered after reaction 3h by control water temperature, water outlet chlorophenol concentration exists
3.4mg/l, adsorbance is 15.5mg/g.Detection parachlorophenol clearance is 93.2%
Embodiment 3
Graphite powder and potassium permanganate are according to mass ratio 1:3, and adding sulphuric acid with phosphoric acid volume ratio is the nitration mixture of 6:1,50 DEG C of water
Bath 2h.Will oxidation after graphite filter, dry, pulverize standby.
Graphite oxide quality and deionized water volume are pressed 1g:50ml, mixes, disperse 5～10min to prepare 0.02g/ml's
The suspension of graphene oxide.
By Fe (NO3)3`2H2O with NaOH adds in 100ml deionized water according to thing mass ratio 0.5:1 and mixes 30min,
The baking oven of 120 DEG C keeps 24 hours preparing.
Being mixed according to 1g:50ml with deionized water volume by prepared hydroxyl oxidize weight of iron, dispersion 5min prepares 0.2g/ml
FeOOH suspension.Finely dispersed FeOOH suspension is joined the most scattered graphene oxide suspended
In liquid, and mixed liquor is disperseed 5～10min, the baking oven of 120 DEG C keeps 24h.
Prepared iron oxyhydroxide/graphenoxide oxide composite material is used for the process of phenol wastewater, specifically comprises the following steps that
Take FeOOH/graphene oxide composite adsorption material 5g input 1000ml is the waste water of 60mg/l containing parachlorophenol concentration
In, constant-temperature table fully shakes, waste water filtering, at 25 DEG C, is filtered after reaction 3h by control water temperature, water outlet chlorophenol concentration exists
5.2mg/l, adsorbance is 11mg/g.Detection parachlorophenol clearance is 91.3%.
The present invention is open and the preparation method of a kind of iron oxyhydroxide/graphenoxide oxide composite material that proposes and at water
Application in process, those skilled in the art can suitably change the links such as condition route realize by using for reference present disclosure, although
The method of the present invention and technology of preparing are described by preferred embodiment, person skilled substantially can without departing from
In present invention, spirit and scope, methods and techniques described herein route is modified or reconfigures, realize
Whole technology of preparing.Special needs to be pointed out is, all similar replacements and change are aobvious for a person skilled in the art
And be clear to, they are considered as being included in present invention spirit, scope and content.
Claims (5)
1. the preparation method of an iron oxyhydroxide/graphenoxide oxide composite material；It is characterized in that by graphene oxide is suspended
The suspension of liquid and FeOOH is composited by hydro-thermal method after according to volume ratio 1:1～2 mixing, dispersion.
2. the method for claim 1, is characterized in that FeOOH component is to utilize hydro-thermal method by Fe (NO3)3`2H2O with
NaOH adds according to mass ratio 0.5～1.2:1 and mixes 30min in 100ml deionized water, keeps in the baking oven of 120～150 DEG C
24 hours, prepare after centrifugal drying.
3. the method for claim 1, it is characterized in that graphite oxide be graphite powder with potassium permanganate according to mass ratio 1:1～
3, add concentrated sulphuric acid and the nitration mixture that strong phosphoric acid volume ratio is 6～8:1,50 DEG C of heating in water bath 2h prepare.
4. the method for claim 1, is characterized in that step is as follows:
1) take the oxidation graphite solid of 1g, add 50ml deionized water, disperse 5～10min, i.e. prepare mass body fraction and be about
The graphene oxide suspension of 0.02g/ml；
2) by taking the FeOOH of 0.5～1g in 50ml deionized water, disperse 5min, i.e. prepare mass body fraction 0.1
～the suspension of 0.2g/ml FeOOH；
3) finely dispersed FeOOH suspension is joined in the most scattered graphene oxide suspension, and will mixing
Liquid dispersion 5～10min, keeps 12～24h in the baking oven of 120 DEG C, i.e. prepares described composite after centrifugal drying.
5. utilize iron oxyhydroxide/graphenoxide oxide composite material to carry out the processing method of phenol wastewater, it is characterized in that taking hydroxyl
What ferrum oxide/graphene oxide composite adsorption material 0.5～5g put into 1000ml is 10～60mg/l containing parachlorophenol concentration
In waste water, shaking on constant-temperature table, control water temperature is at 25 DEG C, and by waste water filtering after reaction 3h, detection parachlorophenol clearance is
87～93.2%, water outlet chlorophenol concentration is 1.3～5.2mg/l, and adsorbance is 11～17.4mg/l.
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Cited By (8)
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| CN107855129A (en) * | 2017-11-23 | 2018-03-30 | 安徽大学 | A kind of preparation method and applications of high-performance molybdenum disulfide/graphene oxide/iron oxide yellow composite catalyst |
| CN108057422A (en) * | 2017-12-14 | 2018-05-22 | 中国科学院生态环境研究中心 | A kind of alcohol bridging enhancing porous hydroxyapatite iron oxide-graphene nano composite hydrogel and preparation method and application |
| CN108424617A (en) * | 2018-03-15 | 2018-08-21 | 厦门大学 | A kind of preparation method and applications of iron oxide hydroxide load graphene oxide fire retardant |
| CN110026153A (en) * | 2019-01-18 | 2019-07-19 | 闽南师范大学 | A kind of synthetic method and absorption property of graphene oxide-samaric hydroxide composite material |
| CN110026152A (en) * | 2019-01-18 | 2019-07-19 | 闽南师范大学 | A kind of graphene oxide-europium hydroxide composite material, preparation method and applications |
| CN110787771A (en) * | 2019-10-25 | 2020-02-14 | 天津大学 | Modified blue algae biochar and preparation method and application thereof |
| CN111139637A (en) * | 2020-01-06 | 2020-05-12 | 江南大学 | Coated fabric substrate and preparation method and using method thereof |
| CN114042387A (en) * | 2022-01-10 | 2022-02-15 | 中国科学院宁波材料技术与工程研究所 | Photocatalytic degradation dye wastewater separation multilayer composite membrane and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107855129A (en) * | 2017-11-23 | 2018-03-30 | 安徽大学 | A kind of preparation method and applications of high-performance molybdenum disulfide/graphene oxide/iron oxide yellow composite catalyst |
| CN108057422A (en) * | 2017-12-14 | 2018-05-22 | 中国科学院生态环境研究中心 | A kind of alcohol bridging enhancing porous hydroxyapatite iron oxide-graphene nano composite hydrogel and preparation method and application |
| CN108424617A (en) * | 2018-03-15 | 2018-08-21 | 厦门大学 | A kind of preparation method and applications of iron oxide hydroxide load graphene oxide fire retardant |
| CN110026153A (en) * | 2019-01-18 | 2019-07-19 | 闽南师范大学 | A kind of synthetic method and absorption property of graphene oxide-samaric hydroxide composite material |
| CN110026152A (en) * | 2019-01-18 | 2019-07-19 | 闽南师范大学 | A kind of graphene oxide-europium hydroxide composite material, preparation method and applications |
| CN110787771A (en) * | 2019-10-25 | 2020-02-14 | 天津大学 | Modified blue algae biochar and preparation method and application thereof |
| CN111139637A (en) * | 2020-01-06 | 2020-05-12 | 江南大学 | Coated fabric substrate and preparation method and using method thereof |
| CN114042387A (en) * | 2022-01-10 | 2022-02-15 | 中国科学院宁波材料技术与工程研究所 | Photocatalytic degradation dye wastewater separation multilayer composite membrane and preparation method and application thereof |
| CN114042387B (en) * | 2022-01-10 | 2022-04-26 | 中国科学院宁波材料技术与工程研究所 | Photocatalytic degradation dye wastewater separation multilayer composite membrane and preparation method and application thereof |
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