CN104226289B - A kind of Graphene/anionic clay composite photo-catalyst and preparation method thereof and application - Google Patents
A kind of Graphene/anionic clay composite photo-catalyst and preparation method thereof and application Download PDFInfo
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Abstract
The invention discloses a kind of Graphene/anionic clay composite photo-catalyst and preparation method thereof and application.Described preparation method comprises the following steps: after preparing graphene oxide solution and mixed salt solution, graphene oxide solution mixed with mixed salt solution；Then the carbamide of certain mass is joined in mixed solution, and back flow reaction of transferring to be hydrolyzed in electric heating device；Product centrifuge washing is with dried in 700～800 DEG C of calcinings, and grinding is sieved, and obtains described Graphene/anionic clay composite photo-catalyst.The present invention utilizes the growth masterplate that graphene oxide is anionic clay fast to prepare Graphene/anionic clay composite photo-catalyst, can be developed into the new catalyst being applied to efficiently simultaneously process Organic substance/Cr (VI) combined pollution under visible light, be of great immediate significance to realizing improvement organic wastewater Han chromium.
Description
Technical field
The invention belongs to environment functional material field, be specifically related to a kind of Graphene/anionic clay complex light and urge
Agent and preparation method thereof and application.
Background technology
The pollution containing chromium (typically Cr VI) organic wastewater is mostly derived from commercial pigments waste water, leather preparation gives up
Water, electroplating wastewater etc., this type of waste water its can biochemical treatment degree low, intractability is big.At present, senior oxygen
Catalyst used in change technology, often can only solely process organic contamination, and can not have both process simultaneously
The ability of the heavy metals such as Cr VI.Therefore, exploitation one effectively can process Organic substance under visible light simultaneously
The new catalyst of/Cr (VI) combined pollution, is of great immediate significance to realizing improvement organic wastewater Han chromium.
Photocatalysis technology be one at environment and the green technology of energy field extensive application prospect, tool can
Seeing that the composite photo-catalyst of photoactive new and effective multifunction is researched and developed is that on high-level oxidation technology grinds
Study carefully focus.
Carbon atom in Graphene is arranged in graphene planes with hexatomic ring form, so has four valency electricity
The C atom of son contributes the valency electron of a non-bonding.These valency electron are tied at the two dimensional crystal of monoatomic layer
Direction vertical with plane in structure forms the delocalization big π key of conjugation, and therefore electronics can move freely in crystal,
Graphene is caused to have the electronic conductivity energy of excellence.The excellent electric conductivity of Graphene make its photocatalysis,
Optical Electro-Chemistry field has a good application prospect, and can be used to manufacture and has semiconductor composite, the sun
Energy battery, ultracapacitor etc..Additionally, Graphene also has the mechanical performance of excellence and the high transmission to light
Property and high-specific surface area, can be used to prepare various functionalization composite based on Graphene.Graphene
Outstanding properties and workability thereof make it have good application prospect in fields such as photocatalysis, leading of its excellence
Electrical property, can walk light induced electron transporting with express delivery, efficiently separates light induced electron and photohole, fall
Their recombination probability low.
Anionic clay (anionic clay) is the stratified material formed by two or three metal hydroxides,
Can synthetic, its laminate positively charged, interlayer carries out charge balance by anion, therefore claims anionic clay.
Anionic clay has the lamellar compound of bigger specific surface and interlamellar spacing more flexibly, and some have light and urge
Change the metallic element of activity, such as ferrum, zinc, titanium, nickel etc., coprecipitation method can be passed through, generate and there is certain lattice
Structure, character metastable anionic clay photocatalyst.It addition, some aniones, such as Cr2O7 2-,
AsO2-, PO4 3-Anionic clay or calcining can be adsorbed onto by ion exchange or reconstruct effect etc. anion
After the interlayer of anionic clay.The Cr (VI) being enriched to material surface or anionic clay interlayer territory can be
Light induced electron provides electron acceptor, and suppression photohole and electronics are combined probability, and highly toxic Cr (VI) can
Can be reduced to hypotoxic Cr (III).
Summary of the invention
In place of shortcoming and defect for solution prior art, the primary and foremost purpose of the present invention is to provide a kind of graphite
The preparation method of alkene/anionic clay composite photo-catalyst.
Another object of the present invention is to the Graphene/anionic clay complex light providing above-mentioned preparation method to obtain
Catalyst.
It is still another object of the present invention to provide Graphene/anionic clay complex light that above-mentioned preparation method obtains
The application of catalyst.
For achieving the above object, the present invention adopts the following technical scheme that
The preparation method of a kind of Graphene/anionic clay composite photo-catalyst, comprises the following steps:
(1) add graphene oxide in deionized water, and stir and ultrasonic make graphene oxide fully dissolve,
Dispersion, obtains graphene oxide solution；Deionization is added by preparing the mixed metal salt needed for anionic clay
Stirring and dissolving in water, obtains mixed salt solution；Then graphene oxide solution is molten with mixed metal salt
Liquid mixes, and stirring is the most ultrasonic, makes metal cation pass through electrostatic interaction and fully adsorbs on graphene oxide,
Obtain the mixed solution of graphene oxide and metal ion；
(2) carbamide of certain mass is joined graphene oxide and metal ion that step (1) prepares
In mixed solution, be then transferred in electric heating device being hydrolyzed back flow reaction, make anionic clay crystal with
Graphene oxide is template slow crystalline growth in the above；Product is used deionized water centrifuge washing, is dried,
Obtain graphene oxide/anionic clay composite；
(3) graphene oxide step (2) obtained/anionic clay composite calcining, then grinds
And sieve, obtain described Graphene/anionic clay composite photo-catalyst.
Preferably, the graphene oxide solution concentration described in step (1) is 1.0～2.0g/L.
Preferably, step (1) is described prepare anionic clay needed for mixed metal salt be zinc salt and aluminium salt,
Or the mixing of zinc salt, nickel salt and aluminium salt.Can make one's options according to specific needs.
Preferably, in the mixed solution of step (1) described graphene oxide and metal ion, graphene oxide
Being 1:1～2:1 with the mol ratio of total metal ion, wherein graphene oxide molecular formula is reduced to C and calculates.
Preferably, step (1) is described by graphene oxide solution and the mixed stirring of mixed salt solution
Time is 12～24h, and ultrasonic time is 2～4h.
Preferably, the carbamide described in step (2) with formed total metal ion used by anionic clay mole
Than being (5.00～6.25): 1.00.
Preferably, step (2) described hydrolysis backflow refers to make mixed solution stably boil at 103～105 DEG C of constant temperature
Rise, steam condensing reflux 24～48h.
Preferably, step (3) described calcining is 700～800 DEG C of calcinings under vacuum or atmosphere of inert gases,；
Described sieving was the sieve of 200 mesh.During calcining, graphene oxide can be Graphene by thermal reduction.
It is furthermore preferred that described noble gas is nitrogen or argon.
Graphene/anionic clay composite photo-catalyst that above-mentioned preparation method obtains, wherein Graphene is compound
Mass content in photocatalyst is about 0.5%～1.0%.
Graphene/anionic clay composite photo-catalyst that above-mentioned preparation method obtains can be applicable under visible ray same
Step processes Organic substance/Cr (VI) combined pollution.
The principle of the present invention is: based on anionic clay to Cr2O7 2-The absorption property superpower etc. anion and stone
The ink alkene facilitation to anionic clay photocatalysis performance, this facilitation mainly shows themselves in that one is stone
Ink alkene has photosensitization to anionic clay photocatalyst, promotes its absorption rate to visible ray；Two are
Graphene can promote that to the super transporting capability of electronics anionic clay photocatalyst light induced electron and photoproduction are empty
The separation in cave.Meanwhile, the Cr of absorption2O7 2-Can promote further as electron acceptor etc. anion
Anionic clay photocatalyst light induced electron and the separation of photohole.Therefore, the graphite prepared by the present invention
Alkene/anionic clay composite can apply to synchronization process Organic substance/Cr (VI) combined pollution, the most organic dirt
Dye thing is by photocatalytic oxidation degradation, and highly toxic Cr (VI) is adsorbed is hypotoxic with photo catalytic reduction
Cr(III)。
Advantages of the present invention and beneficial effect:
Graphene oxide is first well-dispersed in water dissolution by the present invention, adds required metal ion and adds
In graphene oxide solution, in the adsorption of metal ions of positively charged to electronegative graphene oxide.Pass through
Hydrolysis, allows anionic clay in situ slowly growth on graphene oxide, obtain graphene oxide/the moon from
Sub-clay composite material, then calcine through vacuum high-temperature, during this vacuum calcining, graphene oxide heat
It is reduced to Graphene, forms Graphene/anionic clay composite photo-catalyst.Compared with prior art, this
Bright simplify synthesis technique, optimize anionic clay materials, prepare low cost, anion that yield is high
Clay/graphite alkene composite photo-catalyst.
Accompanying drawing explanation
Fig. 1 is the Graphene/ZnAl anionic clay composite photo-catalyst outside drawing of embodiment 1 preparation.
Fig. 2 is the XRD figure of the Graphene/ZnAl anionic clay composite photo-catalyst of embodiment 1 preparation.
Fig. 3 is the TEM figure of the Graphene/ZnAl anionic clay composite photo-catalyst of embodiment 1 preparation.
Fig. 4 is that the composite catalyst of embodiment 1 preparation is under visible light to methylene blue and the removal of Cr (VI)
Effect.
Fig. 5 is the Raman of the Graphene/ZnNiAl anionic clay composite photo-catalyst of embodiment 2 preparation
Figure.
Fig. 6 is that the composite catalyst of embodiment 2 preparation is under visible light to methylene blue and the removal of Cr (VI)
Effect.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but the embodiment party of the present invention
Formula is not limited to this.
Embodiment 1
A kind of can apply to processes the Graphene/anionic clay composite photocatalyst containing chromium organic wastewater under visible ray
The preparation of agent (Graphene/ZnAl anionic clay composite photo-catalyst), comprises the following steps:
(1) (used graphene oxide powder is by literary composition accurately to weigh 0.1g graphene oxide powder
Offer the improvement Hummers method reported for work prepare (Marcano, D.C., Kosynkin, D.V., et al., 2010.
Improved Synthesis of Graphene Oxide.Acs Nano, 4 (8): 4806-4814.)) join equipped with
In the 500mL three neck round bottom flask of 100mL deionized water, through sufficient magnetic agitation and supersound process
(the most about 12h) so that graphene oxide is completely dispersed into brownish black transparent colloidal solution, obtains aoxidizing stone
Ink alkene solution；
Accurately weigh Zn (NO3)2·6H2O 17.85g (0.060mol), Al (NO3)3·9H2O 7.50g(0.02
Mol), NaNO30.85g (0.01mol) joins in 125mL deionized water, stirs and ultrasonic makes it dissolve (this
Time gained mixing salt solution metal cation molar concentration Zn:Al=3:1), obtain mixed salt solution；
Graphene oxide solution and mixed salt solution are mixed in 500mL three neck round bottom flask, passes through
Magnetic agitation 12h, supersound process 4h, metal ion is enriched on graphene oxide, obtains graphene oxide
With the mixed solution of metal ion, now graphene oxide is about 1:1 with the mol ratio of total metal ion；
(2) accurately weigh carbamide 24.02g (0.4mol), join that step (1) obtains equipped with metal from
Son is with the three neck round bottom flask of the mixed solution of graphene oxide, and carbamide is then transferred in electric jacket after dissolving
Carrying out constant temperature 103 DEG C to boil, be hydrolyzed back flow reaction 24h；The product deionized water 4000 that will obtain
Rpm centrifuge washing 5 times, 50 DEG C of vacuum drying 12h, obtain graphene oxide/anionic clay composite；
(3) graphene oxide/anionic clay composite that step (2) is obtained under vacuum 800
DEG C calcining, ground 200 mesh sieves of product after calcining, obtain described Graphene/anionic clay complex light and urge
Agent, the Graphene content in obtained composite photo-catalyst is about 0.5wt% and (utilizes TG-DSC same
Step thermal analyzer records).(in the catalyst now obtained, Graphene is by step with the mass ratio of anionic clay
Suddenly the amount of the graphene oxide that (1) weighs and determine)
The outward appearance of embodiment 1 final products as it is shown in figure 1, as can be seen from FIG., gained Graphene/anion
The most fluffy easy mill of clay composite photo-catalyst quality.
The X-ray diffraction (XRD) of embodiment 1 final products can be found in Fig. 2, as can be seen from FIG. 2 θ=
30-40 ° is ZnAl2O4Characteristic peak, ZnAl2O4Light-catalyzed reaction plays a leading role.Due to Graphene
Content relatively low, this XRD figure fails to demonstrate the characteristic peak of Graphene.
The transmission electron microscope (TEM) of embodiment 1 final products can be found in Fig. 3, it can be clearly seen that forge from figure
After burning, anionic clay is attached on Graphene.During light-catalyzed reaction, Graphene can preferably transporting
Light induced electron.
Take the prepared Graphene/ZnNiAl anionic clay composite photo-catalyst of 0.05g embodiment 1 to join
100mL contains 10mg/L methylene blue and 10mg/L K2Cr2O7Mixed solution in, magnetic agitation.300
The xenon lamp (PLS-SXE) of W is visible light source, and optical filter filters off the light of λ < 420nm.This composite photo-catalyst
To the removal effect of methylene blue and Cr (VI) as shown in Figure 4, as can be seen from FIG., methylene blue can be by light
Catalytic degradation degradation and decolorization, and highly toxic Cr (VI) was adsorbed to Graphene/ZnNiAl anionic clay before this
Composite photo-catalyst, is re-used as electron acceptor absorbing light elder generation electronics, thus is reduced to the Cr (III) of low toxicity.
Embodiment 2
A kind of can apply to processes the Graphene/anionic clay composite photocatalyst containing chromium organic wastewater under visible ray
The preparation of agent (Graphene/ZnNiAl anionic clay composite photo-catalyst), comprises the following steps:
(1) (used graphene oxide powder is by literary composition accurately to weigh 0.2g graphene oxide powder
Offer the improvement Hummers method reported for work prepare (Marcano, D.C., Kosynkin, D.V., et al., 2010.
Improved Synthesis of Graphene Oxide.Acs Nano, 4 (8): 4806-4814.)) join equipped with
In the 500mL three neck round bottom flask of 100mL deionized water, through sufficient magnetic agitation and supersound process
(the most about 12h) so that graphene oxide is completely dispersed into brownish black transparent colloidal solution, obtains aoxidizing stone
Ink alkene solution；
Accurately weigh Zn (NO3)2·6H2O 13.39g (0.045mol), Ni (NO3)2·6H2O 4.36g(0.015
Mol), Al (NO3)3·9H2O 7.50g (0.02mol), NaNO30.85g (0.01mol) joins 125mL
In deionized water, stir and ultrasonic make dissolving metal salts (now gained mixing salt solution metal cation mole is dense
Degree Zn:Ni:Al=9:3:4, M (II): M (III)=3:1), obtain mixed salt solution；
Graphene oxide solution and mixed salt solution are mixed in 500mL three neck round bottom flask, passes through
Magnetic agitation 24h, supersound process 2h, metal ion is enriched on graphene oxide, obtains graphene oxide
With the mixed solution of metal ion, now graphene oxide is about 2:1 with the mol ratio of total metal ion；
(2) accurately weigh carbamide 30.03g (0.5mol), join that step (1) obtains equipped with metal from
Son is with the three neck round bottom flask of the mixed solution of graphene oxide, and carbamide is then transferred in electric jacket after dissolving
Carrying out constant temperature 105 DEG C to boil, be hydrolyzed back flow reaction 48h；The product deionized water 4000 that will obtain
Rpm centrifuge washing 5 times, 50 DEG C of vacuum drying 12h, obtain graphene oxide/anionic clay composite；
(3) graphene oxide/anionic clay composite that step (2) is obtained under vacuum 700
DEG C calcining, ground 200 mesh sieves of product after calcining, obtain described Graphene/anionic clay complex light and urge
Agent.The obtained Graphene content in composite photo-catalyst is about 1.0wt% and (utilizes TG-DSC same
Step thermal analyzer records).
The Raman figure of the final products Graphene of embodiment 2/ZnNiAl anionic clay composite photo-catalyst
Can be found in Fig. 5, as can be seen from FIG. 1331 and 1593cm-1Two peak-to-peak signals at place are originated from material with carbon element
A1gBreathing pattern (the breathing mode of point photons of A of point of symmetry vibration quantum1g
And the sp of carbon atom symmetry)2One-level scattering (the first order scattering of E of key E1g vibration quantum1g
phonon of sp2C atoms), D band and the G of the most corresponding Graphene in the two peak carry.Anionic clay exists
Raman spectrum does not goes out peak.
Comparing embodiment 1, embodiment 2 adds Ni element in preparation process, and the incorporation of Ni can promote
The utilization rate of visible ray in photocatalytic process, thus improve the treatment effeciency containing chromium organic wastewater, but reaction
During have the dissolution of trace Ni, cause secondary pollution.Accordingly, it would be desirable to consider whether as the case may be
Mix Ni element.
Take the prepared Graphene/ZnNiAl anionic clay composite photo-catalyst of 0.05g embodiment 2 to join
100mL contains 10mg/L methylene blue and 10mg/L K2Cr2O7Mixed solution in, magnetic agitation.300
The xenon lamp (PLS-SXE) of W is visible light source, and optical filter filters off the light of λ < 420nm.This composite photo-catalyst
To the removal effect of methylene blue and Cr (VI) as shown in Figure 6, as can be seen from FIG., methylene blue can be by light
Catalytic degradation degradation and decolorization, and highly toxic Cr (VI) was adsorbed to Graphene/ZnNiAl anionic clay before this
Composite photo-catalyst, is re-used as electron acceptor absorbing light elder generation electronics, thus is reduced to the Cr (III) of low toxicity.?
In embodiment 2, it is (corresponding real that methylene blue can be higher than embodiment 1 by the speed of photocatalytic degradation degradation and decolorization
Execute example 1 Fig. 4), mix that promote can absorbing of seeing of light owing to Ni.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-mentioned reality
Execute the restriction of example, the change made under other any spirit without departing from the present invention and principle, modification,
Substitute, combine, simplify, all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (8)
1. the preparation method of Graphene/anionic clay composite photo-catalyst, it is characterised in that include with
Lower step:
(1) add graphene oxide in deionized water, and stirring makes graphene oxide fully dissolve with ultrasonic
Dispersion, obtains graphene oxide solution；Deionization is added by preparing the mixed metal salt needed for anionic clay
Stirring and dissolving in water, obtains mixed salt solution；Then graphene oxide solution is molten with mixed metal salt
Liquid mixes, and stirring is the most ultrasonic, obtains the mixed solution of graphene oxide and metal ion；
(2) carbamide of certain mass is joined graphene oxide and metal ion that step (1) prepares
In mixed solution, be then transferred in electric heating device being hydrolyzed back flow reaction, make anionic clay crystal with
Graphene oxide is template crystalline growth in the above；Product is used deionized water centrifuge washing, is dried,
To graphene oxide/anionic clay composite；
(3) graphene oxide step (2) obtained/anionic clay composite calcining, then grinds
And sieve, obtain described Graphene/anionic clay composite photo-catalyst；
Step (1) is described prepare anionic clay needed for mixed metal salt be zinc salt and aluminium salt, or zinc salt,
Nickel salt and the mixing of aluminium salt；
In the mixed solution of step (1) described graphene oxide and metal ion, graphene oxide and total metal
The mol ratio of ion is 1:1～2:1, and wherein graphene oxide molecular formula is reduced to C and calculates.
Preparation method the most according to claim 1, it is characterised in that the oxidation described in step (1)
Graphene solution concentration is 1.0～2.0g/L.
Preparation method the most according to claim 1, it is characterised in that step (1) is described will oxidation
Graphene solution and the mixed mixing time of mixed salt solution are 12～24h, and ultrasonic time is 2～4h.
Preparation method the most according to claim 1, it is characterised in that step (2) described hydrolysis is returned
Stream refers to make mixed solution stably seethe with excitement at 103～105 DEG C of constant temperature, steam condensing reflux 24～48h.
Preparation method the most according to claim 1, it is characterised in that the carbamide described in step (2)
It is (5.00～6.25) with the mol ratio of the total metal ion formed used by anionic clay: 1.00.
Preparation method the most according to claim 1, it is characterised in that step (3) described calcining is
700～800 DEG C of calcinings under vacuum or atmosphere of inert gases；Described sieving was the sieve of 200 mesh.
7. Graphene/anionic clay composite photo-catalyst, it is characterised in that by claim 1～6
Described in any one preparation method obtain, wherein Graphene mass content in composite photo-catalyst be 0.5%～
1.0%.
8. Graphene described in claim 7/anionic clay composite photo-catalyst synchronization process under visible light has
Application in machine thing/Cr (VI) combined pollution；Described Organic substance is methylene blue.
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| CN105327694A (en) * | 2015-11-01 | 2016-02-17 | 华南理工大学 | Fullerene/anionic clay compound photocatalyst and preparation method and application thereof |
| CN105289578A (en) * | 2015-11-24 | 2016-02-03 | 华南理工大学 | Metal oxide/carbon nanotube composite photocatalyst, and preparation method and application thereof |
| CN105618089B (en) * | 2016-01-20 | 2018-09-14 | 华南理工大学 | A kind of Ag@AgCl modification fullerene/anionic clay composite photo-catalyst and its preparation and application |
| CN109569561A (en) * | 2018-11-22 | 2019-04-05 | 华南农业大学 | A kind of graphene/ZnAlTi hydrotalcite-like composite material and its preparation method and application |
| CN113979786B (en) * | 2021-10-26 | 2023-03-21 | 宜宾五粮液股份有限公司 | Graphene composite pottery jar and preparation method thereof |
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| CN103107023A (en) * | 2013-03-06 | 2013-05-15 | 江南大学 | Preparation method of graphene/zinc-aluminium oxide composite material and application of composite material in super capacitor |
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