CN106824081A - A kind of Graphene titanium dioxide attapulgite composite material and its preparation method and application - Google Patents
A kind of Graphene titanium dioxide attapulgite composite material and its preparation method and application Download PDFInfo
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- CN106824081A CN106824081A CN201710128711.0A CN201710128711A CN106824081A CN 106824081 A CN106824081 A CN 106824081A CN 201710128711 A CN201710128711 A CN 201710128711A CN 106824081 A CN106824081 A CN 106824081A
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- titanium dioxide
- graphene
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- attapulgite composite
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 77
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 42
- 229960000892 attapulgite Drugs 0.000 title claims abstract description 38
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 38
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000725 suspension Substances 0.000 claims abstract description 24
- 239000002689 soil Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000010936 titanium Substances 0.000 claims description 33
- 229910052719 titanium Inorganic materials 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 10
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 9
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000012286 potassium permanganate Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000010865 sewage Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 28
- 230000001699 photocatalysis Effects 0.000 abstract description 17
- 238000010521 absorption reaction Methods 0.000 abstract description 10
- 241000233866 Fungi Species 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 235000011167 hydrochloric acid Nutrition 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 150000008282 halocarbons Chemical class 0.000 description 2
- 150000002391 heterocyclic compounds Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 231100000611 venom Toxicity 0.000 description 1
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—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 surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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Abstract
The present invention discloses a kind of Graphene titanium dioxide attapulgite composite material and its preparation method and application.The method includes：Prepare graphene oxide aaerosol solution；Prepare titanium dioxide suspension；Using hydro-thermal reaction method is by graphene oxide aaerosol solution, titanium dioxide suspension and concavo-convex is mixed to get Graphene titanium dioxide attapulgite composite material.The present invention is combined by the Graphene and titanium dioxide with elite clone performance and with the big recessed soil of specific surface area, comprehensive three kinds of advantages of material, prepare the Graphene titanium dioxide attapulgite composite material with electron conductivity high, high recyclability, high-specific surface area, high absorption capacity, high intensity, photocatalytic effect high and removing other fungus and purifying ability high；The method preparation cost is low, and operation is simple, is conducive to the carrying out of large-scale production.
Description
Technical field
Present invention relates particularly to a kind of Graphene-titanium dioxide-attapulgite composite material and its preparation method and application.
Background technology
Photocatalyst is a kind of photosemiconductor material with photo-catalysis function, is most safe and most clean in the world at present
Surrounding purifying material.It has a low energy consumption, catalytic rate high, long service life, reusable, the features such as sterilized, purification, extensively
Apply to the fields such as sterilization engineering, greasy dirt degraded engineering, cleaning project.Stability that photocatalyst is shown in application process and
Reliability is gradually accepted by everybody, is a kind of new surrounding purifying material.Produced as new type purification industry is related to new purification
Product are continued to bring out, and photocatalyst excellent degradation characteristic and photocatalysis characteristic be increasingly becoming the main material of the large-scale depollution of environment.
The relational expression K=1240/Eg of light absorbs threshold value and band gap according to photocatalyst（Wherein K is light absorbs threshold value, and Eg is band gap）And sky
Cave electrons spread equation：t=d2/k2D（D is particle diameter, and k is constant, and D is diffusion coefficient）, show the width of photocatalytic semiconductor material
The big degree of band gap determines light absorption wavelength threshold value, and particle diameter determines the probability of electronics and hole-recombination.Therefore, the more band is more carried out
The photocatalytic semiconductor material that gap is small, particle diameter is big is applied to the research and production of the depollution of environment.But photocatalytic semiconductor material
Bigger its specific surface area of particle diameter is just smaller, is unfavorable for that object is contacted with catalyst.Simultaneously pure photocatalytic semiconductor material light
Ripple absorption region is small, specific surface area is small, and solar energy absorptivity is low under natural light, reduces photocatalysis efficiency.Due also to receiving
Rice catalysis material is small-sized, and the electron hole pair that photocatalysis is produced easily is combined again, reduces discomposing effect.Meanwhile, mesh
The synthetic method that preceding people prepare optic catalytic composite material is more complicated and cumbersome, and accessory substance is more, and the property of can be recycled is poor, only
Change harmful substance species few.Secondly, the price for reacting used titanium source is high, reduce optic catalytic composite material performance and
Practical value.Under study for action, preferably, its oxidability is strong, and stable chemical nature is nontoxic for the photocatalysis effect of titanium dioxide, so
The composite titania material for preparing the big reusable edible of its specific surface area has significant role in terms of the depollution of environment.When TiO2 receives
Rice grain there is also the small shortcoming of specific surface area, hinders it and is widely applied in purification industry.
Recessed soil is the generally acknowledged material in sewage treating material research with great potential.Its main cause includes：(a)
Due to internal porous road, specific surface is big, up to 500m2. g-1More than.B () stable electrochemical property, is difficult to be wadded a quilt with cotton by electrolyte
It is solidifying, had good stability in high temperature and salt solution.Recessed soil has Active sites, in addition to absorption, also catalytic action.(C) exist
In sewage disposal, Concave-convex clay rod can regenerate, and it consumes energy few, can decolourize, can also deodorant taste removal, except carcinogen, it is right
Environmental protection is highly beneficial.(d）The ability of recessed soil absorption is strong, the heavy metal ion such as its lead, chromium and aldehydes, lipid, hydro carbons etc.
The organic molecule of sizing, directly can be adsorbed into duct.Meanwhile, recessed soil also has sterilizing, detoxification, pesticidal work(
Energy.
Graphene is the generally acknowledged material in conductive material research with great potential.Its main cause includes（a）Stone
Black alkene theoretical specific surface area is up to 2630 m2 g-1, be conducive to absorption largely can molecule be degraded（b）Carrier intrinsic mobility
Up to 200 000 cm2 V-1 s-1, be conducive to the quick transmission of electronics；（c）Graphene has very excellent mechanical performance,
Paper-like graphene film has up to 217 kgf mm-2 Hardness, be the twice of carbon steel hardness.
Therefore, Graphene and titanium dioxide and attapulgite material are combined the shortcoming that can overcome pure titinium dioxide, and have three concurrently
Person's advantage, while effectively improving photocatalytic effect and detergent power, and realizes the reusable edible of composite.Wherein, graphite
Alkene has excellent electric conductivity, is a good electron acceptor, can rapidly turn when titanium dioxide produces photocatalytic effect
Electronics is moved, the probability of electronics and hole-recombination is reduced, photocatalytic effect is promoted.Recessed soil and Graphene all have super large simultaneously
Specific surface area, its absorption type and quantity increase, improve adsorption capacity, overcome pure titinium dioxide adsorption capacity small
Contradiction.And recessed soil itself can be decomposed, adsorbent, effectively removes the species of pollutant.And the material for being adsorbed is such as
There is effectively degraded in photocatalyst surface in organophosphor, phenols, halogenated hydrocarbons, fragrant hydrocarbons and their derivates and heterocyclic compound etc., and
It is finally decomposed to inorganic molecules material；Mercury, chromium, lead and oxide for being adsorbed etc. are in the strong of titanium dioxide optical catalyst
Innocuous substance is degraded under redox ability, solves the problems, such as that recessed native capacity of decomposition is small, can so adsorbed again, reached and follow
The purpose that ring is utilized.The material that the method is prepared has electron conductivity high, high recyclability, high-specific surface area, suction high
Attached ability, high intensity, photocatalytic effect high and removing other fungus and purifying ability high, are a kind of very excellent photocatalytic degradation composite woods
Material.
The content of the invention
It is an object of the present invention to provide a kind of Graphene-titanium dioxide-attapulgite composite material and its preparation method and application；
The method is answered nano titanium oxide with the Graphene with elite clone performance and with the big recessed soil of specific surface area
Close, obtain three-dimensional porous Graphene-titanium dioxide-attapulgite composite material, the material not only can using recessed soil and Graphene compared with
Big specific surface area and stronger absorption property harmful substance in the short period of time in quick adsorption air or sewage, having
Evil material is fixed in the material, moreover it is possible to by the preferable electric conductivity of photocatalysis performance and Graphene of titanium dioxide, by these
Adsorbed and fixed harmful substance is slowly decomposed and discharges nontoxic material；The composite realizes venomous injurant
Matter quickly absorbs fast decoupled and material reusable edible performance.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：There is provided a kind of Graphene-titanium dioxide-recessed soil compound
The preparation method of material, comprises the following steps：
（1）Prepare graphene oxide aaerosol solution；
（2）Prepare titanium dioxide suspension：Concentrated hydrochloric acid, water and ammonium sulfate are mixed, stirring, then be slowly added dropwise metatitanic acid thereto
Four butyl esters, stir 2-3 hours, are obtained；
（3）Graphene oxide aaerosol solution, titanium dioxide suspension and recessed soil are placed in by hydro-thermal reaction using hydro-thermal reaction method
In kettle, in isothermal reaction 20-24 hours at 160-200 DEG C, the graphene oxide-titanium dioxide with three-D space structure is obtained
Titanium-attapulgite composite material；Hydro-thermal method is simple and easy to apply, while redox graphene and titanium dioxide is prepared, by controlling to react
Temperature and reaction time can effectively adjust titanium dioxide crystal form.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement：
Step（1）Detailed process be：
（11）Graphite powder is mixed with the concentrated sulfuric acid carries out ice bath, then is gradually added potassium permanganate to it and is added in 1-3 hours, obtains
To mixed solution；
（12）By step（11）The mixed solution for obtaining be placed in 30-50 DEG C at isothermal reaction 0.5-2 hours, be stirred for 20-24 small
When, then in being reacted 0.5-2 hours at 70-90 DEG C, filtering obtains mud cake mass, then added in above-mentioned mud cake mass
Distilled water, in 3000-4000r ﹒ min-1Centrifugation 10-20 minutes, is centrifuged 2-3 times, obtains graphene oxide aaerosol solution.
Further, step（11）In, graphite powder is 8-12 with the mass volume ratio of the concentrated sulfuric acid：210-230；Potassium permanganate
It is 48-52 with the mass volume ratio of the concentrated sulfuric acid：210-230.
Further, step（12）In, by step（11）The mixed solution for obtaining be placed in 35 DEG C at isothermal reaction 0.5 hour,
It is stirred for 24 hours, then in being reacted 0.5 hour at 85 DEG C, filtering obtains mud cake mass, then in above-mentioned mud cake mass
Distilled water is added, in 4000r ﹒ min-1Centrifugation 10 minutes, is centrifuged 2 times, obtains graphene oxide aaerosol solution.
Further, step（2）Detailed process be：
（21）Concentrated hydrochloric acid, deionized water and ammonium sulfate are mixed into 4min-6min, then after being slowly added dropwise butyl titanate, is stirred
Mix 2-3 hours, obtain titanium dioxide suspension；The concentrated hydrochloric acid, water, ammonium sulfate and butyl titanate（v：v：w：v）It is 18-
20：10-20：0.36-0.38:4-4.5.
Further, step（3）Detailed process be：
（31）Graphene oxide aaerosol solution, titanium dioxide suspension and recessed soil are mixed, supersonic oscillations 10-30 minutes,
Obtain mixed solution；
（32）By step（31）Obtained mixed solution is placed in water heating kettle, small in isothermal reaction 20-24 at 160-200 DEG C
When, then washed with absolute ethyl alcohol and deionized water to neutrality, most after 70-80 DEG C of drying, obtain three-dimensional porous Graphene-two
Titanium oxide-attapulgite composite material.
Further, step（32）In, by step（31）Gained mixing suspension is transferred in water heating kettle, in 180 DEG C of constant temperature
Reaction 24 hours, then washed with absolute ethyl alcohol and deionized water to neutrality, most after 70 DEG C of drying, obtain three-dimensional porous graphite
Alkene-titanium dioxide-attapulgite composite material.
Graphene-the titanium dioxide prepared using the preparation method of above-mentioned Graphene-titanium dioxide-attapulgite composite material
Titanium-attapulgite composite material.
Above-mentioned Graphene-application of the titanium dioxide-attapulgite composite material in terms of sewage disposal and cleaning harmful gas.
Compared with prior art, the beneficial effects of the invention are as follows：
1）The method carries out titanium dioxide with the Graphene with elite clone performance and with the big recessed soil of specific surface area
Compound, comprehensive three kinds of advantages of material prepare electron conductivity high, high recyclability, high-specific surface area, high absorption capacity, height
Graphene-titanium dioxide-the attapulgite composite material of intensity, photocatalytic effect high and removing other fungus and purifying ability high, by Graphene and
The addition of recessed soil, further improves composite specific surface area, electron conductivity.
2）Be combined for Graphene and titanium dioxide and recessed soil by the present invention, improves the conduction efficiency of electronics so that titanium dioxide
The photo-generated carrier on titanium surface is transferred to graphenic surface, so as to reduce TiO2The combined efficiency of middle electron hole pair, improves
Photocatalysis efficiency.
3）The specific surface area of composite is big, improves adsorption capacity, effectively eliminates the pollutant in sewage, and
The material for being adsorbed such as organophosphor, phenols, halogenated hydrocarbons, fragrant hydrocarbons and their derivates and heterocyclic compound etc. are sent out in photocatalyst surface
Raw effectively degraded, and it is finally decomposed to inorganic molecules material；Mercury, chromium, lead and oxide for being adsorbed etc. are in titanium dioxide
Innocuous substance is degraded under the Strong oxdiative reducing power of photochemical catalyst, can so be adsorbed again again, reach the mesh for recycling
's.
4）In hydrothermal reaction process of the invention, the functional group on graphene oxide surface（- OH ,-COOH etc.）Occur
Fracture, the л electrons and TiO of the non-bonding in part2Surface free electron bonding, forms Ti-O-C keys, so as to improve TiO2Valency
Band height, reduces its energy gap so that the absorption line red shift of UV-Vis diffusing reflectance spectras, increased visible absorption efficiency；
Meanwhile, in hydrothermal reaction process, different conditions water in recessed native crystal structure is removed, internal structure is become loose porous, from
And increase specific surface area, strengthen its adsorption capacity.
5）Operation is simple for the inventive method, and low cost is more environmentally friendly, is conducive to the carrying out of large-scale production.
Specific embodiment
The present invention will be described in detail below, and example is served only for explaining the present invention, is not intended to limit the present invention
Scope.
Embodiment 1：
A kind of preparation method of Graphene-titanium dioxide-attapulgite composite material, comprises the following steps：
（1）Prepare graphene oxide aaerosol solution；
（11）8g graphite powders are mixed with the 210ml concentrated sulfuric acids carries out ice bath, then to be gradually added 230ml potassium permanganate to it small in 1
When it is interior add, obtain mixed solution；
（12）By step（11）The mixed solution for obtaining be placed in 30 DEG C at isothermal reaction 0.5 hour, then be positioned over magnetic stirrer
Upper stirring 20 hours, reacts 0.5 hour at 90 DEG C, filtering, obtains mud cake mass, then add in above-mentioned mud cake mass
Enter distilled water, in 3000-4000r ﹒ min-1Centrifugation 10 minutes, is centrifuged 2-3 times, obtains graphene oxide aaerosol solution.
（2）Prepare titanium dioxide suspension：18ml concentrated hydrochloric acids, 10ml water and 0.36g ammonium sulfate are mixed, stirring, then
4ml butyl titanates are slowly added dropwise thereto, are stirred 2-3 hours, be obtained.
（3）Prepare Graphene-titanium dioxide-attapulgite composite material
（31）By 3ml graphene oxides aaerosol solution, 20ml titanium dioxide suspensions and the recessed soil of 6mg
It is added to supersonic oscillations 10-20 minutes in beaker, obtains mixing suspension；
（32）By step（31）Gained mixing suspension is transferred in water heating kettle, is placed in vacuum drying chamber, and constant temperature is anti-at 160 DEG C
Answer 20 hours, after reaction terminates, reaction final product is washed to neutrality, most after at 70 DEG C with absolute ethyl alcohol and deionized water
Drying, obtains with the porous Graphene-titanium dioxide-attapulgite composite material of three-D space structure.
Embodiment 2：
A kind of preparation method of Graphene-titanium dioxide-attapulgite composite material, comprises the following steps：
（1）Prepare graphene oxide aaerosol solution；
（11）12g graphite powders are mixed with the 220ml concentrated sulfuric acids carries out ice bath, then to be gradually added 210ml potassium permanganate to it small in 3
When it is interior add, obtain mixed solution；
（12）By step（11）The mixed solution for obtaining be placed in 50 DEG C at isothermal reaction 2 hours, then be positioned on magnetic stirrer
Stirring 24 hours, is reacted 2 hours at 70 DEG C, filtering, obtains mud cake mass, then steaming is added in above-mentioned mud cake mass
Distilled water, in 4000r ﹒ min-1Centrifugation 20 minutes, is centrifuged 2-3 times, obtains graphene oxide aaerosol solution.
（2）Prepare titanium dioxide suspension：20ml concentrated hydrochloric acids, 20ml water and 0.38g ammonium sulfate are mixed, stirring, then
4.5ml butyl titanates are slowly added dropwise thereto, are stirred 2-3 hours, be obtained.
（3）Prepare Graphene-titanium dioxide-attapulgite composite material
（31）5ml graphene oxides aaerosol solution, 25ml titanium dioxide suspensions and the recessed soil of 10mg are added in beaker and are surpassed
Sonication 10-20 minutes, obtain mixing suspension；
（32）By step（31）Gained mixing suspension is transferred in water heating kettle, is placed in vacuum drying chamber, and constant temperature is anti-at 200 DEG C
Answer 24 hours, after reaction terminates, reaction final product is washed to neutrality, most after at 80 DEG C with absolute ethyl alcohol and deionized water
Drying, obtains with the porous Graphene-titanium dioxide-attapulgite composite material of three-D space structure.
Embodiment 3：
A kind of preparation method of Graphene-titanium dioxide-attapulgite composite material, comprises the following steps：
（1）Prepare graphene oxide aaerosol solution；
（11）10g graphite powders are mixed with the 230ml concentrated sulfuric acids carries out ice bath, then to be gradually added 220ml potassium permanganate to it small in 2
When it is interior add, obtain mixed solution；
（12）By step（11）The mixed solution for obtaining be placed in 40 DEG C at isothermal reaction 1 hour, then be positioned on magnetic stirrer
Stirring 22 hours, is reacted 1 hour at 80 DEG C, filtering, obtains mud cake mass, then steaming is added in above-mentioned mud cake mass
Distilled water, in 3000r ﹒ min-1Centrifugation 10 minutes, is centrifuged 2-3 times, obtains graphene oxide aaerosol solution.
（2）Prepare titanium dioxide suspension：20ml concentrated hydrochloric acids, 20ml water and 0.38g ammonium sulfate are mixed, stirring, then
4.5ml butyl titanates are slowly added dropwise thereto, are stirred 2-3 hours, be obtained.
（3）Prepare Graphene-titanium dioxide-attapulgite composite material：
（31）4ml graphene oxides aaerosol solution, 22ml titanium dioxide suspensions and the recessed soil of 8mg are added to ultrasound in beaker
Ripple vibrates 10-20 minutes, obtains mixing suspension；
（32）By step（31）Gained mixing suspension is transferred in water heating kettle, is placed in vacuum drying chamber, and constant temperature is anti-at 180 DEG C
Answer 22 hours, after reaction terminates, reaction final product is washed to neutrality, most after at 75 DEG C with absolute ethyl alcohol and deionized water
Drying, obtains with the porous Graphene-titanium dioxide-attapulgite composite material of three-D space structure.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of Graphene-titanium dioxide-attapulgite composite material, it is characterized in that, comprise the following steps：
（1）Prepare graphene oxide aaerosol solution；
（2）Prepare titanium dioxide suspension：Concentrated hydrochloric acid, water and ammonium sulfate are mixed, stirring, then be slowly added dropwise metatitanic acid thereto
Four butyl esters, stir 2-3 hours, are obtained；
（3）Graphene oxide aaerosol solution, titanium dioxide suspension and recessed soil are placed in by hydro-thermal reaction using hydro-thermal reaction method
In kettle, in isothermal reaction 20-24 hours at 160-200 DEG C, the graphene oxide-titanium dioxide with three-D space structure is obtained
Titanium-attapulgite composite material；The graphene oxide solution and titania solution and recessed soil（v：v：w）Envelope-bulk to weight ratio be 3-
5：20-25：0.006-0.01.
2. the preparation method of Graphene-titanium dioxide-attapulgite composite material according to claim 1, it is characterized in that, step
（1）Detailed process be：
（11）Graphite powder is mixed with the concentrated sulfuric acid carries out ice bath, then is gradually added potassium permanganate to it and is added in 1-3 hours, obtains
To mixed solution；
（12）By step（11）The mixed solution for obtaining be placed in 30-50 DEG C at isothermal reaction 0.5-2 hours, be stirred for 20-24 small
When, then in being reacted 0.5-2 hours at 70-90 DEG C, filtering obtains mud cake mass, then added in above-mentioned mud cake mass
Distilled water, in 3000-4000r ﹒ min-1Centrifugation 10-20 minutes, is centrifuged 2-3 times, obtains graphene oxide aaerosol solution.
3. the preparation method of Graphene-titanium dioxide-attapulgite composite material according to claim 2, it is characterized in that：
Step（11）In, graphite powder is 8-12 with the mass volume ratio of the concentrated sulfuric acid：210-230；The matter of potassium permanganate and the concentrated sulfuric acid
Amount volume ratio is 48-52：210-230.
4. the preparation method of Graphene-titanium dioxide-attapulgite composite material according to claim 2, it is characterized in that：
Step（12）In, by step（11）The mixed solution for obtaining be placed in 35 DEG C at isothermal reaction 0.5 hour, be stirred for 24 small
When, then in being reacted 0.5 hour at 85 DEG C, filtering obtains mud cake mass, then distillation is added in above-mentioned mud cake mass
Water, in 4000r ﹒ min-1Centrifugation 10 minutes, is centrifuged 2 times, obtains graphene oxide aaerosol solution.
5. the preparation method of Graphene-titanium dioxide-attapulgite composite material according to claim 1, it is characterized in that, step
（2）Detailed process be：
（21）Concentrated hydrochloric acid, water and ammonium sulfate are mixed into 4-6min, then after being slowly added dropwise butyl titanate, are stirred 2-3 hours,
Obtain titanium dioxide suspension；The concentrated hydrochloric acid, water, ammonium sulfate and butyl titanate（v：v：w：v）It is 18-20：10-20：
0.36-0.38:4-4.5。
6. the preparation method of Graphene-titanium dioxide-attapulgite composite material according to claim 1, it is characterized in that, step
（3）Detailed process be：
（31）Graphene oxide aaerosol solution, titanium dioxide suspension and recessed soil are mixed, supersonic oscillations 10-30 minutes,
Obtain mixed solution；
（32）By step（31）Obtained mixed solution is placed in water heating kettle, small in isothermal reaction 20-24 at 160-200 DEG C
When, then washed with absolute ethyl alcohol and deionized water to neutrality, most after 70-80 DEG C of drying, obtain three-dimensional porous Graphene-two
Titanium oxide-attapulgite composite material.
7. the preparation method of Graphene-titanium dioxide-attapulgite composite material according to claim 6, it is characterized in that：
Step（32）In, by step（31）Gained mixing suspension is transferred in water heating kettle, in 180 DEG C of isothermal reactions 24 hours,
Washed with absolute ethyl alcohol and deionized water again to neutrality, most after 70 DEG C of drying, obtain three-dimensional porous Graphene-titanium dioxide-
Attapulgite composite material.
8. prepared using the preparation method of the Graphene-titanium dioxide-attapulgite composite material described in any one of claim 7
Graphene-titanium dioxide-attapulgite composite material.
9. Graphene-titanium dioxide-the attapulgite composite material described in claim 8 is in terms of sewage disposal and cleaning harmful gas
Application.
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| CN112495449A (en) * | 2020-12-04 | 2021-03-16 | 中国矿业大学 | Kaolinite-titanium dioxide-graphene composite photocatalyst with nano support holes and preparation method thereof |
| CN112495450A (en) * | 2020-12-04 | 2021-03-16 | 中国矿业大学 | Palygorskite-titanium dioxide-graphene quantum dot composite photocatalyst and preparation method thereof |
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