CN106395800A - Preparation method of TiO2 intercalated graphene oxide - Google Patents

Preparation method of TiO2 intercalated graphene oxide Download PDF

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Publication number
CN106395800A
CN106395800A CN201610747189.XA CN201610747189A CN106395800A CN 106395800 A CN106395800 A CN 106395800A CN 201610747189 A CN201610747189 A CN 201610747189A CN 106395800 A CN106395800 A CN 106395800A
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graphene oxide
preparation
tio
intercalation
water
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CN106395800B (en
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姚理荣
李小娟
袁国秋
徐山青
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Suzhou Huazong Textile New Material Technology Co ltd
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Nantong University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts

Abstract

The invention discloses a preparation method of TiO2 intercalated graphene oxide. The method includes: taking expanded graphite as the raw material, preparing graphene oxide by an improved way, then inserting interlayer water into the graphene oxide lamella, conducting dehydration and drying, then adding a small amount of carbon tetrachloride, adding quantitative butyl titanate, carrying out ultrasonic dispersion under a sealed condition, then performing washing with anhydrous alcohol, conducting pumping filtration, and then carrying out reaction in a hydrothermal reaction kettle for a certain period of time, thus obtaining TiO2 intercalated graphene oxide. The experimental method is simple and efficient, the prepared TiO2 intercalated graphene oxide has good stability, high catalytic degradation efficiency and reusability, and has good application prospect in air and water treatment, catalytic degradation and electrode materials.

Description

A kind of preparation method of TiO2 intercalation graphene oxide
Technical field
The present invention relates to field of nanometer material technology is and in particular to a kind of TiO2The preparation method of intercalation graphene oxide.
Background technology
Graphene is a kind of bi-dimensional cellular shape lattice structure carbonaceous material by the tightly packed one-tenth of monolayer carbon atom.Graphene More excellent performance is had based on special nanostructured, its material is in optics, magnetics, catalysis, sensor, electronics etc. There is huge application benefit in a lot of fields.TiO2It is a kind of to there is nontoxic, optimal opacity, optimal whiteness and brightness Amphoteric oxide, it is stable, the characteristic of environmentally safe becomes one of optimal catalysis material.
In the last few years for Graphene and TiO2The research of composite emerges in an endless stream, but majority is using chemical oxidation again Method synthesizing graphite alkene/the TiO of reduction2Composite.As Yongbing Tang etc. adopts chemical decomposition method by graphene oxide It is attached to TiO2Film on, method that they adjust graphene oxide depth is to control oxidization time, to synthesize composite wood with this Material, and confirm graphene oxide/TiO2Laminated film there is bigger specific surface area, more dyestuffs can be absorbed, conversion Efficiency is substantially improved；Using Graphene, ultrasonic a period of time in dehydrated alcohol makes it fully dispersed to Lei Yun etc., side Stirring side adds butyl titanate, glacial acetic acid, distilled water and continues to stir to being thoroughly mixed, and places and makes it fully solidifying for a period of time Glue, is dried, and grinds roasting, obtains Graphene/TiO2Composite.Zhang Xiaoyan of Fudan University etc. adopt sol-gel process with Butyl titanate and Graphene are prepared for titanium dioxide (TiO for parent material2) and Graphene composite photocatalyst material.Research Photocatalytic hydrogen production by water decomposition activity under ultraviolet-visible light and visible light conditions for this composite, result shows its light The speed of catalytic decomposition be far above with the conditions of business P25 catalytic efficiency；As Chinese invention patent " a kind of Graphene and dioxy In change titanium composite material and its low temperature preparation and methods for using them " (CN 103117171A), disclose a kind of low-temperature thermal decomposition process and close Become Graphene and TiO2Composite.This invention is by TiO2Powder body adds the bromo- 9,9'- dianthranide (C of 10,10'- bis-28H16Br2) In tetrahydrofuran solution, add for 0.1-1.0wt.% according to graphite compositely proportional, after being stirred vigorously, oxolane evaporated, Then residue (mixed powder) is processed 30min at 200 DEG C, then in noble gases (N2Or Ar gas) lower 400 DEG C of calcining 1-3 Hour, that is, obtain Graphene and the TiO of different content2Composite.This invention advantage is：Low for equipment requirements, repeatability Good, meet environmental requirement, synthesize low cost.Shortcoming is the use of solvent, not environmentally, high cost；In addition TiO2It is attached to graphite Alkene surface, property is unstable, and application is poor.
Content of the invention
For problem above, the invention provides a kind of TiO2The preparation method of intercalation graphene oxide, it simply efficiently, Safe and reliable, novel and unique, can be with the problem in effectively solving background technology.
To achieve these goals, the technical solution used in the present invention is as follows：A kind of TiO2The system of intercalation graphene oxide Preparation Method, comprises the steps of：
1) a certain amount of expanded graphite and appropriate concentrated sulphuric acid (98%H are taken2SO4) be placed in glass container, fill under ice-water bath Divide stirring.It is slowly added to a certain amount of potassium permanganate (KMnO4) until KMnO4Total overall reaction, adds a certain amount of deionized water Mechanical agitation at different temperatures, adds a certain amount of hydrogen peroxide (H after mix homogeneously2O2), solution becomes bright orange by brownish black Color.With cleaning solution under the conditions of hydrochloric acid and deionized water Centrifugal dispersion to neutral, obtain graphene oxide.
2) take the graphene oxide of above-mentioned preparation in hydrothermal reaction kettle, under the conditions of uniform temperature, ultrasonic being obtained contains intermediary water Graphene oxide.
3) the above-mentioned graphene oxide containing intermediary water preparing is dried, weighed.With certain water content meter, add micro Carbon tetrachloride (CCl4) butyl titanate that equation is according to the specified mole of addition is hydrolyzed with butyl titanate；Super under air-proof condition Sound is dispersed to abundant reaction；Anhydrous alcohol cleans a sucking filtration；Add a small amount of anhydrous alcohol, under uniform temperature in hydrothermal reaction kettle Reaction is obtained TiO2Intercalation graphene oxide.
Further, the mesh number of described expanded graphite is in 200-10000 mesh.
Further, shown expanded graphite and concentrated sulphuric acid mass ratio are 1:30-1:40.
Further, described expanded graphite and the mass ratio of potassium permanganate are 1:1-1:6.
Further, described expanded graphite and the mass ratio of hydrogen peroxide are 1:3-1:10.
Further, during described graphene oxide hydro-thermal reaction, Graphene concentration is 2-10wt.%.
Further, described hydrochloric acid and the volume ratio of deionized water are 1:5-1:10；The consumption of deionized water is 50- 3000ml.
Further, described churned mechanically temperature is 5-95 DEG C, and rotating speed is 100-1000 rev/min, and the time is 10- 60min；The time of ultrasonic disperse is 1-10h.
Further, when prepared by the described graphene oxide containing intermediary water, ultrasonic temperature is 100-250 DEG C, time 1-10h.
Further, described TiO2During the preparation of intercalation graphene oxide, hydrothermal temperature is 150-180 DEG C, and the time is 1-10h.
Further, described TiO2During the preparation of intercalation graphene oxide, water content is 5-60wt.%.
Further, the volume of described carbon tetrachloride accounts for the 5-10% of graphene aqueous solution volume.
Further, described preparation TiO2During intercalation graphene oxide, butyl titanate is rubbed with graphene oxide water content That ratio is 1:1-5:1.
Beneficial effects of the present invention：
1) experiment condition is simple, raw materials used cheap and easily-available；
2) mature preparation process of graphene oxide, high yield rate；
3) adopt graphene oxide intermediary water hydrolysis butyl titanate preparation TiO2, can be by TiO2Size is effectively controlled nanometer Level, and be firmly combined with Graphene, difficult for drop-off, catalysis activity is high, is difficult to lose efficacy.
4) present invention is that exploitation novel graphite alkene intercalation nano functional material provides positive thinking.
In fields such as water process, air-treatment, photocatalytic degradation, dyestuff degradeds, application is extremely notable.
Brief description
Fig. 1 is that the embodiment of the present invention 2 prepares TiO2Intercalation graphene oxide picture.
Fig. 2 is embodiment of the present invention sample and common graphite cyclohexene carboxaldehyde clearance comparison diagram.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to Limit the present invention.
Referring to Fig. 1-2；Wherein
In Fig. 1, the internal indistinctly graininess of red circle is nano-TiO2Granule, due to TiO2It is inserted between graphene layer, therefore not clear Aobvious.
Fig. 2 is embodiment of the present invention sample and common graphite cyclohexene carboxaldehyde clearance comparison diagram.Common graphite alkene PARA FORMALDEHYDE PRILLS(91,95) has There is certain adsorption, after certain time, reach saturation.The TiO2 intercalation graphene oxide with catalysiss has and holds Long goes formaldehyde function.
Embodiment 1
1) take the sulphuric acid (H of 5g 300 mesh expanded graphite and 180g 98%2SO4), it is placed in 5000mL container.In ice-water bath In, under conditions of 200 revs/min mechanical agitation so as to be sufficiently mixed；When temperature is less than 5 DEG C, it is slowly added to 15g permanganic acid Potassium (KMnO4) until KMnO4Total overall reaction.Move in 40 DEG C of oil baths, operate under conditions of 300 revs/min 30min.Add 250mL deionized water, reacts 15min at 95 DEG C；Continuously add 450mL deionized water, stir, add 25g 30% mistake Hydrogen oxide (H2O2) aqueous solution, solution gradually becomes glassy yellow by brownish black.By hydrochloric acid and deionized water with 1:9 ratio is made into Solution adds (each 250mL, point 3 additions, ultrasonic disperse 30min after adding every time) in above-mentioned mixed solution；Add 1500mL deionized water stands a night.Add deionized water, clean to neutrality after 4000 revs/min of lower Centrifugal dispersions, obtain Graphene oxide.
2) take the above-mentioned graphene oxide preparing in hydrothermal reaction kettle, ultrasonic 5-6h under the conditions of 135 DEG C of sealing, obtain Graphene oxide containing intermediary water.
3) the above-mentioned graphene oxide containing intermediary water preparing is dried, weighed.With 35% water content meter, add 10g Carbon tetrachloride (CCl4), with butyl titanate and TiO2During the preparation of intercalation graphene oxide, the mol ratio of water content is 1:4 addition 6.9g Butyl titanate；Ultrasonic disperse 5-6h under air-proof condition；Time sucking filtration of alcohol washes；Add a small amount of ethanol, 180 DEG C of hydrothermal reaction kettle Under the conditions of react 10h, obtain TiO2Intercalation graphene oxide.
Embodiment 2
1) take the sulphuric acid (H of 1g 1000 mesh expanded graphite and 36g 98%2SO4), it is placed in 250mL container.In ice-water bath In, under conditions of 200 revs/min mechanical agitation so as to be sufficiently mixed.When temperature is less than 5 DEG C, it is slowly added to 3g potassium permanganate (KMnO4) until KMnO4Total overall reaction.Move in 40 DEG C of oil baths, operate under conditions of 300 revs/min 30min.Add 50mL Deionized water, reacts 15min at 95 DEG C；Continuously add 150mL deionized water, stir.Add 5g 30% peroxidating Hydrogen (H2O2) aqueous solution, solution gradually becomes glassy yellow by brownish black.By hydrochloric acid and deionized water with 1:9 ratio wiring solution-forming Add (each 50mL, point 3 additions, ultrasonic disperse 30min after adding every time) in above-mentioned mixed solution；Add 300mL go from Sub- water stands a night.Add deionized water, clean to neutrality after 4000 revs/min of lower Centrifugal dispersions, obtain graphene oxide.
2) take the above-mentioned graphene oxide preparing in hydrothermal reaction kettle, ultrasonic 6-7h under the conditions of 130 DEG C of sealing, obtain Graphene oxide containing intermediary water.
3) the above-mentioned graphene oxide containing intermediary water preparing is dried, weighed.With 40% water content meter, add 2g tetra- Chlorination carbon (CCl4), with butyl titanate and TiO2During the preparation of intercalation graphene oxide, the mol ratio of water content is 1:4 addition 1.38g Butyl titanate, ultrasonic disperse 5-6h under air-proof condition, anhydrous alcohol cleans a sucking filtration, adds a small amount of anhydrous alcohol, hydro-thermal React 10h under the conditions of 180 DEG C of reactor, obtain TiO2Intercalation graphene oxide.
Embodiment 3
1) take the sulphuric acid (H of 2g 2000 mesh expanded graphite and 200g 98%2SO4), it is placed in 1000mL container.In frozen water In bath, under conditions of 500 revs/min, mechanical agitation is so as to be sufficiently mixed；When temperature is less than 5 DEG C, it is slowly added to 50g Gao Meng Sour potassium (KMnO4) until KMnO4Total overall reaction.Move in 40 DEG C of oil baths, operate under conditions of 400 revs/min 30min.Add 500mL deionized water, reacts 30min at 95 DEG C；Continuously add 1500mL deionized water, stir, add 80g 40% Hydrogen peroxide (H2O2) aqueous solution, solution gradually becomes glassy yellow by brownish black.By hydrochloric acid and deionized water with 1:8 ratio is joined Solution is become to add (each 600mL, point 3 additions, ultrasonic disperse 40min after adding every time) in above-mentioned mixed solution；Add 3000mL deionized water stands a night.Add deionized water, clean to neutrality after 4000 revs/min of lower Centrifugal dispersions, obtain Graphene oxide.
2) take the above-mentioned graphene oxide preparing in hydrothermal reaction kettle, surpass in reverse sound 6-7h under the conditions of 140 DEG C of sealing, obtain Arrive graphene oxide containing intermediary water.
3) the above-mentioned graphene oxide containing intermediary water preparing is dried, weighed.With 45% water content meter, add 20g Carbon tetrachloride (CCl4), with butyl titanate and TiO2During the preparation of intercalation graphene oxide, the mol ratio of water content is 1:4 additions 15.8g butyl titanate；Ultrasonic disperse 5-6h under air-proof condition, cleans a sucking filtration with anhydrous alcohol, adds a small amount of no watery wine Essence, reacts 8h under the conditions of 190 DEG C of hydrothermal reaction kettle, obtains TiO2Intercalation graphene oxide.
Embodiment 4
To embodiment 1-3 gained TiO2Intercalation graphene oxide carries out the identification of correlation, and its result is referring to Figure of description.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.

Claims (10)

1. a kind of TiO2The preparation method of intercalation graphene oxide, comprises the steps of：It is characterized in that,
1) a certain amount of expanded graphite and appropriate concentrated sulphuric acid (98%H are taken2SO4) it is placed in glass container, fully stir under ice-water bath Mix；It is slowly added to a certain amount of potassium permanganate (KMnO4) until KMnO4Total overall reaction, adds a certain amount of deionized water not Synthermal lower mechanical agitation, adds a certain amount of hydrogen peroxide (H after mix homogeneously2O2), solution becomes glassy yellow by brownish black； With cleaning solution under the conditions of hydrochloric acid and deionized water Centrifugal dispersion to neutral, obtain graphene oxide；
2) take the graphene oxide of above-mentioned preparation in hydrothermal reaction kettle, the ultrasonic oxygen being obtained containing intermediary water under the conditions of uniform temperature Graphite alkene；
3) the above-mentioned graphene oxide containing intermediary water preparing is dried, weighed；With certain water content meter, add micro tetrachloro Change carbon (CCl4) butyl titanate that equation is according to the specified mole of addition is hydrolyzed with butyl titanate；Ultrasonic point under air-proof condition It is dissipated to abundant reaction；Anhydrous alcohol cleans a sucking filtration；Add a small amount of anhydrous alcohol, react under uniform temperature in hydrothermal reaction kettle Prepared TiO2Intercalation graphene oxide.
2. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide it is characterised in that：Described is swollen The mesh number of graphite is in 200-10000 mesh.
3. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide it is characterised in that：Shown is swollen Graphite and concentrated sulphuric acid mass ratio are 1:30-1:40.
4. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide it is characterised in that：Described is swollen Graphite is 1 with the mass ratio of potassium permanganate:1-1:6.
5. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide it is characterised in that：Described is swollen Graphite is 1 with the mass ratio of hydrogen peroxide:3-1:10.
6. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide it is characterised in that：Described oxidation During Graphene hydro-thermal reaction, Graphene concentration is 2-10wt%.
7. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide it is characterised in that：Described salt Acid is 1 with the volume ratio of deionized water:5-1:10；The consumption of deionized water is 50-3000ml.
8. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide it is characterised in that：Described machine The temperature of tool stirring is 5-95 DEG C, and rotating speed is 100-1000 rev/min, and the time is 10-60min；The time of ultrasonic disperse is 1- 10h.
9. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide it is characterised in that：Described contains During the graphene oxide preparation of intermediary water, ultrasonic temperature is 100-250 DEG C, time 1-10h.
10. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide it is characterised in that：Described TiO2During the preparation of intercalation graphene oxide, hydrothermal temperature is 150-180 DEG C, and the time is 1-10h；Described TiO2Intercalation oxygen During the preparation of graphite alkene, water content is 5-60wt%；The volume of described carbon tetrachloride accounts for the 5- of graphene aqueous solution volume 10%；Described preparation TiO2During intercalation graphene oxide, butyl titanate is 1 with the mol ratio of graphene oxide water content:1- 5:1.
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Cited By (5)

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CN107051229A (en) * 2017-04-17 2017-08-18 江苏大学 A kind of preparation method and its usage of graphene oxide/titanium dioxide stratiform composite membrane of polyethyleneimine crosslinking
CN107321340A (en) * 2017-06-29 2017-11-07 南通大学 A kind of graphene composite photocatalyst aeroge of hierarchical porous structure and preparation method thereof
CN108841358A (en) * 2018-05-24 2018-11-20 南通大学 A kind of nano-sheet Fe3O4The preparation method of intercalation graphene oxide composite wave-suction material
CN109137264A (en) * 2018-07-07 2019-01-04 东莞市联洲知识产权运营管理有限公司 A method of antibacterial medical dressing is prepared using electrostatic spinning
CN113845346A (en) * 2021-10-28 2021-12-28 北华大学 High-water-permeability concrete combined with acrylic acid and preparation method thereof

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CN103028387A (en) * 2012-12-28 2013-04-10 聊城大学 Preparation method of graphene/titanium dioxide photocatalyst
CN104492409A (en) * 2014-11-20 2015-04-08 华中科技大学 Preparation method for TiO2 crystal/graphene nanocomposite

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107051229A (en) * 2017-04-17 2017-08-18 江苏大学 A kind of preparation method and its usage of graphene oxide/titanium dioxide stratiform composite membrane of polyethyleneimine crosslinking
CN107321340A (en) * 2017-06-29 2017-11-07 南通大学 A kind of graphene composite photocatalyst aeroge of hierarchical porous structure and preparation method thereof
CN108841358A (en) * 2018-05-24 2018-11-20 南通大学 A kind of nano-sheet Fe3O4The preparation method of intercalation graphene oxide composite wave-suction material
CN108841358B (en) * 2018-05-24 2021-03-16 南通大学 Nano-flake Fe3O4Preparation method of intercalated graphene oxide composite wave-absorbing material
CN109137264A (en) * 2018-07-07 2019-01-04 东莞市联洲知识产权运营管理有限公司 A method of antibacterial medical dressing is prepared using electrostatic spinning
CN113845346A (en) * 2021-10-28 2021-12-28 北华大学 High-water-permeability concrete combined with acrylic acid and preparation method thereof
CN113845346B (en) * 2021-10-28 2022-12-23 北华大学 High-water-permeability concrete combined with acrylic acid and preparation method thereof

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