CN106395800B - A kind of preparation method of TiO2 intercalation graphene oxide - Google Patents
A kind of preparation method of TiO2 intercalation graphene oxide Download PDFInfo
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- CN106395800B CN106395800B CN201610747189.XA CN201610747189A CN106395800B CN 106395800 B CN106395800 B CN 106395800B CN 201610747189 A CN201610747189 A CN 201610747189A CN 106395800 B CN106395800 B CN 106395800B
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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 kind of TiO2The preparation method of intercalation graphene oxide, using expanded graphite as raw material, graphene oxide is prepared using improved method, intermediary water is inserted into graphene oxide layer, a small amount of carbon tetrachloride is added after dewatered drying, quantitative butyl titanate is added, is cleaned after ultrasonic disperse with absolute alcohol under air-proof condition, reacts certain time in hydrothermal reaction kettle after filtering and TiO is made2Intercalation graphene oxide.Simple, efficient, the prepared TiO of experimental method of the present invention2Intercalation graphene oxide stability is good, catalytic degradation efficiency is high and reusable, there is good application prospect on air, water process, catalytic degradation, electrode material.
Description
Technical field
The present invention relates to field of nanometer material technology, and in particular to a kind of TiO2The preparation method of intercalation graphene oxide.
Background technique
Graphene be it is a kind of by single layer of carbon atom it is tightly packed at bi-dimensional cellular shape lattice structure carbonaceous material.Graphene
Possess more excellent performance based on special nanostructure, material is in optics, magnetics, catalysis, sensor, electronics etc.
There is huge application benefit in many fields.TiO2It is a kind of with nontoxic, optimal opacity, best whiteness and brightness
Amphoteric oxide, stablize, the characteristic of no pollution to the environment becomes one of optimal catalysis material.
In recent years for graphene and TiO2The research of composite material emerges one after another, but majority is to use chemical oxidation again
Method synthesizing graphite alkene/TiO of reduction2Composite material.Such as Yongbing Tang uses chemical decomposition method by graphene oxide
It is attached to TiO2Film on, method that they adjust graphene oxide depth is control oxidization time, synthesizes composite wood with this
Material, and confirm graphene oxide/TiO2Laminated film have bigger specific surface area, more dyestuffs can be absorbed, convert
Efficiency is obviously improved;Using graphene, ultrasound a period of time in dehydrated alcohol keeps its fully dispersed to Lei Yun etc., side
Stirring side is added butyl titanate, glacial acetic acid, distilled water and continues stirring to being thoroughly mixed, and place makes it sufficiently solidifying for a period of time
Glue, dry, grinding roasting obtains graphene/TiO2Composite material.The Zhang Xiaoyan etc. of Fudan University use sol-gel method with
Butyl titanate and graphene are that starting material is prepared for titanium dioxide (TiO2) and graphene composite photocatalyst material.Research
Photocatalytic hydrogen production by water decomposition activity of the composite material under ultraviolet-visible light and visible light conditions, the results showed that its light
The rate of catalytic decomposition is much higher than the catalytic efficiency of the business P25 under the conditions of;Such 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), a kind of low-temperature thermal decomposition process conjunction is disclosed
At graphene and TiO2Composite material.The invention is by TiO2The bromo- 9,9'- dianthranide (C of 10,10'- bis- is added in powder28H16Br2)
In tetrahydrofuran solution, it is 0.1-1.0wt.% addition according to graphite compositely proportional, after being vigorously stirred, tetrahydrofuran is evaporated,
Then by residue (mixed powder) in 200 DEG C of processing 30min, then in inert gas (N2Or Ar gas) lower 400 DEG C of calcinings 1-3
Hour is to get the graphene and TiO for arriving different content2Composite material.The invention advantage is: low for equipment requirements, reproducibility
It is good, meet environmental requirement, synthesis cost is low.The disadvantage is that solvent has been used, it is not environmentally, at high cost;Furthermore TiO2It is attached to graphite
Alkene surface, property is unstable, and application is poor.
Summary of the invention
In view of the above problems, the present invention provides a kind of TiO2The preparation method of intercalation graphene oxide, it is simple and efficient,
Securely and reliably, novel and unique can effectively solve the problems in background technique.
To achieve the goals above, The technical solution adopted by the invention is as follows: a kind of TiO2The system of intercalation graphene oxide
Preparation Method comprising the steps of:
1) a certain amount of expanded graphite and the suitable concentrated sulfuric acid (98%H are taken2SO4) be placed in glass container, it is filled 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
A certain amount of hydrogen peroxide (H is added in mechanical stirring at different temperatures after mixing2O2), solution becomes bright orange by brownish black
Color.With cleaning solution under the conditions of hydrochloric acid and deionized water Centrifugal dispersion to neutrality, graphene oxide is obtained.
2) take the graphene oxide of above-mentioned preparation in hydrothermal reaction kettle, ultrasound, which is made, under the conditions of certain temperature contains intermediary water
Graphene oxide.
3) by above-mentioned graphene oxide drying, the weighing containing intermediary water prepared.With certain water content meter, it is added micro
Carbon tetrachloride (CCl4) butyl titanate of specified mole is added for foundation with butyl titanate hydrolysis equation;Surpass under air-proof condition
Sound is dispersed to abundant reaction;Absolute alcohol cleans a suction filtration;A small amount of absolute alcohol is added, in hydrothermal reaction kettle under certain temperature
It reacts and TiO is made2Intercalation graphene oxide.
Further, the mesh number of the expanded graphite is in 200-10000 mesh.
Further, expanded graphite shown in and concentrated sulfuric acid mass ratio are 1:30-1:40.
Further, the mass ratio of the expanded graphite and potassium permanganate is 1:1-1:6.
Further, the mass ratio of the expanded graphite and hydrogen peroxide is 1:3-1:10.
Further, when the graphene oxide hydro-thermal reaction, graphene concentration is 2-10wt.%.
Further, the volume ratio of the hydrochloric acid and deionized water is 1:5-1:10;The dosage of deionized water is 50-
3000ml。
Further, the churned mechanically temperature is 5-95 DEG C, and revolving speed is 100-1000 revs/min, time 10-
60min;The time of ultrasonic disperse is 1-10h.
Further, ultrasonic temperature is 100-250 DEG C when the graphene oxide preparation containing intermediary water, time 1-10h.
Further, the TiO2Hydrothermal temperature is 150-180 DEG C when the preparation of intercalation graphene oxide, and the time is
1-10h。
Further, the TiO2Water content is 5-60wt.% when prepared by intercalation graphene oxide.
Further, the volume of the carbon tetrachloride accounts for the 5-10% of graphene aqueous solution volume.
Further, the preparation TiO2When intercalation graphene oxide, butyl titanate rubs with graphene oxide water content
You are than being 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) TiO is prepared using graphene oxide interlayer water hydrolysis butyl titanate2, can be by TiO2Size is effectively controlled nanometer
Grade, and be firmly combined with graphene, not easily to fall off, catalytic activity is high, not vulnerable.
4) present invention provides positive thinking for exploitation novel graphene intercalation nano functional material.
Extremely significant in fields, applications such as water process, air-treatment, photocatalytic degradation, dyestuff degradations.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 2 prepares TiO2Intercalation graphene oxide picture.
Fig. 2 is sample of the embodiment of the present invention and common graphite cyclohexene carboxaldehyde removal rate comparison diagram.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Referring to Fig. 1-2;Wherein
In Fig. 1, indistinctly graininess is nano-TiO inside red circle2Particle, due to TiO2It is inserted between graphene layer, therefore unknown
It is aobvious.
Fig. 2 is sample of the embodiment of the present invention and common graphite cyclohexene carboxaldehyde removal rate comparison diagram.Common graphite alkene PARA FORMALDEHYDE PRILLS(91,95) tool
There is certain suction-operated, reaches saturation after a certain period of time.TiO2 intercalation graphene oxide with catalysis, which has, to be held
Long goes formaldehyde function.
Embodiment 1
1) sulfuric acid (H of 5g 300 mesh expanded graphite and 180g 98% is taken2SO4), it is placed in 5000mL container.In ice-water bath
In, mechanical stirring under conditions of 200 revs/min, mix them thoroughly;When temperature is lower than 5 DEG C, it is slowly added to 15g permanganic acid
Potassium (KMnO4) until KMnO4Total overall reaction.It moves in 40 DEG C of oil baths, operates 30min under conditions of 300 revs/min.It is added
250mL deionized water reacts 15min at 95 DEG C;450mL deionized water is continuously added, is stirred evenly, 30% mistake of 25g is added
Hydrogen oxide (H2O2) aqueous solution, solution gradually becomes glassy yellow by brownish black.Hydrochloric acid and deionized water are made into the ratio of 1:9
(each 250mL, is added three times, ultrasonic disperse 30min after being added every time) is added in above-mentioned mixed solution in solution;It is added
1500mL deionized water stands a night.Deionized water is added, cleaning is obtained to neutrality after 4000 revs/min of lower Centrifugal dispersions
Graphene oxide.
2) take the above-mentioned graphene oxide prepared in hydrothermal reaction kettle, ultrasound 5-6h under the conditions of 135 DEG C of sealing is obtained
Graphene oxide containing intermediary water.
3) by above-mentioned graphene oxide drying, the weighing containing intermediary water prepared.With 35% water content meter, 10g is added
Carbon tetrachloride (CCl4), with butyl titanate and TiO2The molar ratio of water content is that 6.9g is added in 1:4 when prepared by intercalation graphene oxide
Butyl titanate;Ultrasonic disperse 5-6h under air-proof condition;Alcohol washes one time suction filtration;It is added a small amount of alcohol, 180 DEG C of hydrothermal reaction kettle
Under the conditions of react 10h, obtain TiO2Intercalation graphene oxide.
Embodiment 2
1) sulfuric acid (H of 1g 1000 mesh expanded graphite and 36g 98% is taken2SO4), it is placed in 250mL container.In ice-water bath
In, mechanical stirring under conditions of 200 revs/min, mix them thoroughly.When temperature is lower than 5 DEG C, it is slowly added to 3g potassium permanganate
(KMnO4) until KMnO4Total overall reaction.It moves in 40 DEG C of oil baths, operates 30min under conditions of 300 revs/min.50mL is added
Deionized water reacts 15min at 95 DEG C;150mL deionized water is continuously added, is stirred evenly.Add 30% peroxidating of 5g
Hydrogen (H2O2) aqueous solution, solution gradually becomes glassy yellow by brownish black.By hydrochloric acid and deionized water with the ratio wiring solution-forming of 1:9
(each 50mL, is added three times, ultrasonic disperse 30min after being added every time) is added in above-mentioned mixed solution;Be added 300mL go from
Sub- water stands a night.Deionized water is added, cleaning obtains graphene oxide to neutrality after 4000 revs/min of lower Centrifugal dispersions.
2) take the above-mentioned graphene oxide prepared in hydrothermal reaction kettle, ultrasound 6-7h under the conditions of 130 DEG C of sealing is obtained
Graphene oxide containing intermediary water.
3) by above-mentioned graphene oxide drying, the weighing containing intermediary water prepared.With 40% water content meter, 2g tetra- is added
Chlorination carbon (CCl4), with butyl titanate and TiO2The molar ratio of water content is that 1.38g is added in 1:4 when prepared by intercalation graphene oxide
Butyl titanate, ultrasonic disperse 5-6h under air-proof condition, absolute alcohol clean a suction filtration, add a small amount of absolute alcohol, hydro-thermal
10h is reacted under the conditions of 180 DEG C of reaction kettle, obtains TiO2Intercalation graphene oxide.
Embodiment 3
1) sulfuric acid (H of 2g 2000 mesh expanded graphite and 200g 98% is taken2SO4), it is placed in 1000mL container.In ice water
In bath, mechanical stirring under conditions of 500 revs/min, mix them thoroughly;When temperature is lower than 5 DEG C, it is slowly added to 50g Gao Meng
Sour potassium (KMnO4) until KMnO4Total overall reaction.It moves in 40 DEG C of oil baths, operates 30min under conditions of 400 revs/min.It is added
500mL deionized water reacts 30min at 95 DEG C;1500mL deionized water is continuously added, is stirred evenly, 80g 40% is added
Hydrogen peroxide (H2O2) aqueous solution, solution gradually becomes glassy yellow by brownish black.Hydrochloric acid and deionized water are matched with the ratio of 1:8
(each 600mL, is added three times, ultrasonic disperse 40min after being added every time) is added in above-mentioned mixed solution at solution;It is added
3000mL deionized water stands a night.Deionized water is added, cleaning is obtained to neutrality after 4000 revs/min of lower Centrifugal dispersions
Graphene oxide.
2) it takes the above-mentioned graphene oxide prepared in hydrothermal reaction kettle, surpasses in reverse sound 6-7h under the conditions of 140 DEG C of sealing, obtain
To graphene oxide containing intermediary water.
3) by above-mentioned graphene oxide drying, the weighing containing intermediary water prepared.With 45% water content meter, 20g is added
Carbon tetrachloride (CCl4), with butyl titanate and TiO2The molar ratio of water content is 1:4 addition when prepared by intercalation graphene oxide
15.8g butyl titanate;Ultrasonic disperse 5-6h under air-proof condition is added on a small quantity with time suction filtration of absolute alcohol cleaning without watery wine
Essence reacts 8h under the conditions of 190 DEG C of hydrothermal reaction kettle, obtains TiO2Intercalation graphene oxide.
Embodiment 4
To TiO obtained by embodiment 1-32Intercalation graphene oxide carries out relevant identification, and result is referring to Figure of description.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of TiO2The preparation method of intercalation graphene oxide comprising the steps of: it is characterized in that,
1) a certain amount of expanded graphite and suitable 98% concentrated sulfuric acid (98%H are taken2SO4 it) is placed in glass container, is filled 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
A certain amount of hydrogen peroxide (H is added in mechanical stirring at different temperatures after mixing2O2), solution becomes bright orange by brownish black
Color;With cleaning solution under the conditions of hydrochloric acid and deionized water Centrifugal dispersion to neutrality, graphene oxide is obtained;
2) take the graphene oxide of above-mentioned preparation in hydrothermal reaction kettle, the obtained oxygen containing intermediary water of ultrasound under the conditions of certain temperature
Graphite alkene;
3) by above-mentioned graphene oxide drying, the weighing containing intermediary water prepared;With certain water content meter, micro tetrachloro is added
Change carbon (CCl4) butyl titanate of specified mole is added for foundation with butyl titanate hydrolysis equation;Ultrasound point under air-proof condition
It is dissipated to abundant reaction;Absolute alcohol cleans a suction filtration;A small amount of absolute alcohol is added, is reacted under certain temperature in hydrothermal reaction kettle
TiO is made2Intercalation graphene oxide;The volume of the carbon tetrachloride accounts for the 5-10% of graphene aqueous solution volume;Described
Prepare TiO2When intercalation graphene oxide, the molar ratio of butyl titanate and graphene oxide water content is 1:1-5:1.
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 in it is swollen
Graphite and concentrated sulfuric 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
The mass ratio of graphite and potassium permanganate is 1:1-1:6.
5. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide, it is characterised in that: described is swollen
The mass ratio of graphite and hydrogen peroxide is 1:3-1:10.
6. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide, it is characterised in that: the oxidation
When 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: the salt
The volume ratio of acid and deionized water is 1:5-1:10;The dosage 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: the machine
The temperature of tool stirring is 5-95 DEG C, and revolving speed is 100-1000 revs/min, time 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
Ultrasonic temperature is 100-250 DEG C when the graphene oxide preparation of intermediary water, time 1-10h.
10. a kind of TiO according to claim 12The preparation method of intercalation graphene oxide, it is characterised in that: described
TiO2Hydrothermal temperature is 150-180 DEG C when the preparation of intercalation graphene oxide, time 1-10h;The TiO2Intercalation oxygen
Water content is 5-60wt% when prepared by graphite alkene;The volume of the carbon tetrachloride accounts for the 5- of graphene aqueous solution volume
10%;The preparation TiO2When intercalation graphene oxide, the molar ratio of butyl titanate and graphene oxide water content is 1:1-
5:1。
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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 |
CN107321340B (en) * | 2017-06-29 | 2019-08-16 | 南通大学 | A kind of graphene composite photocatalyst aeroge of hierarchical porous structure and preparation method thereof |
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 |
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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CN102492313A (en) * | 2011-11-21 | 2012-06-13 | 四川大学 | Titanium dioxide and graphene oxide composite nano-grade sheet material and preparation method thereof |
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