CN104874347B - A kind of TiO2Load the preparation method and applications of nitrogen-doped graphene sponge - Google Patents
A kind of TiO2Load the preparation method and applications of nitrogen-doped graphene sponge Download PDFInfo
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Abstract
A kind of preparation method and applications of TiO2 loads nitrogen-doped graphene sponge, belong to technical field of function materials.Preparation method is to be added to contain titanium precursors in the alcohol dispersion liquid containing graphene oxide, deionized water is slowly added dropwise again, it stirs evenly to form mixed liquor, hydro-thermal reaction is carried out at 180~240 DEG C 12~48 hours, it takes out and is freeze-dried molding under the conditions of 80~75 DEG C, it is transferred to again in vacuum tube furnace and leads to high-purity nitrogenous gas, and be warming up in 400~800 DEG C and roast 3~12 hours, obtain the three-dimensional porous nitrogen-doped graphene sponge containing 5~10%TiO2.The material preparation method of the present invention is simple, its both adsorbable a large amount of formaldehyde or benzene-like compounds gas, and formaldehyde degradation by photocatalytic oxidation process or benzene-like compounds gas can be passed through under ultra violet lamp, avoid adsorption saturation phenomenon, absorption is carried out at the same time with degradation, it is complete to absorption, realize the purpose of efficient, rapid purification air.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of to have absorption and the difunctional TiO that degrades2Load
The preparation method and applications of nitrogen-doped graphene sponge.
Background technology
Due to science and technology development, at present city dweller either live or work, most times are all indoors
It spends, indoor air conditions will have a direct impact human body.Coating, paint used in house decoration at present and household,
It is gradually distributed from coating and household containing organic pollutants, these gases such as formaldehyde, benzene, ammonias in the materials such as foam stuffing
Out, great injury is caused to the body of people.The common processing method of indoor air pollutants is mainly inhaled by physics
Attached method removes, and common adsorbent has cellular and spheric active carbon, activated carbon fibre and molecular sieve etc., and this method is simply easy
Row, but adsorptive selectivity is poor, renewable difficulty.The method that another kind effectively removes indoor air pollutants is to utilize semiconductor light
Catalysis material is decomposed into harmless tasteless substance by poisonous and harmful, and it is nanometer most to have the photocatalysis catalyst of Commercial Prospect
TiO2, the functional material for having both absorption and photocatalytic degradation functions at present is also more rare.Graphene sponge is a kind of new
The three-dimensional porous carbon material of type, with larger specific surface area, graphene sponge is mainly used for greasy dirt and organic solvent at present
Absorption, report is studied not yet to the absorption of gas pollutant in air.
Invention content
For the above-mentioned problems in the prior art, the purpose of the present invention is to provide one kind to have absorption and degradation double
Function, and the preparation method and applications for the TiO2 load nitrogen-doped graphene sponges that adsorption capacity is strong, degradation speed is fast.
A kind of TiO2Load the preparation method of nitrogen-doped graphene sponge, it is characterised in that preparation method is as follows：
It is added in the alcohol dispersion liquid containing graphene oxide and contains titanium precursors, then deionized water is slowly added dropwise, stir evenly to form mixing
Liquid, hydro-thermal reaction is carried out at 180~240 DEG C 12~48 hours, is taken out and is freeze-dried molding under the conditions of -80~-75 DEG C, then turns
Enter and lead to high-purity nitrogenous gas in vacuum tube furnace, and be warming up in 400~800 DEG C and roast 3~12 hours, obtains containing 5~10%
TiO2Three-dimensional porous nitrogen-doped graphene sponge.
A kind of TiO2Load the preparation method of nitrogen-doped graphene sponge, it is characterised in that containing graphene oxide
A concentration of 1-2mg/ml of graphene oxide in alcohol dispersion liquid.
A kind of TiO2Load the preparation method of nitrogen-doped graphene sponge, it is characterised in that the dropwise addition of deionized water
Time is 30-60min, and the hydro-thermal reaction time is 20-24 hours.
A kind of TiO2Load the preparation method of nitrogen-doped graphene sponge, it is characterised in that lead to high-purity nitrogenous gas
Flow be 100ml/ minute, heating rate be 5 DEG C/min.
A kind of TiO2Load the preparation method of nitrogen-doped graphene sponge, it is characterised in that described 400~800
Lead to high-purity nitrogenous gas in DEG C 3~12 hours, calcination temperature is 600~750 DEG C, and roasting time is 3~4 hours.
A kind of TiO2Load the preparation method of nitrogen-doped graphene sponge, it is characterised in that described contains titanium precursor
Body is butyl titanate or titanium tetrachloride.
A kind of TiO2Load the preparation method of nitrogen-doped graphene sponge, it is characterised in that the preparation method
It is specific as follows：
1）The alcohol dispersion liquid of the graphene oxide of the mg/ml containing 1-2 is measured, is added and contains titanium precursors, then be slowly added dropwise
Ionized water forms mixed liquor, stirs evenly, alcohol dispersion liquid, butyl titanate and the deionized water of the graphene oxide
The volume ratio that feeds intake is 45-55:5:2
2）By step 1）Obtained mixed liquor pours into hydrothermal reaction kettle, and hydro-thermal reaction 12~48 is carried out at 180~240 DEG C
Hour, then natural cooling, obtains TiO2The Graphene gel of load；
3）By step 2）Obtained Graphene gel obtained three-dimensional porous in -80~-75 DEG C of frozen dryings 24 hours
TiO2Load graphene sponge；
4）By step 3）Obtain three-dimensional porous TiO2Load graphene sponge is placed in vacuum tube furnace, by 100ml/
The flow of min is passed through high-purity nitrogenous gas, is warming up in 400~800 DEG C by 5 DEG C/min and roasts 3~12 hours to get to containing 4
~5 % TiO2The nitrogen-doped graphene sponge of load.
The TiO2Load application of the nitrogen-doped graphene sponge in absorption formaldehyde in air or benzene-like compounds.
The TiO2Load the application of nitrogen-doped graphene sponge, it is characterised in that formaldehyde adsorption or benzene-like compounds
Afterwards, then by photocatalysis by formaldehyde or benzene-like compounds carbon dioxide, water are degraded to.
The TiO2Load the application of nitrogen-doped graphene sponge, it is characterised in that the benzene-like compounds include
Benzene, toluene and phenol.
By using above-mentioned technology, compared with prior art, beneficial effects of the present invention are as follows：
1）The TiO of the present invention2The preparation for loading nitrogen-doped graphene sponge is to form compound by being prepared in situ, behaviour
Make simple, low for equipment requirements, can be widely applied in industrial production；
2）The TiO of the present invention2Loading nitrogen-doped graphene sponge has difunctional effect, both can strong adsorption formaldehyde or benzene
Class chemical compound gas, while it can be made to be degraded to the nontoxic gas such as carbon dioxide by photocatalysis fast degradation, it is real
The purpose for now purifying air efficiently, rapidly, with the unique advantage in performance；
3）The TiO of the present invention2Nitrogen-doped graphene sponge is loaded using after a certain period of time, it can be by the letters such as washing, roasting
Folk prescription method activating and regenerating, reuses, therefore reduce use cost, improves economic benefit；
4）The TiO of the present invention2It is simple to load nitrogen-doped graphene sponge preparation method, it has dual function, can both inhale
Attached a large amount of formaldehyde or benzene-like compounds gas, and formaldehyde degradation by photocatalytic oxidation process or benzene-like compounds gas can be passed through under ultra violet lamp
Body is realized the purpose for purifying air efficiently, rapidly, is suitable for popularization and application.
Specific implementation mode
The invention will be further described with reference to embodiments, but protection scope of the present invention is not limited to that：
A kind of TiO2The preparation method of nitrogen-doped graphene sponge is loaded, it is specific as follows：In graphite oxide containing 1-2mg/ml
The alcohol dispersion liquid of alkene, which is added, contains titanium precursors, then slowly in 30-
Deionized water is added dropwise in 60min, stirs evenly to form mixed liquor, hydro-thermal reaction 12~48 is carried out at 180~240 DEG C
Hour, preferred reaction time is 20-24 hours, takes out be freeze-dried molding under the conditions of -80~-75 DEG C after reaction, then
It is transferred in vacuum tube furnace and high-purity nitrogenous gas was led to 100ml/ minutes flows, and with 5 DEG C/min of gradient increased temperature to 400
It is roasted in~800 DEG C 3~12 hours, preferably calcination temperature is 600~750 DEG C, and preferably roasting time is 3~4 hours, is contained
5~10%TiO2Three-dimensional porous nitrogen-doped graphene sponge.
In the present invention, described containing titanium precursors is butyl titanate or titanium tetrachloride, high-purity nitrogenous gas be nitrogen or
Ammonia, purity are 99.9% or more, and alcohol dispersion liquid, butyl titanate and the deionized water of graphene oxide feed intake volume ratio
For 45-55:5:2
The TiO that the present invention obtains2Nitrogen-doped graphene sponge is loaded, there is difunctional effect, it can not only adsorb air
The benzene-like compounds such as middle formaldehyde or benzene, toluene and phenol, moreover it is possible to by photocatalysis by the formaldehyde being adsorbed onto or benzene class chemical combination
Object is degraded to carbon dioxide, water, and TiO2Load nitrogen-doped graphene sponge can be continued with by roasting, regenerating.
Embodiment 1：5%TiO2The preparation method for loading nitrogen-doped graphene sponge is as follows：
1) alcohol dispersion liquid of graphene oxides of 50 ml containing 2 mg/ml is measured, and 5ml butyl titanates are added, then
2ml deionized waters are added dropwise in 30min, forms mixed liquor, stirs evenly；
2）Mixed liquor is poured into 100ml hydrothermal reaction kettles, 180 DEG C of isothermal reactions 24 hours, then natural cooling, is unscrewed
Hydrothermal reaction kettle can be obtained TiO2The Graphene gel of load；
3）By obtained Graphene gel in -78 DEG C of frozen dryings 24 hours, you can obtain three-dimensional porous TiO2
Load graphene sponge；
4）It will obtain three-dimensional porous TiO2Load graphene sponge is placed in vacuum tube furnace, by the stream of 100ml/min
Amount is passed through high-purity ammonia（99.999%）, it is warming up to 600 DEG C by 5 DEG C/min and roasts 3 hours, you can obtains containing 5%TiO2Load
Nitrogen-doped graphene sponge.
Using：It will obtain containing 5%TiO2The nitrogen-doped graphene sponge of load is put into 100ml photo catalysis reactors, input
0.3mg/M3Formaldehyde, take in reactor gas GC to analyze content of formaldehyde after sealing in half an hour, obtain content of formaldehyde at this time
For 0.2 mg/M3, illustrate that the nitrogen-doped graphene sponge PARA FORMALDEHYDE PRILLS(91,95) gas of the present invention has certain suction-operated, then again
Illumination experiment is carried out with the ultraviolet lamp of 30W, 2 hours i.e. complete by the Degradation Formaldehyde in reactor.
In the embodiment, butyl titanate, high-purity nitrogenous gas is replaced to be replaced with nitrogen with titanium tetrachloride containing titanium precursors
Ammonia can obtain same technique effect.
Embodiment 2：6%TiO2The preparation method for loading nitrogen-doped graphene sponge is as follows：
1）The alcohol dispersion liquid of graphene oxides of the 45ml containing 1mg/ml is measured, and 5ml titanium tetrachlorides are added, then
2ml deionized waters are added dropwise in 60min, forms mixed liquor, stirs evenly；
2）Mixed liquor is poured into 100ml hydrothermal reaction kettles, 200 DEG C of isothermal reactions 24 hours, then natural cooling, is unscrewed
Hydrothermal reaction kettle can be obtained TiO2The Graphene gel of load；
3）By obtained Graphene gel in -80 DEG C of frozen dryings 24 hours, you can obtain three-dimensional porous TiO2
Load graphene sponge；
4）It will obtain three-dimensional porous TiO2Load graphene sponge was placed in vacuum tube furnace, by 100 ml/ minutes
Flow is passed through high pure nitrogen（99.999%）, it is warming up to 400 DEG C by 5 DEG C/min and roasts 12 hours, you can obtains 6%TiO2Load
Nitrogen-doped graphene sponge；
5）It will obtain 4%TiO2The nitrogen-doped graphene sponge of load is put into homemade photo catalysis reactor, input
0.5mg/M3Toluene, take in reactor gas GC to analyze toluene level after sealing in half an hour, obtain toluene level at this time
For 0.35 mg/M3, illustrate that nitrogen-doped graphene sponge has certain suction-operated to toluene gas.Then use 50W's again
Ultraviolet lamp carries out illumination experiment, and 4 hours i.e. complete by the degradation of toluene in reactor.
Embodiment 3：7%TiO2The preparation method for loading nitrogen-doped graphene sponge is as follows：
1）The alcohol dispersion liquid of graphene oxides of 55 ml containing 1.5mg/ml is measured, and 6ml titanium tetrachlorides are added, then
2.5 ml deionized waters are added dropwise in 45min, forms mixed liquor, stirs evenly；
2）Mixed liquor is poured into 100ml hydrothermal reaction kettles, 180 DEG C of isothermal reactions 48 hours, then natural cooling, is unscrewed
Hydrothermal reaction kettle can be obtained TiO2The Graphene gel of load；
3）By obtained Graphene gel in -75 DEG C of frozen dryings 48 hours, you can obtain three-dimensional porous TiO2
Load graphene sponge；
4）It will obtain three-dimensional porous TiO2Load graphene sponge was placed in vacuum tube furnace, by 100 ml/ minutes
Flow is passed through high pure nitrogen（99.999%）, it is warming up to 800 DEG C by 5 DEG C/min and roasts 3 hours, you can obtains 7%TiO2Load
Nitrogen-doped graphene sponge；
5）It will obtain 7%TiO2The nitrogen-doped graphene sponge of load is put into photo catalysis reactor, puts into 0.2mg/M3's
Phenol takes gas GC analysis of Phenol contents in reactor in half an hour after sealing, show that phenol content is 0.35 mg/ at this time
M3, illustrate that nitrogen-doped graphene sponge Pyrogentisinic Acid's gas has certain suction-operated.Then carried out again with the ultraviolet lamp of 50W
Illumination experiment, 3 hours i.e. complete by the phenol degrading in reactor.
Example IV：5%TiO2The preparation method for loading nitrogen-doped graphene sponge is as follows：
1）The alcohol dispersion liquid of graphene oxides of the 50ml containing 2mg/ml is measured, and 6ml butyl titanates are added, then
2.5 ml deionized waters are added dropwise in 50min, forms mixed liquor, stirs evenly；
2）Mixed liquor is poured into 100ml hydrothermal reaction kettles, 240 DEG C of isothermal reactions 12 hours, then natural cooling, is unscrewed
Hydrothermal reaction kettle can be obtained TiO2The Graphene gel of load；
3）By obtained Graphene gel in -78 DEG C of frozen dryings 48 hours, you can obtain three-dimensional porous TiO2
Load graphene sponge；
4）It will obtain three-dimensional porous TiO2Load graphene sponge was placed in vacuum tube furnace, by 100 ml/ minutes
Flow is passed through high-purity ammonia（99.999%）, it is warming up to 700 DEG C by 5 DEG C/min and roasts 4 hours, you can obtains 5%TiO2Load
Nitrogen-doped graphene sponge.
The 5%TiO that will be obtained2The nitrogen-doped graphene sponge of load is put into photo catalysis reactor, puts into 0.3mg/M3's
Formaldehyde and 0.3mg/M3Toluene, take in reactor gas GC to analyze formaldehyde and toluene level after sealing in half an hour, at this time
Show that content of formaldehyde is 0.25 mg/M3, toluene level 0.2mg/M3.Then illumination experiment is carried out with the ultraviolet lamp of 50W again, 4
Hour i.e. by reactor formaldehyde and degradation of toluene it is complete.
A kind of preparation method of TiO2 load nitrogen-doped graphene sponges of the present invention is simple, and the obtained material has double
Weight function, solves the problems, such as adsorption saturation in currently available technology, can degrade while absorption, until toxic gas quilt
Absorption is complete, achievees the purpose that purify air rapidly.
Claims (6)
1. a kind of TiO2Load the preparation method of nitrogen-doped graphene sponge, it is characterised in that the preparation method is specific as follows：
1）The alcohol dispersion liquid of the graphene oxide of the mg/ml containing 1-2 is measured, is added and contains titanium precursors, then deionization is slowly added dropwise
Water forms mixed liquor, stirs evenly, and described is titanium tetrachloride, the alcohol dispersion liquid of graphene oxide, tetrachloro containing titanium precursors
It is 45 to change titanium and the deionized water volume ratio that feeds intake:5:2 or 55：6：2.5；
2）By step 1）Obtained mixed liquor pours into hydrothermal reaction kettle, and it is small that hydro-thermal reaction 12~48 is carried out at 180~240 DEG C
When, then natural cooling, obtains TiO2The Graphene gel of load；
3）By step 2）Obtained Graphene gel obtained three-dimensional porous in -80~-75 DEG C of frozen dryings 24 hours
TiO2Load graphene sponge；
4）By step 3）Obtain three-dimensional porous TiO2Load graphene sponge is placed in vacuum tube furnace, by the stream of 100ml/min
Amount is passed through high-purity nitrogenous gas, is warming up in 400~800 DEG C by 5 DEG C/min and roasts 3~12 hours to get to containing 4~5 %
TiO2The nitrogen-doped graphene sponge of load.
2. a kind of TiO according to claim 12Load nitrogen-doped graphene sponge preparation method, it is characterised in that go from
The time for adding of sub- water is 30-60min, and the hydro-thermal reaction time is 20-24 hours.
3. a kind of TiO according to claim 12Load the preparation method of nitrogen-doped graphene sponge, it is characterised in that step
4）In, calcination temperature is 600~750 DEG C, and roasting time is 3~4 hours.
4. a kind of TiO that preparation method as described in claim 1 obtains2Load nitrogen-doped graphene sponge first in adsorbing air
Application in aldehyde or benzene-like compounds.
5. application as claimed in claim 4, it is characterised in that after formaldehyde adsorption or benzene-like compounds, then pass through photocatalysis
Formaldehyde or benzene-like compounds are degraded to carbon dioxide, water.
6. application as claimed in claim 4, it is characterised in that the benzene-like compounds include benzene, toluene and phenol.
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| CN103359709B (en) * | 2012-03-27 | 2016-08-03 | 海洋王照明科技股份有限公司 | The preparation method of nitrogen-doped graphene |
| CN102941042B (en) * | 2012-10-25 | 2016-03-09 | 北京理工大学 | A kind of Graphene/metal oxide hybrid aeroge, preparation method and application thereof |
| EP2767337B1 (en) * | 2013-02-14 | 2016-11-02 | Directa Plus S.p.A. | Method and apparatus for fabricating solid support metal catalyst composites |
| CN103265019B (en) * | 2013-05-25 | 2015-04-15 | 桂林理工大学 | Preparation method for highly-nitrogen-doped graphene light-weight ferromagnetic material |
| CN104415772A (en) * | 2013-08-23 | 2015-03-18 | 国家纳米科学中心 | Nitrogen-doped reduced graphene oxide / nitrogen-doped titanium dioxide composite material and preparation method and application thereof |
| CN103706337B (en) * | 2013-12-30 | 2015-10-07 | 成都纺织高等专科学校 | A kind of except formaldehyde nano-mixture and preparation method thereof |
| CN104098089B (en) * | 2014-07-25 | 2015-11-11 | 西南民族大学 | A kind of preparation method of doped graphene foam |
| CN104355600A (en) * | 2014-10-22 | 2015-02-18 | 华文蔚 | Ceramic composite with high absorptive property and preparation method of ceramic composite |
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