CN102101051B - Method for preparing carbon nano tube supported nano photocatalysis material capable of degrading nitrogen oxides - Google Patents
Method for preparing carbon nano tube supported nano photocatalysis material capable of degrading nitrogen oxides Download PDFInfo
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- CN102101051B CN102101051B CN 201110026187 CN201110026187A CN102101051B CN 102101051 B CN102101051 B CN 102101051B CN 201110026187 CN201110026187 CN 201110026187 CN 201110026187 A CN201110026187 A CN 201110026187A CN 102101051 B CN102101051 B CN 102101051B
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- nano titanium
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000000463 material Substances 0.000 title claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 230000000593 degrading effect Effects 0.000 title claims abstract description 14
- 230000001699 photocatalysis Effects 0.000 title abstract description 25
- 238000007146 photocatalysis Methods 0.000 title abstract description 24
- 239000002041 carbon nanotube Substances 0.000 title abstract description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 title abstract description 6
- 238000000034 method Methods 0.000 title abstract description 3
- 239000013078 crystal Substances 0.000 claims abstract description 30
- 238000012986 modification Methods 0.000 claims abstract description 16
- 230000004048 modification Effects 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 23
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 23
- 238000006555 catalytic reaction Methods 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 101710134784 Agnoprotein Proteins 0.000 claims 1
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 11
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract description 7
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract description 5
- 229910021392 nanocarbon Inorganic materials 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000005284 excitation Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000005923 long-lasting effect Effects 0.000 description 2
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for preparing a carbon nano tube supported modified nano photocatalysis material capable of degrading nitrogen oxides, which comprises the following steps of: ultrasonically dispersing nano titanium dioxide mixed crystal in water for 20 to 30 minutes, then putting the dispersion into 0.3 to 0.5mol/L AgNO3 solution, adding partial ethanol and then stirring for 30 to 40 minutes; putting the solution under an ultraviolet lamp, continuously stirring the solution for 90 minutes, filtering, and calcining the filter residue for 2 to 3 hours at the temperature of between 400 and 450 DEG C to obtain modified nano titanium dioxide mixed crystal; and mixing the modified nano titanium dioxide mixed crystal and carbon nano tube for 2 to 4 hours in a ratio of 1:0.01-0.015 to obtain the carbon nano tube supported modified nano photocatalysis material capable of degrading the nitrogen oxides. The preparation process is simple; the prepared carbon nano tube supported modified nano photocatalysis material has better nitrogen oxide photocatalysis effect because of silver ion modification and nano carbon tube support, particularly the effect under visible light is obviously improved, and meanwhile, the long-term effectiveness of the photocatalysis effect is remarkably improved.
Description
Technical field
The present invention relates to a kind of preparation method of carbon nanometer tube loaded type modified Nano catalysis material of the nitrogen oxide of degrading.
Background technology
Proposed since Fujishima in 1972 since " these are many---liana " effect of semi-conducting material, adopt the research of harmful liquid stable under the photocatalysis technology degraded normal temperature and gas to become the study hotspot of scientific circles, yet because the restriction of excitation wavelength and photocatalysis quantum generation rate and catalytic efficiency is low, the actual outdoor catalytic effect of existing catalysis material is very limited, must carry out the modification of catalysis material.At present, existing more research aspect modification, such as adopting the especially inertia noble metals such as thulium doping vario-property, surface deposition Au, Pt, Ag of ion, or adopt the sensitising agent such as pigment to apply the catalysis material surface, adopt porous carrier technology etc., expectation reach reduce between light induced electron and the hole compound, improve the firing rate of visible light and the effect of photocatalytic activity.
The present invention combines doping vario-property and the effective carrier technology of nano-photocatalyst material, on the one hand existing nano titanium oxide mixed crystal is carried out the silver ion doping vario-property, reaches the effect that improves the photocatalysis efficiency under the visible light; On the other hand, adopt multiple-wall carbon nanotube as effective carrier, so that catalysis material can fully contact with nitrogen oxide and react, significantly reduce simultaneously the recombination probability between light induced electron and the hole, significantly improve photocatalysis efficiency and long-lasting effect thereby reach.
Summary of the invention
The object of the invention is to overcome the preparation method that deficiency of the prior art provides the carbon nanometer tube loaded type nano-photocatalyst material of the nitrogen oxide of degrading.
The preparation method of the carbon nanometer tube loaded type modified Nano catalysis material of the nitrogen oxide of degrading of the present invention may further comprise the steps:
(1) the nano titanium oxide mixed crystal is placed the ultrasonic dispersion of water 20～30 minutes, then put into the AgNO3 solution of 0.3～0.5mol/L, add part ethanol and then stir 30～40min;
(2) place continuation stirring 90min under the uviol lamp, after the filtration filter residue is placed on 400～450 ℃ of lower calcinings 2～3 hours, obtain the nano titanium oxide mixed crystal of modification;
(3) with the nano titanium oxide mixed crystal of modification and the CNT ratio batch mixing 2～4h by weight 1: 0.01～0.015, the preparation method of the carbon nanometer tube loaded type modified Nano catalysis material of the nitrogen oxide that obtains degrading.
Among the present invention, Detitanium-ore-type and rutile-type account for respectively 75% and 25% in the described nano titanium oxide mixed crystal; The caliber of described CNT is that 30～40nm, length are the multi-walled carbon nano-tubes about 1um.
Compared with prior art, the invention has the beneficial effects as follows:
Preparation technology of the present invention is simple, the carbon nanometer tube loaded type modified Nano catalysis material that makes is because through silver ion modification and nano-carbon tube load, possessed better nitrogen oxide photocatalysis effect, especially the effect under the visible light be improved significantly, simultaneously the long-lasting of photocatalysis effect also significantly improves.For this most frequently used nano-photocatalyst material of nano titanium oxide mixed crystal, because the restriction of its valence band width is so that excitation wavelength is positioned at ultraviolet region, photocatalysis effect under the visible light is very poor, after mixing by silver ion, excitation wavelength generation red shift so that the photocatalysis effect under the visible light be improved; In addition, because huge specific area easy adsorption of modification nano titanium oxide mixed crystal and the nitrogen oxide of CNT, effectively avoided the reunion of modified nano-titanium dioxide mixed crystal, also increased the contact probability of modified nano-titanium dioxide mixed crystal and nitrogen oxide, so that photocatalysis efficiency is further promoted, the electronics more than needed of while CNT and the translational speed that excellent conductive performance has also enlarged electronics and hole are poor, thereby reduced the probability of burying in oblivion of electron hole pair, therefore this carbon nanometer tube loaded type modified Nano catalysis material possesses very good photo-catalysis function.
The specific embodiment
Below the present invention is further described by example.
Embodiment 1
(1) the nano titanium oxide mixed crystal is placed the ultrasonic dispersion of water 25 minutes, then put into the AgNO3 solution of 0.3mol/L, add part ethanol and then stir 30min;
(2) place continuation stirring 90min under the uviol lamp, after the filtration filter residue is placed on 400 ℃ of lower calcinings 2 hours, obtain the nano titanium oxide mixed crystal of modification;
(3) with the nano titanium oxide mixed crystal of modification and the CNT ratio batch mixing 2h by weight 1: 0.01, the carbon nanometer tube loaded type modified Nano catalysis material of the nitrogen oxide that obtains degrading.
This material can (wherein the light intensity of 254nm, 290nm, 365nm and 420nm is respectively 4.2,1.5,19 and 165 μ W/cm2) photochemical catalytic oxidation be passed through continuously under the solar simulated condition concentration be the nitrogen dioxide gas of 30ppm, its photocatalysis efficiency reaches 73.3%, after the successive reaction 7.5 hours, photocatalysis efficiency still reaches 46.6%.
Embodiment 2
(1) the nano titanium oxide mixed crystal is placed the ultrasonic dispersion of water 30 minutes, then put into the AgNO3 solution of 0.5mol/L, add part ethanol and then stir 40min;
(2) place continuation stirring 90min under the uviol lamp, after the filtration filter residue is placed on 450 ℃ of lower calcinings 4 hours, obtain the nano titanium oxide mixed crystal of modification;
(3) with the nano titanium oxide mixed crystal of modification and the CNT ratio batch mixing 2h by weight 1: 0.01, the carbon nanometer tube loaded type modified Nano catalysis material of the nitrogen oxide that obtains degrading.
This material can (wherein the light intensity of 254nm, 290nm, 365nm and 420nm is respectively 4.3,1.5,17 and 166 μ W/cm2) photochemical catalytic oxidation be passed through continuously under the solar simulated condition concentration be the nitrogen dioxide gas of 30ppm, its photocatalysis efficiency reaches 75.1%, after the successive reaction 7.5 hours, photocatalysis efficiency still reaches 47.8%.
Embodiment 3
(1) the nano titanium oxide mixed crystal is placed the ultrasonic dispersion of water 30 minutes, then put into the AgNO3 solution of 0.5mol/L, add part ethanol and then stir 40min;
(2) place continuation stirring 90min under the uviol lamp, after the filtration filter residue is placed on 450 ℃ of lower calcinings 4 hours, obtain the nano titanium oxide mixed crystal of modification;
(3) with the nano titanium oxide mixed crystal of modification and the CNT ratio batch mixing 4h by weight 1: 0.015, the carbon nanometer tube loaded type modified Nano catalysis material of the nitrogen oxide that obtains degrading.
This material can (wherein the light intensity of 254nm, 290nm, 365nm and 420nm is respectively 4.3,1.5,18 and 167 μ W/cm2) photochemical catalytic oxidation be passed through continuously under the solar simulated condition concentration be the nitrogen dioxide gas of 30ppm, its photocatalysis efficiency reaches 76.5%, after the successive reaction 7.5 hours, photocatalysis efficiency still reaches 48.3%.
Method of the present invention is mixed by silver ion on the one hand and has been reduced the bandwidth of nano titanium oxide mixed crystal, so that excitation wavelength is to the visible region red shift, thereby has improved the photocatalysis efficiency under the visible light; On the other hand, adopt nano-carbon tube load modified nano-titanium dioxide mixed crystal, effectively prevent the nano titanium oxide mixed crystal reunion, promote effective dispersion of nano titanium oxide mixed crystal and contact with the effective of nitrogen oxide, electronics more than needed and the good conductive function of while CNT, more help to reduce the probability of burying in oblivion of electron hole pair, thereby give nano-carbon tube load modified nano-titanium dioxide mixed crystal nitrogen oxide photo-catalysis function good and steady in a long-term is arranged.
What more than enumerate only is specific embodiments of the invention.Obviously, the invention is not restricted to above examples of implementation, in the protection domain of spirit of the present invention and claim, to any modification and the change that the present invention makes, all should think protection scope of the present invention.
Claims (2)
1. the preparation method of the carbon nanometer tube loaded type modified Nano catalysis material of the nitrogen oxide of degrading may further comprise the steps:
(1) the nano titanium oxide mixed crystal is placed the ultrasonic dispersion of water 20～30 minutes, then put into the AgNO of 0.3～0.5mol/L
3In the solution, add part ethanol and then stir 30～40min;
(2) place continuation stirring 90min under the uviol lamp, after the filtration filter residue is placed on 400～450 ℃ of lower calcinings 2～3 hours, obtain the nano titanium oxide mixed crystal of modification;
(3) with the nano titanium oxide mixed crystal of modification and the CNT ratio batch mixing 2～4h by weight 1: 0.01～0.015, the carbon nanometer tube loaded type modified Nano catalysis material of the nitrogen oxide that obtains degrading;
Wherein Detitanium-ore-type and rutile-type account for respectively 75% and 25% in the nano titanium oxide mixed crystal.
2. the preparation method of the carbon nanometer tube loaded type modified Nano catalysis material of the nitrogen oxide of degrading according to claim 1, the caliber that it is characterized in that described CNT is that 30～40nm, length are the multi-walled carbon nano-tubes about 1 μ m.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102500356A (en) * | 2011-11-11 | 2012-06-20 | 东华大学 | Preparation method for carbon nanotube-nano-bismuth vanadate composite photocatalyst |
| CN104787841B (en) * | 2015-04-30 | 2017-01-11 | 扬州大学 | Preparation method of three-dimensional macroporous carbon/carbon nanotube/titanium dioxide/silver composite material capable of catalytically degrading unsymmetrical dimethylhydrazine |
| CN106752113B (en) * | 2016-12-14 | 2019-02-19 | 浙江恒逸高新材料有限公司 | A kind of preparation method and application of modifying titanium dioxide |
| CN109012744B (en) * | 2018-09-20 | 2021-06-11 | 四川文理学院 | Method for degrading nitrogen oxide by visible light catalysis |
| CN110184632A (en) * | 2019-06-20 | 2019-08-30 | 佛山市众之助新材料科技有限公司 | A method of in metal surface nickel plating ferrophosphor(us) |
| CN111085107A (en) * | 2019-11-25 | 2020-05-01 | 苏交科集团股份有限公司 | Method for purifying vehicle tail gas by porous asphalt pavement loaded composite modified photocatalyst |
| CN113058580B (en) * | 2021-03-26 | 2022-07-15 | 曲阜师范大学 | Preparation method of carbon nano tube/silver nano particle/titanium dioxide visible-light-driven photocatalyst |
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|---|---|---|---|---|
| CN1680023A (en) * | 2004-07-15 | 2005-10-12 | 清华大学 | Light catalyst for nanometer carrier |
| CN1868589A (en) * | 2006-06-22 | 2006-11-29 | 厦门大学 | Method for preparing carbon nanometer tube/titanium dioxide composite photocatalyst |
| CN101704641A (en) * | 2009-11-23 | 2010-05-12 | 浙江大学 | Preparation method of nano-photocatalytic admixture for cement-based material |
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| JP2004148305A (en) * | 2002-10-11 | 2004-05-27 | Osaka Gas Co Ltd | Photocatalyst and air cleaner using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1680023A (en) * | 2004-07-15 | 2005-10-12 | 清华大学 | Light catalyst for nanometer carrier |
| CN1868589A (en) * | 2006-06-22 | 2006-11-29 | 厦门大学 | Method for preparing carbon nanometer tube/titanium dioxide composite photocatalyst |
| CN101704641A (en) * | 2009-11-23 | 2010-05-12 | 浙江大学 | Preparation method of nano-photocatalytic admixture for cement-based material |
Non-Patent Citations (2)
| Title |
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| JP特开2004-148305A 2004.05.27 |
| Shuo Wang et al..Preparation and photocatalytic properties of silver nanoparticles loaded on CNTs/TiO2 composite.《Applied Surface Science》.2009,第255卷8063-8066. * |
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