CN105771951A - Carbon-titanium composite nanofiber supported catalyst and preparation method and application thereof - Google Patents
Carbon-titanium composite nanofiber supported catalyst and preparation method and application thereof Download PDFInfo
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- CN105771951A CN105771951A CN201610153723.4A CN201610153723A CN105771951A CN 105771951 A CN105771951 A CN 105771951A CN 201610153723 A CN201610153723 A CN 201610153723A CN 105771951 A CN105771951 A CN 105771951A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 86
- 239000002121 nanofiber Substances 0.000 title claims abstract description 79
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- CYKMNKXPYXUVPR-UHFFFAOYSA-N [C].[Ti] Chemical compound [C].[Ti] CYKMNKXPYXUVPR-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000003197 catalytic effect Effects 0.000 claims abstract description 16
- 239000010936 titanium Substances 0.000 claims abstract description 15
- 229910000314 transition metal oxide Inorganic materials 0.000 claims abstract description 12
- 238000009987 spinning Methods 0.000 claims abstract description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 239000007833 carbon precursor Substances 0.000 claims abstract description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 7
- 150000001299 aldehydes Chemical class 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 150000002576 ketones Chemical class 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 5
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 16
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 16
- 239000005030 aluminium foil Substances 0.000 claims description 14
- 238000010041 electrostatic spinning Methods 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 230000005685 electric field effect Effects 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- 229910044991 metal oxide Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 239000000356 contaminant Substances 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 239000003112 inhibitor Substances 0.000 claims description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- -1 carbon metal oxide Chemical class 0.000 claims description 3
- 238000006477 desulfuration reaction Methods 0.000 claims description 3
- 230000023556 desulfurization Effects 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229940049706 benzodiazepine Drugs 0.000 claims description 2
- 150000001557 benzodiazepines Chemical class 0.000 claims description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 2
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 2
- 238000005421 electrostatic potential Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 2
- AXLMPTNTPOWPLT-UHFFFAOYSA-N prop-2-enyl 3-oxobutanoate Chemical compound CC(=O)CC(=O)OCC=C AXLMPTNTPOWPLT-UHFFFAOYSA-N 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 2
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 2
- 238000001523 electrospinning Methods 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 22
- 238000013019 agitation Methods 0.000 description 8
- 239000012855 volatile organic compound Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 230000009257 reactivity Effects 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 102100021935 C-C motif chemokine 26 Human genes 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 101000897493 Homo sapiens C-C motif chemokine 26 Proteins 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
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- Biomedical Technology (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention relates to a carbon-titanium composite nanofiber supported catalyst and a preparation method and application thereof. By carbon-titanium composite nanofibers serving as supporters and transition metal oxides serving as active components, the active components are led into a spinning solution in situ to obtain the catalyst with supporting capacity being 0-50%. The preparation method includes: preparing a precursor solution containing carbon precursors, titanium precursors and the active components; obtaining nanofibers of precursor components according to an electrospinning method; performing high-temperature calcination in a nitrogen atmosphere. The catalyst which takes the carbon-titanium composite nanofibers as the supporters integrates advantages of large specific area and favorable low-temperature activity of carbon supporters and advantages of property stability and large quantity of acid sites of TiO2 supporters and has a wide catalytic temperature window and favorable reaction activity. In addition, the preparation method is simple in process, the raw materials are easy to acquire, and the carbon-titanium composite nanofiber supported catalyst is a novel high-efficiency low-cost catalyst applicable to catalytic oxidation removal of volatile organic pollutants such as ketones and aldehydes.
Description
Technical field
The invention belongs to chemical catalyst and preparing technical field thereof, concretely relate to a kind of loaded catalyst and its preparation method and application being carrier with carbon titanium composite nano fiber.
Background technology
China is an energy-consuming big country, primary energy consumption structure based on coal, coal combustion generate SO2、NOx, hydrargyrum, two English, the pollutant such as volatile organic matter make China become one of country the most serious of atmospheric pollution in the world.Wherein volatile organic matter (VolatileOrganicCompounds, it is called for short VOCs) refer to that under room temperature, saturated vapor pressure, more than the boiling point organic compound lower than 260 DEG C under 70Pa, normal pressure, mainly includes aromatic hydrocarbon, aliphatic hydrocarbon, halogenated hydrocarbons, alcohols, aldehydes, ketone and esters etc..The discharge of VOCs not only results in the environmental problems such as greenhouse effect, depletion of the ozone layer, photochemical fog, but also health can produce serious harm.The General Office of the State Council proposes to carry out volatile organic matter prevention and cure of pollution work from State-level to first official for 2010 in " about advancing atmospheric pollution groupcontrol job guide suggestion ", is classified as the priority pollutant of atmospheric pollution groupcontrol.Therefore, the discharge how efficiently and economically reducing volatile organic matter (VOCs) has great significance for administering China's atmospheric pollution.
In the control technology of VOCs, introduce the catalysed oxidation processes after catalyst owing to having the significant advantages such as can carry out, removal efficiency is higher, applied widely, operation is simple at low concentrations, thus become most one of removal methods with application prospect at present.In prior art, the carrier of catalyst is substantially the employing organic material such as metal-oxide or graphite, activated carbon, resin.Chinese patent CN102824909A discloses a kind of with Al2O3For carrier, the catalyst being active component with precious metals pd, the oxidation reaction of the VOCs such as benzene,toluene,xylene, ethyl acetate, ethanol, propane is had significantly high catalysis activity.Chinese patent CN104138756A discloses a kind of loaded catalyst RTCC-1 being carrier with TSC-1 mesoporous carbon, and active component is a kind of in conjunction with one or more metal-oxides in copper oxide, cerium oxide, zirconium oxide, silicon oxide, aluminium oxide in Pd or Pt noble metal.But in above-mentioned catalyst, although with the organic material such as mesoporous carbon, graphite be carrier catalyst there is good low temperature active, but owing to carrier surface acid site is less, the carrying out of catalytic reaction is had certain restriction；With Al2O3、TiO2Deng the catalyst that metal-oxide is carrier, there is when high temperature good reactivity, but the catalysis activity when low-temp reaction is poor.Although and the introducing of noble metal active component enhances reactivity in catalyst, but also improving the preparation cost of catalyst, hardly resulting in and being widely applied.
Therefore, how to prepare and there is wider reaction temperature window, good catalysis activity, prepare catalyst simple, with low cost and become in current VOCs catalytic eliminating technology most one of direction with Research Prospects.
Summary of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of loaded catalyst and its preparation method and application being carrier with carbon titanium composite nano fiber.Catalyst of the present invention is big in combination with carbon carrier specific surface area, low temperature active is good advantage and TiO2The advantage that support is stable, sour site is many, there is wider catalytic temperature window and good reactivity, simultaneously preparation process is simple, raw material is easy to get, it is the catalyst of a kind of New high-efficient low-cost, it is adaptable to industry and the catalytic eliminating of the volatile organic contaminant such as aromatics, ketone, aldehydes in life.
A kind of be carrier with carbon titanium composite nano fiber loaded catalyst, the carbon titanium composite nano fiber that described catalyst is prepared with electrostatic spinning technique is for carrier, and with transition metal oxide for active component, wherein, the load capacity of described active component is 0～50%.
As preferably, described transition metal oxide is V2O5、Co3O4、MnO2、Cr2O3In the combination in any of one or two or more kinds.
As preferably, described carbon titanium composite nano fiber diameter is 100～500nm.
As preferably, described active component particles diameter is 2～100nm.
As preferably, the specific surface area of described catalyst is 50～200m2/g。
The preparation method of a kind of loaded catalyst being carrier with carbon titanium composite nano fiber, comprises the following steps:
(1) preparation solution
Taking polyvinylpyrrolidone and add in dehydrated alcohol as carbon precursor, stirring, to being completely dissolved, adds titanium precursors, active component presoma and hydrolysis inhibitor, and under room temperature, stirring obtains the precursor solution of spinning；
(2) electrostatic spinning
Precursor solution is irrigated jet by syringe, solution jet is stretched by high voltage electric field effect, is solidified, and to be wrapped in the accepter as fiber of the aluminium foil on cylinder, obtains the nanofiber of presoma component；
(3) calcining
In a nitrogen atmosphere, the nanofiber obtained after spinning is carried out high-temperature calcination, naturally cool to room temperature subsequently, finally give the catalyst of the carbon metal oxide-loaded active component of titanium composite nano fiber.
As preferably, the molal weight of described polyvinylpyrrolidone is 45000～55000g/mol.
As preferably, described titanium precursors is the combination in any of one or two or more kinds in butyl titanate, isopropyl titanate, titanium tetrachloride, titanium sulfate, titanyl sulfate；Described hydrolysis inhibitor is the combination in any of one or two or more kinds in glacial acetic acid, hydrochloric acid, triethanolamine, acrylic acid, neck Benzodiazepines, acetoacetic acid allyl ester, acetylacetone,2,4-pentanedione, sulphuric acid, nitric acid, phosphoric acid.
As preferably, in the preparation process of catalyst, the electrostatic potential that electrostatic spinning applies is 5～30kV, and receiving range is 10～25cm, and drum rotation speed is 50～100r/min, and syringe rate of flooding is 0.5～3mL/min；In calcination process, heating rate is 1～10 DEG C/min, and calcining heat is 400～500 DEG C.
The application of a kind of loaded catalyst being carrier with carbon titanium composite nano fiber, described catalyst is for aromatics, ketone, aldehydes volatile organic contaminant catalytic oxidative desulfurization in industrial tail gas and life.
The advantages such as the catalyst of the present invention has that preparation technology is simple, raw material is easy to get, removal efficiency height, long service life, the suitability are wide, it is adaptable to industrial tail gas and the volatile organic contaminant catalytic oxidative desulfurization such as aromatics, ketone, aldehydes in living.The present invention, with carbon titanium composite nano fiber for carrier, combines carbon carrier specific surface area is big, low temperature active is good advantage and TiO2The advantage that support is stable, sour site is many, has wider catalytic temperature window and good reactivity, has opened up the preparation method and application field of new catalytic filtering material, have stronger economy and good application prospect.
Accompanying drawing explanation
Fig. 1 is the XRD diffraction pattern of the nano-fiber catalyst obtained in embodiment 1；
Fig. 2 is the XRD diffraction pattern of the nano-fiber catalyst obtained in embodiment 2；
Fig. 3 is the XRD diffraction pattern of the nano-fiber catalyst obtained in embodiment 3；
Fig. 4 is the XRD diffraction pattern of the nano-fiber catalyst obtained in embodiment 4；
Fig. 5 is the scanning electron microscope image of the nano-fiber catalyst obtained in embodiment 3；
Fig. 6 is the curve that the conversion ratio of acetone catalytic oxidation is varied with temperature by the nano-fiber catalyst obtained in the embodiment of the present invention 1～4.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described, but invention which is intended to be protected is not limited to this.The technology related in embodiment, unless stated otherwise, is routine operation known in the art；The reagent that used, instrument, unless stated otherwise, all can be obtained by public approach.
Embodiment 1
A kind of be carrier with carbon titanium composite nano fiber loaded catalyst, the carbon titanium composite nano fiber that described catalyst is prepared with electrostatic spinning technique is for carrier, and with transition metal oxide for active component, wherein, the load capacity of described active component is 0%.
Described carbon titanium composite nano fiber diameter is 150nm, and the specific surface area of described catalyst is 122.6m2/g。
The preparation method of the above-mentioned loaded catalyst being carrier with carbon titanium composite nano fiber, specifically includes following steps:
(1) preparation solution
Take 1.5g polyvinylpyrrolidone (PVP, molal weight is 55000g/mol) as carbon precursor, add in 15mL dehydrated alcohol, magnetic agitation 30min to PVP is completely dissolved, add 3mL butyl titanate and 3mL glacial acetic acid, being made into the solution of V/Ti=0%, under room temperature, magnetic agitation 18h obtains precursor solution；
(2) electrostatic spinning
Plastic injector takes 9mL precursor solution, is fixed on the position of distance centre of the drum 15cm, and cylinder wraps up the aluminium foil reception device as nanofiber；Add high pressure power supply 15kV, drum rotation speed 50r/min at syringe rustless steel syringe needle place, and syringe rate of flooding is 1mL/min；Solution jet is stretched by high voltage electric field effect, solidifies, obtain the nanofiber of presoma component.
(3) calcining
After spinning terminates, take off aluminium foil in room temperature environment, place 12h, make nanofiber be fully hydrolyzed；Aluminium foil after placing is contained in crucible, puts into tube furnace and calcine in a nitrogen atmosphere, make fibers carbonization and remove organic component；Programming rate with 1 DEG C/min, it is heated to 200 DEG C from room temperature and keeps 1h, it is warming up to 500 DEG C with the speed of 1 DEG C/min again and keeps 1h, naturally cooling to room temperature, finally giving the catalyst (C-TiO of the carbon metal oxide-loaded active component of titanium composite nano fiber2Nano-fiber catalyst).
The XRD diffraction pattern of the nano-fiber catalyst that said method prepares is as shown in Figure 1.
Embodiment 2
A kind of be carrier with carbon titanium composite nano fiber loaded catalyst, the carbon titanium composite nano fiber that described catalyst is prepared with electrostatic spinning technique is for carrier, with transition metal oxide for active component, wherein, the load capacity of described active component is 10%, and described transition metal oxide is V2O5。
Described carbon titanium composite nano fiber diameter is 187nm, and described active component particles diameter is 5.8nm, and the specific surface area of described catalyst is 83.2m2/g。
The preparation method of the above-mentioned loaded catalyst being carrier with carbon titanium composite nano fiber, specifically includes following steps:
(1) preparation solution
Take 1.5g polyvinylpyrrolidone (PVP, molal weight is 55000g/mol) as carbon precursor, add in 15mL dehydrated alcohol, magnetic agitation 30min to PVP is completely dissolved, add 3mL butyl titanate, 0.213g vanadyl acetylacetonate and 3mL glacial acetic acid, being made into the solution of V/Ti=10%, under room temperature, magnetic agitation 18h obtains precursor solution；
(2) electrostatic spinning
Plastic injector takes 9mL precursor solution, is fixed on the position of distance centre of the drum 15cm, and cylinder wraps up the aluminium foil reception device as nanofiber；Add high pressure power supply 15kV, drum rotation speed 50r/min at rustless steel syringe needle place, and syringe rate of flooding is 1mL/min；Solution jet is stretched by high voltage electric field effect, solidifies, obtain the nanofiber of presoma component；
(3) calcining
After spinning terminates, take off aluminium foil in room temperature environment, place 12h, make nanofiber be fully hydrolyzed；Aluminium foil after placing is contained in crucible, puts into tube furnace and calcine in a nitrogen atmosphere, make fibers carbonization and remove organic component；With the programming rate of 1 DEG C/min, it is heated to 200 DEG C from room temperature and keeps 1h, then be warming up to 500 DEG C with the speed of 1 DEG C/min and keep 1h, naturally cool to room temperature, finally give the V/C-TiO of V/Ti=10%2Nano-fiber catalyst.
The XRD diffraction pattern of the nano-fiber catalyst that said method prepares is as shown in Figure 2.
Embodiment 3
A kind of be carrier with carbon titanium composite nano fiber loaded catalyst, the carbon titanium composite nano fiber that described catalyst is prepared with electrostatic spinning technique is for carrier, with transition metal oxide for active component, wherein, the load capacity of described active component is 20%, and described transition metal oxide is V2O5。
Described carbon titanium composite nano fiber diameter is 192nm, and described active component particles diameter is 6.7nm, and the specific surface area of described catalyst is 68.8m2/g。
The preparation method of the above-mentioned loaded catalyst being carrier with carbon titanium composite nano fiber, specifically includes following steps:
(1) preparation solution
Take 1.5g polyvinylpyrrolidone (PVP, molal weight is 55000g/mol) as carbon precursor, add in 15mL dehydrated alcohol, magnetic agitation 30min to PVP is completely dissolved, add 3mL butyl titanate, 0.425g vanadyl acetylacetonate and 3mL glacial acetic acid, being made into the solution of V/Ti=20%, under room temperature, magnetic agitation 18h obtains precursor solution；
(2) electrostatic spinning
Plastic injector takes 9mL precursor solution, is fixed on the position of distance centre of the drum 15cm, and cylinder wraps up the aluminium foil reception device as nanofiber；Add high pressure power supply 15kV, drum rotation speed 50r/min at rustless steel syringe needle place, and syringe rate of flooding is 1mL/min；Solution jet is stretched by high voltage electric field effect, solidifies, obtain the nanofiber of presoma component；
(3) calcining
After spinning terminates, take off aluminium foil in room temperature environment, place 12h, make nanofiber be fully hydrolyzed.Aluminium foil after placing is contained in crucible, puts into tube furnace and calcine in a nitrogen atmosphere, make fibers carbonization and remove organic component；With the programming rate of 1 DEG C/min, it is heated to 200 DEG C from room temperature and keeps 1h, then be warming up to 500 DEG C with the speed of 1 DEG C/min and keep 1h, naturally cool to room temperature, finally give the V/C-TiO of V/Ti=20%2Nano-fiber catalyst.
The XRD diffraction pattern of the nano-fiber catalyst that said method prepares as it is shown on figure 3, scanning electron microscope image as shown in Figure 5.
Embodiment 4
A kind of be carrier with carbon titanium composite nano fiber loaded catalyst, the carbon titanium composite nano fiber that described catalyst is prepared with electrostatic spinning technique is for carrier, with transition metal oxide for active component, wherein, the load capacity of described active component is 50%, and described transition metal oxide is V2O5。
Described carbon titanium composite nano fiber diameter is 198nm, and described active component particles diameter is 7.8nm, and the specific surface area of described catalyst is 53.7m2/g。
The preparation method of the above-mentioned loaded catalyst being carrier with carbon titanium composite nano fiber, specifically includes following steps:
(1) preparation solution
Take 1.5g polyvinylpyrrolidone (PVP, molal weight is 55000g/mol) as carbon precursor, add in 15mL dehydrated alcohol, magnetic agitation 30min to PVP is completely dissolved, add 3mL butyl titanate, 1.062g vanadyl acetylacetonate and 3mL glacial acetic acid, being made into the solution of V/Ti=50%, under room temperature, magnetic agitation 18h obtains precursor solution；
(2) electrostatic spinning
Plastic injector takes 9mL precursor solution, is fixed on the position of distance centre of the drum 15cm, and cylinder wraps up the aluminium foil reception device as nanofiber；Add high pressure power supply 15kV, drum rotation speed 50r/min at rustless steel syringe needle place, and syringe rate of flooding is 1mL/min；Solution jet is stretched by high voltage electric field effect, solidifies, obtain the nanofiber of presoma component；
(3) calcining
After spinning terminates, take off aluminium foil in room temperature environment, place 12h, make nanofiber be fully hydrolyzed；Aluminium foil after placing is contained in crucible, puts into tube furnace and calcine in a nitrogen atmosphere, make fibers carbonization and remove organic component；With the programming rate of 1 DEG C/min, it is heated to 200 DEG C from room temperature and keeps 1h, then be warming up to 500 DEG C with the speed of 1 DEG C/min and keep 1h, naturally cool to room temperature, finally give the V/C-TiO of V/Ti=50%2Nano-fiber catalyst.
The XRD diffraction pattern of the nano-fiber catalyst that said method prepares is as shown in Figure 4.
Catalytic performance is tested
Grinding is sieved, and the granule taking 40～60 order sizes carries out catalytic eliminating performance test in VOCs removal efficiency experimental apparatus for testing.
The nano-fiber catalyst taking 45mg is placed on the central authorities of reactor, and unstrpped gas general gas flow is 60ml/min, and corresponding gas hourly space velocity (GHSV) is 20000h-1, unstrpped gas comprises 500ppm acetone and 5%O2, N2As Balance Air.
In order to ensure the safety and reliability of experiment, blank experiment is with rubble sand (40～60 order), in identical unstripped gas condition, and less than the 300 DEG C thermal decompositions not finding acetone.
The temperature E type thermocouple of catalytic bed and tubular heater is measured automatically, and the acetone concentration of entrance and exit measures with on-line gas chromatography (Agilent789A, USA) and flame ionization ditector (FID) at 60 DEG C.The computing formula of acetone removal efficiency is as follows:
In formula: η acetone conversion
cin,coutThe concentration of import and export place acetone
Each embodiment with carbon titanium composite nano fiber be carrier loaded catalyst (nano-fiber catalyst) when 300 DEG C the removal efficiency result of acetone is as shown in table 1:
Table 1
| Nano-fiber catalyst | Acetone removal efficiency |
| Embodiment 1 | 90% |
| Embodiment 2 | 96% |
| Embodiment 3 | 100% |
| Embodiment 4 | 87% |
The curve that the conversion ratio of acetone catalytic oxidation is varied with temperature by the nano-fiber catalyst obtained in embodiment 1～4 is as shown in Figure 6.
From test result it can be seen that the nano-fiber catalyst of embodiment 3 shows higher reactivity, at acetone concentration 500ppm, air speed 20000h-1When, removal efficiency when 300 DEG C can reach 100%, and the removal efficiency of the nano-fiber catalyst of embodiment 4 is only 87%.This is due to the V/C-TiO in embodiment 32Nano-fiber catalyst has higher active component content and bigger specific surface area, catalytic oxidation can promote to the mass transport process such as reactant and the diffusion of product, Adsorption and desorption be attached, concurrently facilitate the active component avtive spot in the high degree of dispersion of catalyst surface, increase reaction, thus there is good catalytic reaction activity.
Above-described embodiment is only the preferred embodiment of the present invention, its object is to be more fully understood that the technology design of the present invention and feature, can not limit the scope of the invention with this.Described embodiment can be made amendment or supplements or adopt equivalent way to substitute by the research worker of art, without departing from the range of definition of the present invention.
Claims (10)
1. the loaded catalyst that a kind is carrier with carbon titanium composite nano fiber, it is characterized in that: the carbon titanium composite nano fiber that described catalyst is prepared with electrostatic spinning technique is for carrier, with transition metal oxide for active component, wherein, the load capacity of described active component is 0～50%.
2. according to claim 1 be carrier with carbon titanium composite nano fiber loaded catalyst, it is characterised in that: described transition metal oxide is V2O5、Co3O4、MnO2、Cr2O3In the combination in any of one or two or more kinds.
3. according to claim 1 be carrier with carbon titanium composite nano fiber loaded catalyst, it is characterised in that: described carbon titanium composite nano fiber diameter is 100～500nm.
4. according to claim 1 be carrier with carbon titanium composite nano fiber loaded catalyst, it is characterised in that: described active component particles diameter is 2～100nm.
5. according to claim 1 be carrier with carbon titanium composite nano fiber loaded catalyst, it is characterised in that: the specific surface area of described catalyst is 50～200m2/g。
6. the preparation method of catalyst described in a claim 1, it is characterised in that comprise the following steps:
(1) preparation solution
Taking polyvinylpyrrolidone and add in dehydrated alcohol as carbon precursor, stirring, to being completely dissolved, adds titanium precursors, active component presoma and hydrolysis inhibitor, and under room temperature, stirring obtains the precursor solution of spinning；
(2) electrostatic spinning
Precursor solution is irrigated jet by syringe, solution jet is stretched by high voltage electric field effect, is solidified, and to be wrapped in the reception device as fiber of the aluminium foil on cylinder, obtains the nanofiber of presoma component；
(3) calcining
In a nitrogen atmosphere, the nanofiber obtained after spinning is carried out high-temperature calcination, naturally cool to room temperature subsequently, finally give the catalyst of the carbon metal oxide-loaded active component of titanium composite nano fiber.
7. the preparation method of catalyst according to claim 6, it is characterised in that: the molal weight of described polyvinylpyrrolidone is 45000～55000g/mol.
8. the preparation method of catalyst according to claim 6, it is characterised in that: described titanium precursors is the combination in any of one or two or more kinds in butyl titanate, isopropyl titanate, titanium tetrachloride, titanium sulfate, titanyl sulfate；Described hydrolysis inhibitor is the combination in any of one or two or more kinds in glacial acetic acid, hydrochloric acid, triethanolamine, acrylic acid, neck Benzodiazepines, acetoacetic acid allyl ester, acetylacetone,2,4-pentanedione, sulphuric acid, nitric acid, phosphoric acid.
9. the preparation method of catalyst according to claim 6, it is characterized in that: in the preparation process of catalyst, the electrostatic potential that electrostatic spinning applies is 5～30kV, and receiving range is 10～25cm, drum rotation speed is 50～100r/min, and syringe rate of flooding is 0.5～3mL/min；In calcination process, heating rate is 1～10 DEG C/min, and calcining heat is 400～500 DEG C.
10. the application of the catalyst described in a claim 1, it is characterised in that: described catalyst is for aromatics, ketone, aldehydes volatile organic contaminant catalytic oxidative desulfurization in industrial tail gas and life.
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