CN108097204A - Ultra-thin coated by titanium dioxide aerosil column of toxic gas and preparation method thereof can be purified - Google Patents
Ultra-thin coated by titanium dioxide aerosil column of toxic gas and preparation method thereof can be purified Download PDFInfo
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- CN108097204A CN108097204A CN201810119375.8A CN201810119375A CN108097204A CN 108097204 A CN108097204 A CN 108097204A CN 201810119375 A CN201810119375 A CN 201810119375A CN 108097204 A CN108097204 A CN 108097204A
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- Prior art keywords
- titanium dioxide
- ultra
- column
- aerosil
- thin coated
- Prior art date
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 242
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 116
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 229910002012 Aerosil® Inorganic materials 0.000 title claims abstract description 74
- 239000002341 toxic gas Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 33
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 33
- 239000001301 oxygen Substances 0.000 claims description 33
- 229910052760 oxygen Inorganic materials 0.000 claims description 33
- 229910052719 titanium Inorganic materials 0.000 claims description 33
- 239000010936 titanium Substances 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 238000010926 purge Methods 0.000 claims description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 238000000137 annealing Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 9
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical group CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 9
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 9
- 239000012498 ultrapure water Substances 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 18
- 238000007146 photocatalysis Methods 0.000 abstract description 14
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 238000005253 cladding Methods 0.000 abstract description 12
- 239000011148 porous material Substances 0.000 abstract description 11
- 239000003054 catalyst Substances 0.000 abstract description 9
- 239000003463 adsorbent Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 239000002250 absorbent Substances 0.000 abstract description 2
- 230000002745 absorbent Effects 0.000 abstract description 2
- 229960005196 titanium dioxide Drugs 0.000 description 94
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 14
- 239000000243 solution Substances 0.000 description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 241000790917 Dioxys <bee> Species 0.000 description 8
- 229910003978 SiClx Inorganic materials 0.000 description 7
- 238000012512 characterization method Methods 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 5
- 238000001237 Raman spectrum Methods 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000004965 Silica aerogel Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- 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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
-
- 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
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- 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
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/08—Silica
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/405—Oxides of refractory metals or yttrium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/106—Silica or silicates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20707—Titanium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/80—Type of catalytic reaction
- B01D2255/802—Photocatalytic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/93—Toxic compounds not provided for in groups B01D2257/00 - B01D2257/708
Abstract
The present invention relates to physical absorbents and chemical photo-catalysts technical field, and in particular to a kind of ultra-thin coated by titanium dioxide aerosil column for purifying toxic gas and preparation method thereof.It solves catalyst in the prior art and is carried on the method for adsorbent surfaces externally and internally easily to make its mesoporous the technical issues of with transparency reduction absorption property and photocatalysis performance being caused to reduce of narrowing.The present invention realizes ultra-thin cladding of the titanium dioxide in aerosil column surfaces externally and internally using technique for atomic layer deposition, hardly changes the original pore passage structure of airsetting rubber column gel column, so as to ensure the high absorption property of composite material；It ensure that the high grade of transparency of composite material to greatest extent, the uniform light capture of airsetting rubber column gel column inside and outside titanium dioxide realized, so as to ensure the high photocatalysis performance of composite material.
Description
Technical field
The present invention relates to physical absorbents and chemical photo-catalysts technical field, and in particular to one kind can purify toxic gas
Ultra-thin coated by titanium dioxide aerosil column and preparation method thereof.
Background technology
Today's society, the safety of toxic gas serious threat mankind air environment.In view of the mankind to air environment
Continuing reliance on property, the method that searching effectively removes toxic gas in a short time are then particularly important.Physical absorption can will have
Poisonous gas quick adsorption is a kind of fast effective treating method, however absorption belongs to physical world, it is impossible to really drop in surface
Solve toxic gas.On the contrary, toxic gas can be thoroughly degraded to harmless by-product by chemical photochemical catalytic oxidation using solar energy, so
And toxic gas needs the regular hour in the decomposition of photocatalyst surface.Integrate the advantage of the two, physical absorption and chemical light
The quick of concentration of toxic gases, which can be achieved, in the combination of catalysis oxidation reduces and sustainedly and stably decomposes.
Effectively to combine physical absorption and chemical photochemical catalytic oxidation, the selection of adsorbent and catalyst is most important.It is inhaling
Subsidiary formula face, aerosil column have higher specific surface area and abundant mesopore orbit, can largely and rapidly adsorb
Toxic gas.Aerosil column has higher optical clarity simultaneously, is good catalyst carrier.In catalysis side
Face, titanium dioxide have many advantages, such as suitable position of energy band, physical and chemical stability, nontoxic, are a kind of potential light
Catalysis material.
Design the combination of adsorbent and catalyst, can by titanium dichloride load aerosil column interior appearance
Face.However, the method that general catalyst is carried on adsorbent surfaces externally and internally easily makes its mesoporous narrows be reduced with transparency, so as to
Its specific surface area and light capture ability are influenced, is unfavorable for its absorption property and photocatalysis performance.Therefore, need to find a kind of rational
Carried titanium dioxide makes it retain the original duct of aeroge to greatest extent in the method for aerosil column inner surface
With transparency, to ensure high absorption property and photocatalysis performance.
The content of the invention
The method of adsorbent surfaces externally and internally is carried on the invention solves catalyst in the prior art easily makes its mesoporous narrow
The technical issues of with transparency reduction absorption property and photocatalysis performance being caused to reduce, provides and a kind of purifies the super of toxic gas
Thin coated by titanium dioxide aerosil column and preparation method thereof.
In order to solve the above-mentioned technical problem, technical scheme is specific as follows：
A kind of ultra-thin coated by titanium dioxide aerosil column for purifying toxic gas is to utilize atomic layer deposition
Product (ALD) technology is by coated by titanium dioxide in composite material made from aerosil column surfaces externally and internally.
In the above-mentioned technical solutions, the mass percentage of the titanium dioxide is 0.32%-1.25%.
In the above-mentioned technical solutions, the mass percentage of the titanium dioxide is 0.60%.
In the above-mentioned technical solutions, the titanium dioxide is anatase phase titanium dioxide.
A kind of preparation method for the ultra-thin coated by titanium dioxide aerosil column for purifying toxic gas is specific to wrap
Include following steps：
Aerosil column is positioned in ald chamber body by step 1, using high pure nitrogen as carrier gas, sets cavity pressure
It is by force 0.1torr~0.2torr, cavity temperature is 200 DEG C~300 DEG C, and it is 80 DEG C~100 DEG C that titanium source, which keeps temperature, and oxygen source is protected
Temperature is held as 20 DEG C~40 DEG C, opening time of titanium source electronic valve is 0.08s~0.2s, and purge time is 30s~180s, oxygen
The opening time of source electronic valve is 0.015s~0.02s, and purge time is 30s~180s, and cycle-index is followed for 100~400
Ring, operation program obtain sample to be annealed after EP (end of program), the titanium source is isopropyl titanate, and the oxygen source is ultra-pure water；
The sample to be annealed obtained in step 1 is put into Muffle furnace by step 2, and the heating rate for setting Muffle furnace is 5
DEG C/min~25 DEG C/min, annealing temperature be 400 DEG C~800 DEG C, annealing time be 1h~5h, rate of temperature fall for 5 DEG C/min~
25 DEG C/min, obtain ultra-thin coated by titanium dioxide aerosil column.
In the above-mentioned technical solutions, the mass percentage of the titanium dioxide is 0.32%-1.25%.
In the above-mentioned technical solutions, the mass percentage of the titanium dioxide is 0.60%.
In the above-mentioned technical solutions, the titanium dioxide is anatase phase titanium dioxide.
In the above-mentioned technical solutions, it is 0.1torr that chamber pressure is set in step 1, and cavity temperature is 200 DEG C, and titanium source is protected
Temperature is held as 80 DEG C, it is 20 DEG C that oxygen source, which keeps temperature, and titanium source electronic valve opens 0.08s, purges 30s, and oxygen source electronic valve is opened
0.015s is opened, purges 30s, cycle-index is 200 Xun Huans.
In the above-mentioned technical solutions, in step 2 annealing temperature be 500 DEG C, annealing time 3h, heating rate for 10 DEG C/
Min, rate of temperature fall are 10 DEG C/min.
The present invention chooses titanium dioxide and titanium dioxide to obtain the composite material with high absorption property and photocatalysis performance
Silica aerogel column is not limited only to titanium dioxide and aerosil column as photochemical catalyst and adsorbent,
The photochemical catalyst that other available ALD techniques are operated and the mesoporous supports materials theory that transparency is higher and specific surface area is larger
Upper is also feasible.
The beneficial effects of the invention are as follows：
(1) present invention realizes ultra-thin cladding of the titanium dioxide in aerosil column surfaces externally and internally using ALD technique,
Hardly change the original pore passage structure of airsetting rubber column gel column, so as to ensure the high absorption property of composite material；
(2) present invention realizes ultra-thin cladding of the titanium dioxide in aerosil column surfaces externally and internally using ALD technique,
It ensure that the high grade of transparency of composite material to greatest extent, realize the uniform light capture of airsetting rubber column gel column inside and outside titanium dioxide, from
And ensure the high photocatalysis performance of composite material.
Description of the drawings
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
To be illustrated more clearly that the technical solution of the application, attached drawing needed in the embodiment will be made below simple
Ground introduction, it should be apparent that, the accompanying drawings in the following description is only some embodiments described in the present invention, general for this field
For logical technical staff, other attached drawings are can also be obtained according to these attached drawings.
Fig. 1 is ultra-thin coated by titanium dioxide prepared by original aeroge, the embodiment of the present invention 1, embodiment 2 and embodiment 3
The shape appearance figure of aerosil column；
Fig. 2 is ultra-thin coated by titanium dioxide silica airsetting prepared by the embodiment of the present invention 1, embodiment 2 and embodiment 3
The content of titanium dioxide figure of rubber column gel column；
Fig. 3 is ultra-thin coated by titanium dioxide silica airsetting prepared by the embodiment of the present invention 1, embodiment 2 and embodiment 3
Raman spectrum (Raman) collection of illustrative plates of rubber column gel column；
Fig. 4 is ultra-thin coated by titanium dioxide prepared by original aeroge, the embodiment of the present invention 1, embodiment 2 and embodiment 3
The nitrogen adsorption of aerosil column-desorption isothermal curve and pore distribution curve；
Fig. 5 is ultra-thin coated by titanium dioxide prepared by original aeroge, the embodiment of the present invention 1, embodiment 2 and embodiment 3
The transmitance collection of illustrative plates of aerosil column；
Fig. 6 is ultra-thin coated by titanium dioxide silica airsetting prepared by the embodiment of the present invention 1, embodiment 2 and embodiment 3
The acetaldehyde degradation curve of rubber column gel column and carbon dioxide formation curve.
Specific embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
The present invention provides a kind of ultra-thin coated by titanium dioxide aerosil column for purifying toxic gas, is profit
With ALD technique by coated by titanium dioxide in composite material made from aerosil column surfaces externally and internally.It is preferred that the cladding
Titanium dioxide mass percentage for 0.32%-1.25%, the quality hundred of the titanium dioxide of the further preferred cladding
It is 0.60% to divide content.The titanium dioxide is anatase phase titanium dioxide.
The present invention also provides a kind of systems for the ultra-thin coated by titanium dioxide aerosil column for purifying toxic gas
Preparation Method specifically includes following steps：
Aerosil column is positioned in ald chamber body by step 1, using high pure nitrogen as carrier gas, sets cavity pressure
It is by force 0.1torr~0.2torr, cavity temperature is 200 DEG C~300 DEG C, and it is 80 DEG C~100 DEG C that titanium source, which keeps temperature, and oxygen source is protected
Temperature is held as 20 DEG C~40 DEG C, opening time of titanium source electronic valve is 0.08s~0.2s, and purge time is 30s~180s, oxygen
The opening time of source electronic valve is 0.015s~0.02s, and purge time is 30s~180s, and cycle-index is followed for 100~400
Ring, operation program obtain sample to be annealed after EP (end of program), the titanium source is isopropyl titanate, and the oxygen source is ultra-pure water；
Preferred embodiment is：It is 0.1torr that chamber pressure is set in step 1, and cavity temperature is 200 DEG C, and titanium source keeps temperature
For 80 DEG C, it is 20 DEG C that oxygen source, which keeps temperature, and titanium source electronic valve opens 0.08s, purges 30s, and oxygen source electronic valve is opened
0.015s, purges 30s, and cycle-index is 200 Xun Huans.
The sample to be annealed obtained in step 1 is put into Muffle furnace by step 2, and the heating rate for setting Muffle furnace is 5
DEG C/min~25 DEG C/min, annealing temperature be 400 DEG C~800 DEG C, annealing time be 1h~5h, rate of temperature fall for 5 DEG C/min~
25 DEG C/min, obtain ultra-thin coated by titanium dioxide aerosil column.It is preferred that annealing temperature is 500 DEG C, annealing time is
3h, heating rate are 10 DEG C/min, and rate of temperature fall is 10 DEG C/min.
It is preferred that the mass percentage of the titanium dioxide is 0.32%-1.25%, the two of the further preferred cladding
The mass percentage of titanium oxide is 0.60%.The titanium dioxide is anatase phase titanium dioxide.
Embodiment 1
The preparation of ultra-thin coated by titanium dioxide aerosil column, specific implementation step are as follows：
Step 1：Aerosil column is positioned in ald chamber body, using high pure nitrogen as carrier gas, ald chamber is set
Body pressure is 0.1torr, and cavity temperature is 200 DEG C, and it is 80 DEG C that titanium source, which keeps temperature, and it is 20 DEG C that oxygen source, which keeps temperature, and program is set
It is fixed as follows：Titanium source electronic valve opens 0.08s, purges 30s, and oxygen source electronic valve opens 0.015s, purges 30s, and Xun Huan is above-mentioned
Step 100 time is to terminating.Operation program after EP (end of program), obtains sample to be annealed；The titanium source be isopropyl titanate, the oxygen
Source is ultra-pure water；
Step 2：The sample to be annealed that step 1 is obtained is positioned in Muffle furnace, and heating rate is set as 10 DEG C/min, drop
Warm rate is set as 10 DEG C/min, and Muffle furnace program setting is as follows：20 DEG C are 500 DEG C by 48min to temperature, and constant temperature time is
3h is cooled to 20 DEG C using 48min.Operation program takes out sample after EP (end of program), is ultra-thin coated by titanium dioxide dioxy
SiClx airsetting rubber column gel column, the mass percentage of the titanium dioxide of cladding is 0.32%.
Embodiment 2
The preparation of ultra-thin coated by titanium dioxide aerosil column, specific implementation step are as follows：
Step 1：Aerosil column is positioned in ald chamber body, using high pure nitrogen as carrier gas, ald chamber is set
Body pressure is 0.1torr, and cavity temperature is 200 DEG C, and it is 80 DEG C that titanium source, which keeps temperature, and it is 20 DEG C that oxygen source, which keeps temperature, and program is set
It is fixed as follows：Titanium source electronic valve opens 0.08s, purges 30s, and oxygen source electronic valve opens 0.015s, purges 30s, and Xun Huan is above-mentioned
Step 200 time is to terminating.Operation program after EP (end of program), obtains sample to be annealed；The titanium source be isopropyl titanate, the oxygen
Source is ultra-pure water；
Step 2：The sample to be annealed that step 1 is obtained is positioned in Muffle furnace, and heating rate is set as 10 DEG C/min, drop
Warm rate is set as 10 DEG C/min, and Muffle furnace program setting is as follows：20 DEG C are 500 DEG C by 48min to temperature, and constant temperature time is
3h is cooled to 20 DEG C using 48min.Operation program takes out sample after EP (end of program), is ultra-thin coated by titanium dioxide dioxy
SiClx airsetting rubber column gel column, the mass percentage of the titanium dioxide of cladding is 0.60%.
Embodiment 3
The preparation of ultra-thin coated by titanium dioxide aerosil column, specific implementation step are as follows：
Step 1：Aerosil column is positioned in ald chamber body, using high pure nitrogen as carrier gas, ald chamber is set
Body pressure is 0.1torr, and cavity temperature is 200 DEG C, and it is 80 DEG C that titanium source, which keeps temperature, and it is 20 DEG C that oxygen source, which keeps temperature, and program is set
It is fixed as follows：Titanium source electronic valve opens 0.08s, purges 30s, and oxygen source electronic valve opens 0.015s, purges 30s, and Xun Huan is above-mentioned
Step 400 time is to terminating.Operation program after EP (end of program), obtains sample to be annealed；The titanium source be isopropyl titanate, the oxygen
Source is ultra-pure water；
Step 2：The sample to be annealed that step 1 is obtained is positioned in Muffle furnace, and heating rate is set as 10 DEG C/min, drop
Warm rate is set as 10 DEG C/min, and Muffle furnace program setting is as follows：20 DEG C are 500 DEG C by 48min to temperature, and constant temperature time is
3h is cooled to 20 DEG C using 48min.Operation program takes out sample after EP (end of program), is ultra-thin coated by titanium dioxide dioxy
SiClx airsetting rubber column gel column, the mass percentage of the titanium dioxide of cladding is 1.25%.
Embodiment 4
The preparation of ultra-thin coated by titanium dioxide aerosil column, specific implementation step are as follows：
Step 1：Aerosil column is positioned in ald chamber body, using high pure nitrogen as carrier gas, ald chamber is set
Body pressure is 0.1torr, and cavity temperature is 200 DEG C, and it is 80 DEG C that titanium source, which keeps temperature, and it is 20 DEG C that oxygen source, which keeps temperature, and program is set
It is fixed as follows：Titanium source electronic valve opens 0.08s, purges 30s, and oxygen source electronic valve opens 0.015s, purges 30s, and Xun Huan is above-mentioned
Step 100 time is to terminating.Operation program after EP (end of program), obtains sample to be annealed；The titanium source be isopropyl titanate, the oxygen
Source is ultra-pure water；
Step 2：The sample to be annealed that step 1 is obtained is positioned in Muffle furnace, and heating rate is set as 25 DEG C/min, drop
Warm rate is set as 25 DEG C/min, and Muffle furnace program setting is as follows：20 DEG C are 400 DEG C by 15min to temperature, and constant temperature time is
1h is cooled to 20 DEG C using 15min.Operation program takes out sample after EP (end of program), is ultra-thin coated by titanium dioxide dioxy
SiClx airsetting rubber column gel column, the mass percentage of the titanium dioxide of cladding is 0.32%.
Phase structure, pore structure, the light of the ultra-thin coated by titanium dioxide aerosil column finally prepared penetrate energy
Power, absorption property are similar to photocatalysis performance and embodiment 1.
Embodiment 5
The preparation of ultra-thin coated by titanium dioxide aerosil column, specific implementation step are as follows：
Step 1：Aerosil column is positioned in ald chamber body, using high pure nitrogen as carrier gas, ald chamber is set
Body pressure is 0.1torr, and cavity temperature is 200 DEG C, and it is 80 DEG C that titanium source, which keeps temperature, and it is 20 DEG C that oxygen source, which keeps temperature, and program is set
It is fixed as follows：Titanium source electronic valve opens 0.08s, purges 30s, and oxygen source electronic valve opens 0.015s, purges 30s, and Xun Huan is above-mentioned
Step 100 time is to terminating.Operation program after EP (end of program), obtains sample to be annealed；The titanium source be isopropyl titanate, the oxygen
Source is ultra-pure water；
Step 2：The sample to be annealed that step 1 is obtained is positioned in Muffle furnace, and heating rate is set as 5 DEG C/min, drop
Warm rate is set as 5 DEG C/min, and Muffle furnace program setting is as follows：20 DEG C are 800 DEG C by 156min to temperature, and constant temperature time is
5h is cooled to 20 DEG C using 156min.Operation program takes out sample after EP (end of program), is ultra-thin coated by titanium dioxide two
Silica aerogel column, the mass percentage of the titanium dioxide of cladding is 0.32%.
Phase structure, pore structure, the light of the ultra-thin coated by titanium dioxide aerosil column finally prepared penetrate energy
Power, absorption property are similar to photocatalysis performance and embodiment 1.
Embodiment 6
The preparation of ultra-thin coated by titanium dioxide aerosil column, specific implementation step are as follows：
Step 1：Aerosil column is positioned in ald chamber body, using high pure nitrogen as carrier gas, ald chamber is set
Body pressure is 0.2torr, and cavity temperature is 300 DEG C, and it is 100 DEG C that titanium source, which keeps temperature, and it is 40 DEG C that oxygen source, which keeps temperature, and program is set
It is fixed as follows：Titanium source electronic valve opens 0.2s, purges 180s, and oxygen source electronic valve opens 0.02s, purges 180s, and Xun Huan is above-mentioned
Step 100 time is to terminating.Operation program after EP (end of program), obtains sample to be annealed；The titanium source be isopropyl titanate, the oxygen
Source is ultra-pure water；
Step 2：The sample to be annealed that step 1 is obtained is positioned in Muffle furnace, and heating rate is set as 10 DEG C/min, drop
Warm rate is set as 10 DEG C/min, and Muffle furnace program setting is as follows：20 DEG C are 500 DEG C by 48min to temperature, and constant temperature time is
3h is cooled to 20 DEG C using 48min.Operation program takes out sample after EP (end of program), is ultra-thin coated by titanium dioxide dioxy
SiClx airsetting rubber column gel column, the mass percentage of the titanium dioxide of cladding is 0.32%.
Phase structure, pore structure, the light of the ultra-thin coated by titanium dioxide aerosil column finally prepared penetrate energy
Power, absorption property are similar to photocatalysis performance and embodiment 1.
Embodiment 7
The pattern of ultra-thin coated by titanium dioxide aerosil column prepared by the present invention is characterized with ingredient：
To utilizing ultra-thin the two of ALD technique preparation in original aeroge, the embodiment of the present invention 1, embodiment 2 and embodiment 3
Titanium-oxide-coated aerosil column carries out morphology characterization, and the results are shown in Figure 1, from original aeroge to embodiment 3, this
The appearance color for inventing the ultra-thin coated by titanium dioxide aerosil column prepared is gradually deepened.To the embodiment of the present invention 1,
The ultra-thin coated by titanium dioxide aerosil column prepared in embodiment 2 and embodiment 3 using ALD technique carries out component list
Sign, as shown in Fig. 2, from embodiment 1 to embodiment 3, the ultra-thin coated by titanium dioxide silica airsetting of the invention being prepared
The content of titanium dioxide of rubber column gel column is gradually increased to 1.25% from 0.32%, therefore can illustrate, is prepared using the method for the present invention
The content of titanium dioxide of ultra-thin coated by titanium dioxide aerosil column be proportionate with cycle-index.
Embodiment 8
The phase structure characterization of ultra-thin coated by titanium dioxide aerosil column prepared by the present invention：
Using Raman spectrum (Raman) in the embodiment of the present invention 1, embodiment 2 and embodiment 3 ALD technique being utilized to prepare
Ultra-thin coated by titanium dioxide aerosil column carry out phase structure characterization, test result is as shown in figure 3, the present invention
The peak positions of the ultra-thin coated by titanium dioxide aerosil column Raman spectrum being prepared and anatase phase titanium dioxide
The peak position of Raman spectrum is consistent, therefore can illustrate, the ultra-thin coated by titanium dioxide dioxy being prepared using the method for the present invention
Catalyst component in SiClx airsetting rubber column gel column is anatase phase titanium dioxide.
Embodiment 9
The Pore Characterization of ultra-thin coated by titanium dioxide aerosil column prepared by the present invention：
Using nitrogen adsorption instrument to utilizing ALD skills in original aeroge, the embodiment of the present invention 1, embodiment 2 and embodiment 3
Ultra-thin coated by titanium dioxide aerosil column prepared by art carries out Pore Characterization, and test result is as shown in figure 4, this hair
The bright ultra-thin coated by titanium dioxide aerosil column nitrogen adsorption-desorption isothermal curve and pore distribution curve being prepared
Nitrogen adsorption-desorption the isothermal curve and pore distribution curve of equal and original airsetting rubber column gel column are almost consistent, therefore can illustrate, using this
Ultra-thin coated by titanium dioxide aerosil column prepared by inventive method hardly changes the original pore structure of airsetting rubber column gel column.
Embodiment 10
The light of ultra-thin coated by titanium dioxide aerosil column prepared by the present invention penetrates capability representation：
Using UV-Vis DRS absorption spectrum (UV-Vis) to original aeroge, the embodiment of the present invention 1, embodiment 2
Light, which is carried out, with the ultra-thin coated by titanium dioxide aerosil column prepared in embodiment 3 using ALD technique penetrates capability list
Sign, test result is as shown in figure 5, from original aeroge to embodiment 3, light of the sample in 350nm~800nm wave-length coverages is saturating
Crossing rate reduces but successively for 0, therefore can illustrate, the ultra-thin coated by titanium dioxide dioxy being prepared using the method for the present invention
SiClx airsetting rubber column gel column can largely keep the original light of airsetting rubber column gel column to penetrate ability.
Embodiment 11
The absorption property of ultra-thin coated by titanium dioxide aerosil column prepared by the present invention and photocatalysis performance table
Sign：
The ultra-thin coated by titanium dioxide two that ALD technique will be utilized to prepare in the embodiment of the present invention 1, embodiment 2 and embodiment 3
Silica aerogel column is applied in the acetaldehyde degradation experiment under ultraviolet light conditions, is given birth to using acetaldehyde degradation curve and carbon dioxide
The characterization test of absorption property and photocatalysis performance, tool are carried out to ultra-thin coated by titanium dioxide aerosil column into curve
Body embodiment is as follows：
(1) the ultra-thin coated by titanium dioxide aerosil column for preparing embodiment 1, embodiment 2 and embodiment 3 is put
In closed reactor and closed reactor gaseous environment is handled, is as follows：
Ultra-thin coated by titanium dioxide aerosil column is positioned in 500mL quartz photo catalysis reactors.To anti-
Device is answered to be continually fed into high pure air (O2(20%)+N2(80%)) it is, after 20min that its is closed.
(2) absorption property is carried out to ultra-thin coated by titanium dioxide aerosil column using gas chromatograph to urge with light
Change performance characterization test, specific embodiment is as follows：
Gas chromatograph is opened, the test condition for setting gas chromatograph is as follows：1 temperature of post case is 100 DEG C, 2 temperature of post case
It spends for 180 DEG C, 1 temperature of detector is 380 DEG C, and 2 temperature of detector is 200 DEG C, and hydrogen generator flow velocity is 40mL/min, high-purity
Atmospheric pressure 0.45pa, high pure nitrogen pressure are 0.45pa；
5 μm of ol (220ppm) aldehydes gas are injected into closed reactor, secretly adsorb 1h, it then will be ultra-thin in reactor
Coated by titanium dioxide aerosil column, which is placed under ultraviolet light, to be irradiated, ultraviolet ray intensity 3mW/cm2, wavelength is
350nm~400nm takes in reactor under dark adsorption conditions every 1h and carries out acetaldehyde and two in 1mL gases injection gas chromatograph
Concentration of carbon acquisition is aoxidized, is taken under ultraviolet light irradiation every 10min in reactor and carries out acetaldehyde in 1mL gases injection gas chromatograph
It is gathered with gas concentration lwevel.
The acetaldehyde degradation curve of ultra-thin coated by titanium dioxide aerosil column and carbon dioxide formation curve such as Fig. 6
Shown, acetaldehyde concentration of all samples under dark adsorption conditions has and largely reduces, while ultraviolet light irradiation condition
Under carbon dioxide generation it is very fast, wherein the dioxy with the ultra-thin coated by titanium dioxide aerosil column in embodiment 2
Change carbon generation best results, therefore can illustrate, the ultra-thin coated by titanium dioxide silica being prepared using the method for the present invention
Airsetting rubber column gel column has good absorption property and photocatalysis performance.
Obviously, the above embodiments are merely examples for clarifying the description, and is not intended to limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. a kind of ultra-thin coated by titanium dioxide aerosil column for purifying toxic gas, which is characterized in that it is profit
With technique for atomic layer deposition by coated by titanium dioxide in composite material made from aerosil column surfaces externally and internally.
2. the ultra-thin coated by titanium dioxide aerosil column according to claim 1 for purifying toxic gas,
It is characterized in that, the mass percentage of the titanium dioxide is 0.32%-1.25%.
3. the ultra-thin coated by titanium dioxide aerosil column according to claim 2 for purifying toxic gas,
It is characterized in that, the mass percentage of the titanium dioxide is 0.60%.
4. the ultra-thin coated by titanium dioxide silica gas for purifying toxic gas according to claim 1-3 any one
Gel column, which is characterized in that the titanium dioxide is anatase phase titanium dioxide.
5. a kind of system of the ultra-thin coated by titanium dioxide aerosil column described in claim 1 for purifying toxic gas
Preparation Method, which is characterized in that specifically include following steps：
Aerosil column is positioned in ald chamber body by step 1, and using high pure nitrogen as carrier gas, setting chamber pressure is
0.1torr~0.2torr, cavity temperature are 200 DEG C~300 DEG C, and it is 80 DEG C~100 DEG C that titanium source, which keeps temperature, and oxygen source keeps temperature
It spends for 20 DEG C~40 DEG C, the opening time of titanium source electronic valve is 0.08s~0.2s, and purge time is 30s~180s, and oxygen source is electric
The opening time of sub- valve is 0.015s~0.02s, and purge time is 30s~180s, and cycle-index is 100~400 Xun Huans, is transported
Line program obtains sample to be annealed after EP (end of program), the titanium source is isopropyl titanate, and the oxygen source is ultra-pure water；
The sample to be annealed obtained in step 1 is put into Muffle furnace by step 2, and the heating rate for setting Muffle furnace is 5 DEG C/min
~25 DEG C/min, annealing temperature be 400 DEG C~800 DEG C, annealing time be 1h~5h, rate of temperature fall for 5 DEG C/min~25 DEG C/
Min obtains ultra-thin coated by titanium dioxide aerosil column.
6. the system of the ultra-thin coated by titanium dioxide aerosil column according to claim 5 for purifying toxic gas
Preparation Method, which is characterized in that the mass percentage of the titanium dioxide is 0.32%-1.25%.
7. the system of the ultra-thin coated by titanium dioxide aerosil column according to claim 6 for purifying toxic gas
Preparation Method, which is characterized in that the mass percentage of the titanium dioxide is 0.60%.
8. the ultra-thin coated by titanium dioxide silica gas for purifying toxic gas according to claim 5-7 any one
The preparation method of gel column, which is characterized in that the titanium dioxide is anatase phase titanium dioxide.
9. the system of the ultra-thin coated by titanium dioxide aerosil column according to claim 8 for purifying toxic gas
Preparation Method, which is characterized in that it is 0.1torr that chamber pressure is set in step 1, and cavity temperature is 200 DEG C, and titanium source holding temperature is
80 DEG C, it is 20 DEG C that oxygen source, which keeps temperature, and titanium source electronic valve opens 0.08s, purges 30s, and oxygen source electronic valve opens 0.015s,
30s is purged, cycle-index is 200 Xun Huans.
10. the ultra-thin coated by titanium dioxide aerosil column according to claim 8 for purifying toxic gas
Preparation method, which is characterized in that annealing temperature is 500 DEG C, annealing time 3h in step 2, and heating rate is 10 DEG C/min, is dropped
Warm rate is 10 DEG C/min.
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