CN108855169A - Porous silicon carbide as filler/modifying titanium dioxide composite photo-catalyst preparation method - Google Patents
Porous silicon carbide as filler/modifying titanium dioxide composite photo-catalyst preparation method Download PDFInfo
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- CN108855169A CN108855169A CN201810957164.1A CN201810957164A CN108855169A CN 108855169 A CN108855169 A CN 108855169A CN 201810957164 A CN201810957164 A CN 201810957164A CN 108855169 A CN108855169 A CN 108855169A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 20
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 13
- 239000000945 filler Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000004408 titanium dioxide Substances 0.000 title claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 7
- 238000012986 modification Methods 0.000 claims abstract description 7
- 238000012545 processing Methods 0.000 claims abstract description 5
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 19
- 239000003054 catalyst Substances 0.000 claims description 11
- 150000001298 alcohols Chemical class 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 229960000935 dehydrated alcohol Drugs 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000001228 spectrum Methods 0.000 abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000012876 carrier material Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 239000004113 Sepiolite Substances 0.000 description 1
- -1 Titanium alkoxides Chemical class 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
- B01J27/224—Silicon carbide
-
- B01J35/39—
Abstract
The present invention provides a kind of porous silicon carbide as filler/modification TiO2Composite photo-catalyst preparation method belongs to photocatalyst technology field, solves current nano-TiO2Response spectrum narrow range, it is easy to reunite, be easy to run off, photocatalysis effect is poor, the problem of difficult life.Graphene is added in dehydrated alcohol and deionized water by the present invention first, and graphene solution A is made in ultrasonic disperse processing;Again by TiO2It is added to absolute ethanol, is added to after ultrasonic disperse in graphene solution A, adjust solution ph, obtained solution B;Porous silicon carbide Si powder is added in dehydrated alcohol and deionized water, is added in solution B after ultrasonic disperse processing, is agitated to form gel;Gel is transferred in reaction kettle, is reacted 12 hours at 200 DEG C, is ground obtained powdery porous silicon carbide/modification TiO after dry2Composite photo-catalyst.Preparation method of the present invention improves TiO2Photocatalysis efficiency promotes catalytic degradation effect, has good popularization and application foreground.
Description
Technical field
The present invention is a kind of porous silicon carbide as filler/modifying titanium dioxide (TiO2) composite photo-catalyst preparation side
Method belongs to photocatalyst technology field.
Background technique
Light-catalyzed reaction refers to that semiconductor material absorbs extraneous radiation luminous energy excitation and generates conduction band and valence band hole, Jin Eryu
The process of a series of chemical reaction occurs for the substance being adsorbed on catalyst surface.Photocatalysis technology has the advantage that:To have
Degradable machine pollutant is CO2、H2Inorganic pollution is aoxidized or is reduced to harmless object by O etc.;Do not need other electronics by
Body (such as H2O2);Suitable photochemical catalyst has many advantages, such as cheap, nontoxic, stable and may be reused;Can use take no
As light source activation photochemical catalyst, operating condition is easy to control most solar energy, oxidability is strong, without secondary pollution.
In recent years, related TiO2Research it is increasing in different field, and in industrial circle by TiO2Product and its derivative
The benefit that object is created also is being doubled and redoubled.TiO2Nontoxic with its, self-cleaning, safety, chemical property stabilization, catalytic activity height etc. are excellent
Point, is widely used in the energy and environmental area, such as sewage treatment, dye-sensitized solar cells, sensor, electrochromism device
Part etc., and be considered as using one of optimal semiconductor catalyst of photocatalysis field.
By TiO2Being carried on porous media is to solve photochemical catalyst to be easy to run off, improve photochemical catalyst absorption pollutant ability
Effective way.TiO2Composite carrier is in recent years for raising TiO2Photocatalytic activity and the new method proposed, this method master
If the advantages that using carrier material strong adsorption, large specific surface area, strong nontoxic and corrosion resistance, with bentonite, diatomite,
New carbon etc. is that carrier material forms compound system.Work as TiO2With insulator compound tense, Al2O3、SiO2、ZrO2Equal insulators
Also what is mostly play a part of is carrier, however since between carrier and active component particularity can be generated because of interaction
Matter, such as acidity change, so that composite oxides show higher acidity than single component oxide.
Common carrying method has powder sintering method, sol-gal process, sedimentation, sputtering method, hydro-thermal method etc..Powder sintering
Method directlys adopt the methods of ultrasonic disperse TiO2Powder and certain solution are made suspension and with carrier impregnations, deposit certain
TiO2Drying and roasting can be obtained simply after particle, and this method can be mass-produced and catalyst activity is higher, but stability
It is poor with reproducibility.Sol-gal process passes through external force stirring water in certain medium using inorganic titanium salt or Titanium alkoxides as precursor
Solution, condensation form colloidal sol, then are aged into gel, load on carrier it by Best-Effort request, rotary coating or the method for spraying
High-temperature roasting can be obtained afterwards, although operation is relative complex, reaction process is mild, is easy to control.
Sedimentation, which refers to, makes TiO by the methods of laser, high temperature2As steam or the higher liquid phase of dispersion degree, then low
The lower contact carrier of temperature, and condense on carrier a kind of method for forming film, can carry out under normal pressure, and required equipment is simple but film
Uniformity it is poor.Sputtering method is also plasma processing method, and the plasma in gas has under the action of electric field is with magnetic field
There are very high speed and energy, these plasma bombardments TiO2The surface of solid, makes Ti4+Ion is detached from TiO2Lattice ease
Out, it shifts and deposits to carrier surface and form film, still, since sputtering method need to operate in an electrical or magnetic field, required temperature
It is higher, therefore carrier should select heat-resisting material.
Load TiO2Method in the past typically to solve in TiO2Reaction after be easy to run off be not easily recycled regeneration and
TiO2Easy to reunite, the problems such as contact area is small, or prepare composite material to improve catalytic performance, relevant test result also table
It is bright, TiO2It can effectively improve reactivity with the synergistic effect of support materials.Therefore, the present invention is stronger according to porous silicon carbide
Adsorption capacity and its aperture and modified TiO2With good matching, gives full play to the two collaboration and thank to grain husk, improve light and urge
Change performance, to reach better catalytic degradation effect.
Summary of the invention
(1) technical problem
It is an object of the present invention to provide a kind of porous silicon carbide as filler/modification TiO2Composite photo-catalyst preparation side
Method, this method is adsorbed using porous silicon carbide and nano-TiO2The synergistic effect that light is urged solves current nano-TiO2Response spectrum model
Enclose it is narrow, easy to reunite, be easy to run off, photocatalysis effect is poor, the problem of difficult life, to effectively improve TiO2Photocatalytic degradation effect.
(2) technical solution
In view of current TiO2There is a problem of it is easy to reunite, be easy to run off, photocatalysis effect is poor, difficult life, the present invention is from porous
Silicon carbide can effectively adsorb pollutant and the characteristic for reacting it with the modified light catalyst of absorption is started with, and provide one kind and be used as
The porous silicon carbide of filler/modification TiO2Composite photo-catalyst preparation method, to improve the catalytic degradation effect of catalysis material
Fruit, the problems such as alloing catalysis material to be effectively used for a long time and not be lost.Technical solution of the present invention is as follows:First will
Graphene oxide is added in dehydrated alcohol and deionized water, and graphene oxide solution A is made in ultrasonic disperse processing;Then will
TiO2It is added to absolute ethanol, is added to after ultrasonic disperse in graphene oxide solution A, adjust solution ph with ammonium hydroxide, continue
Ultrasonic disperse, obtained solution B;After washing and drying porous silicon carbide Si powder be added to dehydrated alcohol and deionized water
In, it is added in solution B after ultrasonic disperse processing, it is agitated to formation gel;Gel is transferred in closed reactor,
It reacts 12 hours, is washed and dried after dry 12 with deionized water, ground obtained powdery porous silicon carbide/change at 200 DEG C
Property TiO2Composite photo-catalyst.
(3) beneficial effect
TiO2It is a kind of common photochemical catalyst, because it has, itself is nontoxic, oxidability is strong, degradation is thorough, chemically
The advantages that matter is stable and without secondary pollution and by the concern of people, it is considered to be the most catalysis material of development potentiality.
But TiO2Having that response spectrum narrow range, absorption property are poor, are easy to reunion, recycling and reusing difficulty in direct use etc. lacks
It falls into, greatly limits its application, therefore existing research is loaded on porous carrier materials mostly.By TiO2Load to work
Research on the carriers such as property charcoal, Bio-sil, natural crystal, sepiolite it has been reported that but these loads mostly there is at
This more high and low the defects of imitating, making a low multiple use.Porous silicon carbide prepared by the present invention/modification TiO2Composite photo-catalyst can
As filler, TiO is improved2Photocatalysis efficiency promotes catalytic degradation effect, has a good application prospect, to photocatalysis from now on
The development of material is of great practical significance.
Specific embodiment
The present invention provides a kind of porous silicon carbide as filler/modifying titanium dioxide composite photo-catalyst preparation method,
Specific implementation step is as follows:
(1) 20 milligrams of graphene oxides are added in 5 milliliters of dehydrated alcohols and 15 ml deionized waters, at ultrasonic disperse
Graphene oxide solution A is made in reason 20 minutes;
(2) by 60 milligrams of nano-TiOs2It is added in 5 milliliters of dehydrated alcohols, ultrasonic disperse is handled 30 minutes, is added to oxidation
In graphene solution A, solution ph is adjusted with ammonium hydroxide and reaches 9, continue ultrasonic disperse and handle 1 hour, obtained solution B;
(3) 500 milligrams of porous silicon carbide Si powders after deionized water washes and dries are added to 5 milliliters of anhydrous second
In pure and mild 25 ml deionized water, ultrasonic disperse is handled 1 hour, is added in solution B, is stirred evenly, and gel is made;
(4) gel is transferred in closed reactor, is heated to 200 DEG C with 1 DEG C/min heating rate, at 200 DEG C
It is phase reaction 12 hours, 12 hours dry in 100 DEG C of environmental cabinets, ground obtained powdery porous silicon carbide/modification TiO2It is multiple
Light combination catalyst.
Claims (1)
1. a kind of porous silicon carbide as filler/modifying titanium dioxide composite photo-catalyst preparation method, it is characterised in that should
Specific step is as follows for method:
(1) 20 milligrams of graphene oxides are added in 5 milliliters of dehydrated alcohols and 15 ml deionized waters, ultrasonic disperse processing 20
Minute, graphene oxide solution A is made;
(2) by 60 milligrams of nano-TiOs2It is added in 5 milliliters of dehydrated alcohols, ultrasonic disperse is handled 30 minutes, is added to graphene oxide
In solution A, solution ph is adjusted with ammonium hydroxide and reaches 9, continue ultrasonic disperse and handle 1 hour, obtained solution B;
(3) 500 milligrams of porous silicon carbide Si powders after deionized water washes and dries be added to 5 milliliters of dehydrated alcohols and
In 25 ml deionized waters, ultrasonic disperse is handled 1 hour, is added in solution B, is stirred evenly, and gel is made;
(4) gel is transferred in closed reactor, is heated to 200 DEG C with 1 DEG C/min heating rate, is contrary at 200 DEG C
It answers 12 hours, 12 hours dry in 100 DEG C of environmental cabinets, ground obtained powdery porous silicon carbide/modification TiO2Complex light
Catalyst.
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Cited By (2)
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CN110182808A (en) * | 2019-05-24 | 2019-08-30 | 武汉楚能电子有限公司 | A kind of method that silicon-carbon alkene preparation method and its photodegradation vapor water prepare hydrogen |
CN115845890A (en) * | 2022-11-25 | 2023-03-28 | 广东科学技术职业学院 | Reticular photocatalyst material, preparation method, application and equipment thereof |
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CN115845890A (en) * | 2022-11-25 | 2023-03-28 | 广东科学技术职业学院 | Reticular photocatalyst material, preparation method, application and equipment thereof |
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