CN106179293A - A kind of composite photo-catalyst and its preparation method and application - Google Patents
A kind of composite photo-catalyst and its preparation method and application Download PDFInfo
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- CN106179293A CN106179293A CN201610518944.7A CN201610518944A CN106179293A CN 106179293 A CN106179293 A CN 106179293A CN 201610518944 A CN201610518944 A CN 201610518944A CN 106179293 A CN106179293 A CN 106179293A
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- catalyst
- composite photo
- photocatalyst
- porous media
- paint film
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 124
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000576 coating method Methods 0.000 claims abstract description 39
- 239000011248 coating agent Substances 0.000 claims abstract description 38
- 230000032683 aging Effects 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 21
- 230000003197 catalytic effect Effects 0.000 claims abstract description 9
- 239000011148 porous material Substances 0.000 claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 50
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 238000005245 sintering Methods 0.000 claims description 15
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 230000007062 hydrolysis Effects 0.000 claims description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 229910052755 nonmetal Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- -1 semimetal Substances 0.000 claims description 3
- 239000004965 Silica aerogel Substances 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000975 dye Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 241001597008 Nomeidae Species 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 239000003973 paint Substances 0.000 abstract description 53
- 230000001699 photocatalysis Effects 0.000 abstract description 34
- 238000007146 photocatalysis Methods 0.000 abstract description 32
- 230000000694 effects Effects 0.000 abstract description 26
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- 239000000126 substance Substances 0.000 abstract description 11
- 230000000052 comparative effect Effects 0.000 description 20
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- 239000000203 mixture Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- 229910052681 coesite Inorganic materials 0.000 description 7
- 229910052906 cristobalite Inorganic materials 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 229910052682 stishovite Inorganic materials 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 229910052905 tridymite Inorganic materials 0.000 description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
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- 238000005516 engineering process Methods 0.000 description 5
- 229920002521 macromolecule Polymers 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
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- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
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- VAJVDSVGBWFCLW-UHFFFAOYSA-N 3-Phenyl-1-propanol Chemical compound OCCCC1=CC=CC=C1 VAJVDSVGBWFCLW-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- DYUQAZSOFZSPHD-UHFFFAOYSA-N Phenylpropyl alcohol Natural products CCC(O)C1=CC=CC=C1 DYUQAZSOFZSPHD-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 210000004681 ovum Anatomy 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000000886 photobiology Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
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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
- 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
-
- 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
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/651—
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
Abstract
The present invention provides a kind of composite photo-catalyst and its preparation method and application, described composite photo-catalyst is with porous media as carrier, it is filled with photocatalyst aggregate, described composite photo-catalyst is porous three-dimensional network structure, particle size range is 1 100 μm, and the pore size of described porous media is 50 500nm.The catalytic efficiency of the composite photo-catalyst of the present invention is high, easily dispersion, add the coating of the composite photo-catalyst of the present invention, while keeping the photocatalysis effect to little molecule harmful organic substance, avoid the degraded of organic paint film, therefore the ageing-resistant performance of paint film is suitable with the blank paint film not adding photocatalyst, and this paint film has long-acting photocatalysis performance.
Description
Technical field
The invention belongs to catalyst technical field, relate to a kind of composite photo-catalyst and its preparation method and application.
Background technology
Photocatalysis is usually the catalytic organism fall that the photocatalyst using visible/ultraviolet light to carry out being catalyzed makes to be in contact with it
Solve.The form of the photocatalyst the most often used includes: dichloride in anatase type TiO2(such as the HOMBIKAT UV100 of Sha Haliben), with
The TiO that anatase titanium dioxide mixes with rutile-type2(such as the P25 of Degussa), ACF modification TiO2, Au modification TiO2, WXTiO2+3X/SiO2
Aeroge, aeroge physical absorption TiO2It is coated with TiO with nano-porous films2.Above photocatalyst processing mode is (except nanometer is many
Pore membrane cladding TiO2) it being for improving the disposal efficiency of photocatalyst, if but use in organic paint film, also can lead simultaneously
Cause the light degradation of organic paint film.This is because photocatalyst degradation of small molecular harmful substance (NOX, volatile organic matter VOCS)
Meanwhile, paint film is degraded the most simultaneously, and then accelerated ageing and loss of gloss, and the paint film life-span substantially shortens.And photocatalyst photocatalysis fall
The ability solving small organic molecule is the biggest, the degraded of macromolecule paint film and aging the fastest.
N.S Allen at Photocatalytic Coatings for Environmental Applications,
Photochemistry and Photobiology, mentions in 2005,81:279-290, at phenylpropyl alcohol, pure third and polyvinyl alcohol breast
The result of the ultraviolet ageing research adding 10% anatase titania in the paint film based on liquid shows: the purple of 546 hours
After the most aging, these paint films are degraded the mass loss caused more than 97%；J.Auvinen etc. are at The influence of
photocatalytic interior paints on indoor air quality,Atmospheric Environment
Mentioning in 2008,42:4101 4112, within the enclosed space, in a short time, photocatalyst can make indoor harmful little molecular concentration fall
Low；But within the longer-term time, photocatalyst may produce substantial amounts of little molecule during sustaining degradation macromolecule paint film to be had
Machine thing, in making space, the concentration of overall small organic molecule (such as formaldehyde) is bigger than the concentration in blank space.Because it is organic
After adding photocatalyst in paint film, photocatalysis can not only produce carbon dioxide and water by degradable small organic molecule, it is also possible to
In degraded organic varnish membrane process, degraded is not exclusively, and produces substantial amounts of harmful little molecule, and the air making indoor is more harmful.
CN 101784619A discloses to be had photo-catalysis function and has no effect on the photolytic activity TiO of paint film property2.This light is lived
Property TiO2For core shell structure, with nano-TiO2(a diameter of 0.1-1 μm) is core, with SiO2(average thickness is 0.1-10nm) is shell,
SiO2It is coated on TiO2Surface.This photolytic activity TiO2Particle diameter about 1 μm, coating apply in dispersing technology can be had higher
Requirement.
In prior art, report and Patents about having light-catalysed organic paint film are a lot, at these reports with special
In profit, emphasis is emphasizing the photocatalysis effect to small organic molecule in a short time, the photocatalyst shadow to paint film of but avoiding mentioning
Ring and the ageing-resistant performance of paint film.Solving the contradiction of photocatalyst photocatalysis effect and its ageing-resistant performance in organic paint film is light
Catalyst is one of key of actual application in organic paint film.
One of light-catalysed key of photocatalyst is Organic substance and the contacting, because photocatalyst is in specific wavelength illumination of photocatalyst
Electronics-the vacancy of lower generation to only its surface and near just have an effect, can drastically destroy after leaving surface.The most how
Select suitable scheme to make photocatalyst only contact and degradation of small molecular harmful organic substance, completely cut off again itself and paint film base material-height simultaneously
The contact of molecular organic is the problem that this area needs solution badly.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of composite photo-catalyst and preparation method thereof and
Application.
For reaching this goal of the invention, the present invention by the following technical solutions:
On the one hand, the present invention provides a kind of composite photo-catalyst, and described composite photo-catalyst, with porous media as carrier, is filled out
Being filled with photocatalyst aggregate, described composite photo-catalyst is porous three-dimensional network structure, and particle size range is 1-100 μm, described many
The pore size of hole medium is 50-500nm.
The composite photo-catalyst of the present invention had both had higher photocatalysis effect, simultaneously the most non-degradable organic paint film.
The particle diameter of the composite photo-catalyst of the present invention is 1-100 μm, such as 1 μm, 5 μm, 8 μm, 10 μm, 15 μm, 20 μm, 25
μm, 28 μm, 30 μm, 35 μm, 38 μm, 40 μm, 45 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm, preferably 20-40 μm.
Particle size range of the present invention, the size of especially 20-40 μm is relatively low to the requirement of dispersing technology.In general, grain
Footpath is relatively long less than the particle milling time of 20 μm；Less than 1 μm particle dispersion to dispersion intensity and recipe requirements the most very
Height, in the range of less than 1 μm, particle is difficult to scatter, and during storing, easily reunites to micron order；At 20-40
In μ m, particle is more easy to dispersion, and stable storing；The when of higher than 40 μm, easily disperse, it is likely that because particle is too big
Causing sedimentation, and the thickness of major part paint film is both less than 50 μm, the biggest particle can affect paint film appearance.Therefore, in the present invention
In the particle diameter of preferred 20-40 μm.
In the present invention, in described composite photo-catalyst, the pore size of porous media is 50-500nm, such as 50nm,
60nm、70nm、80nm、100nm、120nm、140nm、160nm、180nm、200nm、220nm、250nm、280nm、300nm、
350nm, 400nm, 450nm or 500nm, preferably 50-200nm, such pore diameter range allows little molecule harmful organic substance to pass through
Duct contacts with the photocatalyst of its inside, and under photocatalysis, makes little molecule harmful organic substance be degraded into carbon dioxide and water.By
In porous media such as aerosil, there is adsorption so that the fall of the photocatalyst of composite photo-catalyst of the present invention
Solve efficiency apparently higher than the photocatalyst not improved；On the other hand porous media can avoid photocatalyst directly to contact macromolecule paint
Film, so that paint film is from the catalytic action of light.
Preferably, described porous media is aeroge or derivatives thereof.
Preferably, any during described aeroge is silicon system, carbon system, sulfur system, burning system or metal system aeroge
A kind of or the combination of at least two, preferably silica aerogel, further preferred aerosil.The structure of described aeroge is special
Levy the multi-branched nanoporous three-dimensional net structure being to have high-permeability, have high hole ratio, extremely low density, Gao Bibiao
Area and superelevation pore volume rate.The aperture of this structure provides fixed frame to photocatalyst, and high-specific surface area is conducive to richness
The harmful organic molecule of collection, and then improve photocatalysis efficiency.
Preferably, described photocatalyst is nano-metal-oxide or its alloy with photocatalysis performance, is preferably purple
Outer light-catalysed Detitanium-ore-type TiO2, anatase/rutile mixed type TiO2Or through metal, semimetal, dyestuff or nonmetal
The TiO of the visible light catalytic performance of doping2。
Preferably, any one or the combination of at least two during described metal is gold (Au), silver (Ag) or platinum (Pt)；
Preferably, described nonmetal for carbon and/or nitrogen.
Preferably, in composite photo-catalyst of the present invention, the mol ratio of described porous media and photocatalyst be 1:1～
10:1, such as 1:1,2:1,3:1,4:1,5:1,6:1,7:1,8:1,9:1 or 10:1, preferably 5:1.Set this proportion one
Aspect wishes that major part photocatalyst can be all fixed therein by porous media, and organic little point in the absorption air that can try one's best many
It is big that the amount of son, i.e. porous media should be tried one's best；On the other hand, the amount of photocatalyst can not be too low, even if being otherwise enriched substantial amounts of
Harmful organic molecule, if active center (photocatalyst) to also result in photocatalysis effect very little low.If it is less than this scope, the most
The amount of hole medium is very few, enrichment reduce, photocatalysis efficiency also can reduce, and likely have photocatalyst be free on porous be situated between
Beyond matter, and then cause the degraded of paint film；If higher than this scope, photocatalyst content is the lowest, causes active center density the lowest, meeting
The harmful organic molecule degradation efficiency of impact.When both ratios are 5:1 optimum, porous media can more effectively fix photocatalyst,
And do not affect the photocatalysis of photocatalyst.
Photocatalyst aggregate surface free in the present invention, in described composite photo-catalyst, in the vestibule of porous media
Crossing cladding, it is only in the vestibule sticking and being present in porous media, and the aggregate number of this photocatalyst aggregate is random.Excellent
Selection of land, the particle diameter of described photocatalyst aggregate is 5-100nm, such as 5nm, 8nm, 10nm, 20nm, 30nm, 40nm, 50nm,
60nm, 70nm, 80nm, 90nm or 100nm.
On the other hand, the invention provides the preparation method of described composite photo-catalyst, described method comprises the steps:
(1) photocatalyst is scattered in porous media, hydrolysis, aging, dry, obtain being combined of porous media and photocatalyst
Body；
(2) porous media step (1) prepared is pulverized with the complex of photocatalyst, burns at 500 DEG C-900 DEG C
Tie more than 4 hours；
(3) sintered product of step (2) is disperseed in a solvent, then carry out particulate abrasive and obtain composite photocatalyst
Agent slurry, i.e. obtains described composite photo-catalyst.
The temperature of step (1) described hydrolysis is 30-50 DEG C, such as 30 DEG C, 33 DEG C, 35 DEG C, 38 DEG C, 40 DEG C, 43 DEG C, 45
DEG C, 48 DEG C or 50 DEG C.
Preferably, the time of step (1) described hydrolysis is 10-30 hour, such as 10 hours, 12 hours, 15 hours, 18 little
Time, 20 hours, 23 hours, 25 hours, 28 hours or 30 hours.
Preferably, the described aging temperature of step (1) is 50-70 DEG C, such as 50 DEG C, 53 DEG C, 55 DEG C, 58 DEG C, 60 DEG C, 63
DEG C, 65 DEG C, 68 DEG C or 70 DEG C.
Preferably, step (1) the described aging time is 10-30 hour, such as 10 hours, 12 hours, 15 hours, 18 little
Time, 20 hours, 23 hours, 25 hours, 28 hours or 30 hours.
The porous media that step (1) obtains has loose structure with the complex of photocatalyst aggregate, and has three-dimensional vertical
Body structure, such as Nidus Vespae, TiO2It is distributed in the hole of gel, as ovum stayed by Nidus Vespae.
The temperature of step (2) described sintering is 500 DEG C-900 DEG C, such as 500 DEG C, 530 DEG C, 550 DEG C, 580 DEG C, 600 DEG C,
630 DEG C, 650 DEG C, 680 DEG C, 700 DEG C, 730 DEG C, 750 DEG C, 780 DEG C, 800 DEG C, 830 DEG C, 850 DEG C, 880 DEG C or 900 DEG C.
The time of step (2) described sintering is more than 4 hours, such as 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 little
Time, 6.5 hours, 7 hours, 7.5 hours, 8 hours, 8.5 hours, 9 hours, 9.5 hours, 10 hours, 10.5 hours, 11 hours,
11.5 hours or 12 hours etc., preferably 4-8 hour.
Step (2) carries out the purpose of high temperature sintering and is 2 points: one is so that porous media (such as aeroge) aperture collapses
Collapse, reduce pore size, it is ensured that photocatalyst TiO2The resin that also limit big particle diameter while not flowing out enters, but will not shadow
Ring the entrance of small molecule organic material (major part harmful substance is all small organic molecule)；Two is after porous media caves in, many
Hole Media density rises, and can be dispersed in water, and then can preferably apply in water paint.
In step (2), if the temperature of high temperature sintering less than 500 DEG C or time less than 4h time, porous media is (such as
Aeroge) aperture caves in not, and can cause caving in of porous media skeleton higher than 900 DEG C, affect properties of catalyst.
Preferably, step (3) described solvent is deionized water.
In the present invention, step (3) described dispersion can utilize methods known in the art to carry out, in dispersive process also
Wetting dispersing agent, such as SN-5040 can be added, to promote dispersion.Additionally, particulate abrasive can apply means known in the art
Carry out, such as, can add the zirconium pearl (diameter 2mm) of 2-3 times of formulation weight ratio in system, then at 2500rpm-3000rpm
Under granule is ground, during need condensed water.
Preferably, after particulate abrasive, the size controlling of composite photo-catalyst in described composite photo-catalyst slurry
For 1-100 μm, such as 1 μm, 5 μm, 8 μm, 10 μm, 15 μm, 20 μm, 25 μm, 28 μm, 30 μm, 35 μm, 38 μm, 40 μm, 45 μm,
50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm, preferably 20-40 μm.The present invention can be by known in the art ground
The control method of journey controls the particle diameter of described composite photo-catalyst slurry in 1-100 μm, is preferably controlled within 20-40 μm, this
The particle diameter of sample makes particle easily disperse, and the requirement to dispersing technology is relatively low, and stable storing.
On the other hand, the invention provides a kind of light catalyzed coating, it contains answering according to any one of claim 1-6
Close photocatalyst.
Preferably, described composite photo-catalyst addition in coating is 1-20%, such as 1%, 2%, 3%, 4%,
5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%,
Preferably 5-12%.
The composite catalyst of the present invention is applied and can prepare light catalyzed coating to coating.Wherein said coating is for including
Water paint and oil paint, preferably water paint, the curing mode of coating can be normal temperature cure, heat baking-curing or purple
Outer solidification.
Preferably, the film forming matter of described coating can be conventional macromolecule filming material, such as, can be resin, institute
State resin and include but not limited to alkyd resin, polyester resin, Corvic, acrylic resin, styrene-acrylic resin, siliceous propylene
Any one or the combination of at least two in acid resin, epoxy resin or polyurethane resin, it is also possible to include their blending
Resin (referring to the mixture of two kinds of resins) as and be not limited to epoxy-acrylic resin, polyurethane-acrylic resin etc..Described one-tenth
Membrane substance can also is that emulsion, described emulsion include but not limited to styrene-acrylic emulsion, pure-acrylic emulsion, polyaminoester emulsion, alkyd emulsion
Or any one or the mixture of at least two in epoxy aqueous dispersion or dispersion corresponding to described mixture.
The composite catalyst of the present invention is applied to coating, the photocatalysis to little molecule harmful organic substance can kept
While effect, it is to avoid photocatalyst directly contacts macromolecule paint film, so that paint film is from the catalytic action of light.
Relative to prior art, the method have the advantages that
The catalytic efficiency of the composite photo-catalyst of the present invention is high, easily disperses, adds the composite photo-catalyst of the present invention
Coating, while keeping photocatalysis effect to little molecule harmful organic substance, it is to avoid the degraded of organic paint film, therefore paint film
Ageing-resistant performance suitable with the blank paint film not adding photocatalyst, this paint film has long-acting photocatalysis performance.
Accompanying drawing explanation
Fig. 1 is the structural representation of the composite photo-catalyst of the present invention；
Fig. 2 is the schematic diagram of the composite photocatalyst for degrading organic molecule of the present invention.
Detailed description of the invention
Technical scheme is further illustrated below by detailed description of the invention.Those skilled in the art should be bright
, the only help of described embodiment understands the present invention, is not construed as the concrete restriction to the present invention.Embodiment 1
In the present embodiment, it is prepared by the following method composite photo-catalyst, specifically includes following steps:
A, the preparation of Ludox: taking tetraethyl orthosilicate 83g, ethanol 105g, deionized water 33g, nitric acid 1.4g, under 500rpm
Dispersion 10min, then puts it into airtight in glass jar (50 DEG C, 24h), obtains Ludox.
B, Ludox and TiO2The preparation of complex: by nano-TiO2(NT, aza nano-TiO2) in the feelings of moderate-speed mixer
In Ludox before adding under condition, it is ensured that the mol ratio of silicon and titanium is 5:1, and is added dropwise to 10% ammonia aqueous solution 40, and
After put into be hydrolyzed at 45 DEG C reaction 24h.
C, aging: the Ludox obtained with washes of absolute alcohol hydrolysis and TiO2Complex, and at 60 DEG C preserve
24h, need to clean twice altogether, add after terminating tetraethyl orthosilicate and dehydrated alcohol mixture (tetraethyl orthosilicate: dehydrated alcohol=
1:3；Volume ratio), and aging 24h at 60 DEG C.
D, it is dried: with the product obtained by ethanol purge step C, and at 60 DEG C, preserves 24h, then in 70 DEG C of baking ovens
Dry through 72h, place into aeroge and TiO that 1h at 90 DEG C obtains being dried2Complex powder body.
E, sintering: by the aeroge obtained by step D and TiO2Complex powder body, is put in Muffle furnace and sinters at 600 DEG C
6h；
Prepared by F, composite photo-catalyst slurry: remove ionized water 85g, SN-5040 (wetting dispersing agent) 1g at 500 rpm
Dispersion 10min, adds the composite granule 15g of step E gained, disperses 5min the most at 500 rpm.Add 2-3 times of formulation weight
The zirconium pearl (diameter 2mm) of ratio, disperses 30min (during need condensed water) under 2500rpm-3000rpm, obtain aeroge/
TiO2Slurry, i.e. composite photo-catalyst (aeroge/TiO2), its structure is as shown in Figure 1.
Embodiment 2
Difference from Example 1 is, the nano-TiO used in the present embodiment2For the sharp titanium of UV100: Sha Haliben
Nano-TiO2, the selection of remaining material and preparation method and condition are the most same as in Example 1, obtain composite photo-catalyst.
Embodiment 3
Difference from Example 1 is, the nano-TiO used in the present embodiment2Mixed type for P25: Degussa is received
Rice TiO2(sharp titanium/golden red), the selection of remaining material and preparation method and condition are the most same as in Example 1, obtain complex light
Catalyst.
Embodiment 4
Difference from Example 1 is, in the present embodiment, the mol ratio of silicon and titanium is 10:1, the selection of remaining material with
And preparation method and condition the most same as in Example 1, obtain composite photo-catalyst.
Embodiment 5
Difference from Example 1 is, in the present embodiment, the mol ratio of silicon and titanium is 1:1, the selection of remaining material with
And preparation method and condition the most same as in Example 1, obtain composite photo-catalyst.
Embodiment 6
Difference from Example 1 is, in the present embodiment, step E is sintering 8h, its excess at sintering temperature 500 DEG C
The selection of matter and preparation method and condition are the most same as in Example 1, obtain composite photo-catalyst.
Embodiment 7
Difference from Example 1 is, in the present embodiment, step E is sintering 4h, its excess at sintering temperature 900 DEG C
The selection of matter and preparation method and condition are the most same as in Example 1, obtain composite photo-catalyst.
Comparative example 1-3
In this comparative example, the nano-TiO that will be used2(comparative example 1-3 the most corresponding NT, UV100 and P25) dispersion is inhaled
It is attached to SiO2(by the way of physical mixed), prepares photocatalyst (TiO2+SiO2)。
Comparative example 4
This comparative example is with the difference of embodiment 1, and in this comparative example, the sintering temperature of step E is 450 DEG C, except this
Outside, its preparation method and condition are the most same as in Example 1.
Comparative example 5
This comparative example is with the difference of embodiment 1, and in this comparative example, the sintering temperature of step E is 950 DEG C, except this
Outside, its preparation method and condition are the most same as in Example 1.
Comparative example 6
This comparative example is with the difference of embodiment 1, and in this comparative example, the mol ratio of silicon and titanium is 1:2, except this it
Outward, its preparation method and condition are the most same as in Example 1.
Comparative example 7
This comparative example is with the difference of embodiment 1, and in this comparative example, the mol ratio of silicon and titanium is 12:1, except this it
Outward, its preparation method and condition are the most same as in Example 1.
Comparative example 8-12
With pure TiO2I.e. NT, UV100 and P25 is respectively as comparative example 8-10, with blank aeroge as a comparison case 11, and will
Blank as a comparison case 12.
The composition weight proportioning of the photocatalyst of the preparation of embodiment 1-7 and comparative example 1-12 is as shown in Table 1 and Table 2.
Table 1
Table 2
Application examples 1
This application examples 1 is in coating body by the photocatalyst applications prepared by embodiment 1-7 and comparative example 1-11
System, prepares coating 1-18, as blank, prepares organic varnish being added without the coating (coating 19) of photocatalyst
Film.
Coating 1-18 that the photocatalyst prepared by embodiment 1-7 and comparative example 1-11 prepares and blank
Each constituent content of coating 19 is as shown in Table 3 and Table 4.
Table 3
Table 4
The present invention utilizes coating to the light degradation speed of methylene blue to weigh photocatalysis effect, the light degradation of methylene blue
Speed is that the gray scale difference before and after testing according to Q-UV is weighed: shoot methylene blue on paint film under fixed light source with camera
Photo, analyzes and calculates its grey scale change by the photo imagej obtained, and then with gray scale difference as abscissa, the testing time is
Vertical coordinate is mapped, and slope is the light degradation speed of methylene blue.The light degradation speed of coating is to paint before and after testing according to Q-UV
The weight difference of film is weighed, and weighs the ageing-resistant performance of paint film with this.Test condition is: emittance: 0.71W/m2
(4 fluorescent tubes)；Test temperature: 60 DEG C；Radiation wavelength: UVB-313nm；Photographic light sources: D65, test result is as shown in table 5.
Table 5
Test result shown in table 5 indicates photocatalysis performance and the resistance to ag(e)ing of the light catalyzed coating of different formulations system
Energy.Wherein, methylene blue degradation rate is the highest, represents photocatalysis effect the strongest；Paint film weight-loss ratio is the highest, and photocatalyst pair is described
The damage capability of paint film is the strongest, and the most ageing-resistant ability is the poorest.
Can be drawn by the test result of table 5, coating 15-17 is owing to only adding pure TiO2So that it is ageing-resistant effect is poor,
Cause the loss of paint film weight bigger；Due to SiO in coating 8-102With TiO2Physical mixed so that it is ageing-resistant effect and coating
The ageing-resistant effect of 15-17 is suitable.And the ageing-resistant effect of the coating 1-7 that composite photo-catalyst prepared by the present invention prepares
It is substantially better than the above two, not only there is higher methylene blue degradation rate, and there is relatively low paint film weight-loss ratio, paint film weight
Amount loss is considerably less, and ageing-resistant performance is suitable with the coating 18-19 not adding photocatalyst.Illustrate that the photocatalyst of the present invention can
With while keeping the photocatalysis effect to little molecule harmful organic substance, it is to avoid the degraded to organic paint film.And from photocatalysis
Say in performance, use N hydridization TiO2The catalytic performance of photocatalyst preferable, blank (i.e. coating 19) minimum.This
Bright technology of preparing is applicable to various nano-TiO2, to TiO of the same race2For, the photocatalysis of composite photo-catalyst prepared by the present invention
Effect is preferable, and the degraded to paint film is minimum.
And when in photocatalyst preparation process, sintering temperature is too low, fail to make aeroge aperture cave in, variable density is little,
Reduce with the affinity of water；Aperture is not shunk, and photocatalyst in use dissociates out, and then degraded paint film so that paint film
Degradation rate raises (coating 11)；When sintering temperature is too high, aeroge structure collapse, organic molecule substantially cannot be with photocatalyst
Contact, therefore there is no photocatalysis effect (coating 12), now photocatalysis effect and the blank i.e. photocatalysis effect phase of coating 19
When.As photocatalyst SiO2And TiO2Mol ratio excessive or too small time (such as coating 13, coating 14), its photocatalysis effect is poor,
Analyzing reason is SiO2As porous media, if its content is very few, enrichment reduces, and photocatalysis efficiency can be caused to reduce, and
Very likely result in photocatalyst to be free on beyond porous media, and then cause the degraded of paint film；If TiO2Photocatalyst content is the lowest,
The density causing photocatalyst is the lowest, can affect harmful organic molecule degradation efficiency.
Application examples 2
When application examples 2 is to be added to coating system by different amounts of composite photo-catalyst, investigate Different adding amount to painting
The photocatalysis of material and the impact of ageing-resistant performance.Should prepare coating a-g in use-case 2, concrete formulation for coating material forms such as
Shown in table 6, the photocatalysis and the ageing-resistant performance result that record coating are as shown in table 7.
Table 6
Table 7
From the result of table 7 it follows that (1) is for composite photo-catalyst prepared by the present invention, consumption is the highest, and light is urged
Change effect the best, and do not interfere with paint film stability；(2) the pure TiO to unmodified mistake2For: photocatalysis effect is less than relatively
Composite photo-catalyst (the equivalent TiO answered2Content), paint film is degraded apparently higher than the composite photo-catalyst of the present invention, along with
The rising of its consumption, photocatalyst effect improves, but paint film stability is deteriorated (coating d, e, f).
Applicant states, the present invention illustrates the process of the present invention by above-described embodiment, but the present invention not office
It is limited to above-mentioned processing step, does not i.e. mean that the present invention has to rely on above-mentioned processing step and could implement.Art
Technical staff is it will be clearly understood that any improvement in the present invention, and equivalence to raw material selected by the present invention is replaced and auxiliary element
Interpolation, concrete way choice etc., within the scope of all falling within protection scope of the present invention and disclosure.
Claims (10)
1. a composite photo-catalyst, it is characterised in that described composite photo-catalyst, with porous media as carrier, is filled with light and touches
Matchmaker's aggregate, described composite photo-catalyst is porous three-dimensional network structure, and particle size range is 1-100 μm, described porous media
Pore size is 50-500nm.
Composite photo-catalyst the most according to claim 1, it is characterised in that the particle diameter of described composite photo-catalyst is 20-
40μm；
Preferably, the pore size of described porous media is 50-200nm.
Composite photo-catalyst the most according to claim 1 and 2, it is characterised in that described porous media be aeroge or its
Derivant；
Preferably, any one during described aeroge is silicon system, carbon system, sulfur system, burning system or metal system aeroge
Or the combination of at least two, preferably silica aerogel, further preferred aerosil.
4. according to the composite photo-catalyst according to any one of claim 1-3, it is characterised in that described photocatalyst is for having light
The nano-metal-oxide of catalytic performance or its alloy；
Preferably, described photocatalyst is the Detitanium-ore-type TiO of ultraviolet catalytic2, anatase/rutile mixed type TiO2Or warp
The TiO of the visible light catalytic performance of metal, semimetal, dyestuff or nonmetal doping2In any one or the group of at least two
Close；
Preferably, any one or the combination of at least two during described metal is gold, silver or platinum；
Preferably, described nonmetal for carbon and/or nitrogen.
5. according to the composite photo-catalyst according to any one of claim 1-4, it is characterised in that described porous media touches with light
The mol ratio of matchmaker is 1:1～10:1, preferably 5:1.
6. according to the composite photo-catalyst according to any one of claim 1-5, it is characterised in that described photocatalyst aggregate
Particle diameter is 5-100nm.
7. according to the preparation method of the composite photo-catalyst according to any one of claim 1-6, it is characterised in that described method
Comprise the following steps:
(1) photocatalyst is scattered in porous media, hydrolysis, aging, dry, obtain the complex of porous media and photocatalyst；
(2) porous media step (1) prepared is pulverized with the complex of photocatalyst, sinters 4 little at 500 DEG C-900 DEG C
More than time；
(3) sintered product of step (2) is disperseed in a solvent, then carry out particulate abrasive and obtain composite photo-catalyst slurry
Material, i.e. obtains described composite photo-catalyst.
Preparation method the most according to claim 7, it is characterised in that the temperature of step (1) described hydrolysis is 30-50 DEG C；
Preferably, the time of step (1) described hydrolysis is 10-30 hour；
Preferably, the described aging temperature of step (1) is 50-70 DEG C；
Preferably, step (1) the described aging time is 10-30 hour.
9. according to the preparation method described in claim 7 or 8, it is characterised in that the temperature of step (2) described sintering is 500 DEG C-
900℃；
Preferably, the time of step (2) described sintering is more than 4 hours, preferably 4-8 hour；
Preferably, step (3) described solvent is deionized water；
Preferably, after step (3) described particulate abrasive, the particle diameter of composite photo-catalyst is 1-100 μm, preferably 20-40 μm.
10. a light catalyzed coating, it is characterised in that it contains the composite photo-catalyst according to any one of claim 1-6；
Preferably, described composite photo-catalyst solid addition in coating is 1-20%, preferably 5-12%.
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| CN106693730A (en) * | 2016-12-20 | 2017-05-24 | 济南大学 | Nonmetal multi-doped nTiO2-based visible light catalysis hollow fiber ultrafiltration membrane and preparation method |
| CN107308992A (en) * | 2017-08-23 | 2017-11-03 | 浙江理工大学 | A kind of photocatalytic fiber net and its preparation method and application |
| CN107344749A (en) * | 2017-08-23 | 2017-11-14 | 浙江理工大学 | A kind of photocatalysis landscape tree and its preparation method and application |
| CN107353680A (en) * | 2017-08-23 | 2017-11-17 | 浙江理工大学 | A kind of light catalyzed coating and its preparation method and application |
| CN107365516A (en) * | 2017-08-25 | 2017-11-21 | 安徽智博新材料科技有限公司 | A kind of antifouling Furniture panel of antibacterial and its preparation technology |
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| CN108246319A (en) * | 2016-12-28 | 2018-07-06 | 天津摩根坤德高新科技发展有限公司 | A kind of preparation method of photocatalytic aerogel material |
| CN108610988A (en) * | 2017-06-12 | 2018-10-02 | 郑善 | A kind of absorption of silicon titanium aeroge and photocatalysis interior wall coating |
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| CN106693730B (en) * | 2016-12-20 | 2019-10-25 | 济南大学 | Based on nonmetallic more doping nTiO2Visible light catalytic hollow fiber ultrafiltration membrane and preparation method |
| CN108246319A (en) * | 2016-12-28 | 2018-07-06 | 天津摩根坤德高新科技发展有限公司 | A kind of preparation method of photocatalytic aerogel material |
| CN108610988A (en) * | 2017-06-12 | 2018-10-02 | 郑善 | A kind of absorption of silicon titanium aeroge and photocatalysis interior wall coating |
| CN107308992A (en) * | 2017-08-23 | 2017-11-03 | 浙江理工大学 | A kind of photocatalytic fiber net and its preparation method and application |
| CN107344749A (en) * | 2017-08-23 | 2017-11-14 | 浙江理工大学 | A kind of photocatalysis landscape tree and its preparation method and application |
| CN107353680A (en) * | 2017-08-23 | 2017-11-17 | 浙江理工大学 | A kind of light catalyzed coating and its preparation method and application |
| CN107376885A (en) * | 2017-08-23 | 2017-11-24 | 浙江理工大学 | A kind of photocatalysis artificial flowers and its preparation method and application |
| CN107308992B (en) * | 2017-08-23 | 2022-06-03 | 浙江理工大学 | Photocatalytic fiber net and preparation method and application thereof |
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| CN112870965A (en) * | 2021-01-19 | 2021-06-01 | 黎新安 | Air purification material capable of rapidly degrading formaldehyde and preparation method thereof |
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