CN111635260A - Preparation method of ceramic material for photocatalysis - Google Patents
Preparation method of ceramic material for photocatalysis Download PDFInfo
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- CN111635260A CN111635260A CN202010500645.7A CN202010500645A CN111635260A CN 111635260 A CN111635260 A CN 111635260A CN 202010500645 A CN202010500645 A CN 202010500645A CN 111635260 A CN111635260 A CN 111635260A
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 56
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 97
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims abstract description 21
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000004332 silver Substances 0.000 claims abstract description 8
- -1 silver ions Chemical class 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 229960000583 acetic acid Drugs 0.000 claims description 12
- 108010025899 gelatin film Proteins 0.000 claims description 12
- 239000012362 glacial acetic acid Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000007781 pre-processing Methods 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 230000001954 sterilising effect Effects 0.000 abstract description 5
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 34
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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Abstract
A process for preparing the ceramic material used for photocatalysis includes such steps as choosing carrier, pretreating, preparing titanic acid sol, immersing in ceramic, drying, ageing, high-temp heat treatment and annealing. The invention has simple preparation, effectively enhances the sterilization capability of the photocatalytic ceramic, slows down the reduction rate of photocatalysis of the photocatalytic ceramic, and can increase the sterilization capability of the photocatalytic ceramic by adding silver ions and copper ions.
Description
Technical Field
The invention relates to the field of photocatalytic ceramic preparation, in particular to a preparation method of a ceramic material for photocatalysis.
Background
The water environment pollution of China is very severe, pollution accidents are frequent in recent years, and the sustainable development of the health of residents and the national economy is directly influenced. Meanwhile, China is also a country with relatively serious indoor air quality, and the main reasons are toxic substance volatilization in decoration materials, biological pollution of bacteria and poor ventilation. Therefore, the technology for treating three wastes of the photocatalytic ceramic is developed, the application of the high-technology ceramic in environmental protection and energy conservation is expanded, the national sustainable development strategy is completely met, and the direction of industrial structure adjustment in the ceramic industry is also met.
The existing preparation method of the photocatalytic ceramic mostly adopts butyl titanate as a main raw material, and n-butyl ester or isopropanol as a solvent to soak the ceramic, but the photocatalytic capacity of the photocatalytic ceramic prepared by the method is reduced quickly, the photocatalytic ceramic cannot be used for a long time, and the sterilizing capacity of the photocatalytic ceramic prepared by the method is not strong.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a ceramic material for photocatalysis, which is simple to prepare, effectively enhances the sterilization capability and reduces the reduction rate of the photocatalysis function.
In order to achieve the aim of the invention, the invention adopts the specific scheme that:
a preparation method of a ceramic material for photocatalysis comprises the following steps:
(1) selecting a carrier and preprocessing, selecting common glazed ceramics as the carrier, putting the selected common glazed ceramics into an ultrasonic vibrator, and cleaning for 5 minutes;
(2) preparing a precursor solution, taking butyl titanate as a main raw material, adding water, glacial acetic acid and butyl-n-alcohol, mixing the butyl titanate, the water, the glacial acetic acid and the butyl-n-alcohol according to a molar ratio of 1:3:8:10, and stirring for 10 minutes to obtain titanic acid sol;
(3) completely immersing the pretreated common glazed ceramic into titanic acid sol, keeping for 5 minutes, and then pulling out the common glazed ceramic at a certain speed to obtain the common glazed ceramic with the sol film attached to the surface;
(4) standing the common glazed ceramic with the sol film attached to the surface in a ventilated and shady place, drying and aging for 1 hour to obtain the common glazed ceramic with the gel film attached to the surface;
(5) placing the common glazed ceramic with the surface attached with the gel film into a muffle furnace, keeping the temperature at 500 ℃, firing for 1 hour, taking out the fired common glazed ceramic, and then carrying out annealing treatment to obtain the common glazed ceramic with the surface attached with the photocatalytic film;
(6) and (3) putting the common glazed ceramic with the photocatalytic film attached to the surface into the titanium acid sol, repeating the operation for 1, 2, 5 and 10 times to obtain the common glazed ceramic with different thicknesses of the photocatalytic film attached to the surface.
As an improvement, 3-5% of silver ions or copper ions are added into the titanic acid sol.
As a modification, the speed of pulling out the ordinary glaze ceramic immersed in the titanic acid sol is 3 cm/s.
The invention has the beneficial effects that:
the preparation method is simple, the sterilization capability of the photocatalytic ceramic is effectively enhanced, the reduction rate of photocatalysis of the photocatalytic ceramic is slowed down, and the antibacterial capability of the photocatalytic ceramic can be enhanced through the added silver ions and copper ions.
Detailed Description
The present invention is further described below by way of specific examples, but the present invention is not limited to only the following examples. Variations, combinations, or substitutions of the invention, which are within the scope of the invention or the spirit, scope of the invention, will be apparent to those of skill in the art and are within the scope of the invention.
Example one
A preparation method of a ceramic material for photocatalysis comprises the following steps:
(1) selecting a carrier and preprocessing, selecting common glazed ceramics as the carrier, putting the selected common glazed ceramics into an ultrasonic vibrator, and cleaning for 5 minutes;
(2) preparing a precursor solution, taking butyl titanate as a main raw material, adding water, glacial acetic acid and butyl-n-alcohol, mixing the butyl titanate, the water, the glacial acetic acid and the butyl-n-alcohol according to a molar ratio of 1:3:8:10, stirring for 10 minutes to obtain titanic acid sol, and adding 3-5% of silver ions or copper ions into the titanic acid sol;
(3) completely immersing the pretreated common glazed ceramic into titanic acid sol, keeping for 5 minutes, and then pulling out the common glazed ceramic at the speed of 3cm/s to obtain the common glazed ceramic with the sol film attached to the surface;
(4) standing the common glazed ceramic with the sol film attached to the surface in a ventilated and shady place, drying and aging for 1 hour to obtain the common glazed ceramic with the gel film attached to the surface;
(5) placing the common glazed ceramic with the surface attached with the gel film into a muffle furnace, keeping the temperature at 500 ℃, firing for 1 hour, taking out the fired common glazed ceramic, and then carrying out annealing treatment to obtain the common glazed ceramic with the surface attached with the photocatalytic film;
(6) and putting the common glaze ceramic with the photocatalytic film attached to the surface into a titanium acid sol to obtain the common glaze ceramic with the photocatalytic film attached to the surface.
Example two
A preparation method of a ceramic material for photocatalysis comprises the following steps:
(1) selecting a carrier and preprocessing, selecting common glazed ceramics as the carrier, putting the selected common glazed ceramics into an ultrasonic vibrator, and cleaning for 5 minutes;
(2) preparing a precursor solution, taking butyl titanate as a main raw material, adding water, glacial acetic acid and butyl-n-alcohol, mixing the butyl titanate, the water, the glacial acetic acid and the butyl-n-alcohol according to a molar ratio of 1:3:8:10, stirring for 10 minutes to obtain titanic acid sol, and adding 3-5% of silver ions or copper ions into the titanic acid sol;
(3) completely immersing the pretreated common glazed ceramic into titanic acid sol, keeping for 5 minutes, and then pulling out the common glazed ceramic at the speed of 3cm/s to obtain the common glazed ceramic with the sol film attached to the surface;
(4) standing the common glazed ceramic with the sol film attached to the surface in a ventilated and shady place, drying and aging for 1 hour to obtain the common glazed ceramic with the gel film attached to the surface;
(5) placing the common glazed ceramic with the surface attached with the gel film into a muffle furnace, keeping the temperature at 500 ℃, firing for 1 hour, taking out the fired common glazed ceramic, and then carrying out annealing treatment to obtain the common glazed ceramic with the surface attached with the photocatalytic film;
(6) and (3) putting the common glaze ceramic with the photocatalytic film attached to the surface into the titanium acid sol, repeating the operation for 2 times to obtain the common glaze ceramic with the two photocatalytic films attached to the surface.
EXAMPLE III
A preparation method of a ceramic material for photocatalysis comprises the following steps:
(1) selecting a carrier and preprocessing, selecting common glazed ceramics as the carrier, putting the selected common glazed ceramics into an ultrasonic vibrator, and cleaning for 5 minutes;
(2) preparing a precursor solution, taking butyl titanate as a main raw material, adding water, glacial acetic acid and butyl-n-alcohol, mixing the butyl titanate, the water, the glacial acetic acid and the butyl-n-alcohol according to a molar ratio of 1:3:8:10, stirring for 10 minutes to obtain titanic acid sol, and adding 3-5% of silver ions or copper ions into the titanic acid sol;
(3) completely immersing the pretreated common glazed ceramic into titanic acid sol, keeping for 5 minutes, and then pulling out the common glazed ceramic at the speed of 3cm/s to obtain the common glazed ceramic with the sol film attached to the surface;
(4) standing the common glazed ceramic with the sol film attached to the surface in a ventilated and shady place, drying and aging for 1 hour to obtain the common glazed ceramic with the gel film attached to the surface;
(5) placing the common glazed ceramic with the surface attached with the gel film into a muffle furnace, keeping the temperature at 500 ℃, firing for 1 hour, taking out the fired common glazed ceramic, and then carrying out annealing treatment to obtain the common glazed ceramic with the surface attached with the photocatalytic film;
(6) and putting the common glaze ceramic with the photocatalytic film attached to the surface into the titanium acid sol, repeating the operation for 5 times to obtain the common glaze ceramic with the five photocatalytic films attached to the surface.
Example four
A preparation method of a ceramic material for photocatalysis comprises the following steps:
(1) selecting a carrier and preprocessing, selecting common glazed ceramics as the carrier, putting the selected common glazed ceramics into an ultrasonic vibrator, and cleaning for 5 minutes;
(2) preparing a precursor solution, taking butyl titanate as a main raw material, adding water, glacial acetic acid and butyl-n-alcohol, mixing the butyl titanate, the water, the glacial acetic acid and the butyl-n-alcohol according to a molar ratio of 1:3:8:10, stirring for 10 minutes to obtain titanic acid sol, and adding 3-5% of silver ions or copper ions into the titanic acid sol;
(3) completely immersing the pretreated common glazed ceramic into titanic acid sol, keeping for 5 minutes, and then pulling out the common glazed ceramic at the speed of 3cm/s to obtain the common glazed ceramic with the sol film attached to the surface;
(4) standing the common glazed ceramic with the sol film attached to the surface in a ventilated and shady place, drying and aging for 1 hour to obtain the common glazed ceramic with the gel film attached to the surface;
(5) placing the common glazed ceramic with the surface attached with the gel film into a muffle furnace, keeping the temperature at 500 ℃, firing for 1 hour, taking out the fired common glazed ceramic, and then carrying out annealing treatment to obtain the common glazed ceramic with the surface attached with the photocatalytic film;
(6) and putting the common glazed ceramic with the photocatalytic film attached to the surface into the titanium acid sol, repeating the operation for 10 times to obtain the common glazed ceramic with ten layers of photocatalytic films attached to the surface.
Combining the general glazed ceramics prepared in the first to fourth examples, which have four different numbers of photocatalytic films, at the time of simulating night, namely, under the condition of black light irradiation, the ordinary glazed ceramics with five photocatalytic films has higher photocatalytic activity than the ordinary glazed ceramics with one photocatalytic film and the ordinary glazed ceramics with two photocatalytic films, mainly because the film thickness is increased and the photocatalytic reaction surface area is increased, the absorption capacity to light is enhanced, the photocatalytic activity is improved, but compared with the common glazed ceramics of five photocatalytic films, the common glazed ceramics of ten photocatalytic films have basically no difference in antibacterial performance, this is mainly because an excessive increase in film thickness causes surface agglomeration, increases the grain size during sintering, and relatively decreases the effective particle surface area in the thin film.
In conclusion, the common glaze ceramic with five layers of photocatalytic films not only has stronger antibacterial performance, but also has economical efficiency.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (3)
1. A preparation method of a ceramic material for photocatalysis is characterized by comprising the following steps:
(1) selecting a carrier and preprocessing, selecting common glazed ceramics as the carrier, putting the selected common glazed ceramics into an ultrasonic vibrator, and cleaning for 5 minutes;
(2) preparing a precursor solution, taking butyl titanate as a main raw material, adding water, glacial acetic acid and butyl-n-alcohol, mixing the butyl titanate, the water, the glacial acetic acid and the butyl-n-alcohol according to a molar ratio of 1:3:8:10, and stirring for 10 minutes to obtain titanic acid sol;
(3) completely immersing the pretreated common glazed ceramic into titanic acid sol, keeping for 5 minutes, and then pulling out the common glazed ceramic at a certain speed to obtain the common glazed ceramic with the sol film attached to the surface;
(4) standing the common glazed ceramic with the sol film attached to the surface in a ventilated and shady place, drying and aging for 1 hour to obtain the common glazed ceramic with the gel film attached to the surface;
(5) placing the common glazed ceramic with the surface attached with the gel film into a muffle furnace, keeping the temperature at 500 ℃, firing for 1 hour, taking out the fired common glazed ceramic, and then carrying out annealing treatment to obtain the common glazed ceramic with the surface attached with the photocatalytic film;
(6) and (3) putting the common glazed ceramic with the photocatalytic film attached to the surface into the titanium acid sol, repeating the operation for 1, 2, 5 and 10 times to obtain the common glazed ceramic with different thicknesses of the photocatalytic film attached to the surface.
2. The method for preparing a ceramic material for photocatalysis according to claim 1, wherein: and 3-5% of silver ions or copper ions are added into the titanic acid sol.
3. The method for preparing a ceramic material for photocatalysis according to claim 1, wherein: the speed of pulling out the common glaze ceramic immersed in the titanic acid sol is 3 cm/s.
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Application publication date: 20200908 |