CN102500313B - Preparation method of nano semiconductor material loaded on silicate substrate - Google Patents

Preparation method of nano semiconductor material loaded on silicate substrate Download PDF

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CN102500313B
CN102500313B CN 201110309189 CN201110309189A CN102500313B CN 102500313 B CN102500313 B CN 102500313B CN 201110309189 CN201110309189 CN 201110309189 CN 201110309189 A CN201110309189 A CN 201110309189A CN 102500313 B CN102500313 B CN 102500313B
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silicate
preparation
nano
semiconductor material
carrier
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CN102500313A (en
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徐海
李书耘
李风翠
许慧
李慧芳
伍海波
张强
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Changsha landmark Technology Co., Ltd.
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Hunan Wenxiang Carbon Based Environmental Protection Material Co Ltd
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Abstract

The invention provides a nano semiconductor material loaded on a silicate substrate, which has an excellent air purifying action. The semiconductor material comprises the silicate substrate, wherein a nano TiO2 thin film is attached on the surface of the silicate substrate. The preparation method of the semiconductor material comprises the steps of: preparing a carrier material with one or more silicates as raw materials, preparing a sol with a titanium salt as a precursor, loading the sol containing a photoactive compound on the carrier by an immersion method, drying and calcining. The semiconductor material effectively combines the silicate mineral and titanium salt, and is catalytically decomposed under a visible light condition so as to sufficiently exert the air purifying action.

Description

Load on the preparation method of the nano semiconductor material on the silicate-base
Technical field
The present invention relates to a kind of be used to the preparation methods that purifies air, particularly a kind of preparation method who loads on the nano semiconductor material on the silicate-base.
Background technology
Raising along with development of science and technology and people's living standard, the environment that the mankind depend on for existence has but suffered more and more serious destruction, the situation that indoor air is polluted is also more and more serious, particularly the harmful organic substance in the smoke from cigarette has threatened human beings'health especially, therefore has the materials with function of purifying the air of a room and more and more is subject to people's attention.
Natural silicate mineral such as zeolite, diatomite, attapulgite, vermiculite, perlite have physisorption and ion exchange, and airborne toxic and harmful is had the good adsorption effect, but can not the poisonous and harmful of absorption be decomposed; Nano titanium oxide can be decomposed into nontoxic hydrone and carbon dioxide etc. with airborne catalytic organism under illumination, but does not have suction-operated, and difficulty contacts with harmful molecule, decomposes slowly.
For obtaining a kind of material for air purification that can comparatively fast adsorb and thoroughly remove pernicious gas, the present invention will provide a kind of nano semiconductor material on the silicate-base and preparation method thereof that loads on, and this material can play the effect that purifies the air of a room for a long time.
Summary of the invention
First purpose of the present invention is in order to overcome silicate mineral and the titanium salt defective that its effect that purifies air can not be given full play to when separately using, a kind of nano semiconductor material that loads on the silicate-base is provided, this material effectively combines silicate mineral and titanium salt, catalytic decomposition under the visible light condition makes it give full play to the effect that purifies air.
Second purpose of the present invention provides a kind of preparation method for the production of above-mentioned material.
The objective of the invention is to realize as follows: the described nano semiconductor material on the silicate-base and preparation method thereof that loads on, be to be the feedstock production carrier material with one or more silicate, be that presoma prepares colloidal sol with the titanium salt, the colloidal sol that the recycling infusion process will contain Photoactive compounds loads on the carrier, drying, calcining and make.
Concrete scheme is as follows:
A kind of nano semiconductor material that loads on the silicate-base has silicates basal body, has nano-TiO in the silicate-base surface 2(titanium dioxide) film.
Load on the preparation method of the nano semiconductor material on the silicate-base, may further comprise the steps:
1) preparation carrier:
A: the silicate with particle diameter 20~50 μ m is raw material, adds alkaline solution, and wherein silicate is 100~150:1 with the weight ratio of the alkali compounds of preparation alkaline solution; Be transferred to after mixing that to carry out roasting in the reactor expanded, sintering temperature is 480 ℃~850 ℃, and the still internal pressure is 0.8~1.3MPa, and roasting time is 1~10min; Take out the cooling back and grind screening, the screen size scope is 0.5~30 μ m, obtains Powdered silicate-base carrier;
B: the silicate with particle diameter 20~50 μ m is raw material, adds an amount of alkaline solution, and wherein silicate is 100~150:1 with the weight ratio of the alkali compounds of preparation alkaline solution; Be transferred to after mixing that to carry out roasting in the reactor expanded, sintering temperature is 480 ℃~850 ℃, and the still internal pressure is 0.8-~1.3MPa, and roasting time is 1~10min; Take out the cooling back and grind screening, the screen size scope is 0.5~30 μ m, obtains Powdered silicate-base carrier; Add the water-based adhesive in Powdered silicate-base carrier, the weight ratio of powder silicate and aqueous gel is 5:2~3, fully mixes, and mixture is put into press be pressed into plate, namely gets bulk silicon hydrochlorate base carrier;
2) preparation nano-TiO 2Colloidal sol: titanium salt and absolute ethyl alcohol are stirred 2~10h in acetylacetone,2,4-pentanedione or glacial acetic acid solvent, wherein, titanium salt: absolute ethyl alcohol: the weight ratio of acetylacetone,2,4-pentanedione or glacial acetic acid solvent is 1:1.5~4:0.1~0.2, after fully mixing, adding concentration is 20% ethanolic solution, wherein the weight ratio of titanium salt and 20% ethanolic solution is 1:0.5~1.2, leaves standstill 5~24h and forms nano-TiO 2Colloidal sol;
3) preparation semi-conducting material:
C: adopt method for suppersonic cleaning that the Powdered silicate-base carrier of step (1) A preparation is cleaned, then it is inserted fast in the sol solution of step (2) preparation, after soaking 2~10min, filter, after filter cake dried in the shade naturally, put into drying box drying 10~30min of 100~150 ℃, in the Muffle furnace of inserting again, 500~550 ℃ of roasting temperature 30~60min, naturally take out the cooling back, grind screening, the screen size scope is 0.5~30 μ m, and namely getting Powdered is the nano-titanium dioxide film semi-conducting material of matrix with silicate;
D: adopt method for suppersonic cleaning that the bulk silicon hydrochlorate base carrier for preparing among step (1) B is cleaned, then the silicate-base carrier is inserted fast the nano-TiO of step (2) preparation 2In the colloidal sol, soak after 2~10 minutes, with the speed of 0.5~3mm/s carrier is vertically drawn proposition colloidal sol, make its surface plating layer of even nano-TiO 2Film, after the air dry, the carrier that is coated with film put into 100~150 ℃ the dry 10~30min of drying box, insert roasting 30~60min in 500~550 ℃ Muffle furnace again, naturally take out the cooling back, and what namely obtain bulk is the nano-titanium dioxide film semi-conducting material of matrix with silicate.
Described alkali compounds is selected from a kind of in NaOH, potassium hydroxide, sodium carbonate, sodium acid carbonate, potash, the saleratus.
Described silicate is selected from one or more the mixture in zeolite, diatomite, attapulgite, vermiculite, the perlite.
Described titanium salt is selected from a kind of in tetraethyl titanate, butyl titanate, titanium propanolate, isopropyl titanate, the titanyl sulfate.
The water-based adhesive is selected from one or more the mixture in aqueous polyurethane, water polyacrylic acid, butadiene-styrene latex, acrylate, the neoprene latex.
Natural silicate raw mineral materials such as zeolite, diatomite, attapulgite, vermiculite, perlite sources is abundant, cheap, and has characteristics such as physisorption, ion exchange, chemical property be stable usually because of its some special structures.
The same source of titanium salts such as butyl titanate, titanium propanolate, tetraethyl titanate, isopropyl titanate or titanyl sulfate is abundant, cheap, airborne catalytic organism can be decomposed under illumination, can reach the purpose that purifies air.
Beneficial effect of the present invention: the nano semiconductor material that loads on the silicate-base of the present invention, have that specific area is big, load fastness height, reactivity height, photocatalysis be effective, can be under the visible light condition catalytic decomposition indoor harmful gas, have advantages such as physical absorption and chemical degradation simultaneously concurrently, can be widely used in industries such as high-grade paint, building material, fine chemistry industry, high-grade handicraft.The preparation method who loads on the nano semiconductor material on the silicate-base of the present invention, raw material is easy to get, and technology is simple, and production cost is low, is easy to large-scale production.
Description of drawings
Fig. 1 loads on the structural representation of the nano semiconductor material on the silicate-base;
Fig. 2 is preparation flow figure of the present invention.
Among the figure: 1. silicates basal body, 2. nano-TiO 2Film
The specific embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments.
The invention discloses a kind of nano semiconductor material that loads on the silicate-base, its structure has silicates basal body 1 as shown in fig. 1, has nano-TiO on silicates basal body 1 surface 2Film 2.This silicate-base nano semiconductor material has that specific area is big, load fastness height, photocatalysis are effective, has advantages such as physical absorption and chemical degradation simultaneously concurrently, can be widely used in industries such as high-grade paint, building material, fine chemistry industry, high-grade handicraft.
Its preparation method is flow chart as shown in Figure 2, is the feedstock production carrier material with one or more silicate, obtains the silicate-base carrier through expanded roasting.Be that presoma prepares colloidal sol with the titanium salt, the colloidal sol that the recycling infusion process will contain Photoactive compounds loads on the carrier, drying, calcining and make.
With specific embodiment preparation method of the present invention is described below, its preparation process as shown in Figure 2.
Embodiment 1
(1) be that to add concentration in the diatomite of 20~50 μ m be 15% sodium carbonate liquor 5ml at the 100g particle diameter, mix that be transferred to then that to carry out roasting in the reactor expanded, sintering temperature is 500 ℃, the still internal pressure is 1MPa, and roasting time is 10min.After roasting finishes, the calcining matter taking-up is cooled to room temperature, grinds screening, the screen size scope is 0.5~30 μ m, namely gets Powdered diatomite base carrier.
(2) get the 30g absolute ethyl alcohol and the 20g butyl titanate places container, mix and form mixed liquor together, and to add 2g acetylacetone,2,4-pentanedione solution, 10g concentration in mixed liquor successively be 20% ethanolic solution while stirring, after acetylacetone,2,4-pentanedione solution and ethanol water all add, continue to stir 4h again, stablized, even, transparent light yellow colloidal sol, leave standstill behind the 12h standby.
(3) get the Powdered silicate-base carrier 50g that step (1) prepares, adopt method for suppersonic cleaning that it is cleaned, then it is inserted fast in the sol solution of step (2) preparation, stir, after soaking 2min, filter, after filter cake dried in the shade naturally, put into 100 ℃ the dry 5min of drying box, insert in the Muffle furnace 500 ℃ of roasting temperature 30min again, naturally take out the cooling back, grind screening, the screen size scope is 0.5~30 μ m, and namely getting Powdered is the nano-titanium dioxide film semi-conducting material of matrix with diatomite.
Embodiment 2
(1) be that to add concentration in the zeolite of 20~50 μ m be 20% potassium hydroxide solution 5ml at the 100g particle diameter, mix that be transferred to then that to carry out roasting in the reactor expanded, sintering temperature is 650 ℃, the still internal pressure is 0.8MPa, and roasting time is 5min.After roasting finishes, the calcining matter taking-up is cooled to room temperature, grinds screening, the screen size scope is 0.5~30 μ m, namely gets the zeolite powder base carrier.
(2) get the 80g absolute ethyl alcohol and the 20g titanyl sulfate places container, mix by agitator and to form mixed liquor together, to add 6g glacial acetic acid solution, 24g concentration in mixed liquor successively be 20% ethanolic solution while stirring then, after acetylacetone,2,4-pentanedione solution and ethanol water all add, continue to stir 6h again, stablized, even, transparent light yellow colloidal sol, leave standstill behind the 8h standby.
(3) get the zeolite powder base carrier 50g that step (1) prepares, adopt method for suppersonic cleaning that it is cleaned, then it is inserted fast in the sol solution of step (2) preparation, stir, after soaking 5min, filter, after filter cake dried in the shade naturally, put into 150 ℃ the dry 10min of drying box, insert in the Muffle furnace 520 ℃ of roasting temperature 45min again, naturally take out the cooling back, grind screening, the screen size scope is 0.5~30 μ m, and namely getting Powdered is the nano-titanium dioxide film semi-conducting material of matrix with the zeolite.
Embodiment 3
(1) adding concentration in the silicate mixture that comprises the vermiculite that diatomite that the 80g particle diameter is 20~50 μ m and 70g particle diameter be 20~50 μ m is 20% sodium bicarbonate solution 5ml, mix, be transferred to then that to carry out roasting in the reactor expanded, sintering temperature is 850 ℃, the still internal pressure is 1.3MPa, and roasting time is 3min.After roasting finishes, the calcining matter taking-up is cooled to room temperature, grinds screening, the screen size scope is 0.5~30 μ m, namely gets Powdered silicate carrier.
(2) get the 40g absolute ethyl alcohol and the 20g butyl titanate places container, mix by agitator and to form mixed liquor together, to add 4g acetylacetone,2,4-pentanedione solution, 20g concentration in mixed liquor successively be 20% ethanolic solution while stirring then, after acetylacetone,2,4-pentanedione solution and ethanol water all add, continue to stir 8h again, stablized, even, transparent light yellow colloidal sol, leave standstill behind the 24h standby.
(3) get the Powdered silicate carrier 50g that step (1) prepares, adopt method for suppersonic cleaning that it is cleaned, then it is inserted fast in the sol solution of step (2) preparation, stir, after soaking 3min, filter, after filter cake dried in the shade naturally, put into 130 ℃ the dry 20min of drying box, insert in the Muffle furnace 550 ℃ of roasting temperature 45min again, naturally take out the cooling back, grind screening, the screen size scope is 0.5~30 μ m, and namely getting Powdered is the nano-titanium dioxide film semi-conducting material of matrix with silicate.
Embodiment 4
(1) be that to add concentration in the perlite of 20~50 μ m be 10% sodium hydroxide solution 10ml at the 120g particle diameter, mix that be transferred to then that to carry out roasting in the reactor expanded, sintering temperature is 600 ℃, the still internal pressure is 1.3MPa, and roasting time is 8min.After roasting finishes, the calcining matter taking-up is cooled to room temperature, grinds screening, the screen size scope is 0.5~30 μ m, namely gets Powdered perlite base carrier.
(2) get the 50g absolute ethyl alcohol and the 20g butyl titanate places container, mix by agitator and to form mixed liquor together, to add 4g glacial acetic acid solution, 14g concentration in mixed liquor successively be 20% ethanolic solution while stirring then, after acetylacetone,2,4-pentanedione solution and ethanol water all add, continue to stir 4h again, stablized, even, transparent light yellow colloidal sol, leave standstill behind the 12h standby.
(3) get the Powdered perlite base carrier 50g that step (1) prepares, adopt method for suppersonic cleaning that it is cleaned, then it is inserted fast in the sol solution of step (2) preparation, stir, after soaking 6min, filter, after filter cake dried in the shade naturally, put into 120 ℃ the dry 15min of drying box, insert in the Muffle furnace 510 ℃ of roasting temperature 40min again, naturally take out the cooling back, grind screening, the screen size scope is 0.5~30 μ m, and namely getting Powdered is the nano-titanium dioxide film semi-conducting material of matrix with the perlite.
Embodiment 5
(1) adding concentration in the silicate mixture that comprises diatomite that the 60g particle diameter is 20~50 μ m, attapulgite that the 30g particle diameter is 20~50 μ m, zeolite that the 55g particle diameter is 20~50 μ m is 20% solution of potassium carbonate 5ml, mix, be transferred to then that to carry out roasting in the reactor expanded, sintering temperature is 750 ℃, the still internal pressure is 1MPa, and roasting time is 4min.After roasting finishes, calcining matter is taken out, be cooled to room temperature, grind screening, the screen size scope is 0.5~30 μ m, namely gets Powdered silicate-base carrier.Get Powdered diatomite 50g, add the 20g tetraethyl titanate therein, fully mix, mixture is put into press be pressed into plate, namely get bulk silicon hydrochlorate base carrier.
(2) get the 60g absolute ethyl alcohol and the 20g isopropyl titanate places container, mix by agitator and to form mixed liquor together, to add 2.6g acetylacetone,2,4-pentanedione, 18g concentration in mixed liquor successively be 20% ethanolic solution while stirring then, after acetylacetone,2,4-pentanedione solution and ethanol water all add, continue to stir 7h again, stablized, even, transparent light yellow colloidal sol, leave standstill behind the 5h standby.
(3) adopt method for suppersonic cleaning that the bulk silicon hydrochlorate base carrier of preparation in the step (2) is cleaned, then it is inserted fast soak 10min in the sol solution of step (3) preparation after, speed about adopting homemade pulling machine with 1mm/s lifts vertically upward, and making its surface plating layer of even sol pellicle is nano thin-film.After taking out air dry, the bulk silicon hydrochlorate base carrier that is coated with film put into 150 ℃ the dry 30min of drying box, insert again in the Muffle furnace, 550 ℃ of roasting temperature 60min, cooling back takes out that namely to get block be the nano-titanium dioxide film semi-conducting material of matrix with silicate naturally.
Embodiment 6
(1) be that to add concentration in the attapulgite of 20~50 μ m be 10% potassium hydroxide solution 10ml at the 125g particle diameter, mix, be transferred to then that to carry out roasting in the reactor expanded, sintering temperature is 480 ℃, the still internal pressure is 1.2MPa, and roasting time is 10min.After roasting finishes, calcining matter is taken out, be cooled to room temperature, grind screening, the screen size scope is 0.5~30 μ m, namely gets Powdered attapulgite base carrier.Get Powdered attapulgite 50g, add the 25g acrylate therein, fully mix, mixture is put into press be pressed into plate, namely get block attapulgite base carrier.
(2) get the 70g absolute ethyl alcohol and the 20g butyl titanate places container, mix by agitator and to form mixed liquor together, to add 6g glacial acetic acid, 22g concentration in mixed liquor successively be 20% ethanolic solution while stirring then, after acetylacetone,2,4-pentanedione solution and ethanol water all add, continue to stir 4h again, stablized, even, transparent light yellow colloidal sol, leave standstill behind the 12h standby.
(3) adopt method for suppersonic cleaning that the block attapulgite base carrier of preparation in the step (2) is cleaned, then it is inserted fast soak 8min in the sol solution of step (3) preparation after, speed about adopting homemade pulling machine with 2mm/s lifts vertically upward, and making its surface plating layer of even sol pellicle is nano thin-film.After taking out air dry, the block attapulgite base carrier that is coated with film put into 110 ℃ the dry 20min of drying box, insert again in the Muffle furnace, 530 ℃ of roasting temperature 40min, cooling back takes out that namely to get block be the nano-titanium dioxide film semi-conducting material of matrix with the attapulgite naturally.
Embodiment 7
(1) adding concentration at particle diameter in the perlite 110g of 20~50 μ m is 20% potassium bicarbonate solution 5ml, mixes, and is transferred to then that to carry out roasting in the reactor expanded, and sintering temperature is 500 ℃, and the still internal pressure is 1MPa, and roasting time is 10min.After roasting finishes, calcining matter is taken out, be cooled to room temperature, grind screening, the screen size scope is 0.5~30 μ m, namely gets Powdered diatomite base carrier.Get Powdered diatomite 50g, add 10g butadiene-styrene latex, 10g neoprene latex, 10g acrylate therein, fully mix, mixture is put into press be pressed into plate, namely get block diatom soil matrix carrier.
(2) get the 46g absolute ethyl alcohol and the 20g titanium propanolate places container, mix by agitator and to form mixed liquor together, to add 3g acetylacetone,2,4-pentanedione, 12g concentration in mixed liquor successively be 20% ethanolic solution while stirring then, after acetylacetone,2,4-pentanedione solution and ethanolic solution all add, continue to stir 3h again, stablized, even, transparent light yellow colloidal sol, leave standstill behind the 20h standby.
(3) adopt method for suppersonic cleaning that the block perlite base carrier of preparation in the step (2) is cleaned, then it is inserted fast soak 7min in the sol solution of step (3) preparation after, speed about adopting homemade pulling machine with 0.5mm/s lifts vertically upward, and making its surface plating layer of even sol pellicle is nano thin-film.After taking out air dry, the block perlite base carrier that is coated with film put into 140 ℃ the dry 25min of drying box, insert again in the Muffle furnace, 530 ℃ of roasting temperature 50min, cooling back takes out that namely to get block be the nano-titanium dioxide film semi-conducting material of matrix with the perlite naturally.
Embodiment 8
(1) be that to add concentration in the vermiculite of 20~50 μ m be 15% solution of potassium carbonate 5ml at the 135g particle diameter, mix that be transferred to then that to carry out roasting in the reactor expanded, sintering temperature is 600 ℃, the still internal pressure is 0.9MPa, and roasting time is 9min.After roasting finishes, calcining matter is taken out, be cooled to room temperature, grind screening, the screen size scope is 0.5~30 μ m, namely gets Powdered vermiculite base carrier.Get Powdered vermiculite 50g, add 11g neoprene latex, 11g acrylate therein, fully mix, mixture is put into press be pressed into plate, namely get block vermiculite base carrier.
(2) get the 36g absolute ethyl alcohol and the 20g tetraethyl titanate places container, mix by agitator and to form mixed liquor together, to add 5g glacial acetic acid, 16g concentration in mixed liquor successively be 20% ethanolic solution while stirring then, after acetylacetone,2,4-pentanedione solution and ethanol water all add, continue to stir 7h again, stablized, even, transparent light yellow colloidal sol, leave standstill behind the 5h standby.
(3) adopt method for suppersonic cleaning that the block vermiculite base carrier of preparation in the step (2) is cleaned, then it is inserted fast soak 10min in the sol solution of step (3) preparation after, speed about adopting homemade pulling machine with 3mm/s lifts vertically upward, and making its surface plating layer of even sol pellicle is nano thin-film.After taking out air dry, the block vermiculite base carrier that is coated with film put into 100 ℃ the dry 30min of drying box, insert again in the Muffle furnace, 515 ℃ of roasting temperature 35min, cooling back takes out that namely to get block be the nano-titanium dioxide film semi-conducting material of matrix with the vermiculite naturally.

Claims (5)

1. load on the preparation method of the nano semiconductor material on the silicate-base, this nano semiconductor material has silicates basal body, has nano-TiO in the silicate-base surface 2Film is characterized in that:
1) preparation carrier:
A: the silicate with particle diameter 20~50 μ m is raw material, adds alkaline solution, and wherein contained alkali compounds weight ratio is 100~150:1 in silicate and the aqueous slkali; Be transferred to after mixing that to carry out roasting in the reactor expanded, sintering temperature is 480 ℃~850 ℃, and the still internal pressure is 0.8~1.3MPa, and roasting time is 1~10min; Take out the cooling back and grind screening, the screen size scope is 0.5~30 μ m, obtains Powdered silicate-base carrier;
B: the silicate with particle diameter 20~50 μ m is raw material, adds alkaline solution, and wherein silicate is 100~150:1 with preparing alkali compounds weight ratio contained in the alkaline solution; Be transferred to after mixing that to carry out roasting in the reactor expanded, sintering temperature is 480 ℃~850 ℃, and the still internal pressure is 0.8~1.3MPa, and roasting time is 1~10min; Take out the cooling back and grind screening, the screen size scope is 0.5~30 μ m, obtains Powdered silicate-base carrier; Add the water-based adhesive in Powdered silicate-base carrier, the mass ratio of powder silicate and glue is 5:2~3, fully mixes, and mixture is put into press be pressed into plate, namely gets bulk silicon hydrochlorate base carrier;
2) preparation nano-TiO 2Colloidal sol: titanium salt and absolute ethyl alcohol are stirred 2~10h in acetylacetone,2,4-pentanedione or glacial acetic acid solvent, wherein, the weight ratio of titanium salt, absolute ethyl alcohol, acetylacetone,2,4-pentanedione or glacial acetic acid solvent is 1:1.5~4:0.1~0.3; After fully mixing, adding concentration is 20% ethanolic solution, and wherein the weight ratio of titanium salt and 20% ethanolic solution is 1:0.5~1.2, leaves standstill 5~24h and forms nano-TiO 2Colloidal sol;
3) preparation semi-conducting material:
C: adopt method for suppersonic cleaning that the Powdered silicate-base carrier of step (1) A preparation is cleaned, then it is inserted fast in the sol solution of step (2) preparation, after soaking 2~10min, filter, after filter cake dried in the shade naturally, put into 100~150 ℃ of drying 10~30min in drying box inherence, in the Muffle furnace of inserting again, 500~550 ℃ of roasting temperature 30~60min, naturally take out the cooling back, grind screening, the screen size scope is 0.5~30 μ m, and namely getting Powdered is the nano-titanium dioxide film semi-conducting material of matrix with silicate;
D: adopt method for suppersonic cleaning that the bulk silicon hydrochlorate base carrier for preparing among step (1) B is cleaned, then the silicate-base carrier is inserted fast the nano-TiO of step (2) preparation 2In the colloidal sol, soak after 2~10 minutes, with the speed of 0.5~3mm/s carrier is vertically drawn proposition colloidal sol, make its surface plating layer of even nano-TiO 2Film, after the air dry, the carrier that is coated with film put into 100~150 ℃ the dry 10~30min of drying box, insert roasting 30~60min in 500~550 ℃ the Muffle furnace again, naturally take out the cooling back, and what namely obtain bulk is the nano-titanium dioxide film semi-conducting material of matrix with silicate.
2. the preparation method who loads on the nano semiconductor material on the silicate-base described in claim 1 is characterized in that: described alkali compounds is selected from a kind of in NaOH, potassium hydroxide, sodium carbonate, sodium acid carbonate, potash, the saleratus.
3. the preparation method who loads on the nano semiconductor material on the silicate-base described in claim 1 is characterized in that: described silicate is selected from one or more the mixture in zeolite, diatomite, attapulgite, vermiculite, the perlite.
4. the preparation method who loads on the nano semiconductor material on the silicate-base described in claim 1 is characterized in that: described titanium salt is selected from a kind of in tetraethyl titanate, butyl titanate, titanium propanolate, isopropyl titanate, the titanyl sulfate.
5. the preparation method who loads on the nano semiconductor material on the silicate-base described in claim 1 is characterized in that: the water-based adhesive is selected from one or more the mixture in aqueous polyurethane, water polyacrylic acid, butadiene-styrene latex, acrylate, the neoprene latex.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1419476A (en) * 2000-03-29 2003-05-21 德古萨股份公司 Process for the production of a titanium silicalite shaped article
CN1639064A (en) * 2002-03-07 2005-07-13 昭和电工株式会社 Titanosilicate, process for its production, and its use in producing oxidized compound
CN101062475A (en) * 2006-04-29 2007-10-31 宝山钢铁股份有限公司 Metasilicate hole material assembled nano titanium oxide composite material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1419476A (en) * 2000-03-29 2003-05-21 德古萨股份公司 Process for the production of a titanium silicalite shaped article
CN1639064A (en) * 2002-03-07 2005-07-13 昭和电工株式会社 Titanosilicate, process for its production, and its use in producing oxidized compound
CN101062475A (en) * 2006-04-29 2007-10-31 宝山钢铁股份有限公司 Metasilicate hole material assembled nano titanium oxide composite material and preparation method thereof

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