CN111468089A - Preparation method of gas-induced synthesis ultrafine yellow photocatalyst - Google Patents
Preparation method of gas-induced synthesis ultrafine yellow photocatalyst Download PDFInfo
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Images
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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
- 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
-
- B01J35/39—
-
- B01J35/394—
-
- B01J35/40—
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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
-
- 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
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- 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
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/033—Using Hydrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a preparation method of a gas-induced synthesized ultrafine yellow photocatalyst, which comprises the following steps; preparation of ultrafine white TiO2Nanopowder as the raw material; placing the raw materials in inert atmosphere heat treatment equipment, heating the interior of the inert atmosphere heat treatment equipment to 100-250 ℃, and keeping the temperature in the furnace for 15-30 min; introducing reducing hydrocarbon gas into inert atmosphere heat treatment equipment, and then preserving heat for 5 s-5 min to obtain the superfine yellow TiO2A photocatalyst. The invention relates to gas-induced synthesis of superfine yellow TiO2The preparation method of the photocatalyst has the technical characteristics of simple operation, low equipment requirement, good dispersibility, high repeatability and success rate, and is suitable for large-scale production and use.
Description
Technical Field
The invention relates to a preparation technology of a photocatalyst material, belonging to the technical field of preparation of photocatalyst materials; in particular to a gasInduced synthesis of superfine yellow TiO2A method for preparing a photocatalyst. Meanwhile, the invention also discloses a method for synthesizing superfine yellow TiO based on the gas induction2Superfine yellow TiO prepared by photocatalyst preparation method2A photocatalyst.
Background
Hitherto, people find a large amount of toxic organic pollutants in surface water, underground water and even drinking water, which seriously threatens the production life and life safety of human beings, and the toxic organic pollutants need to be completely treated, and the treatment methods of the toxic organic pollutants are more, wherein the catalytic degradation of the refractory toxic organic matters by using the photocatalyst is a more advanced water pollution treatment method in the existing water purification method.
The photocatalyst catalysis is mainly made of titanium dioxide (TiO)2) The photocatalytic activity of semiconductor photocatalysts as a representative, catalytic degradation of toxic organic pollutants, titanium dioxide (TiO)2) Stable chemical property, low cost and great development potential, however, pure TiO2The forbidden band width of the light source is 3.2eV, the response of the light source to light waves in a visible light wave band is limited, and the utilization rate of the light source to visible light is low. Hoffmann et al found titanium dioxide (TiO)2) The time of oxidation-reduction reaction of electrons and holes on the surface is in the order of microseconds or even milliseconds, but the recombination time is in the order of nanoseconds, so that the recombination rate of the electrons and the holes is a main factor limiting the photocatalytic efficiency, and therefore, the oxidation-reduction reaction is carried out on TiO2The modification is carried out, and the reduction of the forbidden band width and the electron hole recombination rate is particularly important.
In recent years, hydrogen (H) gas has been used2) Synthesizing black or red TiO with different forbidden band widths by chemical vapor deposition under atmosphere2The research on photocatalytic degradation of organic matters has received extensive attention.
Chen et al (Chen et al, Science 2011,331(6018),746) at high pressure H2Under the atmosphere of (2), reacting at 200 ℃ for 5 days to successfully react with white TiO2The black color is changed, and the photocatalytic performance under visible light is greatly improved. Chinese patent 201610244981 discloses a method for preparing titanium foam by etching with alkali solution,Hydrogen ion replacement and calcination are carried out, and finally red TiO with a wedge-shaped structure is prepared2The photoelectrode method not only improves TiO2The light absorption capacity in the visible region and strong absorption in the near infrared region. Chinese patent 201810104208 discloses TiCl3Taking a titanium source, taking a graphite-phase carbon nitride nanosheet as a carrier and alcohol as a solvent, and carrying out hydrothermal treatment in a hydrothermal kettle at the temperature of 70-180 ℃ for 1-12 hours to obtain the superfine TiO2The nano particles are uniformly loaded on the surface of the graphite phase carbon nitride nanosheet to form the composite photocatalyst, so that pollutants in water and air can be effectively removed under the sunlight. However, the above method has many problems, not only is the operation complicated and the conditions harsh, but also the repeatability is not high, and is not suitable for large-scale production.
Disclosure of Invention
Based on the technical problems, the invention provides a method for synthesizing superfine yellow TiO by gas induction2The preparation method of the photocatalyst has the technical effects of simple operation, low equipment requirement, good dispersibility and high repeatability. Meanwhile, the gas is used for inducing and synthesizing the superfine yellow TiO2The invention also discloses a preparation method of the photocatalyst and a superfine yellow TiO2Photocatalyst, the ultrafine yellow TiO2The photocatalyst has the technical effects of low electron hole recombination rate, wide absorption band and high photocatalytic efficiency.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
gas-induced synthesis of superfine yellow TiO2A method for preparing a photocatalyst, the method comprising the steps of;
A. preparation of ultrafine white TiO2Nano powder to obtain raw material;
B. placing the raw materials in inert atmosphere heat treatment equipment, heating the interior of the inert atmosphere heat treatment equipment to 100-250 ℃, and keeping the temperature in the furnace for at least 15 min;
C. introducing reducing hydrocarbon gas into inert atmosphere heat treatment equipment, and then preserving heat for 5 s-5 min to obtain the superfine yellow TiO2A photocatalyst.
Further, theIn step A, ultrafine white TiO2The nano powder is prepared based on a catalytic chemical vapor deposition method and a hydrolysis method.
Further, the preparation based on the catalytic chemical vapor deposition method and the hydrolysis method comprises the following steps:
a. measuring a hydrolysis solvent, heating the hydrolysis solvent to 40-70 ℃, and keeping the temperature constant;
b. dropwise adding a titanium source into the hydrolysis solvent and continuously stirring for at least 24 hours until the solution becomes a white suspension;
c. centrifuging the white suspension to obtain a white precipitate;
d. washing, drying and grinding the white precipitate to obtain the superfine white TiO2And (4) nano powder.
Further, in the step b, the mass ratio of the dropwise added titanium source to the hydrolysis solvent is 1: 20-1: 60.
further, the titanium source is butyl titanate.
Further, in the step d, the white precipitate is washed by using absolute ethyl alcohol and tetrahydrofuran alternately for at least three times, the centrifugal treatment is also carried out after each washing, and the white precipitate is dried in a dry environment for at least 12 hours after the washing is finished.
Further, in the step B, the inert atmosphere heat treatment equipment is a horizontal furnace, and the raw materials are placed in the middle of the horizontal furnace through a quartz boat.
Further, the temperature rise rate of the horizontal furnace is 3-15 ℃/min.
Furthermore, the particle size of the raw material is 1-20 nm.
Furthermore, in the step C, the time for introducing the original hydrocarbon gas is 1 s-3 min, and the reaction time is 5 s-3 min.
Further, in the step C, after the reducing hydrocarbon gas is introduced into the inert atmosphere heat treatment equipment, the volume fraction of the reducing hydrocarbon gas is 5-20%, and the volume fraction of the inert gas is 80-95%.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: the preparation method comprises mixing the raw materialsReacting at 100-250 ℃ by using reducing hydrocarbon gas, and inducing and changing the energy band structure and the surface electronic structure of the raw material by using gas at the temperature range to form yellow superfine TiO with an ultrathin carbon layer on the surface2The photocatalyst has the technical characteristics of simple operation, low equipment requirement, good dispersibility, high repeatability and success rate, and is suitable for large-scale production and use.
Meanwhile, the invention also discloses superfine yellow TiO2Photocatalyst, the ultrafine yellow TiO2Photocatalyst for synthesis of superfine yellow TiO based on gas induction2The photocatalyst is prepared by a preparation method.
The superfine yellow TiO of the invention2The photocatalyst has the technical characteristics of low electron hole recombination rate, wide absorption band and high photocatalytic efficiency due to the adoption of the preparation method.
Drawings
FIG. 1 shows the yellow TiO compound obtained in example 12TEM images of the photocatalyst;
FIG. 2 shows the yellow TiO obtained in example 12XPS spectra of the photocatalyst;
FIG. 3 shows white TiO obtained in example 12Nanopowder and yellow TiO2A methyl orange curve graph drawn by a photocatalyst;
FIG. 4 shows the yellow TiO obtained in example 22TEM images of the photocatalyst;
FIG. 5 shows white TiO obtained in example 22Nanopowder and yellow TiO2A methyl orange curve graph drawn by a photocatalyst;
FIG. 6 shows the yellow TiO compound obtained in example 32TEM images of the photocatalyst;
FIG. 7 shows yellow TiO produced in example 42TEM images of the photocatalyst;
FIG. 8 shows the yellow TiO compound obtained in example 52TEM images of the photocatalyst;
FIG. 9 shows white TiO obtained in example 52Nanopowder and yellow TiO2A methyl orange curve graph drawn by a photocatalyst;
wherein the content of the first and second substances,
in the attached drawingsIs/are as follows
The line segments represent white T iO in different embodiments2A nanopowder methyl orange curve;
in the attached drawings
The line segments represent yellow T iO in different embodiments2Photocatalyst methyl orange curve.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
The invention relates to gas-induced synthesis of superfine yellow TiO2A method for preparing a photocatalyst, the method comprising the steps of;
A. preparation of ultrafine white TiO2Nano powder to obtain raw material;
in particular, ultra-fine white TiO2The nano powder can be prepared by combining a catalytic chemical vapor deposition method and a hydrolysis method, and the combined preparation method specifically comprises the following steps:
a. measuring a hydrolysis solvent, heating the hydrolysis solvent to 40-70 ℃, and keeping the temperature constant; the hydrolysis solvent can be isopropanol or toluene. And can be thermostated by adopting a constant temperature heating device.
b. Dropwise adding a titanium source into the hydrolysis solvent and continuously stirring for at least 24 hours until the solution becomes a white suspension; the mass ratio of the dropwise added titanium source to the hydrolysis solvent is 1: 20-1: 60, the dropwise added titanium source can be butyl titanate.
c. Centrifuging the white suspension to obtain a white precipitate; the centrifugal treatment can be performed by adopting a high-speed centrifuge for centrifugation, wherein the centrifugation speed of the high-speed centrifuge is 10000-15000 r/min, and the centrifugation time is 10-20 min.
d. Washing, drying and grinding the white precipitate to obtain the superfine white TiO2And (4) nano powder. Washing can adoptWashing with anhydrous ethanol and tetrahydrofuran alternately for more than 3 times, and drying in a drying environment for at least 12 hr.
B. Placing the raw materials in inert atmosphere heat treatment equipment, heating the interior of the inert atmosphere heat treatment equipment to 100-250 ℃, and keeping the temperature in the furnace for at least 15 min;
specifically, the inert atmosphere heat treatment equipment is a horizontal furnace, the raw materials are placed in the middle of the horizontal furnace through a quartz boat, and the temperature rise rate of the horizontal furnace is 3-15 ℃/min. Inert gas such as argon is introduced into the inert atmosphere heat treatment equipment, so that an inert atmosphere is formed inside the inert atmosphere heat treatment equipment.
In this step, the ultrafine TiO can be purified2The nanoparticles remove the residual solvent and allow it to become activated.
C. Introducing reducing hydrocarbon gas into inert atmosphere heat treatment equipment, and reacting to obtain the superfine yellow TiO2A photocatalyst.
Specifically, the time for introducing the reducing hydrocarbon gas is 1 s-3 min, and the reaction time is 5 s-3 min. The reducing hydrocarbon gas can be acetylene gas, the flow rate is 40ml/min, and after the reducing hydrocarbon gas is introduced into the inert atmosphere heat treatment equipment, the volume fraction of the reducing hydrocarbon gas is 5-20%, and the volume fraction of the inert gas is 80-95%.
In the step, the strong reducibility of the reducing hydrocarbon gas and the nanometer ultrafine TiO are utilized2High surface energy of (2) so that the ultrafine TiO2Further cracking to obtain smaller nano particles, reconstructing the surface of the nano particles, and simultaneously generating a large number of defects, thereby changing the energy band structure and the surface electronic structure of the nano particles, wherein the macro structure is white superfine TiO2Turning yellow.
Based on the above superfine yellow TiO2The invention also discloses a preparation method of the photocatalyst and a superfine yellow TiO2Photocatalyst, the ultrafine yellow TiO2The photocatalyst is prepared by the preparation method.
Is superfine yellow TiO2The preparation method of the photocatalyst is better implemented, and specific data and parameters are combined belowConditions and the like will further explain the present invention.
Detailed description of the preferred embodiment 1
Gas-induced synthesis of superfine yellow TiO2A method for preparing a photocatalyst, the method comprising the steps of;
step 1: preparation of nano TiO2The method comprises the following steps of respectively measuring 2-10 ml of butyl titanate and 40-80 m L hydrolysis solvent isopropanol by using a measuring tool such as a measuring cylinder, adding the isopropanol into a beaker, placing the beaker into a constant-temperature heating device-constant-temperature electromagnetic water bath kettle, heating the water bath kettle to 40-70 ℃ and keeping the temperature constant, slowly adding the butyl titanate into the isopropanol dropwise, continuously and violently stirring, sealing the beaker after stirring, sealing the beaker by using a sealing cover, a preservative film and the like, reacting for 48 hours after sealing until the solution becomes white turbid liquid, placing the white turbid liquid into a high-speed centrifuge for centrifugation at a high-speed centrifuge centrifugation speed of 10000-15000 r/min for 10-20 min, obtaining white precipitate after centrifugation, washing the white precipitate for at least 3 times by using absolute ethyl alcohol and tetrahydrofuran, carrying out centrifugation treatment in the same way of washing, and drying the washed and centrifuged white precipitate in dry air for 12 hours to obtain nano white TiO2Grinding into powder to obtain superfine white TiO2And (3) preparing a nano powder raw material.
Step 2: preparation of yellow TiO2Photocatalyst: taking the superfine white TiO prepared in the step 12Uniformly spreading 1g of nano powder in a quartz boat, placing the quartz boat in the middle of a quartz tube of a horizontal furnace, checking the gas tightness, introducing inert gas-argon into the quartz tube at the rate of 20ml/min, introducing for 15 minutes, removing air in the quartz tube, slowly heating the horizontal furnace to 180-210 ℃ at the heating rate of 3-15 ℃/min, keeping the temperature for 25 minutes, continuously introducing the argon, and introducing reductive hydrocarbon gas-acetylene (C) into the tubular furnace at the rate of 40ml/min2H2) Reacting for 5 s-5 min, stopping introducing the reducing hydrocarbon gas after the reaction is finished, continuously introducing argon, and cooling to room temperature along with the furnace under the protection of the argon, thus changing the superfine TiO2So that it has a white color and turns yellow to obtain yellow TiO2A photocatalyst.
Specific example 2
Gas-induced synthesis of ultrafine yellow TiO in this example2The preparation method of the photocatalyst is basically the same as that of the embodiment 1, except that: the temperature in the horizontal furnace of the embodiment is changed from 180-210 ℃ to 140-180 ℃.
The method specifically comprises the following steps:
gas-induced synthesis of superfine yellow TiO2A method for preparing a photocatalyst, the method comprising the steps of;
step 1: preparation of nano TiO2The method comprises the following steps of respectively measuring 2-10 ml of butyl titanate and 40-80 m L hydrolysis solvent isopropanol by using a measuring tool such as a measuring cylinder, adding the isopropanol into a beaker, placing the beaker into a constant-temperature heating device-constant-temperature electromagnetic water bath kettle, heating the water bath kettle to 40-70 ℃ and keeping the temperature constant, slowly adding the butyl titanate into the isopropanol dropwise, continuously and violently stirring, sealing the beaker after stirring, sealing the beaker by using a sealing cover, a preservative film and the like, reacting for 48 hours after sealing until the solution becomes white turbid liquid, placing the white turbid liquid into a high-speed centrifuge for centrifugation at a high-speed centrifuge centrifugation speed of 10000-15000 r/min for 10-20 min, obtaining white precipitate after centrifugation, washing the white precipitate for at least 3 times by using absolute ethyl alcohol and tetrahydrofuran, carrying out centrifugation treatment in the same way of washing, and drying the washed and centrifuged white precipitate in dry air for 12 hours to obtain nano white TiO2Grinding into powder to obtain the superfine white TiO2And (4) nano powder.
Step 2: preparation of yellow TiO2Photocatalyst: taking the superfine white TiO prepared in the step 12Uniformly spreading 1g of nano powder in a quartz boat, placing the quartz boat in the middle of a quartz tube of a horizontal furnace, checking the gas tightness, introducing inert gas-argon into the quartz tube at the rate of 20ml/min, introducing for 15 minutes, removing air in the quartz tube, slowly heating the horizontal furnace to 140-180 ℃ at the heating rate of 3-15 ℃/min, keeping the temperature for 25 minutes, continuously introducing the argon, and introducing reductive hydrocarbon gas-acetylene (C) into the tubular furnace at the rate of 40ml/min2H2) Reacting for 5 s-5 min, stopping introducing the reducing hydrocarbon gas after the reaction is finished, continuously introducing argon, and cooling to room temperature along with the furnace under the protection of the argon, thus changing the superfine TiO2So that it has a white color and turns yellow to obtain yellow TiO2A photocatalyst.
Specific example 3
Gas-induced synthesis of ultrafine yellow TiO in this example2The preparation method of the photocatalyst is basically the same as that of the embodiment 1, except that: the temperature in the horizontal furnace of the embodiment is changed from 180-210 ℃ to 100-140 ℃.
The method specifically comprises the following steps:
gas-induced synthesis of superfine yellow TiO2A method for preparing a photocatalyst, the method comprising the steps of;
step 1: preparation of nano TiO2The method comprises the following steps of respectively measuring 2-10 ml of butyl titanate and 40-80 m L hydrolysis solvent isopropanol by using a measuring tool such as a measuring cylinder, adding the isopropanol into a beaker, placing the beaker into a constant-temperature heating device-constant-temperature electromagnetic water bath kettle, heating the water bath kettle to 40-70 ℃ and keeping the temperature constant, slowly adding the butyl titanate into the isopropanol dropwise, continuously and violently stirring, sealing the beaker after stirring, sealing the beaker by using a sealing cover, a preservative film and the like, reacting for 48 hours after sealing until the solution becomes white turbid liquid, placing the white turbid liquid into a high-speed centrifuge for centrifugation at a high-speed centrifuge centrifugation speed of 10000-15000 r/min for 10-20 min, obtaining white precipitate after centrifugation, washing the white precipitate for at least 3 times by using absolute ethyl alcohol and tetrahydrofuran, carrying out centrifugation treatment in the same way of washing, and drying the washed and centrifuged white precipitate in dry air for 12 hours to obtain nano white TiO2Grinding into powder to obtain the superfine white TiO2And (4) nano powder.
Step 2: preparation of yellow TiO2Photocatalyst: taking the superfine white TiO prepared in the step 121g of nano powder is evenly spread in a quartz boat, the quartz boat is placed in the middle of a quartz tube of a horizontal furnace, after checking the air tightness, inert gas-argon gas is introduced into the quartz tube at the speed of 20ml/min,introducing for 15 minutes, removing air in the quartz tube, slowly heating the horizontal furnace to 100-140 ℃ at the heating rate of 3-15 ℃/min, keeping the temperature for 25min, continuously introducing argon, and introducing reductive hydrocarbon gas-acetylene (C) into the tubular furnace at the rate of 40ml/min2H2) Reacting for 5 s-5 min, stopping introducing the reducing hydrocarbon gas after the reaction is finished, continuously introducing argon, and cooling to room temperature along with the furnace under the protection of the argon, thus changing the superfine TiO2So that it has a white color and turns yellow to obtain yellow TiO2A photocatalyst.
Specific example 4
Gas-induced synthesis of ultrafine yellow TiO in this example2The preparation method of the photocatalyst is basically the same as that of the embodiment 1, except that: the temperature in the horizontal furnace of the embodiment is changed from 180-210 ℃ to 210-250 ℃.
The method specifically comprises the following steps:
gas-induced synthesis of superfine yellow TiO2A method for preparing a photocatalyst, the method comprising the steps of;
step 1: preparation of nano TiO2The method comprises the following steps of respectively measuring 2-10 ml of butyl titanate and 40-80 m L hydrolysis solvent isopropanol by using a measuring tool such as a measuring cylinder, adding the isopropanol into a beaker, placing the beaker into a constant-temperature heating device-constant-temperature electromagnetic water bath kettle, heating the water bath kettle to 40-70 ℃ and keeping the temperature constant, slowly adding the butyl titanate into the isopropanol dropwise, continuously and violently stirring, sealing the beaker after stirring, sealing the beaker by using a sealing cover, a preservative film and the like, reacting for 48 hours after sealing until the solution becomes white turbid liquid, placing the white turbid liquid into a high-speed centrifuge for centrifugation at a high-speed centrifuge centrifugation speed of 10000-15000 r/min for 10-20 min, obtaining white precipitate after centrifugation, washing the white precipitate for at least 3 times by using absolute ethyl alcohol and tetrahydrofuran, carrying out centrifugation treatment in the same way of washing, and drying the washed and centrifuged white precipitate in dry air for 12 hours to obtain nano white TiO2Grinding into powder to obtain the superfine white TiO2And (4) nano powder.
Step 2: system for makingPreparation of yellow TiO2Photocatalyst: taking the superfine white TiO prepared in the step 12Uniformly spreading 1g of nano powder in a quartz boat, placing the quartz boat in the middle of a quartz tube of a horizontal furnace, checking the gas tightness, introducing inert gas-argon into the quartz tube at the rate of 20ml/min, introducing for 15 minutes, removing air in the quartz tube, slowly increasing the temperature of the horizontal furnace to 210-250 ℃ at the heating rate of 3-15 ℃/min, keeping the temperature for 25 minutes, continuously introducing the argon, and introducing reductive hydrocarbon gas-acetylene (C) into the tube furnace at the rate of 40ml/min2H2) Reacting for 5 s-5 min, stopping introducing the reducing hydrocarbon gas after the reaction is finished, continuously introducing argon, and cooling to room temperature along with the furnace under the protection of the argon, thus changing the superfine TiO2So that it has a white color and turns yellow to obtain yellow TiO2A photocatalyst.
Specific example 5
Gas-induced synthesis of ultrafine yellow TiO in this example2The preparation method of the photocatalyst is basically the same as that of the embodiment 1, except that: the hydrolysis solvent of this example was changed from isopropanol to toluene.
The method specifically comprises the following steps:
gas-induced synthesis of superfine yellow TiO2A method for preparing a photocatalyst, the method comprising the steps of;
step 1: preparation of nano TiO2The method comprises the following steps of respectively measuring 2-10 ml of butyl titanate and 40-80 m L of hydrolysis solvent toluene by using a measuring tool such as a measuring cylinder, adding the toluene into a beaker, placing the beaker into a constant-temperature heating device-constant-temperature electromagnetic water bath kettle, heating the water bath kettle to 40-70 ℃ and keeping the temperature constant, slowly adding the butyl titanate dropwise into the toluene, continuously and violently stirring, sealing the beaker after stirring, sealing by using a sealing cover, a preservative film and the like, reacting for 48 hours after sealing until the solution becomes white turbid liquid, placing the white turbid liquid into a high-speed centrifuge for centrifugation, wherein the centrifugation speed of the high-speed centrifuge is 10000-15000 r/min, the centrifugation time is 10-20 min, obtaining white precipitate after centrifugation, washing the white precipitate for at least 3 times by using absolute ethyl alcohol and tetrahydrofuran, and washing the same timeCentrifuging, and drying the washed and centrifuged white precipitate in dry air for 12 hours to obtain the nanometer white TiO2Grinding into powder to obtain superfine white TiO2And (3) preparing a nano powder raw material.
Step 2: preparation of yellow TiO2Photocatalyst: taking the superfine white TiO prepared in the step 12Uniformly spreading 1g of nano powder in a quartz boat, placing the quartz boat in the middle of a quartz tube of a horizontal furnace, checking the gas tightness, introducing inert gas-argon into the quartz tube at the rate of 20ml/min, introducing for 15 minutes, removing air in the quartz tube, slowly heating the horizontal furnace to 180-210 ℃ at the heating rate of 3-15 ℃/min, keeping the temperature for 25 minutes, continuously introducing the argon, and introducing reductive hydrocarbon gas-acetylene (C) into the tubular furnace at the rate of 40ml/min2H2) Reacting for 5 s-5 min, stopping introducing the reducing hydrocarbon gas after the reaction is finished, continuously introducing argon, and cooling to room temperature along with the furnace under the protection of the argon, thus changing the superfine TiO2So that it has a white color and turns yellow to obtain yellow TiO2A photocatalyst.
In conclusion, for better embodying the present invention, the following yellow TiO compounds were prepared based on the preparation methods shown in specific example 1 to specific example 52The photocatalyst was subjected to the following tests:
preparing 10 mg/L methyl orange solution, dropwise adding 1ml of 10 wt% NaOH solution into the solution, adjusting the pH value to be more than 4.4, setting the wavelength of an ultraviolet spectrophotometer to be 464nm, testing the absorbance of the solution, and calculating the corresponding methyl orange concentration.
Weighing the white TiO of each example2(preparation in step 1) and yellow TiO2Adding 0.1g of each photocatalyst (prepared in step 2) into 10 mg/L of methyl orange solution, placing in a dark room, adjusting to the same stirring speed, stirring for 2h, taking the supernatant, centrifuging for 20min by a high-speed centrifuge, taking the supernatant, testing the absorbance, and calculating the corresponding methyl orange concentration as the initial concentration C0The methyl orange solution mixed with the catalyst was placed under a 5W L ED light source with the liquid level and light source at a distance of 10cm, and the two cups of solution were stirred at the same speed. And taking the upper suspension at intervals of 30min, centrifuging at 10000r/min, taking the supernatant, testing the absorbance of the supernatant, calculating and recording the concentration of the methyl orange, and circulating the steps until the concentration is not reduced, thus obtaining the methyl orange degradation broken line.
Using the above test, the white TiO prepared in example 1-example 52And yellow TiO2The photocatalyst is measured to obtain the measurement graphs shown in fig. 1-9, wherein:
FIG. 1 shows the yellow TiO compound obtained in example 12TEM images of the photocatalyst; FIG. 2 shows the yellow TiO obtained in example 12XPS spectra of the photocatalyst; FIG. 3 shows white TiO obtained in example 12Nanopowder and yellow TiO2A methyl orange curve graph drawn by a photocatalyst; FIG. 4 shows the yellow TiO obtained in example 22TEM images of the photocatalyst; FIG. 5 shows white TiO obtained in example 22Nanopowder and yellow TiO2A methyl orange curve graph drawn by a photocatalyst; FIG. 6 shows the yellow TiO compound obtained in example 32TEM images of the photocatalyst; FIG. 7 shows yellow TiO produced in example 42TEM images of the photocatalyst; FIG. 8 shows the yellow TiO compound obtained in example 52TEM images of the photocatalyst; FIG. 9 shows white TiO obtained in example 52Nanopowder and yellow TiO2A methyl orange curve graph drawn by a photocatalyst;
analysis in conjunction with FIGS. 1-9:
FIG. 1 shows the yellow TiO compound obtained in example 12TEM image (optical image) of photocatalyst to show yellow TiO2The photocatalyst has a particle size of 10nm or less. FIG. 2 shows the yellow TiO obtained in example 12XPS spectra of photocatalyst, indicating treated TiO2The chemical environment of the Ti atom is changed. FIG. 3 shows white TiO obtained in example 12Nanopowder and yellow TiO2Photocatalyst-plotted methyl orange graph illustrating the yellow TiO prepared in example 1290% of methyl orange is catalytically decomposed by photocatalyst under visible light for 60 min. Also, white TiO is clearly seen in FIG. 12The nano powder is particles with the particle size of less than 10nm, and has uniform size and regular shape.
Simultaneously for yellow TiO2The photocatalyst was similarly characterized, and as can be seen from FIG. 1, yellow TiO2Photocatalyst display and white TiO2The crystal forms of the nano-particles are consistent, the crystal phase of anatase is not changed by a catalytic chemical vapor deposition method under an acetylene atmosphere, and the most remarkable effect is that the size of the nano-particles is reduced from 10nm to 2-3 nm. The resulting visible degradation curve for methyl orange, FIG. 3, illustrates the treated yellow TiO2The photocatalyst has higher catalytic activity, and 90 percent of methyl orange is catalytically decomposed within only one hour, compared with white TiO2The raw material is greatly improved, and the catalytic rate is improved by 12 times.
FIG. 4 shows the yellow TiO compound obtained in example 22TEM image of photocatalyst showing TiO2The photocatalyst has a particle size of about 20nm, and FIG. 5 shows white TiO prepared in example 22And yellow TiO2Plotted methyl orange graph. As can be seen from FIGS. 4 and 5, the yellow TiO prepared in example 2 was observed to be visible light260% of methyl orange is catalytically decomposed by photocatalyst under visible light for 90 min. It can be seen that the photocatalyst prepared in embodiment 2 has a poorer effect on the degradation of methyl orange than the photocatalyst prepared in embodiment 1.
FIG. 6 shows the yellow TiO compound obtained in example 32TEM image of photocatalyst showing TiO2The grain size of the photocatalyst is about 30 nm. FIG. 7 shows the yellow TiO compound obtained in example 42TEM image of photocatalyst showing TiO2The grain size of the photocatalyst is about 100 nm.
FIG. 8 shows the yellow TiO compound obtained in example 52TEM image of photocatalyst showing TiO2The photocatalyst particle size is about 80nm, and FIG. 9 shows the white TiO prepared in example 52And yellow TiO2Plotted methyl orange graph. Illustrating the yellow TiO prepared in specific example 5225% of methyl orange is catalytically decomposed under visible light of a photocatalyst for 90 min. It can be seen that the photocatalyst prepared in embodiment 5 is much less effective in degrading methyl orange than the photocatalysts prepared in embodiments 1 and 2.
The above description is an embodiment of the present invention. The foregoing is a preferred embodiment of the present invention, and the preferred embodiments in the preferred embodiments can be combined and used in any combination if not obviously contradictory or prerequisite to a certain preferred embodiment, and the specific parameters in the embodiments and examples are only for the purpose of clearly illustrating the invention verification process of the inventor and are not intended to limit the patent protection scope of the present invention, which is subject to the claims and the equivalent structural changes made by the content of the description and the drawings of the present invention are also included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the superfine yellow photocatalyst by gas induction synthesis is characterized by comprising the following steps;
A. preparation of ultrafine white TiO2Nano powder to obtain raw material;
B. placing the raw materials in inert atmosphere heat treatment equipment, heating the interior of the inert atmosphere heat treatment equipment to 100-250 ℃, and keeping the temperature in the furnace for at least 15 min;
C. introducing reducing hydrocarbon gas into inert atmosphere heat treatment equipment, and then preserving heat for 5 s-5 min to obtain the superfine yellow TiO2A photocatalyst.
2. The method according to claim 1, wherein in the step A, the ultra-fine white TiO is used2The nano powder is prepared based on a catalytic chemical vapor deposition method and a hydrolysis method.
3. The method of claim 2, wherein the steps of preparing based on catalytic chemical vapor deposition and hydrolysis are:
a. measuring a hydrolysis solvent, heating the hydrolysis solvent to 40-70 ℃, and keeping the temperature constant;
b. dropwise adding a titanium source into the hydrolysis solvent and continuously stirring for at least 24 hours until the solution becomes a white suspension;
c. centrifuging the white suspension to obtain a white precipitate;
d. washing, drying and grinding the white precipitate to obtain the superfine white TiO2And (4) nano powder.
4. The preparation method according to claim 3, wherein in the step b, the mass ratio of the dropwise added titanium source to the hydrolysis solvent is 1: 20-1: 60.
5. the method according to claim 4, wherein the titanium source is butyl titanate.
6. The preparation method according to claim 3, wherein in the step d, the white precipitate is washed at least three times by using absolute ethyl alcohol and tetrahydrofuran alternately, each time after washing, the white precipitate is also subjected to centrifugal treatment, and after washing, the white precipitate is dried in a dry environment for at least 12 hours.
7. The method according to claim 1, wherein the particle size of the raw material is 1 to 20 nm.
8. The preparation method according to claim 1, wherein in the step C, the time for introducing the original hydrocarbon gas is 1 s-3 min, and the reaction time is 5 s-3 min.
9. The method according to claim 1, wherein in the step C, after the reducing hydrocarbon gas is introduced into the inert atmosphere heat treatment device, the volume fraction of the reducing hydrocarbon gas is 5% to 20%, and the volume fraction of the inert gas is 80% to 95%.
10. Superfine yellow TiO2A photocatalyst, characterized in that the ultrafine yellow TiO2The photocatalyst is prepared by the preparation method of any one of claims 1 to 9.
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