CN112452350A - Preparation method of photocatalyst - Google Patents
Preparation method of photocatalyst Download PDFInfo
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- CN112452350A CN112452350A CN202011333232.0A CN202011333232A CN112452350A CN 112452350 A CN112452350 A CN 112452350A CN 202011333232 A CN202011333232 A CN 202011333232A CN 112452350 A CN112452350 A CN 112452350A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 71
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- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 16
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910021612 Silver iodide Inorganic materials 0.000 description 1
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- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
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- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
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- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a preparation method of a photocatalyst, and belongs to the technical field of catalysts. The preparation method of the photocatalyst comprises the following steps: step 1: pretreating sepiolite powder; step 2: mixing; and step 3: drying by distillation; and 4, step 4: and (4) high-temperature calcination. The invention overcomes the defects of photocatalyst g-C in the prior art3N4The obtained photocatalyst can simulate sunlight to degrade organic pollutants such as dye wastewater, has the highest degradation rate of 98.5 percent, and has wide applicationAnd (4) foreground.
Description
Technical Field
The invention relates to a preparation method of a photocatalyst, belonging to the technical field of catalysts.
Background
Energy crisis and environmental issues are the biggest challenges facing humans, and finding ways to solve these two issues is the current research focus. Researches on photo-catalysts utilizing sunlight on the aspects of photo-degradation of organic pollutants, promotion of environmental remediation and photocatalytic hydrolysis hydrogen production have attracted extensive attention. Graphite phase carbon nitride (g-C)3N4) The material has the advantages of simple preparation, low price, no toxicity, good chemical and thermal stability, and the forbidden band width is only 2.7eV, so that the material can absorb visible light. The unique structure of the graphite phase carbon nitride determines that the graphite phase carbon nitride has wide application in the field of visible light catalysis, and shows good photocatalytic performance in the aspects of hydrogen production by decomposing water, pollutant photocatalytic degradation, reduction of carbon dioxide discharged during hydrocarbon combustion by photocatalytic reduction and the like.
In the application of the carbon nitride material, the problems mainly faced are that the quantum efficiency is low, the recombination speed of electron-hole pairs is high, and active particles generated by light excitation cannot be fully utilized. By compounding with semiconductor materials, noble metals or other materials, the carbon nitride can obviously prolong the recombination time of electron-hole pairs and improve the spectral response performance and the photocatalytic efficiency.
In the prior art, for loading g-C3N4The carrier is of various kinds, and the semiconductor is TiO2、MoS2CdS and ZnS, etc., and the noble metals are Ag, Pt, Au, etc. In the above support, TiO2The composite material is nontoxic, but the wide application of the composite material is greatly restricted by the defects of low utilization rate of sunlight, high recombination rate of photogenerated electrons and hole pairs and the like. MoS2And the CdS and ZnS have the possibility of dissolving out metal ions in the reaction process, which can cause secondary environmental pollution. Ag, Pt and Au are expensive and too costly.
Sepiolite is a natural mineral substance, has a very large storage capacity, a fibrous morphology, a large specific surface area, and g-C3N4Similarly, the catalyst has good thermal stability and chemical stability, is nontoxic, cheap and environment-friendly, and is very suitable to be used as a carrier or an adsorbent of a catalyst. However, the sepiolite loaded with g-C is not available at present3N4Is related toAnd (4) carrying out the following steps.
Disclosure of Invention
The invention aims to solve the existing defects and provides a preparation method of a photocatalyst. The invention overcomes the defects of photocatalyst g-C in the prior art3N4The obtained photocatalyst can simulate sunlight to degrade organic pollutants such as dye wastewater, has the highest degradation rate of 98.5 percent, and has wide application prospect.
The technical scheme for solving the technical problems is as follows: a preparation method of a photocatalyst comprises the following steps:
step 1: sepiolite powder pretreatment
Soaking sepiolite powder in distilled water, shaking at room temperature, washing precipitate with distilled water, and drying to obtain dried sepiolite powder;
step 2: mixing
Dispersing the dried sepiolite powder, melamine and thiourea obtained in the step 1 into distilled water, heating, stirring and uniformly mixing to obtain a mixture;
and step 3: drying by distillation
Evaporating the water in the mixture obtained in the step 2 to dryness to obtain a mixture with the water evaporated to dryness;
and 4, step 4: high temperature calcination
And (4) grinding the mixture obtained in the step (3) after the water is evaporated to dryness into powder, calcining at high temperature under the protection of nitrogen, and then cooling to room temperature to obtain the photocatalyst.
The principle of the preparation method of the photocatalyst is as follows:
in the step 1 of the invention, the sepiolite powder is pretreated to remove impurities in the sepiolite powder.
In step 2 of the present invention, the mixing is performed so that g-C3N4The precursors melamine and thiourea are more effectively dispersed on the surface and in the pores of the sepiolite, and the g-C generated can be prevented3N4Agglomeration leads to itThe photocatalytic efficiency is reduced.
In step 3 of the present invention, the evaporation to dryness is performed for the subsequent high temperature calcination.
In step 4 of the invention, high temperature calcination can generate g-C3N4And the sepiolite also has activity, thermal stability and chemical stability.
In conclusion, the invention uses the sepiolite and the photocatalyst g-C3N4The composite material with the synergistic functions of adsorption and photocatalysis is prepared by compounding, and has the following advantages:
(1) the low-concentration organic pollutants can be enriched and concentrated on the surface or in the pore channel of the adsorbent by utilizing the action of the adsorbent, so that the organic pollutants are promoted to migrate from the water phase to the adsorbent and then transferred to the surface of the photocatalyst, and the photocatalytic degradation efficiency is greatly improved.
(2) The photocatalyst in the composite material is utilized to degrade organic pollutants adsorbed on the surface of the adsorbent, and the adsorbent can be regenerated, so that the continuous use of the material can be realized, and secondary pollution caused by desorption of the adsorbent due to saturated adsorption is avoided.
(3) The intermediate product generated in the process of the photocatalytic reaction is adsorbed on the surface of the adsorbent, so that the degradation intermediate is completely degraded into carbon dioxide and water before leaving the surface of the photocatalyst particles, and the problem of secondary pollution possibly generated by the degradation intermediate is avoided.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in the step 1, the particle size of the sepiolite powder is 300 meshes.
Further, in the step 1, the soaking time is 22-26 h.
The further effective results are as follows: by adopting the parameters, the soaking effect is better.
Further, in the step 1, the oscillation device is a gas bath oscillator, the oscillation time is 24 hours, and the rotation speed is 170 r/min.
The adoption of the further beneficial effects is as follows: by adopting the parameters, the oscillation effect is better.
Further, in the step 1, the drying temperature is 105 ℃ and the drying time is 24 hours.
The adoption of the further beneficial effects is as follows: by adopting the parameters, the drying effect is better.
Further, in the step 2, the mass ratio of the sepiolite powder, the melamine and the thiourea is 5 (0.05-2) to (0.075-3).
The further effective results are as follows: by adopting the proportion, the obtained photocatalyst has higher visible light catalytic activity and can be recycled.
Further, in step 2, the volume of the distilled water was 25 ml.
Further, in step 2, the heating temperature is 100 ℃.
The adoption of the further beneficial effects is as follows: by adopting the parameters, the mixing effect of the sepiolite powder, the melamine and the thiourea is better.
Further, in step 3, the temperature of the evaporation to dryness is 100 ℃.
The adoption of the further beneficial effects is as follows: by adopting the parameters, the evaporation drying effect is better.
Further, in step 4, the particle size of the powder is 300 mesh.
The adoption of the further beneficial effects is as follows: the parameters are adopted, so that the subsequent high-temperature calcination is facilitated.
Further, in the step 4, the high-temperature calcination is carried out at the temperature of 400-600 ℃ for 3-5 h.
The adoption of the further beneficial effects is as follows: using the above parameters, g-C can be generated3N4And the sepiolite also has activity, thermal stability and chemical stability.
The preparation method of the photocatalyst has the beneficial effects that:
(1) the sepiolite photocatalyst prepared by the invention can be similar to the photocatalyst g-C3N4Interaction occurs to accelerate the separation of electron-hole pairs, thereby improving the catalytic activity of the photocatalyst.
(2) Prior artIntraoperative g-C3N4The nanometer powder photocatalyst often has the problems of difficult separation and recovery, easy agglomeration and inactivation and the like, so the practical application of the nanometer powder photocatalyst is limited, and the sepiolite and the photocatalyst g-C3N4The complex can greatly reduce the agglomeration phenomenon of a single photocatalyst, and the separation and recovery are easier.
(3) The photocatalyst prepared by the invention can be used for degrading dye wastewater and other toxic organic pollutants, and has good visible light catalysis effect. The photocatalyst is adopted to carry out photocatalytic degradation on the dye methylene blue under visible light, and the degradation rate of the methylene blue is over 95 percent at 60 min.
(4) The preparation method has the advantages of simple preparation process, cheap and easily available raw materials, no toxicity, environmental friendliness, wide market prospect and suitability for large-scale production.
Drawings
FIG. 1 is an SEM photograph of the photocatalyst obtained in example 2 of the present invention.
FIG. 2 is an XRD pattern of the photocatalyst obtained in example 2 of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with specific embodiments, which are set forth merely to illustrate the invention and are not intended to limit the scope of the invention.
Example 1
The preparation method of the photocatalyst of the embodiment comprises the following steps:
step 1: sepiolite powder pretreatment
Soaking 5g of sepiolite powder with the particle size of 300 meshes in distilled water for 22h, shaking in a gas bath oscillator at room temperature for 24h at the rotating speed of 170r/min, washing the precipitate with distilled water for 3 times, and drying at 105 ℃ for 24h to obtain the dried sepiolite powder.
Step 2: mixing
And (2) dispersing the dried sepiolite powder obtained in the step (1), 1g of melamine and 1.5g of thiourea into 25ml of distilled water, heating and stirring at 100 ℃ for 30min, and uniformly mixing to obtain a mixture.
And step 3: drying by distillation
And (3) evaporating the water in the mixture obtained in the step (2) at 100 ℃ to dryness to obtain a mixture of which the water is evaporated to dryness.
And 4, step 4: high temperature calcination
And (4) grinding the mixture obtained in the step (3) after the water is evaporated to dryness into powder with the particle size of 300 meshes, calcining the powder at the high temperature of 400 ℃ for 5 hours under the protection of nitrogen, and then cooling the calcined powder to the room temperature to obtain the photocatalyst. In the photocatalyst, g-C3N4The loading amount of (B) is 10% (mass fraction).
Example 2
The preparation method of the photocatalyst of the embodiment comprises the following steps:
step 1: sepiolite powder pretreatment
Soaking 5g of sepiolite powder with the particle size of 300 meshes in distilled water for 24h, shaking in a gas bath oscillator at room temperature for 24h at the rotating speed of 170r/min, washing the precipitate for 3 times by using distilled water, and drying at 105 ℃ for 24h to obtain the dried sepiolite powder.
Step 2: mixing
And (2) dispersing the dried sepiolite powder obtained in the step (1), 0.05g of melamine and 0.75g of thiourea in 25ml of distilled water, heating and stirring at 100 ℃ for 30min, and uniformly mixing to obtain a mixture.
And step 3: drying by distillation
And (3) evaporating the water in the mixture obtained in the step (2) at 100 ℃ to dryness to obtain a mixture of which the water is evaporated to dryness.
And 4, step 4: high temperature calcination
And (4) grinding the mixture obtained in the step (3) after the water is evaporated to dryness into powder with the particle size of 300 meshes, calcining at the high temperature of 500 ℃ for 4 hours under the protection of nitrogen, and then cooling to room temperature to obtain the photocatalyst. In the photocatalyst, g-C3N4The supported amount of (B) was 0.5% (mass fraction).
The SEM image of the photocatalyst obtained in this example is shown in fig. 1.
The XRD pattern of the photocatalyst obtained in this example is shown in fig. 2.
Example 3
The preparation method of the photocatalyst of the embodiment comprises the following steps:
step 1: sepiolite powder pretreatment
Soaking 5g of sepiolite powder with the particle size of 300 meshes in distilled water for 26h, shaking in a gas bath oscillator at room temperature for 24h at the rotating speed of 170r/min, washing the precipitate with distilled water for 3 times, and drying at 105 ℃ for 24h to obtain the dried sepiolite powder.
Step 2: mixing
And (2) dispersing the dried sepiolite powder obtained in the step (1), 0.1g of melamine and 0.15g of thiourea in 25ml of distilled water, heating and stirring at 100 ℃ for 30min, and uniformly mixing to obtain a mixture.
And step 3: drying by distillation
And (3) evaporating the water in the mixture obtained in the step (2) at 100 ℃ to dryness to obtain a mixture of which the water is evaporated to dryness.
And 4, step 4: high temperature calcination
And (3) grinding the mixture obtained in the step (3) after the water is evaporated to dryness into powder with the particle size of 300 meshes, calcining the powder at the high temperature of 600 ℃ for 3 hours under the protection of nitrogen, and then cooling the calcined powder to the room temperature to obtain the photocatalyst. In the photocatalyst, g-C3N4The loading amount of (B) is 1% (mass fraction).
Example 4
The preparation method of the photocatalyst of the embodiment comprises the following steps:
step 1: sepiolite powder pretreatment
Soaking 5g of sepiolite powder with the particle size of 300 meshes in distilled water for 26h, shaking in a gas bath oscillator at room temperature for 24h at the rotating speed of 170r/min, washing the precipitate with distilled water for 3 times, and drying at 105 ℃ for 24h to obtain the dried sepiolite powder.
Step 2: mixing
And (2) dispersing the dried sepiolite powder obtained in the step (1), 0.5g of melamine and 0.75g of thiourea in 25ml of distilled water, heating and stirring at 100 ℃ for 30min, and uniformly mixing to obtain a mixture.
And step 3: drying by distillation
And (3) evaporating the water in the mixture obtained in the step (2) at 100 ℃ to dryness to obtain a mixture of which the water is evaporated to dryness.
And 4, step 4: high temperature calcination
And (4) grinding the mixture obtained in the step (3) after the water is evaporated to dryness into powder with the particle size of 300 meshes, calcining at the high temperature of 450 ℃ for 4.5 hours under the protection of nitrogen, and then cooling to the room temperature to obtain the photocatalyst. In the photocatalyst, g-C3N4The supported amount of (B) was 5% (mass fraction).
Example 5
The preparation method of the photocatalyst of the embodiment comprises the following steps:
step 1: sepiolite powder pretreatment
Soaking 5g of sepiolite powder with the particle size of 300 meshes in distilled water for 24h, shaking in a gas bath oscillator at room temperature for 24h at the rotating speed of 170r/min, washing the precipitate with distilled water for 3 times, and drying at 105 ℃ for 24h to obtain the dried sepiolite powder.
Step 2: mixing
And (2) dispersing the dried sepiolite powder obtained in the step (1), 2g of melamine and 3g of thiourea into 25ml of distilled water, heating and stirring at 100 ℃ for 30min, and uniformly mixing to obtain a mixture.
And step 3: drying by distillation
And (3) evaporating the water in the mixture obtained in the step (2) at 100 ℃ to dryness to obtain a mixture of which the water is evaporated to dryness.
And 4, step 4: high temperature calcination
And (3) grinding the mixture obtained in the step (3) after the water is evaporated to dryness into powder with the particle size of 300 meshes, calcining at the high temperature of 550 ℃ for 3.5 hours under the protection of nitrogen, and then cooling to the room temperature to obtain the photocatalyst. In the photocatalyst, g-C3N4The loading amount of (B) was 20% (mass fraction).
Example 6
The preparation method of the photocatalyst of the embodiment comprises the following steps:
step 1: sepiolite powder pretreatment
Soaking 5g of sepiolite powder with the particle size of 300 meshes in distilled water for 24h, shaking in a gas bath oscillator at room temperature for 24h at the rotating speed of 170r/min, washing the precipitate with distilled water for 3 times, and drying at 105 ℃ for 24h to obtain the dried sepiolite powder.
Step 2: mixing
And (2) dispersing the dried sepiolite powder obtained in the step (1), 2g of melamine and 3g of thiourea into 25ml of distilled water, heating and stirring at 100 ℃ for 30min, and uniformly mixing to obtain a mixture.
And step 3: drying by distillation
And (3) evaporating the water in the mixture obtained in the step (2) at 100 ℃ to dryness to obtain a mixture of which the water is evaporated to dryness.
And 4, step 4: high temperature calcination
And (4) grinding the mixture obtained in the step (3) after the water is evaporated to dryness into powder with the particle size of 300 meshes, calcining at the high temperature of 450 ℃ for 4.2h under the protection of nitrogen, and then cooling to the room temperature to obtain the photocatalyst. In the photocatalyst, g-C3N4The loading amount of (B) was 20% (mass fraction).
Example 7
The preparation method of the photocatalyst of the embodiment comprises the following steps:
step 1: sepiolite powder pretreatment
Soaking 5g of sepiolite powder with the particle size of 300 meshes in distilled water for 24h, shaking in a gas bath oscillator at room temperature for 24h at the rotating speed of 170r/min, washing the precipitate with distilled water for 3 times, and drying at 105 ℃ for 24h to obtain the dried sepiolite powder.
Step 2: mixing
And (2) dispersing the dried sepiolite powder obtained in the step (1), 1.5g of melamine and 2.25g of thiourea into 25ml of distilled water, heating and stirring at 100 ℃ for 30min, and uniformly mixing to obtain a mixture.
And step 3: drying by distillation
And (3) evaporating the water in the mixture obtained in the step (2) at 100 ℃ to dryness to obtain a mixture of which the water is evaporated to dryness.
And 4, step 4: high temperature calcination
Grinding the mixture obtained in the step 3 after the water is evaporated to dryness into powder with the particle size of 300 meshes, calcining the powder at the high temperature of 500 ℃ for 3.5 hours under the protection of nitrogen, and then cooling the calcined powder to the room temperature to obtain the catalystThus obtaining the photocatalyst. In the photocatalyst, g-C3N4The loading amount of (B) was 15% (mass fraction).
Experimental example:
the photocatalysts obtained in the embodiments 1 to 7 are respectively tested for simulating the catalytic degradation of organic dyes by sunlight, and the test specifically comprises the following steps:
putting the photocatalysts obtained in the embodiments 1 to 7 into 50ml quartz tubes respectively, adding 30mg/L methylene blue dye solution, covering the quartz tubes with black plastic bags, standing for 1h, transferring the quartz tubes into a photocatalytic reaction system, starting stirring and photocatalysis, simulating sunlight by using a xenon lamp as a light source, and calculating the photocatalytic degradation efficiency as follows: 93.1%, 98.5%, 81.5%, 91.5%, 93.9%, 89.5% and 86.3%. The sepiolite has no visible light catalytic activity and is pure g-C3N4The visible light catalytic activity is lower, and the degradation rate of methylene blue is only 40% under the same experimental conditions.
The photocatalyst with the first photocatalytic degradation rate of 98.5% is subjected to three recovery experiments, and the catalytic efficiency can still reach 86%.
In the prior art, Li Rong et al use urea to prepare g-C with single component3N4Catalyst, Li jiao and so on adopts concentrated sulfuric acid to protonate and modify block g-C3N4Obtaining nanobelt g-C3N4The dye methylene blue is degraded under ultraviolet light, the reaction time is 2 hours, and the degradation rate of the dye is 94.9 percent and is close to 100 percent respectively. The degradation rate of the dye is high in both preparation methods, but visible light is not utilized. g-C3N4With other ingredients such as Pt, Ag, AgI, WO3Chlorine, TiO2g-C of the same3N4The composite catalyst has the activity of degrading dye by visible light catalysis, but the cost is far higher than that of the sepiolite.
As can be seen, the photocatalysts obtained in examples 1 to 7 of the present invention have a higher g-C ratio than the single component3N4The visible light catalytic efficiency of the photocatalyst or sepiolite is much higher.
Comparative example 1
The difference from the example 2 is that in the comparative example 1, the dried sepiolite powder is not added, and the rest is the same as the example 1, and the specific preparation method is as follows:
step 1: mixing
0.05g of melamine and 0.75g of thiourea were dispersed in 25ml of distilled water, heated and stirred at 100 ℃ for 30min, and mixed uniformly to obtain a mixture.
Step 2: drying by distillation
And (3) evaporating the water in the mixture obtained in the step (1) at 100 ℃ to dryness to obtain a mixture of which the water is evaporated to dryness.
And step 3: high temperature calcination
Grinding the mixture obtained in the step 2 after the water is evaporated to dryness into powder with the particle size of 300 meshes, calcining the powder at the high temperature of 500 ℃ for 4 hours under the protection of nitrogen, and then cooling the calcined powder to the room temperature to obtain the g-C3N4A catalyst.
g-C prepared in comparative example 13N4The catalyst is used for visible light catalytic degradation of methylene blue, and the degradation rate is 40%.
Comparative example 2
The difference from example 2 is that in comparative example 2, no melamine and thiourea are added, and the preparation method is the same as that of example 2:
step 1: sepiolite powder pretreatment
Soaking 5g of sepiolite powder with the particle size of 300 meshes in distilled water for 24h, shaking in a gas bath oscillator at room temperature for 24h at the rotating speed of 170r/min, washing the precipitate for 3 times by using distilled water, and drying at 105 ℃ for 24h to obtain the dried sepiolite powder.
Step 2: mixing
And (3) calcining the dried sepiolite powder obtained in the step (1) at the high temperature of 500 ℃ for 4 hours under the protection of nitrogen, and then cooling to room temperature to obtain the thermally modified sepiolite.
The thermally modified sepiolite prepared in comparative example 2 had no photocatalytic activity under visible light.
In conclusion, the sepiolite photocatalyst prepared by the method can be used together with the photocatalystAgent g-C3N4Interaction occurs to accelerate the separation of electron-hole pairs, thereby improving the catalytic activity of the photocatalyst.
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 invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of a photocatalyst is characterized by comprising the following steps:
step 1: sepiolite powder pretreatment
Soaking sepiolite powder in distilled water, shaking at room temperature, washing precipitate with distilled water, and drying to obtain dried sepiolite powder;
step 2: mixing
Dispersing the dried sepiolite powder, melamine and thiourea obtained in the step 1 into distilled water, heating, stirring and uniformly mixing to obtain a mixture;
and step 3: drying by distillation
Evaporating the water in the mixture obtained in the step 2 to dryness to obtain a mixture with the water evaporated to dryness;
and 4, step 4: high temperature calcination
And (4) grinding the mixture obtained in the step (3) after the water is evaporated to dryness into powder, calcining at high temperature under the protection of nitrogen, and then cooling to room temperature to obtain the photocatalyst.
2. The method for preparing a photocatalyst as claimed in claim 1, wherein in step 1, the sepiolite powder has a particle size of 300 mesh; the soaking time is 22-26 h.
3. The method according to claim 1, wherein in step 1, the oscillating device is a gas bath oscillator, the oscillating time is 24h, and the rotation speed is 170 r/min.
4. The method of claim 1, wherein the drying temperature is 105 ℃ and the drying time is 24 hours in step 1.
5. The method for preparing the photocatalyst according to claim 1, wherein in the step 2, the mass ratio of the sepiolite powder, the melamine and the thiourea is 5 (0.05-2) to (0.075-3).
6. The method of claim 1, wherein the volume of the distilled water in step 2 is 25 ml.
7. The method of claim 1, wherein the heating is performed at 100 ℃ for 30min in step 2.
8. The method according to claim 1, wherein the temperature for evaporating to dryness in step 3 is 100 ℃.
9. The method of claim 1, wherein in step 4, the powder has a particle size of 300 mesh.
10. The method for preparing a photocatalyst as claimed in any one of claims 1 to 9, wherein in step 4, the high-temperature calcination is carried out at a temperature of 400 ℃ to 600 ℃ for a period of 3h to 5 h.
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