CN112337464A - Spray pyrolysis preparation method, synthesis system and application of metal-doped porous carbon-based visible-light-induced photocatalyst - Google Patents

Spray pyrolysis preparation method, synthesis system and application of metal-doped porous carbon-based visible-light-induced photocatalyst Download PDF

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CN112337464A
CN112337464A CN202011109889.9A CN202011109889A CN112337464A CN 112337464 A CN112337464 A CN 112337464A CN 202011109889 A CN202011109889 A CN 202011109889A CN 112337464 A CN112337464 A CN 112337464A
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light
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porous carbon
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刘健
汪璐
陶亮亮
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Hefei University of Technology
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    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
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Abstract

The invention discloses a spray pyrolysis preparation method of a metal-doped porous carbon-based visible-light-induced photocatalyst, which comprises the following steps: mixing a carbon source material, a pore-forming agent and a metal salt solution, and dissolving in deionized water to form a precursor solution; carrying out ultrasonic atomization on the precursor liquid, then sending the precursor liquid into pyrolysis equipment along with carrier gas, and pyrolyzing for 1-2s to form a material precursor; cooling the material precursor and collecting; the invention also discloses a synthesis system for implementing the method and application of the photocatalytic material prepared by the method in catalytic degradation treatment of the dye. The catalyst material has the advantages that the raw materials required by the preparation of the catalyst material are cheap and easy to obtain, the subsequent large-scale utilization is facilitated, the synthesis steps are simple, and the catalyst material can be prepared by one-step pyrolysis after the precursor solution is prepared; the catalyst material can also greatly improve the utilization rate of sunlight, reduce the occurrence of light corrosion and greatly improve and maintain the specific surface area of the catalyst material.

Description

Spray pyrolysis preparation method, synthesis system and application of metal-doped porous carbon-based visible-light-induced photocatalyst
Technical Field
The invention relates to the field of preparation of porous carbon material photocatalysts, in particular to a spray pyrolysis preparation method, a synthesis system and application of a metal-doped porous carbon-based visible-light-induced photocatalyst.
Background
The photocatalyst is a generic name for a semiconductor material having a photocatalytic function represented by nano-sized titanium dioxide. In the case of titanium dioxide, it can generate a substance having a strong oxidizing property (e.g., hydroxyl radical, oxygen gas, etc.) under light irradiation, and can be used for decomposing organic compounds, partially inorganic compounds, bacteria, viruses, etc. However, the existing photocatalytic materials have the following disadvantages: (1) the existing photocatalytic material has low light utilization efficiency, for example, the traditional titanium dioxide-based photocatalyst can only well utilize the light in an ultraviolet band; (2) the existing photocatalytic material has photo-corrosion, and the material can be decomposed and damaged after being used for a period of time, so that the service life of the catalyst is greatly reduced; (3) the specific surface area of the existing photocatalyst material is insufficient, and the specific surface area is also greatly reduced after agglomeration, so that the catalyst cannot be fully and effectively utilized.
In addition, a carbon-based porous material hydrothermal method can be adopted to prepare the photocatalytic material, but the conventional hydrothermal method for synthesizing the carbon-based porous material is that all raw materials are directly put into a reaction kettle for reaction, subsequent carbon materials are required to be cleaned, ground, sieved and the like, so that the stability and uniformity of a sample cannot be ensured, and an additional modification step is required to be carried out during subsequent metal and heteroatom doping, which is very tedious.
Disclosure of Invention
The invention aims to provide a spray pyrolysis preparation method, a synthesis system and application of a metal-doped porous carbon-based visible-light-induced photocatalyst.
The invention realizes the purpose through the following technical scheme:
a spray pyrolysis preparation method of a metal-doped porous carbon-based visible-light-induced photocatalyst comprises the following steps
The method comprises the following steps: mixing a carbon source material, a pore-forming agent and a metal salt solution, and dissolving in deionized water to form a precursor solution;
step two: carrying out ultrasonic atomization on the precursor liquid, then sending the precursor liquid into pyrolysis equipment along with carrier gas, and pyrolyzing for 1-2s to form a catalyst material precursor;
step three: and cooling the catalyst material precursor, collecting, cleaning and modifying to obtain the metal-doped porous carbon-based visible-light-induced photocatalyst material.
The further improvement is that the mass ratio of each component in the precursor solution is 0.5-5% of carbon source material, 0.5-5% of pore-forming agent and 0.1-2% of metal salt solution.
The further improvement is that the carbon source material is sucrose.
In a further improvement, the pore-forming agent is sodium carbonate or sodium chloride.
In a further improvement, the metal salt solution is copper sulfate.
The further improvement is that the carrier gas adopts nitrogen with the flow rate of 0.1-5L/min.
The further improvement is that the temperature of the pyrolysis is 600-800 ℃.
The further improvement is that in the third step, the collected catalyst material precursor is soaked and washed by dilute hydrochloric acid to adjust the surface potential, and after the soaking and washing are completed, the catalyst material precursor is separated, cleaned and dried.
The invention provides a synthesis system for implementing the method, which comprises a spraying device, a pyrolysis device and a collection device, wherein the spraying device consists of a spraying container, an ultrasonic atomizer arranged in the spraying container and a nitrogen tank connected with the spraying container, the collection device is connected with the spraying container through a pipeline, the pyrolysis device is a tubular furnace, and the tubular furnace is arranged on a connecting pipeline between the collection device and the spraying container.
The invention provides an application of a metal-doped porous carbon-based visible-light-induced photocatalyst prepared by the method in catalytic degradation of a dye, wherein the dye is methyl orange, methylene blue or Congo red and the like.
The invention has the beneficial effects that:
1) the synthesis steps are simple, the photocatalyst material can be prepared by one-step pyrolysis after the precursor solution is prepared, and the subsequent operations of cleaning, grinding, sieving and the like and the additional modification operation during the doping of metal and heteroatom are omitted;
2) the traditional photocatalyst mostly utilizes titanium dioxide, the band gap of the titanium dioxide is 3.1-3.2eV, only ultraviolet band light can be utilized, the sunlight utilization efficiency is low, the method loads copper oxide and cuprous oxide nanoparticles with the band gap of 1.2-2.2eV on the surface of the nano-scale porous carbon material through a one-step pyrolysis synthesis method, so that the band gap of the prepared catalyst material is reduced, and the utilization rate of sunlight is greatly improved;
3) the carbon material has a stable structure, and the carbon material is used as a catalyst substrate, so that the occurrence of light corrosion can be greatly reduced, the stable work of the catalyst is ensured, and the service life is prolonged;
4) the nanoscale porous carbon has rich porous structures, the specific surface area of the catalyst material can be greatly increased, and the surface electronegativity of the catalyst material particles can be improved through the loading of metal and corresponding modification adjustment, so that the catalyst material is prevented from agglomerating, and the higher specific surface area is kept in the whole reaction process;
5) the catalyst material can be used for harmless degradation treatment of dyes and other organic pollutants;
6) the raw materials required by the preparation of the catalyst material are cheap and easy to obtain, and the catalyst material is convenient for subsequent large-scale utilization.
Drawings
FIG. 1 is a TEM image of a visible-light-induced photocatalyst prepared by the one-step pyrolysis method of the present invention;
FIG. 2 is a schematic diagram of a spray pyrolysis preparation system of a metal-doped porous carbon-based visible light catalyst;
FIG. 3 is a graph showing the degradation curve of a visible light catalyst methyl orange;
in the figure: 1. a pyrolysis device; 2. a collection device; 3. a spray container; 4. an ultrasonic atomizer; 5. a nitrogen tank; 6. a pipeline.
Detailed Description
The present application will now be described in further detail with reference to the drawings, it should be noted that the following detailed description is given for illustrative purposes only and is not to be construed as limiting the scope of the present application, as those skilled in the art will be able to make numerous insubstantial modifications and adaptations to the present application based on the above disclosure.
Example 1
The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst comprises the following steps:
the method comprises the following steps: mixing a carbon source material, a pore-forming agent and a metal salt solution, and dissolving the mixture in deionized water to form a precursor solution, wherein the mass ratio of each component in the precursor solution is 0.5% of the carbon source material, 0.5% of the pore-forming agent and 0.1% of the metal salt solution;
step two: carrying out ultrasonic atomization on the precursor liquid, then sending the precursor liquid into pyrolysis equipment along with carrier gas (nitrogen with the flow rate of 0.1L/min), and pyrolyzing the precursor liquid for 1.5s at 700 ℃ to form a catalyst material precursor;
step three: and cooling the material precursor, collecting, and soaking and washing the collected material precursor by using dilute hydrochloric acid to adjust the surface potential, improve the dispersibility and prevent subsequent aggregation, and separating, cleaning and drying the precursor material after the soaking and washing are finished.
Example 2
The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst comprises the following steps:
the method comprises the following steps: mixing a carbon source material, a pore-forming agent and a metal salt solution, and dissolving the mixture in deionized water to form a precursor solution, wherein the mass ratio of each component in the precursor solution is 5% of the carbon source material, 5% of the pore-forming agent and 1% of the metal salt solution;
step two: carrying out ultrasonic atomization on the precursor liquid, then sending the precursor liquid into pyrolysis equipment along with carrier gas (nitrogen with the flow rate of 2L/min), and pyrolyzing the precursor liquid for 2s at 600 ℃ to form a catalyst material precursor;
step three: and cooling the material precursor, collecting, and soaking and washing the collected material precursor by using dilute hydrochloric acid to adjust the surface potential, improve the dispersibility and prevent subsequent aggregation, and separating, cleaning and drying the precursor material after the soaking and washing are finished.
Example 3
The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst comprises the following steps:
the method comprises the following steps: mixing a carbon source material, a pore-forming agent and a metal salt solution, and dissolving the mixture in deionized water to form a precursor solution, wherein the mass ratio of each component in the precursor solution is 2% of the carbon source material, 2% of the pore-forming agent and 2% of the metal salt solution;
step two: carrying out ultrasonic atomization on the precursor liquid, then sending the precursor liquid into pyrolysis equipment along with carrier gas (nitrogen with the flow rate of 5L/min), and pyrolyzing the precursor liquid for 1s at 800 ℃ to form a catalyst material precursor;
step three: cooling and collecting the material precursor, soaking and washing the collected material precursor with dilute hydrochloric acid to adjust surface potential, improving dispersibility and preventing subsequent aggregation, separating, cleaning and drying the precursor material after soaking and washing, and obtaining a TEM image of the photocatalyst sample as shown in FIG. 1
In the above embodiment, the carbon source material is sucrose, the pore-forming agent is sodium carbonate, and the metal salt solution is copper sulfate. Of course, in the implementation process of the present invention, the carbon source material, the pore-forming agent, and the metal salt solution may be selected from other substances as needed, for example, the carbon source material may also be selected from glucose, maltose, glycerol, and the like, the pore-forming agent may also be selected from ammonium bicarbonate, calcium carbonate, and the like, and the metal salt solution may also be selected from cerium nitrate, zinc chloride, manganese sulfate, iron nitrate, lanthanum nitrate, praseodymium nitrate, and the like, all of which are within the protection scope of the present invention.
Example 4
As shown in fig. 2, a synthesis system for implementing the above method comprises a spraying device, a pyrolysis device 1 and a collection device 2, wherein the spraying device is composed of a spraying container 3, an ultrasonic atomizer 4 arranged in the spraying container 3 and a nitrogen tank 5 connected to the spraying container 3, the collection device 2 is connected with the spraying container 3 through a pipeline 6, the pyrolysis device 1 is a tubular furnace, and the tubular furnace is arranged on the connecting pipeline 6 between the collection device 2 and the spraying container 3.
This synthesis system is at the during operation, pack into spray container 3 with the prepared precursor liquid earlier, start ultrasonic atomizer 4, become the liquid droplet with precursor liquid ultrasonic atomization, open the discharge valve of nitrogen gas jar 5 simultaneously, in nitrogen gas lets in spray container 3 with certain speed, in nitrogen gas can carry the atomizing liquid droplet and get into pyrolysis device 1 through pipeline 6, pyrolysis device 1 heats the pyrolysis, forms the catalyst material precursor, is cooled down and is collected by collection device 2 at last.
Example 5
The application of the metal-doped porous carbon-based visible-light-induced photocatalyst prepared by the method in catalytic degradation of dyes is methyl orange, methylene blue, Congo red or the like, and can be used for degrading other organic pollutants.
In order to verify the catalytic degradation efficiency of the catalyst material prepared by the invention, a photocatalytic degradation contrast test of methyl orange is carried out as follows:
preparing a catalyst sample prepared in example 2, titanium dioxide and methyl orange into 0.01g/L of dispersion liquid a, b and c respectively;
mixing 5ml of the dispersion liquid a and b with 5ml of the solution c to obtain samples d and e;
thirdly, the solution d and the solution e are subjected to dark ultrasound for 60min to achieve adsorption balance;
exposure to 150000Lx sunlight after 60 min;
sampling at intervals, centrifuging, taking supernatant, filtering and measuring the concentration of methyl orange.
The degradation curve prepared based on the measured concentration of methyl orange is shown in fig. 3, and the experimental results show that the catalyst material prepared in example 2 (i.e., the "sample" curve in the figure) has better photocatalytic effect than titanium dioxide, mainly indicated that the catalyst material prepared in example 2 can degrade methyl orange faster, the time required for reaching 30% degradation rate is about 200min shorter than that of titanium dioxide, and the final degradation rate is 32% higher than that of titanium dioxide.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.

Claims (10)

1. The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst is characterized by comprising the following steps of: the method comprises the steps of
The method comprises the following steps: mixing a carbon source material, a pore-forming agent and a metal salt solution, and dissolving in deionized water to form a precursor solution;
step two: carrying out ultrasonic atomization on the precursor liquid, then sending the precursor liquid into pyrolysis equipment along with carrier gas, and pyrolyzing for 1-2s to form a catalyst material precursor;
step three: and cooling the catalyst material precursor, collecting, cleaning and modifying to obtain the metal-doped porous carbon-based visible-light-induced photocatalyst material.
2. The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst according to claim 1, characterized in that: the mass ratio of each component in the precursor solution is 0.5-5% of carbon source material, 0.5-5% of pore-forming agent and 0.1-2% of metal salt solution.
3. The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst according to claim 1, characterized in that: the carbon source material is sucrose.
4. The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst according to claim 1, characterized in that: the pore-forming agent is sodium carbonate or sodium chloride.
5. The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst according to claim 1, characterized in that: the metal salt solution is copper sulfate.
6. The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst according to claim 1, characterized in that: the carrier gas adopts nitrogen with the flow rate of 0.1-5L/min.
7. The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst according to claim 1, characterized in that: the temperature of the pyrolysis is 600-800 ℃.
8. The spray pyrolysis preparation method of the metal-doped porous carbon-based visible-light-induced photocatalyst according to claim 1, characterized in that: and in the third step, the collected material precursor is soaked and washed by dilute hydrochloric acid to adjust the surface potential, and after the soaking and washing are finished, the catalyst material precursor is separated, cleaned and dried.
9. A synthesis system for carrying out the method of any one of claims 1 to 8, wherein: the synthesis system comprises a spraying device, a pyrolysis device and a collecting device, wherein the spraying device comprises a spraying container, an ultrasonic atomizer arranged in the spraying container and a nitrogen tank connected to the spraying container, the collecting device is connected with the spraying container through a pipeline, the pyrolysis device selects a tubular furnace, and the tubular furnace is arranged on a connecting pipeline between the collecting device and the spraying container.
10. Use of a metal-doped porous carbon-based visible-light-induced photocatalyst prepared by the method according to any one of claims 1 to 8 in dye-catalyzed degradation, wherein: the dye is methyl orange, methylene blue or Congo red.
CN202011109889.9A 2020-10-16 2020-10-16 Spray pyrolysis preparation method, synthesis system and application of metal-doped porous carbon-based visible-light-induced photocatalyst Pending CN112337464A (en)

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