CN111514921B - Bicontinuous-structure mesoporous graphitized carbon nitride and preparation method and application thereof - Google Patents
Bicontinuous-structure mesoporous graphitized carbon nitride and preparation method and application thereof Download PDFInfo
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 28
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- 238000001354 calcination Methods 0.000 claims description 7
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- 230000003197 catalytic effect Effects 0.000 description 4
- 238000001338 self-assembly Methods 0.000 description 4
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000003708 ampul Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
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- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920000361 Poly(styrene)-block-poly(ethylene glycol) Polymers 0.000 description 1
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- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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Abstract
The invention discloses a bicontinuous structure mesoporous graphitized carbon nitride and a preparation method and application thereof, and relates to the field of photocatalytic materials213‑b‑PEO45Preparing silicon dioxide with a bicontinuous structure for a soft template, and preparing ordered bicontinuous mesoporous graphitized carbon nitride by using the silicon dioxide as a template and applying the ordered bicontinuous mesoporous graphitized carbon nitride to a photocatalyst. The invention adopts a method of taking block copolymer as a soft template to prepare mesoporous SiO with a bicontinuous structure2As a hard template, the internal pore structure of the material can be more effectively adjusted; the graphite carbon nitride material of a bicontinuous structure can shorten the diffusion length of carriers generated by photons, which can contribute to achieving high photocatalytic efficiency.
Description
Technical Field
The invention relates to the field of photocatalytic materials, in particular to a bicontinuous mesoporous graphitized carbon nitride and a preparation method and application thereof.
Background
At present, photocatalytic water decomposition hydrogen production is one of the ideal choices for solving many environmental problems nowadays. Although various types of photocatalysts have been developed, the synthesis process is complicated, the cost is high, and the solar energy utilization rate is low. In recent years, graphite carbon nitride (g-CNs) has attracted much attention as a photocatalyst, but the specific surface area is reduced by the absence of pores in the materialSmall area, poor mass transfer and high carrier recombination rate, resulting in low photocatalytic activity. Introduction of a pore structure into a graphite carbon nitride photocatalyst becomes one of important methods for improving the catalytic performance of the graphite carbon nitride photocatalyst. In view of the prior art, the preparation of carbon nitride materials requires the use of mesoporous templates such as mesoporous SiO at elevated temperatures2Can successfully synthesize the mesoporous carbon nitride material. For example, it has been reported that mesoporous silica SBA-16 having a cubic ordered pore structure is prepared by using an ultrasonic and vacuum-assisted melt infiltration method, and a mesoporous carbon nitride material is produced by thermal polycondensation using this as a template and cyanamide as a precursor. But the material has the problems of small specific surface area, poor mass transfer, high carrier recombination rate and the like, thereby influencing H under the irradiation of visible light2The release rate of (a), the photocatalytic performance is reduced.
The bicontinuous structure has three-dimensional through pore channels and is one of ideal mass transfer structures, but at present, the bicontinuous structure is difficult to prepare by the traditional technologies such as photoetching from top to bottom due to the complex pore channel structure. The block polymer self-assembly provides a new idea for preparing the material with the bicontinuous structure. However, due to the narrow phase region of the bicontinuous structure in the phase diagram of the self-assembled morphology of the block copolymer and the difficulty in finding suitable self-assembly parameters, the preparation of the Bicontinuous Porous Material (BPM) based on the self-assembly of the block copolymer still faces a great challenge. At present, the functional materials with bicontinuous structures are few, and the structures are mostly seen in polymer supermolecular assemblies. For example, the Yiyong Mai team self-assembles from solutions of a commercial block copolymer, polystyrene-polyethylene oxide (PS-b-PEO), to obtain porous assemblies having a highly ordered bicontinuous structure, such as the Pn3m lattice structure. The assembly provides an excellent template for preparing the functional material with the bicontinuous structure by a subsequent template method. (Angew. chem.2017,56,7135.)
Therefore, those skilled in the art have been devoted to develop a mesoporous graphitized carbon nitride photocatalyst having an ordered bicontinuous structure.
Disclosure of Invention
In view of the defects in the prior art, the technical problem to be solved by the invention is to introduce a bicontinuous structure which is beneficial to mass transfer into carbon nitride to obtain a mesoporous carbon nitride material with high catalytic performance, and promote the migration and separation of photon-generated carriers by utilizing three-dimensional continuous through pore channels, thereby improving the photocatalytic performance.
In order to achieve the purpose, the invention provides graphitized carbon nitride with a bicontinuous structure, wherein the structure of the graphitized carbon nitride material is an ordered bicontinuous structure mesopore.
The method comprises the following steps: step 1, using PS by EISA method213-b-PEO45Preparing silicon dioxide with a bicontinuous structure for the soft template; and 2, preparing the double-continuous structure mesoporous graphitized carbon nitride by using the silicon dioxide as a template.
Further, the step 1 further comprises: step 1.1, adding PS213-b-PEO45Dissolving in tetrahydrofuran, stirring for 0.5h, adding hydrochloric acid, stirring the mixed solution for 2h, and then adding tetraethyl silicate to obtain a mixture; step 1.2, slowly evaporating the mixture at room temperature in a dryer in the air to remove volatile components, and then volatilizing for a period of time at a certain temperature to obtain a compound; and 1.3, calcining the compound in air at a certain temperature for a period of time to obtain the silicon dioxide with the bicontinuous structure.
Further, the step 2 further comprises: step 2.1, sealing the melamine and the bicontinuous structure silicon dioxide in a 25mL quartz ampoule bottle, synthesizing in a vacuum sealing environment, pumping the ampoule bottle to 3-10mbar, standing for a period of time at a certain temperature in a muffle furnace, and linearly heating to obtain yellow g-CN/SiO2A solid mixture; step 2.2, yellow g-CN/SiO2The solid mixture was treated with HF at room temperature for a period of time to remove the bicontinuous structure silica, followed by water and ethanol in a centrifuge at 1000 rpm-1Washing for three times at a rotating speed, and drying for a period of time at a certain temperature to obtain the bicontinuous mesoporous graphitized carbon nitride.
Further, step 1.1 said PS213-b-PEO45The dosage is 75mg, the dosage is 5mL, the concentration of hydrochloric acid is 2mol L-1The dosage is 500 mu L, and the dosage of the tetraethyl silicate is 640 mu L.
Further, the volatilization temperature in the step 1.2 is 100 ℃, and the time is 24 hours.
Further, the calcination temperature in step 1.3 is 550 ℃ and the calcination time is 6 h.
Further, in the step 2.1, the dosage of the melamine is 60mg, the dosage of the silicon dioxide with the bicontinuous structure is 30mg, the temperature of the muffle furnace is set to be 550 ℃, the standing time is 2 hours, and the linear heating rate is set to be 1 ℃ for min-1。
Further, in step 2.2, the HF concentration is 5 wt%, the treatment time is 12h, the drying temperature is 60 ℃, and the time is 12 h.
The double-continuous structure mesoporous graphitized carbon nitride is applied as a photocatalyst.
The invention has the following technical effects:
1) the mesoporous SiO with the bicontinuous structure is prepared by adopting a method of taking a block copolymer as a soft template2As a hard template, the internal pore structure of the material can be more effectively adjusted;
2) the graphite carbon nitride material of a bicontinuous structure can shorten the diffusion length of carriers generated by photons, which can contribute to achieving high photocatalytic efficiency.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a scanning electron microscope image of a preferred embodiment of the present invention;
FIG. 2 is a transmission electron microscope image of a preferred embodiment of the present invention;
FIG. 3 is the hydrogen generation performance of a preferred embodiment of the present invention;
fig. 4 is a graph of the cycling performance of a preferred embodiment of the present invention.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
Example 1
Induction of self-Assembly (EISA) by solvent Evaporation method with PS213-b-PEO45Preparation of bicontinuous SiO for soft templates2A hard template. First 75mg PS213-b-PEO45Dissolved in 5mL of tetrahydrofuran. After stirring for 0.5h, HCl (500. mu.L, 2mol L) was added to the mixture-1) And the mixed solution was stirred for 2 hours, and TEOS (640 μ L) was further added to the solution. The solution was then slowly evaporated at room temperature in an air desiccator to remove volatile components. Volatilizing the obtained compound at 100 ℃ for 24h, and calcining the product at 550 ℃ in air for 6h to obtain the silicon dioxide with the bicontinuous structure.
60mg of melamine and 30mg of silica of bicontinuous structure were sealed as hard templates in 25mL quartz ampoules, which were evacuated to vacuum. Then, the ampoule was placed in a muffle furnace at 550 ℃ for 2 hours at a linear temperature rise rate of 1 ℃ for min-1. In this process, the polymer produced by the sublimation of melamine is deposited on a silica hard template of bicontinuous structure. Thereafter, the yellow g-CN/SiO obtained2The solid mixture was treated with 5 wt% HF at room temperature for 12h to remove the dual continuous structure of the silica hard template. After HF etching, the sample was sequentially washed with water and ethanol in a centrifuge for 1000 rpm-1Washing for three times at the rotating speed of (1), and drying for 12 hours at the temperature of 60 ℃ to obtain the bicontinuous mesoporous graphitized carbon nitride.
As shown in fig. 1 and 2, the obtained carbon nitride material is shown to be an ordered bicontinuous structure.
As shown in FIG. 3, the resulting carbon nitride material was used as photo-decomposed water driven by visible light to produce H2Having excellent photocatalytic performance, H2The production rate of (2) is as high as 6, 831 mu mol h-1g-1. As shown in fig. 4, the material retains 90% of the primary hydrogen generation after 4 catalytic cycles, and has excellent catalytic cycle stability.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (3)
1. A preparation method of bicontinuous mesoporous graphitized carbon nitride is characterized in that the structure of the graphitized carbon nitride is ordered bicontinuous mesoporous structure, and the method comprises the following steps:
step 1, using PS by EISA method213-b-PEO45The block copolymer is used for preparing silicon dioxide with a bicontinuous structure for a soft template:
step 1.1, adding PS213-b-PEO45Dissolving in tetrahydrofuran, stirring for 0.5h, adding hydrochloric acid, stirring the mixed solution for 2h, and then adding tetraethyl silicate to obtain a mixture; the PS213-b-PEO45The dosage is 75mg, the dosage of tetrahydrofuran is 5mL, the concentration of hydrochloric acid is 2mol/L, the dosage is 500 muL, and the dosage of tetraethyl silicate is 640 muL;
step 1.2, slowly evaporating the mixture at room temperature in a dryer in the air to remove volatile components, and then volatilizing at a certain temperature for a period of time to obtain a compound; the volatilization temperature is 100 ℃, and the time is 24 hours;
step 1.3, calcining the compound in air at a certain temperature for a period of time to obtain the silicon dioxide with the bicontinuous structure; the calcination temperature is 550 ℃, and the calcination time is 6 h;
step 2, preparing the double-continuous structure mesoporous graphitized carbon nitride by using the silicon dioxide as a template:
step 2.1, melamine and the silica of bicontinuous structure are sealed in 25mL quartz ampoules, synthesized in a vacuum-tight environment, the ampoules are evacuated to 3-10mbar, and subsequentlyStanding in a muffle furnace at a certain temperature for a period of time, and linearly heating to obtain yellow g-CN/SiO2A solid mixture; the dosage of the melamine is 60mg, the dosage of the silicon dioxide with the double continuous structure is 30mg, the temperature of the muffle furnace is set to be 550 ℃, the standing time is 2h, and the linear heating rate is set to be 1 ℃/min;
step 2.2, yellow g-CN/SiO2And (3) treating the solid mixture with HF at room temperature for a period of time to remove the silicon dioxide with the bicontinuous structure, then washing the solid mixture with water and ethanol under a centrifuge at the rotating speed of 1000r/min for three times, and drying the solid mixture at a certain temperature for a period of time to obtain the bicontinuous structure mesoporous graphitized carbon nitride.
2. The method for preparing bicontinuous mesoporous graphitized carbon nitride according to claim 1, wherein the HF concentration in step 2.2 is 5 wt%, the treatment time is 12 hours, the drying temperature is 60 ℃, and the drying time is 12 hours.
3. The application of the bicontinuous mesoporous graphitized carbon nitride obtained by the preparation method of claim 1 as a photocatalyst.
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