CN113275030A - Preparation method of ordered mesoporous carbon and carbon nitride composite material - Google Patents

Preparation method of ordered mesoporous carbon and carbon nitride composite material Download PDF

Info

Publication number
CN113275030A
CN113275030A CN202110494216.8A CN202110494216A CN113275030A CN 113275030 A CN113275030 A CN 113275030A CN 202110494216 A CN202110494216 A CN 202110494216A CN 113275030 A CN113275030 A CN 113275030A
Authority
CN
China
Prior art keywords
composite material
carbon
sba
ordered mesoporous
carbon nitride
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110494216.8A
Other languages
Chinese (zh)
Inventor
张俊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN202110494216.8A priority Critical patent/CN113275030A/en
Publication of CN113275030A publication Critical patent/CN113275030A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • B01J35/39
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02Impregnation, coating or precipitation
    • B01J37/0201Impregnation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/082Decomposition and pyrolysis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/725Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

Abstract

The invention discloses a preparation method of an ordered mesoporous carbon and carbon nitride composite material, which specifically comprises the following steps: mixing a certain amount ofDispersing C/SBA-15 and melamine in deionized water, stirring for 2h, and drying the solution at 50 ℃ to obtain a solid; then calcining the solid in a muffle furnace for 2 hours at two temperatures respectively, cooling to room temperature, and grinding to powder; finally, hydrofluoric acid with certain concentration is used for treating for 24 hours, and then OMC/gC is successfully prepared by filtering, washing and drying3N4A composite material. The preparation method of the ordered mesoporous carbon and carbon nitride composite material comprises the step of loading OMC on a lamellar structure g-C3N4The surface of the material has larger specific surface area, stronger absorption of visible light and better separation effect of photogenerated electrons and holes.

Description

Preparation method of ordered mesoporous carbon and carbon nitride composite material
Technical Field
The invention relates to the technical field of photocatalyst material preparation, in particular to a preparation method of an ordered mesoporous carbon and carbon nitride composite material.
Background
g-C3N4The material has the advantages of response to visible light, good thermal stability and chemical stability, no toxicity, low cost, easy preparation and the like by virtue of the narrow forbidden band width, and is concerned by researchers in various countries. However, g-C of a single phase3N4The generated photo-generated electrons and holes are easy to recombine, and the photo-catalytic activity is not high due to the low specific surface area, so that the photo-catalytic activity is difficult to meet the practical application. Therefore, to increase g-C3N4Photocatalytic activity of (1), the students at home and abroad are right for g-C3N4A great deal of modification work is carried out, for example, g-C with mesoporous structure is prepared by using a soft and hard template method3N4Increase the specific surface area to g-C3N4Carrying out doping modification of metal ions or nonmetals to obtain g-C3N4Compounding with other semiconductor material to form composite photocatalyst and preparing g-C in different shapes3N4And so on. Among them, the composite photocatalyst prepared by compounding with semiconductor materials is the most common modification means. When g-C3N4After being compounded with other semiconductors, photo-generated electrons and holes can be rapidly separated by means of complementary potentials, quantum efficiency is improved, and finally photocatalytic activity is enhanced. .
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of an ordered mesoporous carbon and carbon nitride composite material, and provides a preparation scheme of a novel carbon nitride composite material.
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of an ordered mesoporous carbon and carbon nitride composite material specifically comprises the following steps:
s1, preparation of carbon/SBA-15 (C/SBA-15): dispersing SBA-15 into deionized water containing a certain amount of sucrose and concentrated sulfuric acid (98%), continuously stirring for 12h, heating, sequentially treating at 100 ℃ and 160 ℃ for 6h, and grinding to powder. The above impregnation process was repeated once more. Carrying out heat treatment on the obtained material for 5h at 900 ℃ in a protective gas atmosphere to obtain C/SBA-15 composite particles;
s2, ordered mesoporous carbon/carbon nitride (OMC/g-C)3N4) Preparing a composite material: dispersing a certain amount of C/SBA-15 prepared in the step S1 and melamine in deionized water, stirring for 2 hours, and drying the solution at 50 ℃ to obtain a solid;
s3, calcining the solid prepared in the S2 step in a muffle furnace at two temperatures for 2 hours respectively, cooling to room temperature, and grinding to powder;
s4, finally treating the mixture for 24 hours by using hydrofluoric acid with certain concentration, and then filtering, washing and drying the mixture to successfully prepare the OMC/gC3N4A composite material.
Preferably, the shielding gas in step S1 includes one or more of nitrogen, helium, neon, and argon.
Preferably, the two temperatures in the step S3 are 500 ℃ and 520 ℃.
Preferably, the certain concentration in step S4 is 10%.
Advantageous effects
The invention provides a preparation method of an ordered mesoporous carbon and carbon nitride composite material. Compared with the prior art, the method has the following beneficial effects: the preparation method of the ordered mesoporous carbon and carbon nitride composite material comprises the step of loading OMC on a lamellar structure g-C3N4The surface of the material has larger specific surface area, stronger absorption of visible light and better separation effect of photogenerated electrons and holes. The photocatalytic activity of RhB serving as a model pollutant is investigated, and an experimental result shows that OMC/g-C3N4The composite material can adsorb the RhB dye more strongly by virtue of larger specific surface area, the capacity of degrading the RhB dye by photocatalysis is correspondingly enhanced, and the O in the photocatalysis process can be obtained by carrying out a reactive species capture experiment on the catalyst2 -Is the main active component, and the cavity does not play the role of the active component, and in addition, the prepared composite particles have better continuous use capability and structural stability.
Drawings
FIG. 1 shows OMC/g-C of the present invention3N4The preparation process of the composite material is shown schematically;
FIG. 2 shows OMC/g-C of the present invention3N4A TEM image of (B);
FIG. 3 is an ultraviolet-visible absorption spectrogram of the RhB solution under different illumination times of photocatalytic degradation of the composite material of the present invention;
FIG. 4 is a graph showing the adsorption curve of the composite material of the present invention to (A) RhB and the photodegradation curve of (B);
FIG. 5 is a bar graph of the RhB degradation rate constants of the present invention.
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. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-5, the embodiment of the present invention provides three technical solutions: a preparation method of an ordered mesoporous carbon and carbon nitride composite material specifically comprises the following embodiments:
example 1
S1, preparation of carbon/SBA-15 (C/SBA-15): dispersing 1g of SBA-15 into 5g of deionized water containing 1.25g of sucrose and 1g of concentrated sulfuric acid (98%), continuously stirring for 12h, heating, sequentially treating at 100 ℃ and 160 ℃ for 6h, and grinding to powder. The above impregnation process was repeated once more. Carrying out heat treatment on the obtained material for 5h at 900 ℃ in a nitrogen atmosphere to obtain C/SBA-15 composite particles;
s2, ordered mesoporous carbon/carbon nitride (OMC/g-C)3N4) Preparing a composite material: dispersing 0.05g of C/SBA-15 prepared in the step S1 and 3g of melamine in 20ml of deionized water, stirring for 2 hours, and drying the solution at 50 ℃ to obtain a solid;
s3, calcining the solid prepared in the S2 step in a muffle furnace at 500 ℃ and 520 ℃ for 2 hours respectively, cooling to room temperature, and grinding to powder;
s4, finally treating the mixture for 24 hours by 10 percent hydrofluoric acid, and then filtering, washing and drying the mixture to successfully prepare the OMC/gC3N4A composite material.
Example 2
S1, preparation of carbon/SBA-15 (C/SBA-15): dispersing 1g of SBA-15 into 5g of deionized water containing 1.25g of sucrose and 1g of concentrated sulfuric acid (98%), continuously stirring for 12h, heating, sequentially treating at 100 ℃ and 160 ℃ for 6h, and grinding to powder. The above impregnation process was repeated once more. Carrying out heat treatment on the obtained material for 5h at 900 ℃ in a nitrogen atmosphere to obtain C/SBA-15 composite particles;
s2, ordered mesoporous carbon/carbon nitride (OMC/g-C)3N4) Preparing a composite material: dispersing 0.1g of C/SBA-15 prepared in the step S1 and 3g of melamine in 20ml of deionized water, stirring for 2 hours, and drying the solution at 50 ℃ to obtain a solid;
s3, calcining the solid prepared in the S2 step in a muffle furnace at 500 ℃ and 520 ℃ for 2 hours respectively, cooling to room temperature, and grinding to powder;
s4, finally treating the mixture for 24 hours by 10 percent hydrofluoric acid, and then filtering, washing and drying the mixture to successfully prepare the OMC/gC3N4A composite material.
Example 3
S1, preparation of carbon/SBA-15 (C/SBA-15): dispersing 1g of SBA-15 into 5g of deionized water containing 1.25g of sucrose and 1g of concentrated sulfuric acid (98%), continuously stirring for 12h, heating, sequentially treating at 100 ℃ and 160 ℃ for 6h, and grinding to powder. The above impregnation process was repeated once more. Carrying out heat treatment on the obtained material for 5h at 900 ℃ in a nitrogen atmosphere to obtain C/SBA-15 composite particles;
s2, ordered mesoporous carbon/carbon nitride (OMC/g-C)3N4) Preparing a composite material: dispersing 0.2g of C/SBA-15 prepared in the step S1 and 3g of melamine in 20ml of deionized water, stirring for 2 hours, and drying the solution at 50 ℃ to obtain a solid;
s3, calcining the solid prepared in the S2 step in a muffle furnace at 500 ℃ and 520 ℃ for 2 hours respectively, cooling to room temperature, and grinding to powder;
s4, finally treating the mixture for 24 hours by 10 percent hydrofluoric acid, and then filtering, washing and drying the mixture to successfully prepare the OMC/gC3N4A composite material.
To verify the OMC/g-C prepared by the method of the invention3N4The photocatalytic effect of the composite material is that the degradation test of RhB is carried out on composite material samples prepared by putting different amounts of C/SBA-15, please refer to the curve B in figure 4, after the illumination, the single phase g-C3N4The degradation rate for RhB was about 23.6%. To prepare OMC/g-C3N4The activity of the sample for photocatalytic degradation of RhB is generally higher than that of pure g-C3N4In particular, 0.2g of OMC/g-C prepared from C/SBA-15 is added3N4After 60min reaction, the degradation rate of RhB almost reaches 100%. Also, referring to FIG. 3, FIG. 3 shows OMC/g-C3N4Ultraviolet-visible absorption spectrogram of RhB photocatalytic degradation of the composite material. As shown in the figure, the intensity of the absorption peak of RhB is gradually reduced along with the prolonging of the illumination time, and after 1h of reaction, the characteristic peak of RhB completely disappears, which means that RhB is degraded. The above results demonstrate that OMC/g-C is prepared according to the invention3N4The composite material is a photocatalyst with high performance and high efficiency.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (4)

1. A method for preparing an ordered mesoporous carbon and carbon nitride composite material is characterized by comprising the following steps: the method specifically comprises the following steps:
s1, preparation of carbon/SBA-15 (C/SBA-15): dispersing SBA-15 into deionized water containing a certain amount of sucrose and concentrated sulfuric acid (98%), continuously stirring for 12h, heating, sequentially treating at 100 ℃ and 160 ℃ for 6h, and grinding to powder. The above impregnation process was repeated once more. Carrying out heat treatment on the obtained material for 5h at 900 ℃ in a protective gas atmosphere to obtain C/SBA-15 composite particles;
s2, ordered mesoporous carbon/carbon nitride (OMC/g-C)3N4) Preparing a composite material: dispersing a certain amount of C/SBA-15 prepared in the step S1 and melamine in deionized water, stirring for 2 hours, and drying the solution at 50 ℃ to obtain a solid;
s3, calcining the solid prepared in the S2 step in a muffle furnace at two temperatures for 2 hours respectively, cooling to room temperature, and grinding to powder;
s4, finally treating the mixture for 24 hours by using hydrofluoric acid with certain concentration, and then filtering, washing and drying the mixture to successfully prepare the OMC/gC3N4A composite material.
2. The method for preparing the ordered mesoporous carbon and carbon nitride composite material according to claim 1, wherein the method comprises the following steps: the shielding gas in the step S1 includes one or more of nitrogen, helium, neon, and argon.
3. The method for preparing the ordered mesoporous carbon and carbon nitride composite material according to claim 1, wherein the method comprises the following steps: the two temperatures in the step S3 are 500 ℃ and 520 ℃.
4. The method for preparing the ordered mesoporous carbon and carbon nitride composite material according to claim 1, wherein the method comprises the following steps: the certain concentration in step S4 is 10%.
CN202110494216.8A 2021-05-07 2021-05-07 Preparation method of ordered mesoporous carbon and carbon nitride composite material Pending CN113275030A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110494216.8A CN113275030A (en) 2021-05-07 2021-05-07 Preparation method of ordered mesoporous carbon and carbon nitride composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110494216.8A CN113275030A (en) 2021-05-07 2021-05-07 Preparation method of ordered mesoporous carbon and carbon nitride composite material

Publications (1)

Publication Number Publication Date
CN113275030A true CN113275030A (en) 2021-08-20

Family

ID=77278225

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110494216.8A Pending CN113275030A (en) 2021-05-07 2021-05-07 Preparation method of ordered mesoporous carbon and carbon nitride composite material

Country Status (1)

Country Link
CN (1) CN113275030A (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104475140A (en) * 2014-11-07 2015-04-01 江苏大学 Silver-modified carbon nitride composite photocatalytic material and preparation method thereof
CN106810436A (en) * 2015-11-30 2017-06-09 中国科学院大连化学物理研究所 A kind of method that catalysis oxidation glycerine prepares lactic acid

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104475140A (en) * 2014-11-07 2015-04-01 江苏大学 Silver-modified carbon nitride composite photocatalytic material and preparation method thereof
CN106810436A (en) * 2015-11-30 2017-06-09 中国科学院大连化学物理研究所 A kind of method that catalysis oxidation glycerine prepares lactic acid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LEI SHI ET AL.: "Remarkably enhanced photocatalytic activity of ordered mesoporous carbon/g-C3N4 composite photocatalysts under visible light" *

Similar Documents

Publication Publication Date Title
CN107824210B (en) Titanium dioxide composite photocatalyst coated by nitrogen-doped mesoporous carbon and preparation method and application thereof
CN110201703B (en) Preparation method of multi-metal doped carbon nitride composite material
Guo et al. A new heterojunction Ag3PO4/Cr-SrTiO3 photocatalyst towards efficient elimination of gaseous organic pollutants under visible light irradiation
CN108355702B (en) Graphite-phase carbon nitride photocatalyst with large specific surface area carbon deposition defects and preparation method and application thereof
CN109331860B (en) Low-platinum alloy composite nano photocatalyst for air purification and preparation method and application thereof
CN108067281A (en) Porous g-C3N4Photochemical catalyst and its preparation method and application
CN112892521A (en) Oxygen-enriched vacancy echinoid tungsten oxide and preparation method and application thereof
CN114392762B (en) Composite material based on two-dimensional MXene nano structure and preparation method thereof
WO2019076090A1 (en) Supported vocs catalytic combustion catalyst and preparation method therefor
CN109569673B (en) Preparation method of defect BiOI-BiOBr composite photocatalytic material with excellent photocatalytic performance
CN112076738A (en) Boron-doped defective zinc oxide and preparation method and application thereof
CN112958134A (en) Ag modified N-doped porous carbon loaded TiO2Composite material and method of making
CN112473712A (en) CeO treated with different atmospheres2/g-C3N4Heterojunction material, preparation method and application thereof
CN112758927A (en) Preparation method of tea stem-based activated carbon with high specific surface area
CN106975509B (en) Preparation method and application of nitrogen and iron co-doped bismuth vanadate visible-light-driven photocatalyst
CN114849680A (en) Catalyst and preparation method and application thereof
KR100966300B1 (en) Visible Rays Active Titanium Dioxide Codoped Carbon, Nitrogen, Boron, Fluorine and Manufacturing Method Thereof
CN113967481B (en) Spherical MoP-HCCN-like composite photocatalyst and preparation method and application thereof
CN109158117B (en) Full-spectrum-response double-doped lanthanum fluoride/attapulgite up-conversion composite photocatalytic material and preparation method and application thereof
CN113275030A (en) Preparation method of ordered mesoporous carbon and carbon nitride composite material
CN110252375B (en) Iron, nitrogen and cobalt co-doped titanium dioxide/activated carbon compound, preparation method and application as photocatalyst
CN113117660A (en) Cotton carbon fiber monolithic catalyst and preparation method and application thereof
CN113289661B (en) Dual-polarization site co-modified carbon nitride photocatalyst and preparation method thereof
CN111330626A (en) Processing technology of semiconductor photocatalyst material
CN111250115B (en) Preparation method and product of flower-ball-shaped bismuth oxyiodide-titanium dioxide heterojunction photocatalyst

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20210820