CN109569691B - Preparation method of boron-doped carbon nitride, product and application thereof - Google Patents
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 32
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002243 precursor Substances 0.000 claims abstract description 27
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004327 boric acid Substances 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 239000004098 Tetracycline Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000001782 photodegradation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229960002180 tetracycline Drugs 0.000 claims description 2
- 229930101283 tetracycline Natural products 0.000 claims description 2
- 235000019364 tetracycline Nutrition 0.000 claims description 2
- 150000003522 tetracyclines Chemical class 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052796 boron Inorganic materials 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract description 2
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- 241000446313 Lamella Species 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
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- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 231100000317 environmental toxin Toxicity 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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- 239000003607 modifier Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- -1 sodium tetraphenylborate Chemical compound 0.000 description 1
- 230000009466 transformation Effects 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
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention relates to a preparation method of boron-doped carbon nitride and a product and application thereof.A mode of carrying out hydrothermal reaction on melamine and boric acid promotes boron atoms and melamine to carry out chemical reaction so that boron and carbon nitrogen elements form atomic-level mixing on one hand, and carries out hydrothermal reaction on the melamine in an acid environment so that the melamine can form a supermolecular structure, which is beneficial to the separation of a carbon nitride lamellar structure in the subsequent roasting process; and then roasting the precursor synthesized by the reaction to prepare the boron-doped carbon nitride which is uniformly doped and has a thinner lamellar structure. The boron-doped carbon nitride prepared by the method has the advantages of uniform element doping, thinner lamella, better photocatalytic performance, simple preparation operation and lower difficulty, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to a preparation method of boron-doped carbon nitride, a product and application thereof.
Background
Energy crisis and environmental pollution are two major strategic problems in the sustainable development of human society. With the increasing exhaustion of traditional fossil energy sources such as coal, oil, natural gas and the like and a series of environmental problems brought about in the use process, the problems in the fields of purification and control of water and air are urgent and important for the effective utilization of clean energy sources. The photocatalysis process can convert solar energy into chemical energy, and the photocatalytic oxidation reduction reaction is used for realizing the decomposition, degradation and mineralization of environmental toxins, so that the photocatalysis water treatment system has the advantages of stability, high efficiency, no pollution and the like. Therefore, the photocatalytic technology taking the photocatalytic material as the core has very important significance for China in the key period of economic and social transformation.
The polymer semiconductor carbon nitride as a novel nonmetal visible light photocatalyst has the characteristics of unique electronic structure, visible light catalytic activity, good chemical and thermal stability, no toxicity, simple and easy preparation, no metal and the like, but the catalytic activity of the carbon nitride is limited due to the high recombination rate of photoinduced electron-hole pairs, so that the photocatalytic activity is improved by modifying and modifying the photocatalyst in a proper mode, and a visible light response, high-efficiency and stable photocatalytic material is developed.
To improve this disadvantage, doping is now often used to improve the electronic structure and surface properties. After doping, the electronic structure is changed, and the doping elements and the original molecular orbit of the carbon nitride undergo orbital hybridization, so that the energy band structure, the electronic structure and the optical property of the carbon nitride are changed. Research shows that the efficiency of photocatalytic hydrogen production by adopting boron-doped carbon nitride can reach 4.3 times of that before doping, and the boron-doped carbon nitride has good capability of degrading organic dye rhodamine B and shows good light stability. However, the doping preparation method adopted at present is generally prepared by mechanically mixing a carbon nitride precursor with a boron-containing substance in a solid phase and then baking the mixture. For example, urea is used as a precursor, sodium tetraphenylborate is used as a boron-doped source, and boron-doped carbon nitride is prepared by mechanical ball milling, mixing and roasting; also, melamine is used as a precursor, sodium borohydride is used as a boron source and mechanically mixed with the melamine, and then the mixture is roasted to prepare boron-doped carbon nitride; the boron-doped carbon nitride prepared by the methods has the problem of doping uniformity and further influences the photocatalytic performance of the boron-doped carbon nitride. For example, some have prepared more uniformly boron-doped carbon nitride by liquid phase doping, and the photocatalytic hydrogen production efficiency is 2.5 times that of the simple doping, which indicates that the hydrogen production efficiency can be further greatly improved by more uniformly doping the elements, but the above-mentioned liquid phase doping introduces other substances as surface charge modifiers, which introduces impurities on the one hand, and on the other hand, the element doping is not particularly uniform, but is more uniform relative to the solid phase doping.
Disclosure of Invention
Aiming at the defect of uneven element doping in the existing preparation of boron-doped carbon nitride, the invention aims to provide a preparation method of boron-doped carbon nitride.
Yet another object of the present invention is to: provides a boron-doped carbon nitride product prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of boron-doped carbon nitride comprises the following steps of carrying out hydrothermal reaction on melamine and boric acid, and then roasting a precursor synthesized by the reaction to prepare the boron-doped carbon nitride which is uniformly doped and has a thinner lamellar structure, wherein the preparation method comprises the following steps:
1) weighing melamine/boric acid/water according to a mass ratio of (0.01-1) to (5-100), firstly adding melamine, boric acid and water into a hydrothermal reaction kettle, uniformly stirring, then putting into an oven for hydrothermal reaction, and then filtering, washing and vacuum-drying a product to obtain a precursor;
2) and grinding and crushing the obtained precursor, then putting the precursor into a crucible, heating the precursor to 400-600 ℃ in a muffle furnace at a heating rate of 2.5 ℃/min, and preserving the heat for 1-5 hours to obtain powder, namely the boron-doped carbon nitride.
The mechanism of the invention is as follows: the method is characterized in that a hydrothermal reaction mode is carried out on melamine and boric acid, so that on one hand, boron atoms and melamine are promoted to carry out a chemical reaction, and boron and carbon nitrogen elements form atomic-level mixing; on the other hand, the melamine is subjected to hydrothermal treatment in an acid environment, so that a supermolecular structure can be formed, and the separation of a carbon nitride lamellar structure in the subsequent roasting process is facilitated.
The hydrothermal reaction temperature is 100-200 ℃, and the reaction time is 1-12 hours.
The invention also provides boron-doped carbon nitride, which is prepared according to the method.
In addition, the invention also provides application of the boron-doped carbon nitride as a catalyst in the tetracycline photodegradation reaction.
The method can prepare the boron-doped carbon nitride which is uniformly doped and has a thinner lamellar structure, and the boron-doped carbon nitride prepared by the method has the advantages of uniform element doping, thinner lamellar, better photocatalytic performance, simple preparation operation, lower difficulty and suitability for large-scale production.
Drawings
FIG. 1 scanning electron micrograph of boron doped carbon nitride;
figure 2 distribution of boron element in boron doped carbon nitride.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
A preparation method of boron-doped carbon nitride comprises the following steps of carrying out hydrothermal reaction on melamine and boric acid, and then roasting a precursor synthesized by the reaction to prepare the boron-doped carbon nitride which is uniformly doped and has a thinner lamellar structure, wherein the preparation method comprises the following steps:
accurately weighing melamine, boric acid and water, wherein the mass ratio of the melamine to the boric acid is 1:0.1, and the mass ratio of the melamine to the water is 1:50, firstly adding the melamine to the boric acid and the water into a hydrothermal reaction kettle, uniformly stirring, then putting into an oven, heating to a certain temperature (120 ℃) for reaction for a period of time (6 hours), and then filtering, washing and vacuum-drying the product to obtain a precursor;
and grinding and crushing the precursor, and then putting the ground precursor into a crucible for roasting, wherein the heating rate is 2.5 ℃/min, the final roasting temperature is 500 ℃, and the roasting time is 3 hours, so that the obtained powder is the boron-doped carbon nitride. A scanning electron micrograph of the product boron-doped carbon nitride is shown in figure 1. The distribution of boron in boron-doped carbon nitride is shown in fig. 2.
Example 2
A boron-doped carbon nitride prepared in a procedure similar to example 1, by the following steps:
accurately weighing melamine, boric acid and water (wherein the mass ratio of the melamine to the boric acid is 1:0.3, and the mass ratio of the melamine to the water is 1: 80), firstly adding the melamine to the boric acid and the water into a hydrothermal reaction kettle, uniformly stirring, then putting into an oven, heating to a certain temperature (180 ℃) for reaction for a period of time (5 hours), and then filtering, washing and vacuum-drying the product to obtain a precursor;
and grinding and crushing the precursor, and then putting the ground precursor into a crucible for roasting (wherein the heating rate is 2.5 ℃/min, the final roasting temperature is 550 ℃, and the roasting time is 4 hours), so that the obtained powder is the boron-doped carbon nitride.
Example 3
A boron-doped carbon nitride prepared in a procedure similar to example 1, by the following steps:
accurately weighing melamine, boric acid and water (wherein the mass ratio of the melamine to the boric acid is 1:0.05, and the mass ratio of the melamine to the water is 1: 80), firstly adding the melamine to the boric acid and the water into a hydrothermal reaction kettle, uniformly stirring, then putting into an oven, heating to a certain temperature (120 ℃) for reaction for a period of time (5 hours), and then filtering, washing and vacuum-drying the product to obtain a precursor;
and grinding and crushing the precursor, and then putting the ground precursor into a crucible for roasting (wherein the heating rate is 2.5 ℃/min, the final roasting temperature is 600 ℃, and the roasting time is 2 hours), so that the obtained powder is the boron-doped carbon nitride.
Example 4
A boron-doped carbon nitride prepared in a procedure similar to example 1, by the following steps:
accurately weighing melamine, boric acid and water (wherein the mass ratio of the melamine to the boric acid is 1:0.1, and the mass ratio of the melamine to the water is 1: 100), firstly adding the melamine to the boric acid and the water into a hydrothermal reaction kettle, uniformly stirring, then putting into an oven, heating to a certain temperature (150 ℃) for reaction for a period of time (8 hours), and then filtering, washing and vacuum-drying the product to obtain a precursor; and grinding and crushing the precursor, and then putting the ground precursor into a crucible for roasting (wherein the heating rate is 2.5 ℃/min, the final roasting temperature is 500 ℃, and the roasting time is 3 hours), so that the obtained powder is the boron-doped carbon nitride. The content of each element of the boron-doped carbon nitride is shown in an attached table:
Claims (3)
1. a preparation method of boron-doped carbon nitride is characterized in that melamine and boric acid are subjected to hydrothermal reaction, and then a precursor synthesized by the reaction is roasted to prepare the boron-doped carbon nitride which is uniformly doped and has a thinner lamellar structure, and comprises the following steps:
1) weighing melamine/boric acid/water according to a mass ratio of (0.01-1) to (5-100), firstly adding melamine, boric acid and water into a hydrothermal reaction kettle, uniformly stirring, then putting into an oven for hydrothermal reaction, and then filtering, washing and vacuum-drying a product to obtain a precursor;
2) grinding and crushing the obtained precursor, then putting the precursor into a crucible, heating the precursor to 400-600 ℃ in a muffle furnace at a heating rate of 2.5 ℃/min, and preserving the heat for 1-5 hours to obtain powder, namely boron-doped carbon nitride; wherein the content of the first and second substances,
the hydrothermal reaction temperature is 100-200 ℃, and the reaction time is 1-12 hours.
2. A boron-doped carbon nitride produced by the method of claim 1.
3. Use of the boron-doped carbon nitride of claim 2 as a catalyst in a photodegradation reaction of tetracycline.
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| CN114733543B (en) * | 2022-02-28 | 2023-05-30 | 山东大学 | Boron-modified carbon nitride material and preparation method and application thereof |
| CN114931964A (en) * | 2022-05-18 | 2022-08-23 | 扬州大学 | B doping with g-C 3 N 4 Application of catalyst in catalytic synthesis of dimethyl carbonate |
| CN115646530B (en) * | 2022-11-14 | 2023-12-12 | 吉林大学 | Double-promotion boron-doped accordion-shaped graphite carbon nitride photocatalyst and preparation method and application thereof |
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