CN111939962A - Preparation method of iron-doped carbon nitride loaded zinc oxide composite photocatalyst - Google Patents
Preparation method of iron-doped carbon nitride loaded zinc oxide composite photocatalyst Download PDFInfo
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- CN111939962A CN111939962A CN202010909189.1A CN202010909189A CN111939962A CN 111939962 A CN111939962 A CN 111939962A CN 202010909189 A CN202010909189 A CN 202010909189A CN 111939962 A CN111939962 A CN 111939962A
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 55
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 27
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000008367 deionised water Substances 0.000 claims abstract description 30
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 30
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 22
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 17
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000919 ceramic Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 6
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 3
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000005303 weighing Methods 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- 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
-
- B01J35/39—
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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 discloses a preparation method of an iron-doped carbon nitride loaded zinc oxide composite photocatalyst, which is characterized by adding dicyandiamide into a solvent, heating and stirring the mixture to dissolve the dicyandiamide, adding ferric chloride into the mixture, and continuously stirring the mixture until deionized water is evaporated to dryness; cleaning and drying the prepared solid, grinding and crushing the solid, then putting the solid into a ceramic crucible with a cover for heating, preserving heat and roasting, and naturally cooling to obtain iron-doped carbon nitride; adding iron-doped carbon nitride into deionized water, performing ultrasonic treatment to uniformly disperse the iron-doped carbon nitride, adding zinc nitrate, heating the zinc nitrate, adding sodium hydroxide, and finally filtering, cleaning and drying to obtain a solid, namely the iron-doped carbon nitride loaded zinc oxide composite photocatalyst. The iron-doped carbon nitride loaded zinc oxide photocatalyst obtained by the invention has moderate forbidden band width, high light quantum efficiency, high separation efficiency of photo-generated electrons and charges and good effect of photocatalytic degradation of methylene blue; and the preparation process is simple, the yield is high, and the cost is low.
Description
Technical Field
The invention relates to a preparation method of an iron-doped carbon nitride loaded zinc oxide composite photocatalyst, belonging to the technical field of nano material preparation.
Background
With the development and progress of human society, people face two major problems of serious fossil energy shortage and environmental pollution. As is well known, the reserves of resources are not unlimited, and fossil energy is not only limited in reserves and expensive in exploitation, but also pollutes and destroys the ecological environment. Among various renewable energy sources, solar energy resources are favored because of their advantages of huge reserves, safe use, environmental protection, no geographical restrictions, and the like. The photocatalytic technology is a new technology which can utilize solar energy to purify the environment and convert energy and is rapidly developed in recent years. On one hand, low-density solar energy can be converted into high-density chemical energy through a photocatalytic technology, and on the other hand, various pollutants can be decomposed and bacteria and viruses can be killed through the photocatalytic technology. However, the existing photocatalytic materials have the defects of low quantum conversion efficiency and low solar energy utilization rate.
The graphite-like phase carbon nitride is a yellow nano crystal, has excellent optical and electrical properties due to the band gap of about 2.7eV, has rich sources, is easy to synthesize, has low cost and the like, attracts the attention of the world, and has important application prospect in the aspects of solving the problems of energy shortage, environmental pollution and the like. However, carbon nitride still has some problems, such as low utilization rate of visible light, easy recombination of photon-generated carriers, short lifetime, etc., which limit further improvement of carbon nitride performance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the existing carbon nitride photocatalyst has low catalytic efficiency.
In order to solve the technical problem, the invention provides a preparation method of an iron-doped carbon nitride loaded zinc oxide composite photocatalyst, which is characterized by comprising the following steps of:
step 1): adding dicyandiamide into a solvent, heating and stirring to dissolve dicyandiamide, adding ferric chloride, and continuously stirring until deionized water is evaporated to dryness;
step 2): cleaning and drying the solid prepared in the step 1), grinding and crushing, then putting the solid into a ceramic crucible with a cover for heating, keeping the temperature, roasting, and naturally cooling to prepare iron-doped carbon nitride;
step 3): adding the iron-doped carbon nitride prepared in the step 2) into deionized water, performing ultrasonic treatment to uniformly disperse the iron-doped carbon nitride, then adding zinc nitrate, heating the zinc nitrate, adding sodium hydroxide, and finally filtering, cleaning and drying to obtain a solid, namely the iron-doped carbon nitride loaded zinc oxide composite photocatalyst.
Preferably, the mass ratio of dicyandiamide to ferric chloride in the step 1) is 1 (0.001-1); the mass ratio of dicyandiamide to deionized water is 1 (0.1-50).
Preferably, the heating and stirring temperature in the step 1) is 50-100 ℃.
Preferably, the heating rate in the step 2) is 1-20 ℃/min; the roasting temperature is 400-650 ℃, and the roasting time is 0.1-15 h.
Preferably, the mass ratio of the iron-doped carbon nitride to the zinc nitrate in the step 3) is 1 (0.001-10); the mass ratio of the zinc nitrate to the sodium hydroxide is 1 (0.01-10); the mass ratio of the iron-doped carbon nitride to the deionized water is 1 (1-100).
Preferably, the heating temperature in the step 3) is 30-100 ℃.
Compared with non-metal element doping, because the outmost layer of metal ions has empty tracks and the outmost layer of single atoms in the carbon nitride has a large number of lone-pair electrons, the metal doping can enable the metal atoms to exist in gaps of the outmost layer of single atoms, the structure of the carbon nitride cannot be damaged, and the stability of the carbon nitride is improved. According to the invention, metal iron atoms are used as doping elements, so that on one hand, an electron acceptor can be provided, and the electronic structure of carbon nitride is changed, so that the energy band structure of the carbon nitride is changed, and the response to visible light is improved; on the other hand, different from the doping of other non-metal elements, the doping does not replace carbon and nitrogen atoms in the structure, so that the physical structure of the alloy is not changed, and the stability of the alloy is improved. The zinc oxide is loaded by the photocatalyst, so that the separation of photogenerated charges and electrons can be promoted, the existence time of the zinc oxide is prolonged, the photogenerated electrons and holes are more likely to react with pollutants, and the efficiency of degrading the dye by photocatalysis is improved.
The iron-doped carbon nitride loaded zinc oxide photocatalyst prepared by the preparation method provided by the invention has the advantages of moderate forbidden band width, high photon efficiency, high separation efficiency of photo-generated electrons and charges and good effect of photocatalytic degradation of methylene blue; and the preparation process is simple, the yield is high, the cost is low, and the method is suitable for large-scale popularization.
Drawings
FIG. 1 is an electron microscope image of the iron-doped carbon nitride-loaded zinc oxide composite photocatalyst prepared in example 1;
FIG. 2 is a graph showing the photocatalytic degradation efficiency of common zinc oxide on the market and the powder in each example.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
Weighing dicyandiamide, ferric chloride and deionized water (the addition amount of dicyandiamide is 10 g; the addition amount of ferric chloride is 1 g; and the addition amount of dicyandiamide is 70g), firstly adding dicyandiamide into deionized water, heating and stirring (80 ℃) to dissolve the dicyandiamide, then adding ferric chloride, and continuously stirring until the deionized water is evaporated to dryness; then, the prepared solid is washed, dried, ground and crushed, then put into a ceramic crucible with a cover to be heated (the heating rate is 2 ℃/min) to a certain temperature (500 ℃) for heat preservation and roasting for a period of time (3h), and the naturally cooled solid is the iron-doped carbon nitride; adding iron-doped carbon nitride into deionized water (the adding amount of the iron-doped carbon nitride is 1g, and the adding amount of the deionized water is 20g), and performing ultrasonic treatment to uniformly disperse the iron-doped carbon nitride. And then adding a certain amount of zinc nitrate (the addition amount of the zinc nitrate is 0.4g) into the solution, heating the solution to a certain temperature (80 ℃), adding a certain amount of sodium hydroxide (the addition amount of the sodium hydroxide is 0.5g), and then filtering, cleaning and drying to obtain a solid, namely the iron-doped carbon nitride loaded zinc oxide composite photocatalyst.
Example 2
Weighing dicyandiamide, ferric chloride and deionized water (the addition amount of dicyandiamide is 10g, the addition amount of ferric chloride is 0.5g and the addition amount of dicyandiamide is 30g), firstly adding dicyandiamide into deionized water, heating and stirring (95 ℃) to dissolve the dicyandiamide, then adding ferric chloride, and continuously stirring until the deionized water is evaporated to dryness; then, the prepared solid is washed, dried, ground and crushed, then put into a ceramic crucible with a cover to be heated (the heating rate is 5 ℃/min) to a certain temperature (650 ℃) for heat preservation and roasting for a period of time (5h), and the naturally cooled solid is the iron-doped carbon nitride; adding iron-doped carbon nitride into deionized water (the adding amount of the iron-doped carbon nitride is 1g, and the adding amount of the deionized water is 70g), and performing ultrasonic treatment to uniformly disperse the iron-doped carbon nitride. And then adding a certain amount of zinc nitrate (the addition amount of the zinc nitrate is 0.6g) into the solution, heating the solution to a certain temperature (90 ℃), adding a certain amount of sodium hydroxide (the addition amount of the sodium hydroxide is 0.4g), and then filtering, cleaning and drying to obtain a solid, namely the iron-doped carbon nitride loaded zinc oxide composite photocatalyst.
Example 3
Weighing dicyandiamide, ferric chloride and deionized water (the addition amount of dicyandiamide is 10g, the addition amount of ferric chloride is 2g and the addition amount of dicyandiamide is 50g), firstly adding dicyandiamide into deionized water, heating and stirring (75 ℃) to dissolve the dicyandiamide, then adding ferric chloride, and continuously stirring until the deionized water is evaporated to dryness; then, the prepared solid is washed, dried, ground and crushed, then put into a ceramic crucible with a cover to be heated (the heating rate is 10 ℃/min) to a certain temperature (550 ℃), and roasted for a period of time (2h), and the naturally cooled solid is iron-doped carbon nitride; adding iron-doped carbon nitride into deionized water (the adding amount of the iron-doped carbon nitride is 1g, and the adding amount of the deionized water is 30g), and performing ultrasonic treatment to uniformly disperse the iron-doped carbon nitride. And then adding a certain amount of zinc nitrate (the addition amount of the zinc nitrate is 0.2g) into the solution, heating the solution to a certain temperature (70 ℃), adding a certain amount of sodium hydroxide (the addition amount of the sodium hydroxide is 0.1g), and then filtering, cleaning and drying to obtain a solid, namely the iron-doped carbon nitride loaded zinc oxide composite photocatalyst.
Example 4
Weighing dicyandiamide, ferric chloride and deionized water (the addition amount of dicyandiamide is 10g, the addition amount of ferric chloride is 1.5g and the addition amount of dicyandiamide is 100g), firstly adding dicyandiamide into deionized water, heating and stirring (80 ℃) to dissolve the dicyandiamide, then adding ferric chloride, and continuously stirring until the deionized water is evaporated to dryness; then, the prepared solid is washed, dried, ground and crushed, then put into a ceramic crucible with a cover to be heated (the heating rate is 3 ℃/min) to a certain temperature (600 ℃) for heat preservation and roasting for a period of time (4h), and the naturally cooled solid is the iron-doped carbon nitride; adding iron-doped carbon nitride into deionized water (the adding amount of the iron-doped carbon nitride is 1g, and the adding amount of the deionized water is 50g), and performing ultrasonic treatment to uniformly disperse the iron-doped carbon nitride. And then adding a certain amount of zinc nitrate (the addition amount of the zinc nitrate is 1g) into the solution, heating the solution to a certain temperature (85 ℃), adding a certain amount of sodium hydroxide (the addition amount of the sodium hydroxide is 0.2g), and then filtering, cleaning and drying to obtain a solid, namely the iron-doped carbon nitride loaded zinc oxide composite photocatalyst.
The comparative data of the efficiency of the iron-doped carbon nitride-loaded zinc oxide composite photocatalyst prepared in examples 1-4 and the efficiency of the commercially available common zinc oxide for photocatalytic degradation of methylene blue are shown in table 1. The concentration of the dye methylene blue adopted in the photocatalytic degradation experiment is 20mg/L, the mass of the photocatalyst is 0.5g, the methylene blue degradation experiment is carried out under the irradiation of a 300W xenon lamp under the stirring condition, and the concentration of the methylene blue after degradation is measured by an ultraviolet visible absorption spectrum.
TABLE 1
| Sample numbering | The degradation rate% |
| Commercially available ordinary zinc oxide | 65.7 |
| Example 1 | 98.3 |
| Example 2 | 92.5 |
| Example 3 | 89.5 |
| Example 4 | 95.7 |
Claims (6)
1. A preparation method of an iron-doped carbon nitride loaded zinc oxide composite photocatalyst is characterized by comprising the following steps:
step 1): adding dicyandiamide into a solvent, heating and stirring to dissolve dicyandiamide, adding ferric chloride, and continuously stirring until deionized water is evaporated to dryness;
step 2): cleaning and drying the solid prepared in the step 1), grinding and crushing, then putting the solid into a ceramic crucible with a cover for heating, keeping the temperature, roasting, and naturally cooling to prepare iron-doped carbon nitride;
step 3): adding the iron-doped carbon nitride prepared in the step 2) into deionized water, performing ultrasonic treatment to uniformly disperse the iron-doped carbon nitride, then adding zinc nitrate, heating the zinc nitrate, adding sodium hydroxide, and finally filtering, cleaning and drying to obtain a solid, namely the iron-doped carbon nitride loaded zinc oxide composite photocatalyst.
2. The preparation method of the iron-doped carbon nitride-supported zinc oxide composite photocatalyst according to claim 1, wherein the mass ratio of dicyandiamide to ferric chloride in the step 1) is 1 (0.001-1); the mass ratio of dicyandiamide to deionized water is 1 (0.1-50).
3. The preparation method of the iron-doped carbon nitride-supported zinc oxide composite photocatalyst according to claim 1, wherein the heating and stirring temperature in the step 1) is 50-100 ℃.
4. The preparation method of the iron-doped carbon nitride-supported zinc oxide composite photocatalyst as claimed in claim 1, wherein the heating rate in the step 2) is 1-20 ℃/min; the roasting temperature is 400-650 ℃, and the roasting time is 0.1-15 h.
5. The preparation method of the iron-doped carbon nitride-supported zinc oxide composite photocatalyst according to claim 1, wherein the mass ratio of the iron-doped carbon nitride to the zinc nitrate in the step 3) is 1 (0.001-10);
the mass ratio of the zinc nitrate to the sodium hydroxide is 1 (0.01-10); the mass ratio of the iron-doped carbon nitride to the deionized water is 1 (1-100).
6. The preparation method of the iron-doped carbon nitride-supported zinc oxide composite photocatalyst according to claim 1, wherein the heating temperature in the step 3) is 30-100 ℃.
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| CN114308109A (en) * | 2022-01-27 | 2022-04-12 | 杭州师范大学 | ZnO/C-g-C3N4Photocatalyst, preparation method thereof and triclosan wastewater treatment method |
| CN115448266A (en) * | 2022-09-20 | 2022-12-09 | 安徽理工大学 | Preparation method of ferric oxide combined alpha and beta composite phase carbon nitride material |
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| CN112708394A (en) * | 2020-12-31 | 2021-04-27 | 东莞市深丰光电科技有限公司 | Coating glue, protective film and preparation method |
| CN114308109A (en) * | 2022-01-27 | 2022-04-12 | 杭州师范大学 | ZnO/C-g-C3N4Photocatalyst, preparation method thereof and triclosan wastewater treatment method |
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