CN112915987A - TiO with formaldehyde degrading effect2@C3N4Photocatalyst and preparation method thereof - Google Patents
TiO with formaldehyde degrading effect2@C3N4Photocatalyst and preparation method thereof Download PDFInfo
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- CN112915987A CN112915987A CN202110106421.2A CN202110106421A CN112915987A CN 112915987 A CN112915987 A CN 112915987A CN 202110106421 A CN202110106421 A CN 202110106421A CN 112915987 A CN112915987 A CN 112915987A
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000000593 degrading effect Effects 0.000 title claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011858 nanopowder Substances 0.000 claims abstract description 18
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000001699 photocatalysis Effects 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 5
- 239000008139 complexing agent Substances 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- AVBJHQDHVYGQLS-AWEZNQCLSA-N (2s)-2-(dodecanoylamino)pentanedioic acid Chemical compound CCCCCCCCCCCC(=O)N[C@H](C(O)=O)CCC(O)=O AVBJHQDHVYGQLS-AWEZNQCLSA-N 0.000 claims description 2
- QUVMSYUGOKEMPX-UHFFFAOYSA-N 2-methylpropan-1-olate;titanium(4+) Chemical compound [Ti+4].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] QUVMSYUGOKEMPX-UHFFFAOYSA-N 0.000 claims description 2
- GRWPYGBKJYICOO-UHFFFAOYSA-N 2-methylpropan-2-olate;titanium(4+) Chemical compound [Ti+4].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] GRWPYGBKJYICOO-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 2
- 229920001732 Lignosulfonate Polymers 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 2
- -1 alkylbenzene sulfonate Chemical class 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- YEERRUXKIUHGRM-UHFFFAOYSA-N N.O.[Ti+4] Chemical compound N.O.[Ti+4] YEERRUXKIUHGRM-UHFFFAOYSA-N 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000007146 photocatalysis Methods 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 239000002135 nanosheet Substances 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 7
- 239000002131 composite material Substances 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- MRSOZKFBMQILFT-UHFFFAOYSA-L diazanium;oxalate;titanium(2+) Chemical compound [NH4+].[NH4+].[Ti+2].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O MRSOZKFBMQILFT-UHFFFAOYSA-L 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
Images
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/802—Visible light
Abstract
The invention provides TiO with formaldehyde degradation effect2@C3N4The preparation method of the nano-sheet comprises the following steps: firstly, mixing a titanium source compound, a carbon-nitrogen source compound and a complexing agent, crushing, sieving, calcining at the temperature of 450-600 ℃, grinding and crushing a calcined product to obtain TiO2@C3N4And (4) nano powder. Prepared TiO2@C3N4The nanometer powder can effectively utilize sunThe light provides short diffusion distance for charge transmission, and has good photoelectrochemistry and photocatalytic activity under visible light. Has larger application space in the field of solar energy conversion.
Description
Technical Field
The invention relates to the field of preparation of reinforced photoelectrochemical active materials, in particular to TiO2@C3N4Nanometer powder and its preparation method are provided.
Background
TiO2And C3N4The composite material has unique electron optical characteristics and wide application prospects in the fields of photocatalytic organic pollutant decomposition and the like, and people pay attention to the composite material, and the single material has general photoelectrochemical properties, so that the performance of the single material is unsatisfactory when the single material is applied to the field of solar photocatalytic organic matter decomposition, and the composite material capable of enhancing the photocatalytic activity is needed.
Among the various composite nanomaterials, TiO2Is particularly attractive due to appropriate gaps, large surface area and excellent chemical stability, has excellent potential for photocatalytic decomposition of organic substances, but has a narrow photoresponse range, so that TiO has good stability and good stability2The efficiency of the nanosheets is unsatisfactory, so C is3N4The nano-sheet and the nano-sheet are coupled to form the nano-composite material, which is an effective measure for improving the light conversion efficiency.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a TiO2@C3N4Method for preparing nano powder, prepared TiO2@C3N4The nano powder can effectively utilize sunlight and has excellent photocatalytic organic pollutant decomposing capacity.
In order to solve the problems, the invention provides TiO2@C3N4The preparation method of the nano powder comprises the following steps:
firstly, mixing a titanium source compound, a carbon nitrogen source compound and a coordination agent, crushing, and sieving with a 300-mesh and 500-mesh sieve;
calcining the screened material at the temperature of 500-570 ℃;
grinding and crushing the calcined product to obtain TiO2@C3N4A nanopowder powder.
Prepared TiO2@C3N4The nano powder can effectively utilize sunlight and has good photocatalytic activity under visible light.
The molar ratio of the titanium source compound to the carbon nitrogen source compound is 5: 10-100: 1-5.
The time of the calcination treatment is 1-6 hours.
The titanium source compound is selected from one or more of titanium tert-butoxide, titanium trichloride, titanium tetrachloride, ammonium titanyl oxalate, tetraisobutyl titanate, tetra-n-butyl titanate, titanium isopropoxide and titanyl sulfate.
The carbon and nitrogen source compound is selected from one or more of urea, dicyandiamide, melamine, cyanuric chloride and ammonium chloride.
The complexing agent is selected from one or more of lignosulfonate, heavy alkylbenzene sulfonate, alkyl sulfonate, hexadecyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, polyvinyl alcohol, disodium ethylene diamine tetraacetate, lauroyl glutamic acid, sodium octadecyl sulfate and fatty alcohol-polyoxyethylene ether sodium sulfate;
the TiO is2@C3N4The nanometer powder can utilize sunlight effectively and has excellent photocatalytic activity in visible light.
The preparation method provided by the invention has the advantages that the used equipment is simple, the batch production can be carried out only by the most common chemical raw materials, and the pollution degree of the products and the raw materials to the environment is low. And the product can effectively utilize sunlight and has good photocatalytic activity under visible light.
Drawings
FIG. 1 is an XRD pattern of a sample prepared according to example 1 of the present invention;
FIG. 2 is a high resolution TEM image of a sample prepared in example 1 of the present invention;
FIG. 3 is a graph showing the effect of photocatalytic degradation of formaldehyde on samples prepared in example 1 of the present invention;
FIG. 4 is a graph showing the effect of photocatalytic degradation of formaldehyde on samples prepared in example 2 of the present invention;
FIG. 5 is a graph showing the effect of photocatalytic degradation of formaldehyde on samples prepared in example 3 of the present invention;
FIG. 6 is a graph showing the effect of photocatalytic degradation of formaldehyde on samples prepared in example 4 of the present invention;
Detailed Description
To further illustrate the present invention, the following examples are provided to describe the preparation of the TiO2@ C3N4 nanopowder of the present invention in detail.
Examples
Detecting the obtained sample with X-ray diffractometer (model: Philips X' Pert PRO SUPER) to obtain X-ray diffraction pattern shown in figure 1, and determining the sample to be TiO2@C3N4And (3) nano materials.
The obtained sample was examined with a transmission electron microscope (model: JEOL-2010) to obtain a transmission electron microscope photograph as shown in FIG. 2, wherein FIG. 2 is a photograph of TiO provided in example 1 of the present invention2@C3N4Transmission electron micrograph (c). As can be seen from fig. 2: prepared by the implementation of C3N4Encapsulated TiO2。
The formaldehyde degradation effect of the obtained sample was measured by using a formaldehyde degradation test device (laboratory assembly setup device), and the results shown in fig. 3 were obtained. As can be seen in fig. 3: TiO prepared in example 12@C3N4The nanometer powder has good formaldehyde degrading effect.
The same identification and detection analyses as in example 1 were carried out on the samples obtained in examples 4 and 5, and it was confirmed that the obtained sample was TiO2The nano powder can realize certain photocatalytic activity and has a common formaldehyde degradation effect.
The same identification and detection analyses as in example 1 were carried out on the samples obtained in examples 2 and 3, and it was confirmed that the obtained sample was TiO2@C3N4Nano meterThe powder can realize high-efficiency photocatalytic activity and has good formaldehyde degradation effect.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (9)
1. TiO22@C3N4The preparation method of the nano powder is characterized by comprising the following steps:
mixing a titanium source compound, a carbon-nitrogen source compound and a coordination agent, crushing and sieving;
calcining the screened material at the temperature of 450-600 ℃;
grinding and crushing the calcined product to obtain TiO2@C3N4And (4) nano powder.
2. The TiO of claim 12@C3N4The preparation method of the nano powder is characterized in that the molar ratio of the titanium source compound to the carbon nitrogen source compound is 5: 10-100: 1-5.
3. The TiO of claim 12@C3N4The preparation method of the nano powder is characterized in that the sieving is a 300-mesh and 500-mesh sieving sieve.
4. The TiO of claim 12@C3N4The preparation method of the nano powder is characterized in that the calcining treatment time is 1-6 hours.
5. The TiO of claim 12@C3N4The preparation method of the nano powder is characterized in that the titanium source compound is selected from titanium tert-butoxide, titanium trichloride, titanium tetrachloride and titanium-oxygen ammonium oxalateOne or more of tetraisobutyl titanate, tetra-n-butyl titanate, titanium isopropoxide and titanyl sulfate.
6. The TiO of claim 12@C3N4The preparation method of the nano powder is characterized in that the carbon and nitrogen source compound is selected from one or more of urea, dicyandiamide, melamine, cyanuric chloride and ammonium chloride.
7. The TiO of claim 12@C3N4The preparation method of the nano powder is characterized in that the complexing agent is selected from one or more of lignosulfonate, heavy alkylbenzene sulfonate, alkyl sulfonate, hexadecyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, polyvinyl alcohol, disodium ethylene diamine tetraacetate, lauroyl glutamic acid, sodium octadecyl sulfate and sodium fatty alcohol-polyoxyethylene ether sulfate.
8. TiO produced by the production method according to any one of claims 1 to 72@C3N4And (4) nano powder.
9. TiO prepared according to the process of any one of claims 1 to 82@C3N4The nano powder is used for degrading formaldehyde through photocatalysis.
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| CN202110106421.2A CN112915987A (en) | 2021-01-26 | 2021-01-26 | TiO with formaldehyde degrading effect2@C3N4Photocatalyst and preparation method thereof |
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| CN202110106421.2A CN112915987A (en) | 2021-01-26 | 2021-01-26 | TiO with formaldehyde degrading effect2@C3N4Photocatalyst and preparation method thereof |
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Cited By (2)
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| CN114602526A (en) * | 2022-03-30 | 2022-06-10 | 中国科学技术大学先进技术研究院 | Preparation method of titanium nitride coated titanium dioxide nano material |
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