CN113731390A - Spherical HCNs @ TiO2Preparation method of photocatalyst and application of photocatalyst in dye wastewater - Google Patents
Spherical HCNs @ TiO2Preparation method of photocatalyst and application of photocatalyst in dye wastewater Download PDFInfo
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- CN113731390A CN113731390A CN202111134153.1A CN202111134153A CN113731390A CN 113731390 A CN113731390 A CN 113731390A CN 202111134153 A CN202111134153 A CN 202111134153A CN 113731390 A CN113731390 A CN 113731390A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 239000002351 wastewater Substances 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000015556 catabolic process Effects 0.000 claims abstract description 17
- 238000006731 degradation reaction Methods 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001179 sorption measurement Methods 0.000 claims abstract description 10
- RYSXWUYLAWPLES-MTOQALJVSA-N (Z)-4-hydroxypent-3-en-2-one titanium Chemical compound [Ti].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O RYSXWUYLAWPLES-MTOQALJVSA-N 0.000 claims abstract description 9
- 238000010000 carbonizing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 5
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000010865 sewage Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 6
- 238000001354 calcination Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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Classifications
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
- B01J21/185—Carbon nanotubes
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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 the technical field of sewage treatment, in particular to spherical HCNs @ TiO2The preparation method of the photocatalyst and the application of the photocatalyst in dye wastewater comprise the following steps: step (1) of mixing Hollow Carbon Spheres (HCNs) and titanium acetylacetonate (Tio (acac)2) Mixing and dissolving in a solvent, and performing ultrasonic treatment for 30min to obtain a suspension A; step (2), stirring the suspension A obtained in the step (1) at 45 ℃ for 24h, and drying the obtained product in vacuum to obtain a product HCNs @ Tio (acac)2(ii) a Step (3), carbonizing the product obtained in the step (2) to obtain HCNs @ TiO2. The invention and commercial TiO2Compared with the prior art, the prepared spherical HCNs @ TiO2The degradation effect of the photocatalyst is better; the spherical HCNs @ TiO of the invention2Photocatalyst in liquid phase reactionThe composite material has good stability, can achieve the best photocatalytic activity while maintaining excellent adsorption performance, can efficiently treat the active red 3BS dye wastewater, and has remarkable photocatalytic effect; the preparation method is simple and easy to implement, convenient to operate, wide in raw material source and suitable for popularization and application.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to spherical HCNs @ TiO2A preparation method of the photocatalyst and application thereof in dye wastewater.
Background
In recent years, environmental problems caused by water pollution directly harm human health, and particularly, dye wastewater has the characteristics of deep chroma, high concentration, complex organic matter components and difficult treatment. There are several methods for degrading organic pollutants: electrochemical methods, biological decomposition methods, adsorption methods, physical sedimentation methods, photocatalytic oxidation methods, and the like. Through years of research, researchers find that a way of combining an adsorption method and a photocatalytic oxidation method has great significance for the research on the degradation of organic pollutants.
TiO2As a photocatalytic material, the photocatalyst has the characteristics of high catalytic efficiency, stable chemical property, no selectivity to target pollutants, thorough degradation, low cost, no toxicity and the like, and is widely applied to the field of sewage treatment. But due to TiO2The method has the defects of small particle size, difficult recovery, fast recombination of electron-hole pairs and the like. Thus, there is a need for TiO2And (4) carrying out modification. The Hollow Carbon Spheres (HCNs) have the advantages of large surface area, microporous structure, high adsorption capacity, high surface reaction activity and the like, so that the hollow carbon spheres have a good adsorption effect on the dye in the wastewater. Thus, TiO2As a better photocatalyst, the hollow carbon sphere is used as a good adsorbent, and the titanium acetylacetonate is used as a titanium source to be compounded with the hollow carbon sphere to prepare HCNs @ TiO2A photocatalyst. By the modification means, the adsorption performance and TiO of the hollow carbon spheres can be well exerted2Synergistic effect of photocatalysis.
Disclosure of Invention
Aiming at the problems, the invention provides spherical HCNs @ TiO2The photocatalyst has the advantages of wide raw material, simple preparation process, low cost and good catalytic degradation effect, and can be widely used for degrading organic dyes.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
spherical HCNs @ TiO2The preparation method of the photocatalyst comprises the following steps:
mixing and dissolving hollow carbon spheres and titanium acetylacetonate in a solvent, and performing ultrasonic treatment for 30min to obtain a suspension A;
step (2), stirring the suspension A obtained in the step (1) at 45 ℃ for 24h, and drying the obtained product in vacuum to obtain a product HCNs @ Tio (acac)2；
Step (3), carbonizing the product obtained in the step (2) to obtain HCNs @ TiO2。
Preferably, in the step (1), the solvent is absolute ethyl alcohol.
Preferably, in the step (1), the mass ratio of the hollow carbon spheres to the titanium acetylacetonate is 1 (5-15).
Preferably, in the step (3), the calcination is performed to 650 ℃.
By adopting the technical scheme, the spherical HCNs @ TiO2The preparation process of the photocatalyst is simple and convenient and is easy to adjust.
The invention also provides spherical HCNs @ TiO prepared by the preparation method2The application of the photocatalyst in dye sewage is applied to photocatalytic degradation of active red 3 BS.
Preferably, the spherical HCNs @ TiO is used2The photocatalyst is dispersed in a solution containing active red 3BS, dark adsorption is carried out until adsorption-desorption balance is achieved, and then degradation is carried out under the ultraviolet irradiation condition.
The invention has the beneficial effects that:
1. the invention and commercial TiO2Compared with the prior art, the prepared spherical HCNs @ TiO2The degradation effect of the photocatalyst is better.
2. The spherical HCNs @ TiO prepared by the invention2The photocatalyst has good stability in liquid phase reaction, can achieve the best photocatalytic activity while maintaining excellent adsorption performance, can efficiently treat the active red 3BS dye wastewater, and has remarkable photocatalytic effect.
3. The preparation method is simple and easy to implement, convenient to operate, wide in raw material source and suitable for popularization and application.
Drawings
FIG. 1 is a graph showing the degradation effects of different catalysts prepared in examples 1, 2, 3 and 4 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 accompanying drawings, so that those skilled in the art can better understand the advantages and features of the present invention, and thus the scope of the present invention is more clearly defined. The embodiments described herein are only a few embodiments of the present invention, rather than all embodiments, and all other embodiments that can be derived by one of ordinary skill in the art without inventive faculty based on the embodiments described herein are intended to fall within the scope of the present invention.
Example 1
And 2, stirring the suspension A at 45 ℃ for 24 hours, and then carrying out vacuum drying to obtain a solid.
Step 3, carbonizing the solid, calcining to 650 ℃ to obtain spherical HCNs @ TiO2A photocatalyst.
Step 4, taking 10mg of spherical HCNs @ TiO2The photocatalyst is dispersed in 100ml of active red 3BS (20mg/L) solution, magnetically stirred in the dark for 30min to reach adsorption-desorption equilibrium, then subjected to ultraviolet light degradation, an Abs value is measured every 15min, and a degradation effect curve is calculated and drawn, as shown in fig. 1.
Example 2
And 2, stirring the suspension A at 45 ℃ for 24 hours, and then carrying out vacuum drying to obtain a solid.
Step 3, carbonizing the solid, calcining to 650 ℃ to obtain spherical HCNs @ TiO2A photocatalyst.
Step 4, taking 10mg of spherical HCNs @ TiO2The photocatalyst is dispersed in 100ml of active red 3BS (20mg/L) solution, magnetically stirred in the dark for 30min to reach adsorption-desorption equilibrium, then subjected to ultraviolet light degradation, an Abs value is measured every 15min, and a degradation effect curve is calculated and drawn, as shown in fig. 1.
Example 3
And 2, stirring the suspension A at 45 ℃ for 24 hours, and then carrying out vacuum drying to obtain a solid.
Step 3, carbonizing the solid, calcining to 650 ℃ to obtain spherical HCNs @ TiO2A photocatalyst.
Step 4, taking 10mg of spherical HCNs @ TiO2The photocatalyst is dispersed in 100ml of active red 3BS (20mg/L) solution, magnetically stirred in the dark for 30min to reach adsorption-desorption equilibrium, then subjected to ultraviolet light degradation, an Abs value is measured every 15min, and a degradation effect curve is calculated and drawn, as shown in fig. 1.
Example 4
10mg of commercial TiO2 was dispersed in 100ml of active Red 3BS (20mg/L) solution, magnetically stirred in the dark for 30min to reach adsorption-desorption equilibrium, then subjected to ultraviolet light degradation, and Abs values were measured every 15min, and a degradation effect curve was calculated and plotted, as shown in FIG. 1.
It can be seen from the above examples 1, 2, 3 and 4 that the commercial TiO compounds are compatible with2Compared with the spherical HCNs @ TiO prepared by the invention2The degradation effect of the photocatalyst is better; the spherical HCNs @ TiO prepared by the invention2The photocatalyst has good stability in liquid phase reaction, can achieve the best photocatalytic activity while maintaining excellent adsorption performance, can efficiently treat the active red 3BS dye wastewater, and has remarkable photocatalytic effect; meanwhile, the preparation method is simple and easy to implement, convenient to operate, wide in raw material source and suitable for popularization and application.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (6)
1. Spherical HCNs @ TiO2The preparation method of the photocatalyst is characterized by comprising the following steps: the method comprises the following steps:
mixing and dissolving hollow carbon spheres and titanium acetylacetonate in a solvent, and performing ultrasonic treatment for 30min to obtain a suspension A;
step (2), stirring the suspension A obtained in the step (1) at 45 ℃ for 24h, and drying the obtained product in vacuum to obtain a product HCNs @ Tio (acac)2；
Step (3), carbonizing the product obtained in the step (2) to obtain HCNs @ TiO2。
2. A spherical HCNs @ TiO according to claim 12The preparation method of the photocatalyst is characterized by comprising the following steps: in the step (1), the solvent is absolute ethyl alcohol.
3. A spherical HCNs @ TiO according to claim 12The preparation method of the photocatalyst is characterized by comprising the following steps: in the step (1), the mass ratio of the hollow carbon spheres to the titanium acetylacetonate is 1 (5-15).
4. A spherical HCNs @ TiO according to claim 12The preparation method of the photocatalyst is characterized by comprising the following steps: in the step (3), the mixture is calcined to 650 ℃.
5. The application of the spherical HCNs @ TiO2 photocatalyst prepared by the preparation method according to claim 1 in dye wastewater is characterized in that: is applied to photocatalytic degradation of active red 3 BS.
6. Use according to claim 5, characterized in that: and dispersing the spherical HCNs @ TiO2 photocatalyst into a solution containing active red 3BS, carrying out dark adsorption until adsorption-desorption balance is achieved, and then carrying out degradation under the ultraviolet irradiation condition.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0614682A1 (en) * | 1993-03-11 | 1994-09-14 | Fuji Electric Co., Ltd. | Method for removing pollutants and purifying materials |
| CN101733087A (en) * | 2009-12-18 | 2010-06-16 | 南京大学 | Floating type TiO2/floating bead composite photochemical catalyst and preparation method and application thereof |
| CN105016526A (en) * | 2015-07-10 | 2015-11-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Photocatalysis-adsorption flocculation combining technique for organic waste water difficult to degrade |
| CN106040213A (en) * | 2016-05-26 | 2016-10-26 | 河海大学 | TiO2/CNCs composite photocatalyst and preparation method and application thereof |
| CN112973744A (en) * | 2021-02-03 | 2021-06-18 | 华北电力大学 | Novel photoelectric catalyst and preparation method thereof |
-
2021
- 2021-09-27 CN CN202111134153.1A patent/CN113731390A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0614682A1 (en) * | 1993-03-11 | 1994-09-14 | Fuji Electric Co., Ltd. | Method for removing pollutants and purifying materials |
| CN101733087A (en) * | 2009-12-18 | 2010-06-16 | 南京大学 | Floating type TiO2/floating bead composite photochemical catalyst and preparation method and application thereof |
| CN105016526A (en) * | 2015-07-10 | 2015-11-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Photocatalysis-adsorption flocculation combining technique for organic waste water difficult to degrade |
| CN106040213A (en) * | 2016-05-26 | 2016-10-26 | 河海大学 | TiO2/CNCs composite photocatalyst and preparation method and application thereof |
| CN112973744A (en) * | 2021-02-03 | 2021-06-18 | 华北电力大学 | Novel photoelectric catalyst and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 吴海培等: "二氧化钛/还原氧化石墨烯复合材料的制备及其光催化降解脱色性能", 《纺织学报》 * |
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