CN115722264B - Titanium dioxide/PFNBr composite photocatalyst, preparation method and application thereof - Google Patents
Titanium dioxide/PFNBr composite photocatalyst, preparation method and application thereof Download PDFInfo
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- CN115722264B CN115722264B CN202211449479.8A CN202211449479A CN115722264B CN 115722264 B CN115722264 B CN 115722264B CN 202211449479 A CN202211449479 A CN 202211449479A CN 115722264 B CN115722264 B CN 115722264B
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Abstract
The invention discloses a titanium dioxide/PFNBr composite photocatalyst, a preparation method and application thereof, relating to the technical field of photocatalyst preparation 2 Compounding, providing a hydrophilic TiO 2 The composite photocatalyst of PFNBr, which has the hydrophilicity of material maintained, makes conjugated polymer PFNBr wrap TiO by simple process 2 An inorganic-organic hybrid structure is formed, the photoresponse range of the material is expanded, and the recombination rate of photo-generated electrons and holes is reduced. The invention prepares TiO under the same condition 2 Composite photocatalyst of PFNBr and two single phases (TiO 2 PFNBr) photocatalytic degradation and hydrogen production performance were tested. The results show that the prepared TiO 2 The PFNBr composite photocatalyst is obviously superior to two single phases in the degradation and hydrogen production processes.
Description
Technical Field
The invention relates to the technical field of photocatalyst preparation, in particular to a titanium dioxide/PFNBr composite photocatalyst, a preparation method and application thereof.
Background
With the rapid development of society, the world is faced with two major crisis of environmental pollution and energy shortage. The photocatalysis technology utilizes organic photocatalyst hybridized inorganic photocatalyst to generate photo-generated electron-hole with higher redox capability under the irradiation of a specific light source so as to realize the realization of organic pollutantHigh degradation and hydrogen production efficiency, and has great prospect in the fields of environmental management and new energy exploration. TiO (titanium dioxide) 2 Titanium dioxide is used as the most representative n-type semiconductor photocatalyst, has good photocatalytic degradation performance of pollutants and hydrogen production under ultraviolet light, and has been widely paid attention to because of good photochemical stability, no secondary pollution and low cost. But TiO 2 The semiconductor material is a wide forbidden band (3.2 eV) semiconductor material, has weak response to visible light and low light energy utilization rate (only 5% of solar spectrum); at the same time TiO 2 Is easy to combine with photo-generated electron and hole and further limits TiO 2 Industrialization process.
For TiO 2 The modification of the metal-metal hybrid material becomes a key factor for improving the photocatalytic performance of the metal-hybrid material, the overall photocatalytic efficiency mainly depends on factors such as band gap, carrier separation and transmission, energy conversion and the like, and at present, methods such as morphology regulation, metal and nonmetal doping, heterojunction formation and the like are adopted, but the metal-hybrid material is used for TiO 2 The self performance of the light-sensitive element is limited, and the light response range is difficult to break through. Among the numerous modification methods, organic polymers are used for TiO 2 The surface modification is a mild, low-cost and sustainable surface functionalization method, and can be used as TiO 2 And the conjugated polymer has the advantages of adjustable spectrum and controllable main side chain.
TiO is reported in most of the literature 2 Adopts hydrophobic polymer, as Yang Lianli in patent CN 112588322A discloses a super-hydrophobic polymer/titanium-based photocatalysis aerogel block and a preparation method thereof, and in patent CN 112920382A, rain hiding and the like use in-situ polymerization composite TiO 2 And efficient broadening of TiO of conjugated microporous polymers 2 Band gap, the photocatalytic effect is improved, but the band gap can prevent conjugated polymer and TiO to a certain extent 2 Compounding and contacting the surface of the catalyst with pollutants, active substances and the like in a reaction system; as disclosed in patent CN 113634279A, an Ag/TiO 2 The preparation of the PANI photocatalyst effectively improves the adsorptivity and photocatalytic degradation efficiency of the material, but noble metal is introduced in the preparation process; as disclosed in patent CN 111495343A, a TiO 2 Grafted polyacrylic acid hydrogel adsorptionThe degradation material endows the polyacrylic acid-based hydrogel with excellent photocatalytic degradation performance, but the preparation process of the method is complex and the energy consumption is high; as patent CN 111589472A discloses TiO 2 Carboxyl-containing conjugated microporous polymer/TiO 2 The preparation method of the composite material has overlong reaction time and is not beneficial to popularization and application. Based on the method, a photocatalysis composite material which is simple in synthesis, low in energy consumption, good in photocatalysis degradation and hydrogen production performance and free from uneconomical noble metal is designed, and has research significance.
Disclosure of Invention
The invention aims at the prior art that the organic conjugated polymer and the inorganic material TiO 2 Is not easy to compound, is difficult to contact with target pollutants and active substances, and has complex preparation process. Provides a preparation method which is simple and uses TiO 2 Titanium dioxide/PFNBr (TiO) materials that are matched with hydrophilic polymers in terms of both valence and energy bands, widening the photoresponse range 2 PFNBr) and can be applied to the fields of degradation, hydrogen production and other photocatalysis.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a preparation method of a titanium dioxide/PFNBr composite photocatalyst, which comprises the following steps:
step (1) dissolving PFNBr:
adding a hydrophilic conjugated polymer PFNBr into methanol, heating at the boiling point of the methanol, and obtaining a solution after the PFNBr is completely dissolved;
step (2) preparing TiO 2 PFNBr photocatalyst:
TiO is mixed with 2 Dispersing in the solution obtained in the step (1), carrying out ultrasonic treatment, stirring and reduced pressure distillation to obtain the titanium dioxide/PFNBr composite photocatalyst.
Further, the TiO 2 The preparation method of the PFNBr composite photocatalyst comprises the following steps:
step (1) dissolving PFNBr:
PFNBr is added into a flat-bottomed flask, methanol (20-40 mL) is poured into the flask, and the flask is heated under the boiling point of the methanol until the PFNBr is completely dissolved, so as to obtain a solution;
step (2) preparing TiO 2 PFNBr composite photocatalyst:
will purchase the resulting TiO 2 Dispersing in the solution formed in (1), sealing the flat-bottom flask with sealing film, stirring for at least 1 hr after ultrasonic treatment, and distilling at 50deg.C under reduced pressure to obtain TiO 2 PFNBr composite photocatalyst.
Further, tiO 2 And PFNBr is 10: (0-10), tiO 2 The amount of (2) is not 0.
Further, in the step (1), the ultrasonic time is 10-40 min, and the stirring time is 1-3 h.
TiO prepared by the preparation method 2 PFNBr composite photocatalyst.
The TiO 2 Use of a PFNBr composite photocatalyst in degrading a contaminant.
In the process of degrading pollutants, tiO 2 The PFNBr composite photocatalyst is placed in an aqueous solution of target pollutants, stirred in a dark place to ensure that the target pollutants reach adsorption and desorption equilibrium, and irradiated for a period of time under visible light to degrade the target pollutants. The illumination time is 0.5-2 h, and TiO 2 The dosage of the PFNBr composite photocatalyst in the aqueous solution of the target pollutant is 0.4-1g/L.
To test TiO 2 Degradation performance of PFNBr composite photocatalyst on pollutants, the invention uses TiO 2 Adding the PFNBr composite photocatalyst into the prepared target pollutant (RhB) wastewater solution, stirring for 30min in a dark place to reach adsorption and desorption equilibrium, irradiating for a period of time under visible light to degrade the target pollutant, taking 3mL of supernatant at intervals, and centrifuging for 10min. Spectrophotometry was used to test the absorbance of the contaminant stock solution and the supernatant removed for each time period. The illumination time is 0.5-2 h, and the mass concentration of the prepared wastewater solution containing the target pollutant (RhB) is 10-80 mg.L -1 ，TiO 2 The dosage of the PFNBr composite photocatalyst in the aqueous solution of the target pollutant is 0.4-1g/L.
The titanium dioxide/PFNBr composite photocatalyst is applied to hydrogen production.
In the hydrogen production process of the titanium dioxide/PFNBr composite photocatalyst, the titanium dioxide/PFNBr composite photocatalyst is placed in a photocatalytic reaction tank, 20mL of triethanolamine is added as a sacrificial agent, 80mL of water is added, a xenon lamp light source with a 360nm cut-off filter is used for limiting the illumination wavelength range to be lambda not less than 360nm, carrier gas is argon, a hydrogen production experiment is carried out for 5 hours, and data of hydrogen in the system are collected every 1 hour.
The invention discloses the following technical effects:
the invention uses organic conjugated polymer PFNBr and inorganic material TiO 2 Compounding, providing a hydrophilic TiO 2 The composite photocatalyst of PFNBr, which has the hydrophilicity of material maintained, makes conjugated polymer PFNBr wrap TiO by simple process 2 An inorganic-organic hybridized core-shell structure is formed, the photoresponse range of the material is expanded, and the recombination rate of photo-generated electrons and holes is reduced. The invention prepares TiO under the same condition 2 Composite photocatalyst of PFNBr and two single phases (TiO 2 PFNBr) photocatalytic degradation and hydrogen production performance were tested. The results show that the prepared TiO 2 The PFNBr composite photocatalyst is obviously superior to two single phases in the degradation and hydrogen production processes.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a preparation process of the hydrophilic conjugated polymer PFNBr composite titanium dioxide-based photocatalyst;
FIG. 2 is a TiO prepared in example 1 2 PFNBr and TiO 2 An XRD pattern of (b);
FIG. 3 is a TiO film prepared in example 2 2 N of PFNBr 2 Adsorption isotherms;
FIG. 4 is a TiO film prepared in example 3 2 /PFNBr、TiO 2 Infrared spectra with PFNBr;
FIG. 5 shows a real objectExample 2 TiO prepared 2 、TiO 2 A degradation effect diagram of PFNBr on target pollutants in water under an LED lamp;
FIG. 6 is a TiO film prepared in example 2 2 、TiO 2 Graph of photocatalytic hydrogen production effect of PFNBr under xenon lamp.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The preparation process flow chart of the hydrophilic conjugated polymer PFNBr composite titanium dioxide-based photocatalyst is shown in figure 1.
Room temperature in the present invention means 25±2℃.
Unless otherwise indicated, all materials used in the examples of the present invention were commercially available.
The PFNBr in the examples of the present invention was purchased from beggar teclmique, inc.
TiO in the embodiment of the invention 2 Purchased from Shanghai microphone Biochemical technologies Co.
Example 1
10mg of PFNBr was taken and dissolved in a flask containing 20mL of methanol by heating at the boiling point of methanol (64.5 ℃ C.), and 100mg of TiO purchased was added 2 Ultrasonic treating for 30min, adding magneton, sealing the flask with sealing film, stirring for 1 hr (stirring speed is 600 rpm/min), and vacuum distilling at 50deg.C to obtain TiO 2 /PFNBr。TiO 2 With TiO 2 The XRD pattern of the PFNBr is shown in FIG. 2, and the composite photocatalyst mainly shows TiO 2 Mainly because the conjugated polymer PFNBr assumes an amorphous state, tiO 2 Is anatase type.
Example 2
20mg of PFNBr was taken and dissolved in a flask containing 20mL of methanol by heating at the boiling point of methanol (64.5 ℃ C.), and 100mg of TiO purchased was added 2 Ultrasonic treating for 30min, adding magneton, sealing the flask with sealing film, stirring for 1 hr (stirring speed is 600 rpm/min), and vacuum distilling at 50deg.C to obtain TiO 2 /PFNBr。TiO 2 N of PFNBr 2 The adsorption isotherm is shown in figure 3, the specific surface area of the composite material is 135.3m 2 And/g, the average pore diameter is 3.0nm, which shows that the specific surface area of the material is large, the reactive sites are more, and the adsorption performance on target pollutants is good.
Example 3
20mg of PFNBr was charged into a 40mL flask containing methanol in the presence of methanolHeating to dissolve at boiling point (64.5 ℃ C.), adding 100mg of purchased TiO 2 Ultrasonic treating for 30min, adding magneton, sealing the flask with sealing film, stirring for 3 hr (stirring speed is 600 rpm/min), and vacuum distilling at 50deg.C to obtain TiO 2 /PFNBr，TiO 2 、TiO 2 The infrared spectrograms of the PFNBr and the PFNBr are shown in figure 4, the infrared curve displayed by the synthesized composite material mainly shows the functional group peak of the conjugated polymer PFNBr, and the Fourier infrared spectrogram mainly shows the functional group on the surface of the material, which shows that the PFNBr is successfully coated on the TiO 2 Is provided.
Example 4
20mg of PFNBr was taken and dissolved in a 20mL flask containing methanol by heating at the boiling point of methanol (64.5 ℃ C.), and 100mg of TiO purchased was added 2 Ultrasonic treating for 30min, adding magneton, sealing the flask with sealing film, stirring for 3 hr (stirring speed is 600 rpm/min), and vacuum distilling at 50deg.C to obtain TiO 2 /PFNBr。
Example 5
20mg of PFNBr was taken and dissolved in a 20mL flask containing methanol by heating at the boiling point of methanol (64.5 ℃ C.), and 100mg of TiO purchased was added 2 Ultrasonic treating for 10min, adding magneton, sealing with sealing film, stirring for 3 hr (stirring speed is 600 rpm/min), and vacuum distilling at 50deg.C to obtain TiO 2 /PFNBr。
Example 6
20mg of PFNBr was taken and dissolved in a 20mL flask containing methanol by heating at the boiling point of methanol (64.5 ℃ C.), and 100mg of TiO purchased was added 2 Ultrasonic treating for 30min, adding magneton, sealing with sealing film, stirring vigorously for 1 hr (stirring speed is 600 rpm/min), and distilling at 50deg.C under reduced pressure to obtain TiO 2 /PFNBr。
Application example 1
TiO prepared in example 2 2 PFNBr material, degradation performance study was performed as follows: the LED lamp is used as a visible light source, the catalyst dosage is 0.4g/L, and the concentration of 50mL prepared is 10mg.L -1 After adding the catalyst into the RhB aqueous solution, stirring for 0.5h in a dark place to make the RhB aqueous solution absorb and desorb the RhB aqueous solution in balance. Under the LED to performPhotocatalytic photoreaction. Taking 3mL of supernatant at intervals, and centrifuging for 10min. Spectrophotometry was used to test the absorbance of RhB stock solution and the supernatant removed. As shown in FIG. 5, the horizontal axis represents time, the vertical axis represents the content ratio of RhB in solution, the lower curve represents the time-varying curve of RhB in LED light degradation, in the degradation experiment, the RhB is degraded by using a better composite catalyst, the degradation rate is up to 100% and is TiO with the same time 2 Is 2.8 times as large as the above. The material of the invention has obvious degradation effect compared with pure titanium dioxide through comparison, and obviously, the TiO provided by the invention 2 The PFNBr photocatalyst has extremely high efficiency of photocatalytic degradation of RhB.
Application example 2
TiO prepared in example 2 2 PFNBr material, hydrogen production performance study is carried out, and the process is as follows: the xenon lamp is used as a hydrogen-producing light source, the wavelength range is lambda not less than 360nm, the catalyst addition amount is 0.2g/L, the sacrificial agent is 20mL, 80mL of water is added, the reaction tank is vacuumized, argon is used as carrier gas, and H generated in a gas chromatography detection system is used 2 Hydrogen production experiments were performed for 5 hours, and data for hydrogen in the system were collected every 1 hour. Example 2 TiO prepared 2 、TiO 2 The photo-catalytic hydrogen production effect graph of PFNBr under xenon lamp is shown in figure 6, the abscissa is time, the ordinate is hydrogen production, the upper curve is the time-dependent curve of hydrogen production of sample obtained by the method of the invention under xenon lamp by using triethanolamine as sacrificial agent, and the pure titanium dioxide is found to hardly produce hydrogen under near ultraviolet light of 360nm by comparison 2 The yield of PFNBr reaches 2037.5. Mu. Mol/g in 5 h.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (5)
1. The preparation method of the titanium dioxide/PFNBr composite photocatalyst is characterized by comprising the following steps of:
step (1) dissolving PFNBr:
adding PFNBr into methanol, heating at boiling point of methanol until PFNBr is completely dissolved to obtain solution;
step (2) preparing TiO 2 PFNBr photocatalyst:
TiO is mixed with 2 Dispersing the titanium dioxide/PFNBr composite photocatalyst in the solution obtained in the step (1), carrying out ultrasonic treatment, stirring and reduced pressure distillation to obtain the titanium dioxide/PFNBr composite photocatalyst;
TiO 2 and PFNBr is 10: (0-10), tiO 2 The amount of (2) is not 0.
2. The method according to claim 1, wherein in the step (2), the ultrasonic treatment time is 10 to 40 minutes and the stirring time is 1 to 3 hours.
3. A titanium dioxide/PFNBr composite photocatalyst prepared by the preparation method according to any one of claims 1 to 2.
4. Use of the titanium dioxide/PFNBr composite photocatalyst of claim 3 for degrading contaminants.
5. Use of the titanium dioxide/PFNBr composite photocatalyst of claim 3 in hydrogen production.
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| EP2314375A1 (en) * | 2001-12-21 | 2011-04-27 | Showa Denko K.K. | Photocatlyst particles comprising a condensed phosphate |
| US8158005B1 (en) * | 2007-11-02 | 2012-04-17 | University Of South Florida | Functional composites formed from colloidal polymer particles with photocatalytic metal oxide (MOx) nanoparticles |
| PL229796B1 (en) * | 2012-07-23 | 2018-08-31 | Splast Spólka Z Ograniczona Odpowiedzialnoscia Spólka Komandytowa | TiO<sub>2</sub> photocatalytic coating on the surfaces of polymer, sunlight activated, process for their preparation and the use thereof |
| CN102847558B (en) * | 2012-10-09 | 2014-02-26 | 河北科技大学 | Method for preparing conjugated polyene/nano titanium dioxide visible-light-induced photocatalyst by taking natural rubber as raw material |
| US10668458B2 (en) * | 2015-09-23 | 2020-06-02 | University Of Ulsan Foundation For Industry Cooperation | Photocatalyst having high visible-light activity |
| CN105618153B (en) * | 2015-12-28 | 2017-12-26 | 江南大学 | A kind of silicon titanium dioxide polypyrrole three-dimensional bionic composite and application based on level assembling |
| CN105772104B (en) * | 2016-04-21 | 2018-11-13 | 江苏朗逸环保科技有限公司 | A kind of composite photo-catalyst and preparation method thereof based on nano-titanium dioxide and cyclization polyacrylonitrile |
| CN107737945B (en) * | 2017-09-12 | 2020-07-31 | 南京邮电大学 | Synthetic method and application of composite nano gold particles |
| US20210171557A1 (en) * | 2019-12-10 | 2021-06-10 | Nutech Ventures | Wrapping perovskite grains with silica shells for improved stability and efficiency of perovskite electronic devices |
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