CN113413902A - Novel MXene/TiO2/g-C3N4Method for preparing composite material - Google Patents

Novel MXene/TiO2/g-C3N4Method for preparing composite material Download PDF

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CN113413902A
CN113413902A CN202110696898.0A CN202110696898A CN113413902A CN 113413902 A CN113413902 A CN 113413902A CN 202110696898 A CN202110696898 A CN 202110696898A CN 113413902 A CN113413902 A CN 113413902A
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mxene
tio
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叶晓云
张玉梅
顾芳晓
王乾廷
吴益凡
陈龙
马立安
刘雪华
陈文哲
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Fujian University of Technology
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Abstract

The invention discloses a novel MXene/TiO2/g‑C3N4Composite material and method for making the same, where MXene comprises Mo2TiC3、Ti3C2、Ti2C、Nb2C and Nb4C3And the like. In g-C3N4And MXene as substrate, and preparing MXene/TiO by in-situ method2/g‑C3N4A composite material. The process comprises preparing g-C3N4With two-dimensional sheet material MXene, MXene and g-C3N4Adding tetrabutyl titanate, and then adding hydrofluoric acid and absolute ethyl alcohol to obtain MXene/TiO2/g‑C3N4A composite material. The preparation process adopted by the invention is simple, and the prepared mixed phase MXene/TiO2/g‑C3N4TiO in composite material2Distributed on the surface of MXene sheet layer in the form of microspheres, g-C3N4Distributed in TiO2The microsphere and the layered MXene surface enhance the charge separation efficiency of the composite material. The novel MXene/TiO2/g‑C3N4The composite material can be used as a catalyst material in the field of photocatalysis.

Description

Novel MXene/TiO2/g-C3N4Method for preparing composite material
Technical Field
The invention relates to a novel MXene/TiO2/g-C3N4A method for preparing a composite material.
Background
In recent years, with the rapid development of economy in China, the discharge of industrial wastewater and domestic sewage causes serious pollution to water resources, aggravates the shortage of water resources and seriously affects the normal life of people. Therefore, the development of an efficient and environment-friendly wastewater treatment technology to solve the problem of water pollution is urgently needed. In the process of exploring a novel degradation technology, the novel photocatalytic material is widely concerned due to the advantages of cleanness, safety, high efficiency and the like.
TiO2The photocatalyst has stable physical and chemical properties, is nontoxic and low in cost, and becomes one of the most representative semiconductor photocatalysts. But TiO 22The band gap of the optical waveguide is relatively wide (3.2 eV), and the optical response range is limited; meanwhile, the high recombination rate of the photo-generated electron-hole pairs also causes low photocatalytic efficiency. To improve the above disadvantages, the current research is mainly focused on TiO2Compounding with metal, metal oxide or other semiconductor to make it absorb red shift of edge and strengthen TiO2The absorption of visible light and the high-efficiency separation of electron-hole pairs are promoted to achieve the aim of improving the photocatalytic performance.
Transition metal carbide (MXene) materials are two-dimensional (2D) materials emerging in recent years, and abundant physicochemical properties are endowed by abundant elemental composition and structural adjustability and gradually emerge from the 2D materials. MXene has the chemical formula of Mn+1XnTx Wherein M is a transition metal (e.g., Ti, Zr, Hf, V, Nb, Ta, Cr, Sc, etc.), X is C or N (N is generally 1 to 3), and T is a surface group (e.g., -O, -OH, -F, etc.). Ti3C2As one of MXene materials, the surface of the MXene material possesses a large number of hydrophilic groups (-OH, -O, -F and the like), and the functional groups can help Ti3C2And a firm connection is constructed between the semiconductor material and the substrate. Further, Ti3C2Has excellent metal conductivity and can ensure effective carrier migration on the surface, which makes Ti3C2The catalyst has great application potential in the field of photocatalysis as a cocatalyst.
Graphite phase carbon nitride (g-C)3N4) The photocatalyst is a novel non-metal n-type semiconductor photocatalytic material, has great attention due to good chemical stability, easy regulation and control of structure and performance, unique two-dimensional layered structure and good visible light response, and is a photocatalyst with good prospect. However g-C by high temperature calcination3N4The photocatalyst has the defects of small specific surface area, too fast recombination of photon-generated carriers, narrow visible light absorption range, low quantum efficiency and the like, so that the photocatalytic performance of the photocatalyst is still defective. g-C3N4Has abundant surface groups, is suitable for being compounded with other photocatalytic materials to form a heterojunction, and is used for researching the influence of the heterojunction on the performance of the catalyst and the improvement of the photocatalytic efficiency.
Therefore, the invention uses tetrabutyl titanate as a Ti source and generates TiO with HF by a one-step hydrothermal method according to a certain proportion2Microsphere to prepare the three-component composite catalyst MXene/TiO2/g-C3N4. Compact heterojunction is formed among the components of the ternary composite catalyst, and the visible light catalysis performance is effectively improved under the combined action of a charge transfer mechanism and the characteristics of the photocatalytic semiconductor. The photocatalyst has certain potential and prospect in the field of photodegradation.
Disclosure of Invention
The technical problem to be solved by the invention is to provide MXene/TiO2/g-C3N4The composite material has obviously enhanced response to visible light, and the formation of heterojunction inside the material is favorable for charge transfer between catalysts and effective separation of electron-hole pairs.
In order to achieve the purpose, the invention adopts the following technical scheme:
novel MXene/TiO2/g-C3N4The preparation method of the composite material comprises the following steps: the method comprises the following steps:
(1) preparation of g-C3N4: heating melamine in a muffle furnace to obtain yellow powder, and then alternately cleaning and drying with deionized water and absolute ethyl alcohol to obtain g-C3N4Powder;
(2) preparing MXene: weighing a certain amount of MAX powder, etching by using an HF solution, cleaning by using clear water and absolute ethyl alcohol, and drying by using a vacuum oven to obtain MXene powder;
(3) preparation of MXene/TiO2/g-C3N4The composite material comprises the following components: mixing MXene powder with g-C3N4Placing the mixture and n-butyl titanate in polytetrafluoroethylene, adding HF and ethanol, performing ultrasonic thorough mixing, performing hydrothermal reaction, repeatedly cleaning the mixture by using acetone, deionized water and absolute ethyl alcohol, and drying the mixture in a drying oven to obtain MXene/TiO2/g-C3N4And (c) a complex.
Further, the calcination temperature in the step (1) is 550 ℃ and 600 ℃.
Further, in the step (1), the calcination is carried out for 2.5-5 ℃ min-1Heating for 2-6 hours.
Further, in the step (1), the sample is dried at a temperature of 50-80 ℃.
Further, MAX is Ti3AlC2、Nb2AlC、MoTiAlC3、Ti2AlC or Nb4AlC3One or a mixture of several of the powders. The MXene obtained comprises Mo2TiC3、Ti3C2、Ti2C、Nb2C and Nb4C3One or a mixture of several of them.
Further, in the step (2), the mass fraction of the HF solution is 40-49%, and the mass ratio of MAX to HF is 10.75-5: 1.
further, the etching temperature in the step (2) is 60 ℃, and the reaction time is 24 h.
Further, MXene and g-C in the step (3)3N4The mass ratio is 1: 0 to 5.
Further, in the step (3), the mass fraction of the HF solution is 40-49%, and the volume ratio of the hydrofluoric acid solution to the tetrabutyl titanate is 1: 6.25.
Further, in the step (3), the volume ratio of the ethanol to the tetrabutyl titanate is 12: 1.
further, MXene/TiO obtained in step (3)2/g-C3N4The hydrothermal reaction temperature of the composite material is 80 ℃, and the time is 24 h.
The application also provides MXene/TiO2/g-C3N4The composite material is used as a photocatalyst.
The invention has the following advantages: the preparation process is simple and easy to regulate, the preparation raw materials are common and easy to obtain, and the cost is low. The composite material has good chemical stability, wide spectral absorption range and environmental friendliness, and is a clean catalytic material with potential value.
Drawings
Fig. 1 is an SEM image of a sample: (a) g-C3N4; (b) Ti3AlC2; (c) Ti3C2; (d) 0% TiO2/MXene/g-C3N4; (e) 10% TiO2/MXene/g-C3N4; (f) 20% TiO2/MXene/g-C3N4; (g) 30% TiO2/MXene/g-C3N4; (h) 40% TiO2/MXene/g-C3N4。
FIG. 2 shows 20% TiO2/MXene/g-C3N4EDS mapping plot of catalyst.
Figure 3 is an XRD pattern of the sample.
Fig. 4 is a graph of photocatalytic rate for the samples.
FIG. 5 is a plot of the apparent rate constants of samples: (a) 0% TiO2/MXene/g-C3N4; (b) 10% TiO2/MXene/g-C3N4; (c) 20% TiO2/MXene/g-C3N4; (d) 30% TiO2/MXene/g-C3N4; (e) 40% TiO2/MXene/g-C3N4。
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1
Heating melamine in a muffle furnace at 550 deg.C for 2 h at 2.5 deg.C for min-1Is prepared by washing yellow powder with deionized water and anhydrous ethanol for 3 times, and drying at 60 deg.C to obtain g-C3N4And (3) powder.
10 mL of 49% HF solution was weighed into polytetrafluoroethylene, and 1g of Ti was weighed3AlC2Slowly adding the powder, continuously stirring at 60 deg.C for 12 hr, washing the obtained powder with deionized water to pH of about 6-7, centrifuging with ethanol for three times, and drying in vacuum oven at 60 deg.C to obtain Ti3C2And (3) powder.
0.1428 g of Ti were taken3C2An appropriate amount of g-C3N4And 2.5 mL of n-butyl titanate are put into polytetrafluoroethylene, 0.4 mL of 49% HF is added, 30 mL of ethanol is added, ultrasonic treatment is carried out for 40 min, hydrothermal treatment is carried out for 80 ℃ and 24 h, and MXene/TiO is prepared2/g-C3N4Cleaning the sheet composite with acetone, deionized water and absolute ethyl alcohol for three times, and placing the sheet composite into a 60 ℃ ovenAnd (5) drying.
The other steps are not changed, and g-C is controlled3N4Were added in amounts of 0g, 0.079g, 0.178g, 0.306g and 0.476g, respectively, to give TiO2/MXene/ g-C3N4A composite photocatalyst is shown in Table 1.
Table 1 sample formulation table
Figure 810467DEST_PATH_IMAGE002
Note: t is the reaction temperature and T is the reaction time
Example 2
10 mL (49wt%) of HF solution was weighed into a Teflon reactor, and 1g of Nb was weighed2AlC（MoTiAlC3、Ti2AlC、Nb4AlC3) Slowly adding the powder into an HF solution, fully stirring, putting the powder into an oven, heating to 60 ℃, reacting for 24 hours, washing the obtained sample with deionized water until the pH value is about 7, centrifugally washing with ethanol for three times, and finally drying the powder in a vacuum oven at 60 ℃ for 24 hours to obtain MXene powder.
The other steps are not changed to prepare MXene/TiO2/g-C3N4A composite photocatalyst is provided.
g-C obtained in examples 1 to 23N4MXene and MXene/TiO2/ g-C3N4The compound was analyzed using a Field Emission Scanning Electron Microscope (FESEM), EDS spectrometer, X-ray diffractometer (XRD), ultraviolet-visible spectrophotometer (UV-vis). A photocatalytic degradation experiment is carried out by taking a rhodamine B solution as a target dye, and the photocatalytic activity of the rhodamine B solution is evaluated by measuring the absorbance through an ultraviolet-visible spectrophotometer. The specific test results are shown in FIGS. 1 to 4.
FIG. 1 shows g-C3N4、MXene、0% TiO2/MXene/g-C3N4、10% TiO2/MXene/g-C3N4、20% TiO2/MXene/g-C3N4、30% TiO2/MXene/g-C3N4、40% TiO2/MXene/g-C3N4SEM image of the sample. As can be seen from FIG. 1(a), g-C3N4Is an irregular particle consisting of a lamellar structure. From Ti3AlC2(FIG. 1(b)) Ti obtained by HF etching3C2The delamination was evident, and the whole was accordion-shaped (fig. 1 (c)). In the preparation process, in the presence of HF and Ti (OBu)4The volume ratio is 1: TiO formed under the condition of 6.252Agglomerated into a sphere and distributed in Ti3C2The periphery (FIG. 1 (d)). Adding g-C3N4Then, it can be seen that g-C is in the form of flakes3N4Dispersedly attached to TiO2Microspheres and Ti3C2Surface (FIG. 1 (e)), with g-C3N4Increased amount of added, microspherical TiO2Gradually decreasing (fig. 1 (f) - (h)). It is noteworthy that 40% TiO can be seen in FIG. 1(h)2/MXene/g-C3N4Little or no apparent microspherical TiO was observed in the samples2。
FIG. 2 shows 20% TiO2/MXene/g-C3N4EDS mapping map of (a). The elemental content and elemental surface distribution of the samples were analyzed by EDS spectrometer. As is clear from the figure, TiO2/MXene/g-C3N4Contains Ti, O, C, N and F elements, because of TiO2、Ti3C2And g-C3N4The surface of the material is mainly Ti, O, C and N elements. Wherein the F element is formed by etching MAX material by using HF as etchant to form a part of F end group Ti3C2Therefore, a small amount of F element is also present on the surface of the material.
FIG. 3 shows MXene and 0% TiO2/MXene/g-C3N4、10% TiO2/MXene/g-C3N4、20% TiO2/MXene/g-C3N4、30% TiO2/MXene/g-C3N4And 40% TiO2/MXene/g-C3N4XRD pattern of the sample. It can be seen that Ti3C2Characteristic peaks appear at 9.58 °, 18.30 °, 27.43 °, 35.94 °, 41.74 ° and 60.51 °, respectively corresponding to (002), (004), (101), (f) and (f)103) Crystal planes (105), (108), (109) and (110). The characteristic peaks appearing at 25.14 °, 37.55 °, 47.94 °, 54.83 °, 62.49 ° and 75.03 ° respectively correspond to anatase TiO2The (101), (004), (200), (105), (204), (215) crystal planes of (1). g-C3N4The characteristic peaks appearing at 13.17 ° and 23.40 ° correspond to the (100) and (002) crystal planes, respectively. Ti in all samples3C2And TiO2All the characteristic peaks of (a) are present and the peak intensity remains substantially unchanged. With g-C3N4Increase in amount of addition, g-C in sample3N4The characteristic peaks are also enhanced. At the same time, it can be observed that g-C3N4Is obviously stronger than Ti3C2And TiO2The characteristic peaks of (a) are much stronger.
FIG. 4 shows 0% TiO2/MXene/g-C3N4、10%TiO2/MXene/g-C3N4、20% TiO2/MXene/g-C3N4、30% TiO2/MXene/g-C3N4、40% TiO2/MXene/g-C3N4Graph of photocatalytic rate. 50 mL of 20mg/L RhB solution was degraded from 20mg of sample under visible light conditions. As can be seen, 20% TiO2/MXene/g-C3N4The degradation effect is optimal, and the degradation rate of the RhB reaches 95.6 percent in 120 min. And 0% TiO2/MXene/g-C3N4、10% TiO2/MXene/g-C3N4、30% TiO2/MXene/g-C3N4And 40% TiO2/MXene/g-C3N4The degradation rates at 120 min were 64.0%, 71.3%, 87.8% and 94.2%, respectively. It can be seen that g-C was not added during the preparation3N4The degradation effect of the catalyst on RhB was the worst. Compared with 0% TiO2/MXene/g-C3N4With g-C3N4In different proportions of TiO2/MXene/g-C3N4The degradation effect of the sample on RhB is improved to different degrees.
FIG. 5 is 0% TiO2/MXene/g-C3N4、10% TiO2/MXene/g-C3N4、20% TiO2/MXene/g-C3N4、30% TiO2/MXene/g-C3N4、40% TiO2/MXene/g-C3N4Is shown in the figure. To further analyze and compare the degradation rate of the catalyst to RhB in visible light, an apparent rate constant k was introduced to determine the photocatalytic activity of the sample. As shown with g-C3N4The apparent rate constant of the proportionally increasing catalyst exhibits a tendency to increase first and then decrease. Wherein 20% of TiO2/MXene/g-C3N4Has the largest apparent rate constant and the k value of 0.0235 h-1. Further evidence for 20% TiO2/MXene/g-C3N4The photocatalytic performance of the catalyst is best.
From the above characterization, it can be concluded that: ti3C2、g-C3N4With microspherical TiO2The photocatalytic performance of the system is enhanced by the compound. The heterojunction formed between the contact surfaces of the materials greatly improves the degradation rate of organic pollutants.
Although specific embodiments of the invention have been described above, it will be understood by those skilled in the art that the specific embodiments described are illustrative only and are not limiting upon the scope of the invention, and that equivalent modifications and variations can be made by those skilled in the art without departing from the spirit of the invention, which is to be limited only by the appended claims.

Claims (10)

1. Novel MXene/TiO2/g-C3N4The preparation method of the composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of g-C3N4: heating melamine in muffle furnace, cleaning the obtained yellow powder, and drying to obtain g-C3N4Powder;
(2) preparing MXene: weighing a certain amount of MAX powder, etching by using an HF solution, cleaning, and drying by using a vacuum oven to obtain MXene powder;
(3) preparation of MXene/TiO2/g-C3N4The composite material comprises the following components: mixing MXene powder with g-C3N4Placing the powder and tetrabutyl titanate in polytetrafluoroethylene, adding HF and ethanol, fully mixing, and generating TiO by a hydrothermal method2Cleaning and drying to obtain MXene/TiO2/g-C3N4A sheet composite.
2. The novel MXene/TiO according to claim 12/g-C3N4The preparation method of the composite material is characterized by comprising the following steps: the calcination temperature in the step (1) is 550-600 ℃, and the calcination temperature rise rate is 2.5-5 ℃ for min-1The calcination time is 2-6 h.
3. The novel MXene/TiO according to claim 12/g-C3N4The preparation method of the composite material is characterized by comprising the following steps: MAX is Ti3AlC2、Nb2AlC、MoTiAlC3、Ti2AlC or Nb4AlC3One or a mixture of several of the powders.
4. The novel MXene/TiO according to claim 12/g-C3N4The preparation method of the composite material is characterized by comprising the following steps: in the step (2), the mass fraction of the HF solution is 40-49%, and the mass ratio of MAX to HF is 10.75-5: 1.
5. the novel MXene/TiO according to claim 12/g-C3N4The preparation method of the composite material is characterized by comprising the following steps: the etching temperature in the step (2) is 60 ℃, and the reaction time is 24 h.
6. The novel MXene/TiO according to claim 12/g-C3N4The preparation method of the composite material is characterized by comprising the following steps: MXene and g-C in step (3)3N4The mass ratio is 1: 0 to 5.
7. The novel MXene/TiO according to claim 12/g-C3N4The preparation method of the composite material is characterized by comprising the following steps: in the step (3), the mass fraction of the HF solution is 40-49%, and the volume ratio of the hydrofluoric acid solution to the tetrabutyl titanate is 1: 6.25.
8. the novel MXene/TiO according to claim 12/g-C3N4The preparation method of the composite material is characterized by comprising the following steps: MXene/TiO obtained in step (3)2/g-C3N4The hydrothermal reaction temperature of the composite material is 80 ℃, and the time is 24 h.
9. The novel MXene/TiO according to any one of claims 1 to 82/g-C3N4MXene/TiO prepared by preparation method of composite material2/g-C3N4A composite material.
10. MXene/TiO according to any of claims 92/g-C3N4The composite material is used as a photocatalyst.
CN202110696898.0A 2021-06-23 2021-06-23 Novel MXene/TiO2/g-C3N4Method for preparing composite material Pending CN113413902A (en)

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CN115110115B (en) * 2022-07-11 2024-02-09 陕西科技大学 C, N co-doped TiO 2-based composite film photoelectrode and preparation method and application thereof

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