CN113304765B - Antimony nanosheet and graphite-like phase carbon nitride nanosheet composite material and preparation method thereof - Google Patents
Antimony nanosheet and graphite-like phase carbon nitride nanosheet composite material and preparation method thereof Download PDFInfo
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- CN113304765B CN113304765B CN202010118599.4A CN202010118599A CN113304765B CN 113304765 B CN113304765 B CN 113304765B CN 202010118599 A CN202010118599 A CN 202010118599A CN 113304765 B CN113304765 B CN 113304765B
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses an antimony nanosheet and graphite-like phase carbon nitride nanosheet composite material and a preparation method thereof. The material is formed by compounding antimony nano sheets and graphite-like phase carbon nitride in a mass ratio of 2.5: 100-10: 100, a soft chemical method is adopted to realize a sheet compounding process, and the performance of the catalytic material is modulated by controlling the content of Sb. The invention has the advantages of simple raw materials and process, uniform product and the like, and the material has better peroxidase-like property.
Description
Technical Field
The invention belongs to the field of catalytic materials, and particularly relates to a Sb-CN nanosheet composite material, a preparation method and application thereof.
Background
In recent years, the preparation and property research of antimony nanosheets are extensive, and the semiconductor nanomaterial refers to a superfine semiconductor material with a nanometer-scale grain size. Due to the characteristics of the nano material, the nano material plays an important role in the fields of photoelectricity, microelectronics, photocatalysis, sensors, detectors, biological photography and the like. Dresselhaus et al synthesized amorphous or polycrystalline Antimony Nanowires on porous anodized alumina templates using vapor deposition techniques and studied their transmission Properties (Heremans J, Thrush C M, Lin Y, et al, Transport Properties of inorganic Nanowires [ J ]. Phys Rev B, 2001, 63(8): 85406-. The Qiaetai group synthesized Antimony Nanotubes (Hu H, Mo M, Yang B, et al. A radial Synthesis-Reduction Route to analysis Nanotubes [ J ]. New J Chem, 2003, 27(8): 1161-.
The nano enzyme is a kind of existing nano materialThe material has unique performance and catalytic function. The nano enzyme has the characteristics of high catalytic efficiency, stability, economy and large-scale preparation, and is widely applied to the fields of medicine, chemical industry, food, agriculture, environment and the like. g-C 3 N 4 Has similar activity of peroxidase, and can be used in H 2 O 2 In the presence of the catalyst, the micromolecular chromogenic substrate 3,3 ', 5, 5' -tetramethyl benzidine (TMB) is subjected to color change reaction, so that the application range of the nano enzyme in the analysis field is expanded, and a new direction is provided for biomedical detection. As mentioned earlier, although g-C 3 N 4 Has application advantages in more and more fields, but due to the g-C obtained by the traditional preparation method 3 N 4 The specific surface area of the material is small, the recombination rate of current carriers is high, the catalytic efficiency is low, and the g-C is directly limited 3 N 4 The material is applied to future actual industrialization.
Disclosure of Invention
The invention aims to provide an Sb-CN nanosheet composite material and a preparation method thereof. The preparation method is simple in preparation process, the electron transmission capacity is enhanced, more reactive sites are provided by the compounding of the metal Sb nanosheets, and the prepared Sb-CN nanosheet composite material has good hydrogen peroxide catalysis performance.
The technical solution for realizing the purpose of the invention is as follows: an Sb-CN nanosheet composite material comprises antimony nanosheets and graphite-like phase carbon nitride (g-C) in a mass ratio of 2.5: 100-10: 100 (preferably 5: 100) 3 N 4 ) And compounding.
The preparation method of the Sb-CN nanosheet composite material comprises the following specific steps:
and 2, dropwise adding ultrapure water introduced with argon into the mixed solution, finally washing to be neutral, and drying in vacuum to finally obtain the Sb-CN nano sheet of the composite material.
Further, a concentrated sulfuric acid dispersion of antimony was obtained by placing antimony powder in concentrated sulfuric acid, stirring at 25 ℃ for 4 hours, and then standing for 30 min.
Further, the concentrated sulfuric acid dispersion of the graphite-like phase carbon nitride is obtained by placing the graphite-like phase carbon nitride in concentrated sulfuric acid, stirring at 25 ℃ for 4 hours, and then standing for 30 min.
Further, the mass ratio of antimony to the graphite-like phase carbon nitride is 2.5:100 to 10:100, preferably 5: 100.
Further, the argon gas in the ultra-pure water introduced with argon gas is saturated to remove dissolved oxygen in the water.
Further, ultrapure water introduced with argon is added dropwise to the mixed solution at 15-40 ℃.
Further, drying in vacuum at 25-45 ℃.
Compared with the prior art, the invention has the following advantages:
the Sb-CN nanosheet prepared by the invention has a simple preparation process, the electron transmission capability is enhanced, and more reactive sites are provided by compounding the metal Sb nanosheets.
The present invention is described in further detail below with reference to the attached drawing figures.
Drawings
FIG. 1 is an XRD pattern of Sb-CN nanosheet composites in different proportions.
FIG. 2 shows that Sb-CN nano-sheet composite materials with different proportions are activated by 10 mmol/L H 2 O 2 Performance comparison (color comparison of products after catalytic degradation).
FIG. 3 shows that different proportions of Sb-CN nano-sheet composite material activate different concentrations (10 mmol/L/5 mmol/L/1 mmol/L) of H 2 O 2 Comparative graph of catalytic performance.
Detailed Description
The invention is further elucidated with reference to the figures and embodiments.
The Sb-CN nanosheet composite material is prepared by the following steps:
(1) respectively dispersing 0.2g of antimony and 0.2g of graphite-phase carbon nitride by using 20mL of concentrated sulfuric acid, stirring for 4h at 25 ℃, and standing for 30 min;
(2) dropwise adding the concentrated sulfuric acid containing antimony in the step (1) into the concentrated sulfuric acid solution of the graphite-phase carbon nitride prepared in the step (1), and continuously stirring for 2 hours;
(3) and (3) at 25 ℃, dropwise adding 500mL of ultrapure water introduced with argon into the mixed solution obtained in the step (2), finally washing to be neutral, and drying in vacuum to finally obtain the Sb-CN nano sheet composite material.
Comparative example 1: preparation of CN nano-sheet composite material
(1) Dispersing 0.2g of graphite-phase carbon nitride by using 20mL of concentrated sulfuric acid, stirring for 4 hours at 25 ℃, and standing for 30 min;
(2) and (3) dropwise adding 500ml of ultrapure water introduced with argon into the solution obtained in the step (1), finally washing to be neutral at 25 ℃, and drying in vacuum to finally obtain the CN nanosheet.
Example 1: preparation of 2.5% Sb-CN nanosheet composite
(1) Respectively dispersing 0.2g of antimony and 0.2g of graphite-phase carbon nitride by using 20mL of concentrated sulfuric acid, stirring for 4 hours at 25 ℃, and standing for 30 min;
(2) dropwise adding 0.5mL of the concentrated sulfuric acid solution of antimony in the step (1) into 20mL of the concentrated sulfuric acid solution of graphite-phase carbon nitride prepared in the step (1), and continuously stirring for 2 hours;
(3) and (3) at 25 ℃, dropwise adding 500ml of ultrapure water introduced with argon into the mixed solution obtained in the step (2), finally washing to be neutral, and drying in vacuum to finally obtain the 2.5% Sb-CN nano sheet of the composite material.
Example 2: preparation of 5% Sb-CN nanosheet composite material
(1) Respectively dispersing 0.2g of antimony and 0.2g of graphite-phase carbon nitride by using 20mL of concentrated sulfuric acid, stirring for 4 hours at 25 ℃, and standing for 30 min;
(2) dropwise adding 1mL of the concentrated sulfuric acid solution of antimony in the step (1) into 20mL of the concentrated sulfuric acid solution of graphite-phase carbon nitride prepared in the step (1), and continuously stirring for 2 hours;
(3) and (3) at 25 ℃, dropwise adding 500ml of ultrapure water introduced with argon into the mixed solution obtained in the step (2), finally washing to be neutral, and drying in vacuum to finally obtain the 5% Sb-CN nano sheet of the composite material.
Example 3: preparation of 7.5% Sb-CN nanosheet composite material
(1) Respectively dispersing 0.2g of antimony and 0.2g of graphite-phase carbon nitride by using 20mL of concentrated sulfuric acid, stirring for 4 hours at 25 ℃, and standing for 30 min;
(2) dropwise adding 1.5mL of the concentrated sulfuric acid solution of antimony in the step (1) into 20mL of the concentrated sulfuric acid solution of graphite-phase carbon nitride prepared in the step (1), and continuously stirring for 2 hours;
(3) and (3) at 25 ℃, dropwise adding 500ml of ultrapure water introduced with argon into the mixed solution obtained in the step (2), finally washing to be neutral, and drying in vacuum to finally obtain the composite material 7.5% Sb-CN nano sheet.
Example 4: preparation of 10% Sb-CN nanosheet composite material
(1) Respectively dispersing 0.2g of antimony and 0.2g of graphite-phase carbon nitride by using 20mL of concentrated sulfuric acid, stirring for 4 hours at 25 ℃, and standing for 30 min;
(2) dropwise adding 2mL of the concentrated sulfuric acid solution of antimony in the step (1) into 20mL of the concentrated sulfuric acid solution of graphite-phase carbon nitride prepared in the step (1), and continuously stirring for 2 hours;
(3) and (3) at 25 ℃, dropwise adding 500ml of ultrapure water introduced with argon into the mixed solution obtained in the step (2), finally washing to be neutral, and drying in vacuum to finally obtain the composite material 10% Sb-CN nano sheet.
FIG. 1 is a comparison of the XRD patterns of the materials prepared in the comparative example and examples 1-4.
The Sb-CN nanosheet composite materials of examples 1-4 in different proportions are subjected to the same concentration H 2 O 2 The results of the catalytic degradation in the presence of (10 mmol/L) (color comparison of the products after catalytic degradation) are shown in FIG. 2. The result shows that when the composite material is 5% Sb-CN nano-sheet, the color of the product is the darkest, which indicates that the catalytic performance of the material is the best.
Sb-CN nano-sheet composite materials with different contrast ratios and different ratios of examples 1-4 at different concentrations of 10 mmol/L, 5 mmol/L and 1 mmol/LH 2 O 2 The results of the catalytic degradation in the presence of the catalyst (absorbance comparison of the product after catalytic degradation) are shown in FIG. 3. As a result, it was found that when the composite material had a definite timing, H 2 O 2 The higher the concentration, the higher the absorbance of the product, indicating H 2 O 2 In amounts which affect the catalytic properties of the material, H 2 O 2 The higher the content, the higher the catalytic performance of the material; when H is present 2 O 2 When the concentration is fixed, the absorbance of the product is highest when 5% of Sb-CN nano-sheets are used as enzyme, which indicates that the Sb-CN nano-sheets with different proportions have a certain concentration H 2 O 2 In the presence of the Sb-CN nanosheet composite material, the catalytic performance of the Sb-CN nanosheet composite material is different, and the Sb-CN nanosheet composite material with the content of 5% has strong catalytic performance compared with other composite materials.
The catalytic degradation process is as follows:
(1) in a 10 mL glass bottle, 100uL of Sb-CN composite material with the concentration of 10 mg/mL and different proportions and 100uL of H with different concentrations (10 mmol/L, 5 mmol/L and 1 mmol/L) are added 2 O 2 And 200 uL of Phosphate Buffered Saline (PBS) at a concentration of 10 mmol/L pH 4.0.
(2) To (1) was added 100uL of 3,3 ', 5, 5' -Tetramethylbenzidine (TMB) at a concentration of 10 mmol/L. The glass bottle was heated in a 37 ℃ water bath for 30 min.
(3) Centrifuging the substance in the glass bottle in (2) for 20 min.
(4) The supernatant after centrifugation in (3) was measured for absorbance at 652nm using a spectrophotometer.
Claims (11)
1. The antimony nanosheet and graphite-like phase carbon nitride nanosheet composite material is characterized by being compounded from antimony nanosheets and graphite-like phase carbon nitride in a mass ratio of 2.5: 100-10: 100;
the preparation method comprises the following steps:
step 1, dropwise adding the concentrated sulfuric acid dispersion liquid of antimony into the concentrated sulfuric acid dispersion liquid of graphite-like phase carbon nitride, and stirring for 2 hours;
and 2, dropwise adding ultrapure water introduced with argon into the mixed solution, finally washing to be neutral, and drying in vacuum to finally obtain the Sb-CN nanosheet of the composite material.
2. The antimony nanosheet and graphite-like phase carbon nitride nanosheet composite material is characterized by being compounded from antimony nanosheets and graphite-like phase carbon nitride in a mass ratio of 5: 100;
the preparation method comprises the following steps:
step 1, dropwise adding the concentrated sulfuric acid dispersion liquid of antimony into the concentrated sulfuric acid dispersion liquid of graphite-like phase carbon nitride, and stirring for 2 hours;
and 2, dropwise adding ultrapure water introduced with argon into the mixed solution, finally washing to be neutral, and drying in vacuum to finally obtain the Sb-CN nanosheet of the composite material.
3. A preparation method of an antimony nanosheet and graphite-like phase carbon nitride nanosheet composite material is characterized by comprising the following specific steps:
step 1, dropwise adding the concentrated sulfuric acid dispersion liquid of antimony into the concentrated sulfuric acid dispersion liquid of graphite-like phase carbon nitride, and stirring for 2 hours;
and 2, dropwise adding ultrapure water introduced with argon into the mixed solution, finally washing to be neutral, and drying in vacuum to finally obtain the Sb-CN nano sheet of the composite material.
4. A method according to claim 3, wherein the concentrated sulfuric acid dispersion of antimony is obtained by placing antimony powder in concentrated sulfuric acid, stirring for 4 hours at 25 ℃ and then standing for 30 min.
5. The method of claim 3, wherein the concentrated sulfuric acid dispersion of graphite-like phase carbon nitride is obtained by placing graphite-like phase carbon nitride in concentrated sulfuric acid, stirring at 25 ℃ for 4 hours, and then standing for 30 min.
6. The method of claim 3, wherein the mass ratio of antimony to graphite-like phase carbon nitride is 2.5:100 to 10: 100.
7. The method of claim 3, wherein the mass ratio of antimony to graphite-like phase carbon nitride is 5: 100.
8. The method of claim 3, wherein the argon in the argon-sparged ultrapure water is saturated.
9. The method according to claim 3, wherein ultrapure water to which argon is introduced is added dropwise to the mixed solution at 15 to 40 ℃.
10. The method of claim 3, wherein the drying is performed under vacuum at 25-45 ℃.
11. Use of a composite material according to claim 1 or 2 for catalysing the oxidation of a peroxide.
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| CN108424546A (en) * | 2018-02-14 | 2018-08-21 | 东华大学 | A kind of salt, preparation method and its application of hybrid modification phosphoric acid |
| CN110124687A (en) * | 2019-05-16 | 2019-08-16 | 北京化工大学 | A kind of preparation method of the LDH/rGO composite material of ruthenium doping and its application on evolving hydrogen reaction |
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Patent Citations (7)
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| CN105297133A (en) * | 2015-10-28 | 2016-02-03 | 南京理工大学 | Preparation method of single-crystal less-layer antimonene |
| CN107008486A (en) * | 2017-05-19 | 2017-08-04 | 西安工业大学 | A kind of preparation method of carbonitride/stibium doping stannic oxide hetero-junctions |
| CN108187718A (en) * | 2017-12-28 | 2018-06-22 | 江苏大学 | A kind of Preparation method and use of carbonitride/tantalic acid calcium potassium nanosheet composite material |
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| CN110371932A (en) * | 2018-04-12 | 2019-10-25 | 中国科学院化学研究所 | A kind of two-dimensional nano piece and its preparation method and application |
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