A novel urchin-like ordered carbon@iron composite material and a preparation method and application thereof

Abstract

The application provides a novel urchin-like ordered carbon@iron composite material and a preparation method and application thereof, and belongs to the technical field of carbon nanomaterials. The urchin-like silicon template is obtained by using triethanolamine, cetyltrimethylammonium bromide, sodium salicylate and tetraethyl silicate as raw materials, mixing and stirring, hydrothermal reaction, water washing and centrifugation, drying and calcination in an air atmosphere. Then, the silicon template is compounded with dopamine in a Tris solution, and stirring, ultrasonic treatment, standing in the dark, centrifugal drying are carried out to obtain a mesoporous silicon filled with polydopamine. The product is mixed with ferrocene in acetone, hydrogen peroxide solution is added, oil bath stirring is carried out until the solvent volatilizes, drying is carried out, and calcination is carried out in an inert atmosphere. Finally, the new urchin-like ordered carbon@iron composite material is obtained by alkaline solution refluxing, centrifugal drying treatment. The new urchin-like ordered carbon@iron composite material has excellent catalytic activity, and has a good application prospect in the fields of electrocatalysis, engineering materials, energy storage and conversion and the like.

Description

Technical Field

[0001] This invention relates to the field of carbon nanomaterials technology, specifically to a novel sea urchin-like ordered carbon@iron composite material, its preparation method, and its application. Background Technology

[0002] Carbon nanomaterials are abundant, possess excellent electrical conductivity, large and easily tunable specific surface area, high stability, high strength, and strong durability. They have attracted significant attention in fields such as engineering materials, electrocatalysis, environmental applications, and energy conversion, and are commonly used as catalyst supports, such as activated carbon, graphene, and carbon nanotubes. Researchers are continuously developing new carbon nanomaterials, leading to a growing and increasingly complex carbon nanomaterial family. Carbon nanocomposites not only possess tunable porous structures and surface chemistry but also offer numerous advantages as catalyst supports, such as easy reduction of the metallic phase, acid and alkali resistance, high-temperature stability, and low cost, indicating broad application prospects. In the field of engineering materials, carbon nanomaterials can be used to improve the compressive strength and wear resistance of concrete, plastic pipes, and other materials. With further research, the application prospects of carbon nanomaterials in engineering materials will become even broader.

[0003] Transition metals are abundant in the Earth's crust, readily available, and offer a significant cost advantage over precious metals, while also exhibiting good biocompatibility. Their unique electronic structure endows them with numerous active sites and excellent catalytic selectivity, effectively reducing reaction activation energy and enhancing catalytic efficiency. Furthermore, transition metals possess excellent electrical conductivity, enabling them to synergize with other materials, making them ideal alternatives to precious metal catalysts. They are widely used in organic synthesis, electrocatalysis, and other fields.

[0004] The structural advantages of carbon nanomaterials combined with the excellent catalytic properties of transition metals result in performance superior to other materials. The high specific surface area and porous structure of carbon materials inhibit metal particle agglomeration, improving their dispersibility and utilization; while transition metals enhance the electronic conductivity of composite materials and enrich the types of active sites. This combination not only improves the overall catalytic activity and selectivity of the material but also significantly enhances its structural stability and resistance to degradation, while retaining its low cost. It solves the problems of insufficient activity of single carbon materials and easy agglomeration of single metal particles, broadening its application scenarios in energy conversion, catalytic reactions, and engineering materials. Summary of the Invention

[0005] The purpose of this invention is to provide a novel sea urchin-like ordered carbon@iron composite material, its preparation method and application. This composite material exhibits superior performance in both electrocatalysis and engineering materials, and has great application potential.

[0006] This invention is implemented as follows:

[0007] A novel method for preparing sea urchin-like ordered carbon@iron composite materials includes the following steps:

[0008] (1) Dissolve triethanolamine in water, add hexadecyltrimethylammonium bromide and sodium salicylate, mix and stir, then place the solution in an oil bath and stir, then add tetraethyl silicate to the solution and continue stirring; then dry the reaction in a reaction vessel; after the reaction is completed, centrifuge, dry, and finally calcine to obtain a silicon template;

[0009] (2) Take the silicon template and dopamine from step (1) and dissolve them in Tris solution. After stirring, let it stand, then wash with water, centrifuge, and dry to obtain polydopamine-filled mesoporous silicon.

[0010] (3) Add the product from step (2) and ferrocene to acetone, stir evenly, then add hydrogen peroxide solution, stir in an oil bath until the solvent evaporates, wash the powder product with water, centrifuge, dry, and then calcine in an inert atmosphere.

[0011] (4) Add the calcined product from step (3) into a flask, place a magnetic ball in it, reflux it in an alkaline solution, centrifuge and dry it to obtain a novel sea urchin-shaped ordered carbon@iron composite material.

[0012] Preferably, in step (3), the mass ratio of the product to ferrocene in step (2) is 1:2 to 2:1.

[0013] Preferably, the calcination conditions in step (1) are: in an air atmosphere, at 500~600℃ for 5~8h.

[0014] Preferably, the resting conditions in step (2) are: resting in the dark for 20~36 hours.

[0015] Preferably, the calcination conditions in step (3) are: under an inert atmosphere, at 750~850℃ for 3~4 hours.

[0016] Preferably, the heating process during calcination in step (3) is as follows: heating for 450~500 min to 600℃, and then heating for 30~50 min to 750~850℃.

[0017] Preferably, the alkaline solution in step (4) is a sodium hydroxide solution, and the reflux time is 2-3 hours.

[0018] This invention also provides applications of the novel sea urchin-shaped ordered carbon@iron composite material prepared by the above method. Specifically, the novel sea urchin-shaped ordered carbon@iron composite material can be used as a catalyst in the detection of chloramphenicol, and can also be used as an admixture in the preparation of asphalt concrete.

[0019] The preparation method of this invention is environmentally friendly, has a high yield, and involves a mild reaction. The stepwise loading process, including stirring, evaporation, and calcination, loads iron onto ordered carbon, ultimately yielding a novel sea urchin-like ordered carbon@iron composite material. Iron doping enhances the interaction between electrons, generating additional electronic active sites, thereby improving electrocatalytic performance and enhancing the structural function of the composite material.

[0020] The novel sea urchin-like ordered carbon@iron composite material prepared by the method of this invention exhibits excellent electrocatalytic performance, showing a superior detection limit for chloramphenicol reaction, and possesses good stability, reproducibility, and anti-interference capabilities. Furthermore, this novel sea urchin-like ordered carbon@iron composite material can be widely applied in engineering construction. As an admixture in asphalt concrete, it can improve strength, wear resistance, and rutting resistance. Its high specific surface area, high stability, and thermal stability can enhance the sound absorption and noise reduction performance of asphalt pavements, and it also effectively promotes high-temperature ductility and low-temperature crack resistance.

[0021] This invention uses silicon as a soft template and employs a stepwise filling and loading process. Carbon source is filled into the silicon template via dopamine polymerization. Iron loading and material carbonization are simultaneously achieved through solvent evaporation and calcination. The reaction conditions are mild, the reagents used are inexpensive and readily available, and the preparation process is simple and controllable, effectively improving product yield and reducing production costs. The resulting composite material exhibits a unique sea urchin-like morphology, possessing high specific surface area, good stability, and mechanical strength. The synergistic effect of the carbon matrix and iron component endows it with excellent catalytic activity, showing promising application prospects in catalytic degradation, engineering materials, energy storage and conversion, and other fields. Attached Figure Description

[0022] Figure 1 This is a flowchart of the preparation method of the novel sea urchin-shaped ordered carbon@iron composite material of the present invention.

[0023] Figure 2 These are scanning electron microscope (SEM) images of the novel sea urchin-like ordered carbon@iron composite materials prepared in Examples 1-3 at scales of 100 nm and 500 nm; wherein, (A) and (D) are SEM images of the composite material prepared in Example 1, (B) and (E) are SEM images of the composite material prepared in Example 2, and (C) and (F) are SEM images of the composite material prepared in Example 3.

[0024] Figure 3 These are transmission electron microscope (TEM) images of the novel sea urchin-like ordered carbon@iron composite materials prepared in Examples 1-3 at scales of 50 nm and 100 nm; wherein, (A) and (D) are TEM images of the composite material prepared in Example 1, (B) and (E) are TEM images of the composite material prepared in Example 2, and (C) and (F) are TEM images of the composite material prepared in Example 3.

[0025] Figure 4 These are mapping images of the novel sea urchin-shaped ordered carbon@iron composite material prepared in Example 1 at a scale of 250 nm; where (A) is the corresponding transmission electron microscope image of the novel sea urchin-shaped ordered carbon@iron composite material, (B) is the mapping image of all elements, (C) is the mapping image of C element, (D) is the mapping image of N element, (E) is the mapping image of O element, and (F) is the mapping image of Fe element.

[0026] Figure 5 These are X-ray diffraction patterns of the novel sea urchin-shaped ordered carbon@iron composite materials prepared in Examples 1-3.

[0027] Figure 6 The X-ray photoelectron spectrum of the novel sea urchin-shaped ordered carbon@iron composite material prepared in Example 1 is shown below. (A) is the overall spectrum of the composite material, (B) is the C peak spectrum, (C) is the N peak spectrum, (D) is the O peak spectrum, and (E) is the Fe peak spectrum.

[0028] Figure 7 These are comparative graphs showing the performance of the composite materials prepared in Examples 1-3 and Comparative Example 1. In Example (A), the composite material was prepared in a 1M PBS solution at pH 7 at 50 mV s⁻¹. -1 (a) CV curves of chloramphenicol (200µM) for glassy carbon electrodes modified with various composite materials and bare glassy carbon electrodes at the scanning rate of ; (b) EIS spectra of glassy carbon electrodes modified with various composite materials and bare glassy carbon electrodes in potassium ferricyanide solution; (c) CV curves of glassy carbon electrodes modified with various composite materials in potassium ferricyanide solution.

[0029] Figure 8 It is the novel sea urchin-shaped ordered carbon in Example 1 (1) @iron (1) The performance of the composite material / glassy carbon electrode in pH measurement in 500 μM chloramphenicol PBS buffer solution; (A) pH measurement in 1M PBS at 50 mV s -1 The DPV response curve on the composite-modified glassy carbon electrode was obtained by scanning the scanning rate; (B) is a linear relationship between pH and potential; (C) is the relationship between pH and current.

[0030] Figure 9 It is the novel sea urchin-shaped ordered carbon in Example 1 (1) @iron (1) The composite material was used to detect chloramphenicol at different scan rates; where (A) shows the results at different scan rates (10 mVs) in a PBS (pH=7) buffer solution containing 200 μM chloramphenicol. -1 Up to 300 mV s -1(A) shows the CV curve under the current; (B) shows the linear relationship between the scan rate and the peak current.

[0031] Figure 10 The novel sea urchin-like ordered carbon obtained in Example 1 (1) @iron (1) Quantitative test results of the composite material for chloramphenicol. In the figure, (A) is the DPV response curve on the glassy carbon electrode modified with the composite material after adding 0-1000 μM chloramphenicol in 1 M PBS (pH 7.0), and (B) is the linear relationship between chloramphenicol concentration and corresponding response current.

[0032] Figure 11 The novel sea urchin-like ordered carbon obtained in Example 1 (1) @iron (1) Reproducibility results of composite materials. Detailed Implementation

[0033] The present invention will be further described below with reference to the embodiments. The processes and methods not described in detail in the following embodiments are conventional methods known in the art. Unless otherwise stated, the raw materials or reagents used in the embodiments are commercial products that can be purchased through commercial channels. Example 1

[0034] Combination Figure 1 The preparation method of the novel sea urchin-like ordered carbon@iron composite material provided in this embodiment includes the following steps:

[0035] S1. Preparation of dendritic mesoporous silicon (silicon template).

[0036] 0.408 g of triethanolamine was dissolved in 150 mL of water, and 2.28 g of hexadecyltrimethylammonium bromide and 1.61 g of sodium salicylate were added. The mixture was stirred to obtain a transparent, viscous solution. The transparent, viscous solution was placed in an oil bath and stirred at 80 °C for 1 h. Then, 22.43 g of tetraethyl silicate was added to the solution, and the mixture was stirred in an oil bath at 80 °C for 2 h. After stirring, the solution was a milky white liquid. The solution was then placed in a reaction vessel and reacted in an oven at 80 °C for 4 h. The solution was still a milky white liquid after being removed. The solution was washed with water and centrifuged three times. The sample settled at the bottom of the centrifuge tube. The supernatant was poured off, and the sample was dried in an oven at 60 °C for 12 h to obtain a white solid. The white solid was ground into powder, heated to 550°C in a tube furnace for 300 min, calcined in air at 550°C for 6 h, and then cooled to 20°C for 300 min to obtain nanoscale dendritic mesoporous silicon, which is the silicon template (in the shape of a sea urchin).

[0037] S2, filled with dopamine (DA) carbon source.

[0038] Weigh 0.25g of the silicon template powder obtained in step S1 and 0.625g of dopamine and dissolve them in 37.5mL of Tris solution. Stir and sonicate the solution for 10min to dissolve it. Let it stand in the dark at room temperature for 24h. Wash with water three times and centrifuge. Dry at 60℃ for 24h to obtain solid powder polydopamine-filled mesoporous silicon (DMSN@PDA).

[0039] S3, doped with iron.

[0040] Weigh 0.4 g of the polydopamine-filled mesoporous silica obtained in step S2 and 0.4 g of ferrocene, add them to 25 mL of acetone, and stir for 10 min to obtain a mixture. Add 2.0 mL of 25% hydrogen peroxide solution to the mixture and stir in an oil bath at 100 °C for about 20 min until the solvent evaporates completely, leaving only powder. Wash the sample with water and centrifuge twice, then dry it in an oven at 60 °C for 20 h. Afterward, calcine it in a nitrogen atmosphere with the following parameters: heat to 600 °C for 480 min, then heat to 800 °C for 40 min, hold at 800 °C for 3 h, and then cool to 20 °C for 400 min.

[0041] S4. Synthesis of a novel sea urchin-shaped ordered carbon@iron composite material.

[0042] Alkali washing to remove the silicon template: The sample from step S3 was added to a round-bottom flask, a magnetic stir bar was added, 50 mL of sodium hydroxide solution was added, and the mixture was refluxed for 2.5 h. After that, it was centrifuged and dried three times. The resulting composite material was named a novel urchin-shaped ordered carbon. (1) @iron (1) In composite materials, the subscripts for carbon and iron are used to indicate the mass ratio (or parts by mass) of DMSN@PDA and ferrocene. Example 2

[0043] Compared to Example 1, the mass of polydopamine-filled mesoporous silica and ferrocene used in step S3 of this example is 0.2 g and 0.4 g, respectively (i.e., the mass ratio of the two is 1:2), and all other aspects are the same as in Example 1. The composite material obtained in this example is denoted as novel urchin-like ordered carbon. (1) @iron (2) Composite materials. Example 3

[0044] Compared to Example 1, the mass of polydopamine-filled mesoporous silica and ferrocene used in step S3 of this example is 0.4 g and 0.2 g, respectively (i.e., the mass ratio of the two is 2:1), and all other aspects are the same as in Example 1. The composite material obtained in this example is referred to as novel urchin-like ordered carbon. (2) @iron (1) Composite materials.

[0045] Comparative Example 1

[0046] Compared with Example 1, the composite material prepared in this comparative example does not contain iron. The preparation process includes steps S1, S2 and S4 in Example 1, but does not include step S3. The resulting composite material is referred to as a novel sea urchin-shaped ordered carbon composite material.

[0047] The composite materials prepared in Examples 1-3 were structurally characterized, and the results are as follows: Figures 2-6 As shown.

[0048] Figure 2 Scanning electron microscope (SEM) images of the novel sea urchin-shaped ordered carbon@iron composite materials prepared in Examples 1-3 are shown. The microstructure of the novel sea urchin-shaped ordered carbon@iron composite materials at scales of 100 nm and 500 nm can be clearly observed through the SEM images. The ordered carbon morphology is visible, and iron elements are loaded onto the ordered carbon. The SEM images confirm that the novel sea urchin-shaped ordered carbon@iron composite materials were successfully synthesized.

[0049] Figure 3 Transmission electron microscopy (TEM) images of the novel sea urchin-shaped ordered carbon@iron composite materials prepared in Examples 1-3 are shown. The TEM images clearly show the microstructure of the novel sea urchin-shaped ordered carbon@iron composite materials at scales of 50 nm and 100 nm. The microstructure of ordered carbon is visible, and iron is loaded onto the ordered carbon. The TEM images also confirm that the novel sea urchin-shaped ordered carbon@iron composite materials were successfully synthesized.

[0050] Figure 4 This is a mapping image of the novel urchin-like ordered carbon@iron composite material prepared in Example 1 at a scale of 250 nm. Figure 4 This confirms that iron has been successfully loaded onto a carbon-based material, and a novel urchin-like ordered carbon@iron composite material has been successfully synthesized.

[0051] Figure 5 These are X-ray diffraction patterns of the novel sea urchin-like ordered carbon@iron composite materials prepared in Examples 1-3. Figure 5 It can be seen that the composite materials in Examples 1-3 exhibit similar characteristic peaks. 2θ = 44.68°, 65.02°, and 82.33° correspond to the common crystal structures of iron, namely (110), (200), and (211) crystal planes (PDF#06-0696). 2θ = 16.67°, 22.77°, 26.57°, and 34.22° correspond to the (002), (120), (103), and (123) crystal planes of carbon (PDF#50-0926). Therefore, the successful synthesis of the novel urchin-like ordered carbon@iron composite material can be demonstrated, and iron nanoparticles were successfully loaded onto ordered carbon, indicating successful preparation of the composite material.

[0052] Figure 6This is the X-ray photoelectron spectrum of the novel sea urchin-shaped ordered carbon@iron composite material prepared in Example 1. Figure 6 (A) is the full X-ray photoelectron spectrum; (B) shows that C is divided into three peaks: C=C (284.80 eV), CN (286.41 eV), and C=O=C (289.21 eV); (C) shows two peaks for nitrogen, namely pyrrole nitrogen (399.92 eV) and graphitic nitrogen (401.00 eV); (D) shows two peaks for O, namely CO (531.58 eV) and C=O (533.3 eV); (E) shows the peaks for Fe, with peaks at 711.34 eV and 725.5 eV corresponding to ferrous iron, peaks at 715.6 eV and 728.7 eV corresponding to ferric iron, and satellite peaks at 717.4 eV and 735.6 eV.

[0053] The electrocatalytic performance of chloramphenicol prepared in Examples 1-3 and Comparative Example 1 was tested below.

[0054] The composite materials prepared in Examples 1-3 and Comparative Example 1 were applied to the electroanalysis of chloramphenicol to compare their electrochemical performance. The specific steps are as follows:

[0055] (1) A three-electrode testing system (Autolab 302N electrochemical workstation) was used, with silver / silver chloride as the reference electrode, platinum wire as the counter electrode, and the glassy carbon electrode modified with the prepared composite material as the working electrode. The electrolyte solution was PBS solution.

[0056] The working electrode is prepared as follows: 2 mg of the prepared composite material is dispersed in 1 mL of N,N-dimethylformamide solution to make the concentration 2 mg / mL. 5 µL of the dispersion is then dropped onto the surface of the glassy carbon electrode and dried under an infrared lamp (150 W) to obtain the working electrode.

[0057] (2) Place the three electrodes in the electrolytic cell, immerse them in the electrolyte solution, select the electrochemical method, set the parameters, and perform chloramphenicol electrochemical test.

[0058] Test results are available Figure 7-11 , Figure 7 (A) is at 50 mV s -1 The CV curves of the working electrodes made of the composite materials in Examples 1-3 and Comparative Example 1 were obtained at a scan rate of 200 μM chloramphenicol in 1M PBS buffer solution (pH=7). Figure 7 (A) also presents the CV curves of a bare glassy carbon electrode in 1M PBS buffer (pH=7) with a concentration of 200 μM chloramphenicol. Figure 7(A) It can be seen that the larger the peak current value, the better the electrocatalytic performance of the composite material of the modified electrode. The composite material prepared in Example 1 has a higher electrochemical response to 200 µM chloramphenicol (the current response in Example 1 is 12.50 µA, the current response in Example 2 is 12.05 µA, and the current response in Example 3 is 11.14 µA). Therefore, the composite material in Example 1 has the best electrocatalytic performance for chloramphenicol.

[0059] Depend on Figure 7 (B) It can be seen that the composite material prepared in Example 1 has a smaller impedance value compared with the composite materials prepared in Examples 2 and 3 (the impedance values ​​corresponding to Examples 1 to 3 are 48.37 Ω, 104.8 Ω and 107 Ω, respectively).

[0060] Figure 7 (C) is at 50 mV s -1 The CV curve of 100 μM chloramphenicol in potassium ferricyanide solution at the scan rate is shown in the figure. As can be seen from the figure, the novel urchin-like ordered carbon in Example 1... (1) @iron (1) The composite material exhibits the largest partial current, demonstrating a large electrode active surface area, thus indicating superior electrocatalytic performance.

[0061] Figure 8 The novel sea urchin-shaped ordered carbon in Example 1 (1) @iron (1) The pH performance of the composite material in 500 μM chloramphenicol PBS buffer solution was measured. Figure 8 (A) shows the differential pulse voltammetry (DPV) curves of the composite material in Example 1 detecting chloramphenicol in buffer solutions of different pH values ​​(3-11). These solutions were used to test the effect of different pH conditions on electrocatalytic performance. Figure 8 (A) It can be seen that the peak current value increases with increasing pH, and the peak current value increases monotonically only when pH≤7, and then decreases with increasing pH. Therefore, it can be concluded that pH=7 is the optimal pH value for detecting chloramphenicol. Figure 8 (B) shows a linear relationship between pH and potential (E), with the linear equation being E = 0.36298 + 0.02707pH.

[0062] Figure 9 The effect of different scan rates on the detection of chloramphenicol in the composite material in Example 1 is shown. Figure 9 It can be seen that the novel sea urchin-shaped ordered carbon (1) @iron (1) The glassy carbon electrode modified with composite material was tested in 1M PBS (pH=7) buffer solution containing 500 μM chloramphenicol at different scan rates. Figure 9In (A), the different colored lines represent values ​​from 10 mV s. -1 Up to 300 mV s -1 The different scan rates are: 10, 15, 20, 25, 30, 40, 50, 60, 70, 85, 100, 115, 130, 150, 170, 190, 215, 240, 270, and 300, with the unit being mV / s. -1 Under these conditions, the peak current value increases with the increase of the scan rate. Figure 9 (B) shows a linear relationship between the peak current (I) and the scan rate (V), with the linear equation being: I(μA) = 36.7573 + 0.2147 v(mV / s) (R 2 =0.983), proving that chloramphenicol is an adsorption-controlled reaction.

[0063] Figure 10 The novel sea urchin-like ordered carbon in Example 1 is shown. (1) @iron (1) The electrocatalytic performance of the composite material for different concentrations of chloramphenicol ranging from 0 μM to 1000 μM. For example... Figure 10 As shown in (A), the peak current value increases with increasing concentration. Figure 10 (B) shows the linear relationship between peak current and concentration. It can be clearly observed that the increase in peak current with increasing concentration exhibits two linear relationships, corresponding to concentration ranges of 0-100 μM and 100-1000 μM, respectively. Within the concentration range of 0-100 μM, the peak current increases rapidly, and the linear equation is as follows: I (μA) = 11.6882 + 1.1679 c (μM)(R) 2 =0.950); within the concentration range of 100-1000 μM, the peak current increases moderately, and the linear equation is: I (μA)=121.6086+0.05865c (μM) (R 2 =0.964). Where c is the concentration of chloramphenicol.

[0064] Figure 11 The reproducibility test of the composite material in Example 1 on five different electrodes is shown. In the experiment, five different working electrodes were made by modifying the glassy carbon electrode with the composite material in Example 1. The buffer solution was 1M PBS buffer with pH=7 containing 300 μM chloramphenicol. The current value of the peak with a potential of about 0.6V was observed on the CV plot. The calculated relative standard deviation RSD was 1.60%, which shows that the composite material prepared in Example 1 has excellent reproducibility.

[0065] The composite material prepared by this invention can be used not only in the field of electrocatalysis, but also in the field of engineering materials.

[0066] The composite materials prepared in Examples 1-3 and Comparative Example 1 were incorporated into asphalt concrete to improve its performance. Specifically, the composition of the reference asphalt concrete was: 8 parts asphalt, 70 parts crushed stone, 20 parts quartz sand, 10 parts mineral powder, and 30 parts water. The composite materials from Examples 1-3 and Comparative Example 1 were each incorporated into the reference asphalt concrete at a ratio of 5 parts, and then the compressive, tensile, and rutting resistance of the concrete were tested. The test results are shown in Table 1.

[0067] Table 1 Performance test results of benchmark asphalt concrete and asphalt concrete with different composite materials

[0068]

[0069] As shown in Table 1, incorporating a certain amount of the novel sea urchin-shaped ordered carbon@iron composite material prepared in this invention into the benchmark asphalt concrete can effectively improve the strength and rutting resistance of the asphalt concrete. However, incorporating the novel sea urchin-shaped ordered carbon composite material prepared in Comparative Example 1 did not significantly improve the performance of the asphalt concrete.

Claims

1. Use of a novel sea urchin-like ordered carbon@iron composite material, characterized in that, The novel urchin-shaped ordered carbon@iron composite material is used as a catalyst for the detection of chloramphenicol. The preparation method of the novel sea urchin-like ordered carbon@iron composite material includes the following steps: (1) Dissolve triethanolamine in water, add hexadecyltrimethylammonium bromide and sodium salicylate, mix and stir, then place the solution in an oil bath and stir, then add tetraethyl silicate to the solution and continue stirring; then dry the reaction in a reaction vessel; after the reaction is completed, centrifuge, dry, and finally calcine to obtain a silicon template; (2) Take the silicon template and dopamine from step (1) and dissolve them in Tris solution. After stirring, let it stand, then wash with water, centrifuge, and dry to obtain polydopamine-filled mesoporous silicon. (3) Add the product from step (2) and ferrocene to acetone, stir evenly, then add hydrogen peroxide solution, stir in an oil bath until the solvent evaporates, wash the powder product with water, centrifuge, dry, and then calcine in an inert atmosphere. (4) Add an alkaline solution to the calcined product in step (3) and reflux, then centrifuge and dry to obtain a novel sea urchin-shaped ordered carbon@iron composite material.

2. Use of the novel sea urchin-like ordered carbon@iron composite material according to claim 1, characterized in that, In step (3), the mass ratio of the product and ferrocene in step (2) is 1:2 to 2:

1.

3. The application of the novel sea urchin-like ordered carbon@iron composite material according to claim 1, characterized in that, The calcination conditions in step (1) are: in an air atmosphere, at 500~600℃ for 5~8h.

4. The application of the novel sea urchin-like ordered carbon@iron composite material according to claim 1, characterized in that, The resting conditions in step (2) are: rest in the dark for 20~36 hours.

5. The application of the novel sea urchin-like ordered carbon@iron composite material according to claim 1, characterized in that, The calcination conditions in step (3) are: under an inert atmosphere, heat at 750~850℃ for 3~4 hours.

6. The application of the novel sea urchin-like ordered carbon@iron composite material according to claim 5, characterized in that, The heating process during calcination in step (3) is as follows: heat up to 600℃ for 450~500min, and then heat up to 750~850℃ for 30~50min.

7. The application of the novel sea urchin-like ordered carbon@iron composite material according to claim 1, characterized in that, In step (4), the alkaline solution is sodium hydroxide solution, and the reflux time is 2-3 hours.

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