Magnetic response iron-carbon nano-catalyst and preparation method thereof

Abstract

The invention discloses a magnetic response iron-carbon nano-catalyst and a preparation method thereof, and belongs to the technical field of preparation of iron-carbon nano-catalysts. Comprising the following steps: 1, preparing an iron source, a carbon source, a reducing agent and a surfactant; step 2, dissolving an iron source in a first part of solvent, and adding a surfactant to obtain an iron precursor solution; 3, pretreating a carbon source, and dissolving the pretreated carbon source in a second solvent to obtain a carbon precursor solution; 4, mixing the iron precursor solution obtained in the step 2 and the carbon precursor solution obtained in the step 3, and uniformly stirring to obtain a mixed solution; 5, adding a reducing agent into the mixed solution obtained in the step 4; step 6, after the reduction reaction is finished, separating out the magnetic response iron-carbon nano-catalyst by using a magnet, and washing the magnetic response iron-carbon nano-catalyst by using deionized water and ethanol; and step 7, drying and calcining the washed magnetic response iron-carbon nano-catalyst.

Description

Technical Field

[0001] The invention relates to the technical field of preparation of iron-carbon nanocatalysts, in particular to a magnetic responsive iron-carbon nanocatalyst and a preparation method thereof. Background Art

[0002] With the increasingly severe environmental problems and the increasing demand for efficient catalytic reactions, the development of new catalysts has become a research hotspot. Magnetic responsive iron-carbon nanocatalysts combine the magnetism of iron with the stability and catalytic performance of carbon materials, and have broad application prospects in environmental governance, energy conversion, and organic synthesis. However, the existing preparation methods have problems such as complex processes, high costs, and unstable catalytic performance. Therefore, a new preparation method is needed to prepare high-performance magnetic responsive iron-carbon nanocatalysts. Summary of the invention

[0003] The purpose of the present invention is to provide a method for preparing a magnetically responsive iron-carbon nanocatalyst to solve the problems raised in the above-mentioned background technology.

[0004] In view of the above problems, the technical solution proposed by the present invention is: A magnetic responsive iron-carbon nanocatalyst and a preparation method thereof, comprising the following steps: Step 1, preparing an iron source, a carbon source, a reducing agent, and a surfactant, wherein the molar ratio of the iron source, the carbon source, the reducing agent, and the surfactant is iron source: carbon source: reducing agent: surfactant = 1:2:5:0.1; Step 2, dissolving the iron source in the first solvent and adding a surfactant to obtain an iron precursor solution; Specifically, the surfactant can improve the dispersibility of the iron nanoparticles in the iron source.

[0005] Step 3, pretreating the carbon source, and dissolving the pretreated carbon source in a second solvent to obtain a carbon precursor solution; Specifically, pretreatment can improve the solubility and reactivity of the carbon source.

[0006] Step 4, mixing the iron precursor solution obtained in step 2 and the carbon precursor solution obtained in step 3, and stirring them evenly to obtain a mixed solution; Step 5, adding a reducing agent to the mixed solution obtained in step 4, so that the mixed solution undergoes a reduction reaction, and stirring the mixed solution, while ensuring that the mixed solution reacts at 60° C. for 2 hours; Specifically, the temperature and time can ensure the formation of iron nanoparticles and the coating of carbon materials, and stirring can promote the progress of the reaction and the uniformity of the product.

[0007] Step 6, after the reduction reaction is completed, the magnetic responsive iron-carbon nanocatalyst is separated by a magnet, and the magnetic responsive iron-carbon nanocatalyst is washed with deionized water and ethanol; Specifically, deionized water and ethanol can remove impurities and unreacted substances.

[0008] Step seven, drying the washed magnetic responsive iron-carbon nanocatalyst, and calcining the dried magnetic responsive iron-carbon nanocatalyst.

[0009] Specifically, drying can remove the solvent, and calcination can improve the crystallinity and stability of the iron-carbon nanocatalyst.

[0010] As a preferred technical solution of the present invention, the iron source in the step one is one of ferric chloride, ferric sulfate, and ferric nitrate, the carbon source in the step one is one of glucose, sucrose, and starch, the reducing agent in the step one is one of sodium borohydride and hydrazine hydrate, and the surfactant in the step one is one of sodium dodecyl sulfate and hexadecyltrimethylammonium bromide.

[0011] As a preferred technical solution of the present invention, the molar ratio of the iron source and the first solvent in the step 2 is iron source: first solvent = 1:556, and the molar ratio of the carbon source and the second solvent in the step 3 is carbon source: first solvent = 1:278, and the first solvent and the second solvent are both deionized water.

[0012] As a preferred technical solution of the present invention, the pretreatment method in step three is one of heating and ultrasound.

[0013] As a preferred technical solution of the present invention, the magnet in step six is ​​an electromagnet.

[0014] Specifically, the electromagnet will only generate a magnetic field when it is energized. By utilizing this characteristic, the adsorption and separation of magnetically responsive iron-carbon nanocatalysts can be completed.

[0015] As a preferred technical solution of the present invention, the drying in step seven is performed using a drying oven.

[0016] As a preferred technical solution of the present invention, the calcination in step seven is carried out in a tubular furnace.

[0017] On the other hand, the present invention provides a magnetically responsive iron-carbon nanocatalyst, including a magnetically responsive iron-carbon nanocatalyst, wherein the magnetically responsive iron-carbon nanocatalyst is a finished product prepared according to any one of claims 1-7.

[0018] Compared with the prior art, the beneficial effects of the present invention are: the magnetic responsive iron-carbon nanocatalyst and its preparation method, the magnetic responsive iron-carbon nanocatalyst prepared by the above method, have the advantages of simple production process, low cost, high catalytic activity and stability, and effectively solve the problems of complex process, high cost and unstable catalytic performance in the existing preparation method. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a flowchart of a magnetically responsive iron-carbon nanocatalyst and a method for preparing the same disclosed in an embodiment of the present invention. DETAILED DESCRIPTION

[0020] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0021] See also Figure 1 The present invention provides a technical solution: a method for preparing a magnetically responsive iron-carbon nanocatalyst, comprising the following steps: Step 1, prepare 10 mmol of ferric chloride, 20 mmol of glucose, 50 mmol of sodium borohydride, and 1 mmol of sodium dodecyl sulfate; Step 2: dissolve 10 mmol of ferric chloride in 100 ml of deionized water to obtain an iron precursor solution, add 1 mmol of sodium dodecyl sulfate and stir evenly; Step 3, placing 20 mmol of glucose in a drying oven, heating at 40° C. for 4 min, and dissolving 20 mmol of glucose in 100 ml of deionized water to obtain a carbon precursor solution; Step 4, mixing the iron precursor solution obtained in step 2 and the carbon precursor solution obtained in step 3, and stirring them evenly to obtain a mixed solution; Step 5, adding 50 mmol of sodium borohydride to the mixed solution obtained in step 4, so that the mixed solution undergoes a reduction reaction, and stirring the mixed solution, while ensuring that the mixed solution reacts at 60° C. for 2 hours; Step 6, after the reduction reaction is completed, an energized electromagnet is placed on a container containing the mixed solution, and the magnetic responsive iron-carbon nanocatalyst is separated by using the magnetic field generated by the electromagnet. After the adsorption is completed, the electromagnet is turned off to allow the separated magnetic responsive iron-carbon nanocatalyst to fall into another drying container, and the magnetic responsive iron-carbon nanocatalyst is washed three times with deionized water and ethanol respectively; Step seven, placing the washed magnetic responsive iron-carbon nanocatalyst in a drying oven and drying it at 60°C for 12 hours, placing the dried magnetic responsive iron-carbon nanocatalyst in a tubular furnace and calcining it at 400°C for 2 hours, and finally obtaining the magnetic responsive iron-carbon nanocatalyst.

[0022] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] See also Figure 1 The present invention provides a technical solution: a method for preparing a magnetically responsive iron-carbon nanocatalyst, comprising the following steps: Step 1, prepare 10 mmol of ferric sulfate, 20 mmol of sucrose, 50 mmol of hydrazine hydrate, and 1 mmol of hexadecyltrimethylammonium bromide; Step 2: dissolve 10 mmol of ferric sulfate in 100 ml of deionized water to obtain an iron precursor solution, add 1 mmol of hexadecyltrimethylammonium bromide and stir evenly; Step 3, placing 20 mmol of sucrose in a drying oven, heating at 40° C. for 4 min, and dissolving 20 mmol of sucrose in 100 ml of deionized water to obtain a carbon precursor solution; Step 4, mixing the iron precursor solution obtained in step 2 and the carbon precursor solution obtained in step 3, and stirring them evenly to obtain a mixed solution; Step 5, adding 50 mmol of hydrazine hydrate to the mixed solution obtained in step 4, so that the mixed solution undergoes a reduction reaction, and stirring the mixed solution, while ensuring that the mixed solution reacts at 60° C. for 2 hours; Step 6, after the reduction reaction is completed, an energized electromagnet is placed on a container containing the mixed solution, and the magnetic responsive iron-carbon nanocatalyst is separated by using the magnetic field generated by the electromagnet. After the adsorption is completed, the electromagnet is turned off to allow the separated magnetic responsive iron-carbon nanocatalyst to fall into another drying container, and the magnetic responsive iron-carbon nanocatalyst is washed three times with deionized water and ethanol respectively; Step seven, placing the washed magnetic responsive iron-carbon nanocatalyst in a drying oven and drying it at 60°C for 12 hours, placing the dried magnetic responsive iron-carbon nanocatalyst in a tubular furnace and calcining it at 400°C for 2 hours, and finally obtaining the magnetic responsive iron-carbon nanocatalyst.

[0024] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0025] See also Figure 1 The present invention provides a technical solution: a method for preparing a magnetically responsive iron-carbon nanocatalyst, comprising the following steps: Step 1, prepare 10 mmol of ferric nitrate, 20 mmol of starch, 50 mmol of hydrazine hydrate, and 1 mmol of hexadecyltrimethylammonium bromide; Step 2: dissolve 10 mmol of ferric nitrate in 100 ml of deionized water to obtain an iron precursor solution, add 1 mmol of hexadecyltrimethylammonium bromide and stir evenly; Step 3, placing 20 mmol of starch in a drying oven, heating at 40° C. for 4 min, dissolving 20 mmol of starch in 100 ml of deionized water to obtain a carbon precursor solution; Step 4, mixing the iron precursor solution obtained in step 2 and the carbon precursor solution obtained in step 3, and stirring them evenly to obtain a mixed solution; Step 5, adding 50 mmol of hydrazine hydrate to the mixed solution obtained in step 4, so that the mixed solution undergoes a reduction reaction, and stirring the mixed solution, while ensuring that the mixed solution reacts at 60° C. for 2 hours; Step 6, after the reduction reaction is completed, an energized electromagnet is placed on a container containing the mixed solution, and the magnetic responsive iron-carbon nanocatalyst is separated by using the magnetic field generated by the electromagnet. After the adsorption is completed, the electromagnet is turned off to allow the separated magnetic responsive iron-carbon nanocatalyst to fall into another drying container, and the magnetic responsive iron-carbon nanocatalyst is washed three times with deionized water and ethanol respectively; Step seven, placing the washed magnetic responsive iron-carbon nanocatalyst in a drying oven and drying it at 60°C for 12 hours, placing the dried magnetic responsive iron-carbon nanocatalyst in a tubular furnace and calcining it at 400°C for 2 hours, and finally obtaining the magnetic responsive iron-carbon nanocatalyst.

[0026] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] See also Figure 1 The present invention provides a technical solution: a method for preparing a magnetically responsive iron-carbon nanocatalyst, comprising the following steps: Step 1, prepare 10mmol of ferric chloride, 20mmol of glucose, 50mmol of hydrazine hydrate, and 1mmol of hexadecyltrimethylol; Step 2, dissolving 10 mmol of ferric chloride in 100 ml of deionized water to obtain an iron precursor solution, adding 1 mmol of hexadecyltrimethylolpropane and stirring evenly; Step 3, placing 20 mmol of glucose in a cleaning tank, determining the ultrasonic frequency, power and treatment time according to the amount of glucose, starting the ultrasonic cleaner, and starting ultrasonic treatment. After the ultrasonic treatment is completed, turning off the power switch of the ultrasonic cleaner, taking the cleaning tank out of the ultrasonic cleaner, taking out the treated glucose, filtering, drying and characterizing the taken-out glucose, and dissolving 20 mmol of glucose in 100 ml of deionized water to obtain a carbon precursor solution; Step 4, mixing the iron precursor solution obtained in step 2 and the carbon precursor solution obtained in step 3, and stirring them evenly to obtain a mixed solution; Step 5, adding 50 mmol of hydrazine hydrate to the mixed solution obtained in step 4, so that the mixed solution undergoes a reduction reaction, and stirring the mixed solution, while ensuring that the mixed solution reacts at 60° C. for 2 hours; Step 6, after the reduction reaction is completed, an energized electromagnet is placed on a container containing the mixed solution, and the magnetic responsive iron-carbon nanocatalyst is separated by using the magnetic field generated by the electromagnet. After the adsorption is completed, the electromagnet is turned off to allow the separated magnetic responsive iron-carbon nanocatalyst to fall into another drying container, and the magnetic responsive iron-carbon nanocatalyst is washed three times with deionized water and ethanol respectively; Step seven, placing the washed magnetic responsive iron-carbon nanocatalyst in a drying oven and drying it at 60°C for 12 hours, placing the dried magnetic responsive iron-carbon nanocatalyst in a tubular furnace and calcining it at 400°C for 2 hours, and finally obtaining the magnetic responsive iron-carbon nanocatalyst.

[0028] The prepared magnetically responsive iron-carbon nanocatalyst was tested for its performance. In wastewater treatment, the magnetically responsive iron-carbon nanocatalyst can quickly degrade organic pollutants with a removal rate of more than 90%. In energy conversion, the magnetically responsive iron-carbon nanocatalyst can improve the performance of fuel cells, with the power density increased by more than 30%.

Claims

1. A method for preparing a magnetically responsive iron-carbon nanocatalyst, characterized in that: The following steps are involved: Step 1, preparing an iron source, a carbon source, a reducing agent, and a surfactant, wherein the molar ratio of the iron source, the carbon source, the reducing agent, and the surfactant is iron source: carbon source: reducing agent: surfactant = 1:2:5:0.1; Step 2, dissolving the iron source in the first solvent and adding a surfactant to obtain an iron precursor solution; Step 3, pretreating the carbon source, and dissolving the pretreated carbon source in a second solvent to obtain a carbon precursor solution; Step 4, mixing the iron precursor solution obtained in step 2 and the carbon precursor solution obtained in step 3, and stirring them evenly to obtain a mixed solution; Step 5, adding a reducing agent to the mixed solution obtained in step 4, so that the mixed solution undergoes a reduction reaction, and stirring the mixed solution, while ensuring that the mixed solution reacts at 60° C. for 2 hours; Step 6, after the reduction reaction is completed, the magnetic responsive iron-carbon nanocatalyst is separated by a magnet, and the magnetic responsive iron-carbon nanocatalyst is washed with deionized water and ethanol; Step seven, drying the washed magnetic responsive iron-carbon nanocatalyst, and calcining the dried magnetic responsive iron-carbon nanocatalyst.

2. The method for preparing a magnetically responsive iron-carbon nanocatalyst according to claim 1, characterized in that: The iron source in step one is one of ferric chloride, ferric sulfate, and ferric nitrate; the carbon source in step one is one of glucose, sucrose, and starch; the reducing agent in step one is one of sodium borohydride and hydrazine hydrate; and the surfactant in step one is one of sodium dodecyl sulfate and hexadecyltrimethylammonium bromide.

3. The method for preparing a magnetically responsive iron-carbon nanocatalyst according to claim 1, characterized in that: The molar ratio of the iron source to the first solvent in the step 2 is iron source: first solvent = 1:556, and the molar ratio of the carbon source to the second solvent in the step 3 is carbon source: first solvent = 1:

278. Both the first solvent and the second solvent are deionized water.

4. The method for preparing a magnetically responsive iron-carbon nanocatalyst according to claim 1, characterized in that: The pretreatment method in step three is one of heating and ultrasound.

5. The method for preparing a magnetically responsive iron-carbon nanocatalyst according to claim 1, characterized in that: The magnet in step six is ​​an electromagnet.

6. The method for preparing a magnetically responsive iron-carbon nanocatalyst according to claim 1, characterized in that: The drying in step seven is carried out in a drying oven.

7. The method for preparing a magnetically responsive iron-carbon nanocatalyst according to claim 1, characterized in that: The calcination in step seven is carried out using a tubular furnace.

8. A magnetically responsive iron-carbon nanocatalyst, as used in the method for preparing a magnetically responsive iron-carbon nanocatalyst according to claims 1-7, characterized in that: It comprises a magnetically responsive iron-carbon nanocatalyst, and the magnetically responsive iron-carbon nanocatalyst is a finished product prepared according to any one of claims 1-7.

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