CN115722273A - Method for rapidly preparing iron-carbon composite film catalytic material under assistance of laser - Google Patents
Method for rapidly preparing iron-carbon composite film catalytic material under assistance of laser Download PDFInfo
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- CN115722273A CN115722273A CN202211298300.3A CN202211298300A CN115722273A CN 115722273 A CN115722273 A CN 115722273A CN 202211298300 A CN202211298300 A CN 202211298300A CN 115722273 A CN115722273 A CN 115722273A
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Abstract
The invention discloses a method for rapidly preparing an iron-carbon composite film catalytic material under the assistance of laser, which comprises the following specific steps: placing ferrocene in a quartz tube, introducing auxiliary gas into one end of the quartz tube, and fixing the other end of the quartz tube on a rotating motor; placing the quartz tube under a laser to perform laser treatment twice to obtain the quartz tube loaded with the iron-carbon composite film; and then soaking in an acid solution, sequentially soaking in deionized water and absolute ethyl alcohol to wash and remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material. The invention adopts ferrocene as a carbon source and an iron source for the first time and utilizes the laser action to prepare the iron-carbon composite film catalytic material. The laser preparation realizes one-step synthesis and deposition load, has simple and quick process and good repeatability, and is suitable for large-scale preparation.
Description
Technical Field
The invention belongs to the technical field of preparation of iron-carbon composite functional materials, and particularly relates to a method for rapidly preparing an iron-carbon composite film catalytic material under the assistance of laser.
Background
In previous researches, the nano zero-valent iron is loaded on some solid carriers, such as activated carbon, so that the stability of the nano zero-valent iron can be enhanced, and some physical properties of the nano zero-valent iron can be changed. Iron-carbon materials are mainly synthesized by physically mixing, sintering precursors of carbon and iron. The prior art is a ball milling method (CN 110065999A, CN 112604703B), iron salt and polymer are placed in a ball mill reaction kettle and are obtained under the action of mechanical force such as friction, collision, impact and the like; or calcining iron-containing metal skeleton (CN 111111111661A, CN109179594B, CN111112638A, CN 113019420A) by heat treatment, or high-pressure treating iron-containing carbon precursor (CN 105110424A, CN113499776A, CN112548095A, CN110575815A, CN113877637A, CN 109626722A). The carbon shell restrains the metal nano particles in a small space, thereby preventing the mutual aggregation of the metal particles, protecting the metal particles from the influence of the external environment and solving the problem that the nano metal particles can not be stably existed in the air. However, these preparation processes require a large amount of organic solvents, long-time calcination or high-pressure reaction, consume time and materials, and are complicated and tedious in preparation processes except for one-step preparation by a ball milling method. In addition, the prepared carbon shell and the nano zero-valent iron are both powder catalysts, so that the problems of difficult recovery and recycling exist, and the large-scale production is not facilitated. In order to achieve the purposes of green energy conservation and cost saving, it is very important to find an iron-containing precursor which is cheap and easy to obtain. Ferrocene with a sandwich structure has unique molecular structure and aromatic characteristic, and has attracted great interest of chemists of various countries in the world in the processes of organic synthesis and material preparation due to low cost. Ferrocene molecules are composed of two cyclopentadienyl radicals sandwiching an iron atom and are commonly used as a carbon source in the synthesis of materials. At present, no relevant report exists for preparing the iron-carbon composite film catalytic material by taking ferrocene as a carbon source and an iron source through laser assistance.
Disclosure of Invention
The invention solves the technical problem of providing a method for rapidly preparing an iron-carbon composite film catalytic material by laser assistance, which has simple process and good repeatability.
The invention adopts the following technical scheme for solving the technical problems, and the method for rapidly preparing the iron-carbon composite film catalytic material by laser assistance is characterized by comprising the following specific steps of:
s1, placing ferrocene in a quartz tube, introducing auxiliary gas into one end of the quartz tube, setting the flow rate of the auxiliary gas to be 120-180mL/min, fixing the other end of the quartz tube on a rotating motor, and setting the rotating speed of the rotating motor to be 20-50r/min, wherein the auxiliary gas is air, argon-hydrogen mixed gas or nitrogen;
s2, placing the quartz tube under a 1064nm laser, setting the power of the laser to be 50-70% of the total power, the frequency to be 120-180Hz, the scanning speed to be 60-90mm/S, starting a rotating motor and the laser after introducing auxiliary gas for 3-8min, and carrying out laser scanning treatment for 5-20S;
s3, after the laser processing in the S2 is finished, setting the power of the laser to be 2% -8% of the total power, the frequency to be 120-180Hz, the scanning speed to be 60-90mm/S, starting the rotating motor and the laser, and performing laser scanning processing for 10-30min to obtain the quartz tube loaded with the iron-carbon composite film;
and S4, placing the quartz tube loaded with the iron-carbon composite film in an acid solution, soaking for 8-12h at 70-90 ℃, then sequentially soaking in deionized water and absolute ethyl alcohol to wash and remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material.
Further, the total power of the 1064nm laser is 30W.
Further defined, the acidic solution is a sulfuric acid solution, a nitric acid solution, or a hydrochloric acid solution.
Compared with the prior art, the invention has the following advantages and beneficial effects: 1. the invention adopts ferrocene as a carbon source and an iron source for preparing the iron-carbon composite film catalytic material for the first time. 2. The laser preparation of the invention realizes one-step synthesis and deposition load, and the process is simple and quick and is easy to repeat. The structure and composition of the supported thin film catalytic material can be varied by different atmospheric conditions. 3. The quartz tube loaded with the iron-carbon composite film catalytic material prepared by the invention shows stable performance in a circulating advanced oxidation system, and the process method is simple and convenient to operate, has strong repeatability and is convenient for batch production, so that the quartz tube has a very high application prospect.
Drawings
FIG. 1 is an XRD pattern of a quartz tube loaded with an iron-carbon composite thin film catalytic material obtained in examples 1-3;
FIG. 2 is a diagram of a quartz tube loaded with an iron-carbon composite thin film catalytic material obtained in examples 1 to 3;
FIG. 3 is a graph showing the performance of the iron-carbon composite film-loaded catalytic material quartz tube obtained in examples 1-3 as a catalyst for advanced oxidative degradation of tetracycline hydrochloride.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention. The technical means used in the examples are conventional means well known to those skilled in the art.
Example 1
S1, placing ferrocene in a quartz tube, introducing air serving as auxiliary gas into one end of the quartz tube, setting the flow rate of the auxiliary gas to be 150mL/min, fixing the other end of the quartz tube on a rotating motor, and setting the rotating speed of the rotating motor to be 30r/min;
s2, carrying out first laser treatment, namely placing the quartz tube under a 1064nm laser (the total power is 30W), setting the power of the laser to be 60% of the total power, the frequency to be 150Hz, the scanning speed to be 75mm/S, introducing auxiliary gas for 5min, then starting a rotating motor and the laser, and carrying out laser scanning treatment for 10S;
s3, performing second laser processing, after the laser processing in the step S2 is completed, setting the power of the laser to be 5% of the total power, the frequency to be 150Hz, the scanning speed to be 75mm/S, starting the rotating motor and the laser, and performing laser scanning processing for 10min to obtain the quartz tube loaded with the iron-carbon composite film;
and S4, placing the quartz tube loaded with the iron-carbon composite film in a 2M sulfuric acid solution, soaking for 10 hours at 80 ℃, then sequentially soaking in deionized water and absolute ethyl alcohol to wash and remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material.
Example 2
Step S1, placing ferrocene in a quartz tube, introducing argon-hydrogen mixed gas with the volume ratio of 9 to 1 as auxiliary gas into one end of the quartz tube, setting the flow rate of the auxiliary gas to be 150mL/min, fixing the other end of the quartz tube on a rotating motor, and setting the rotating speed of the rotating motor to be 30r/min;
s2, carrying out first laser treatment, namely placing the quartz tube under a 1064nm laser (the total power is 30W), setting the power of the laser to be 60% of the total power, the frequency to be 150Hz, the scanning speed to be 75mm/S, introducing auxiliary gas for 5min, then starting a rotating motor and the laser, and carrying out laser scanning treatment for 10S;
s3, performing second laser processing, after the laser processing in the step S2 is completed, setting the power of the laser to be 5% of the total power, the frequency to be 150Hz, the scanning speed to be 75mm/S, starting the rotating motor and the laser, and performing laser scanning processing for 10min to obtain the quartz tube loaded with the iron-carbon composite film;
and S4, placing the quartz tube loaded with the iron-carbon composite film in a 2M sulfuric acid solution, soaking for 10 hours at 80 ℃, then sequentially soaking in deionized water and absolute ethyl alcohol to wash and remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material.
Example 3
S1, placing ferrocene in a quartz tube, introducing nitrogen as auxiliary gas into one end of the quartz tube, setting the flow rate of the auxiliary gas to be 150mL/min, fixing the other end of the quartz tube on a rotating motor, and setting the rotating speed of the rotating motor to be 30r/min;
s2, carrying out first laser treatment, namely placing the quartz tube under a 1064nm laser (the total power is 30W), setting the power of the laser to be 60% of the total power, the frequency to be 150Hz, the scanning speed to be 75mm/S, introducing auxiliary gas for 5min, then starting a rotating motor and the laser, and carrying out laser scanning treatment for 10S;
s3, performing secondary laser processing, after the laser processing in the S2 is finished, setting the power of the laser to be 5 percent of the total power, the frequency to be 150Hz, the scanning speed to be 75mm/S, starting the rotating motor and the laser, and performing laser scanning processing for 10min to obtain the quartz tube loaded with the iron-carbon composite film;
and S4, placing the quartz tube loaded with the iron-carbon composite film in a 2M sulfuric acid solution, soaking for 10 hours at 80 ℃, then sequentially soaking in deionized water and absolute ethyl alcohol to wash and remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (3)
1. A method for rapidly preparing an iron-carbon composite film catalytic material under the assistance of laser is characterized by comprising the following specific steps:
step S1, placing ferrocene in a quartz tube, introducing auxiliary gas into one end of the quartz tube, setting the flow rate of the auxiliary gas to be 120-180mL/min, fixing the other end of the quartz tube on a rotating motor, and setting the rotating speed of the rotating motor to be 20-50r/min, wherein the auxiliary gas is air, argon-hydrogen mixed gas or nitrogen;
s2, placing the quartz tube under a 1064nm laser, setting the power of the laser to be 50-70% of the total power, the frequency to be 120-180Hz, the scanning speed to be 60-90mm/S, starting a rotating motor and the laser after introducing auxiliary gas for 3-8min, and carrying out laser scanning treatment for 5-20S;
s3, after the laser processing in the step S2 is finished, setting the power of the laser to be 2% -8% of the total power, the frequency to be 120-180Hz, the scanning speed to be 60-90mm/S, starting the rotating motor and the laser, and performing laser scanning processing for 10-30min to obtain the quartz tube loaded with the iron-carbon composite film;
and S4, placing the quartz tube loaded with the iron-carbon composite film in an acid solution, soaking for 8-12h at 70-90 ℃, then sequentially soaking in deionized water and absolute ethyl alcohol to wash and remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material.
2. The method for rapidly preparing the iron-carbon composite film catalytic material under the assistance of the laser according to claim 1, which is characterized in that: the total power of the 1064nm laser is 30W.
3. The method for rapidly preparing the iron-carbon composite film catalytic material under the assistance of the laser according to claim 1, which is characterized in that: the acid solution is a sulfuric acid solution, a nitric acid solution or a hydrochloric acid solution.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6045769A (en) * | 1997-12-08 | 2000-04-04 | Nanogram Corporation | Process for carbon production |
| CN103752313A (en) * | 2013-12-31 | 2014-04-30 | 中国科学院上海硅酸盐研究所 | Fe-supported mesoporous carbon material, and preparation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6045769A (en) * | 1997-12-08 | 2000-04-04 | Nanogram Corporation | Process for carbon production |
| CN103752313A (en) * | 2013-12-31 | 2014-04-30 | 中国科学院上海硅酸盐研究所 | Fe-supported mesoporous carbon material, and preparation method and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| K. ELIHN ET AL.: "Emission spectroscopy of carbon-covered iron nanoparticles in different gas atmospheres", 《APPLIED SURFACE SCIENCE》, vol. 186, pages 573 - 577, XP027323306 * |
| TAKUYA OKAMOTO ET AL.: "Synthesis of Bare Iron Nanoparticles from Ferrocene Hexane Solution by Femtosecond Laser Pulses", 《CHEMPHYSCHEM》, vol. 19, no. 19, pages 2480 - 2485, XP072158025, DOI: 10.1002/cphc.201800436 * |
| 张京等: "激光辐照对二茂铁掺杂单壁碳纳米管的影响", 《高等学校化学学报》, vol. 34, no. 6, pages 1505 - 1509 * |
| 邵玉苓: "激光法合成金属—碳复合材料的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 7, pages 33 * |
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