CN115722273B - Method for rapidly preparing iron-carbon composite film catalytic material with assistance of laser - Google Patents
Method for rapidly preparing iron-carbon composite film catalytic material with assistance of laser Download PDFInfo
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- CN115722273B CN115722273B CN202211298300.3A CN202211298300A CN115722273B CN 115722273 B CN115722273 B CN 115722273B CN 202211298300 A CN202211298300 A CN 202211298300A CN 115722273 B CN115722273 B CN 115722273B
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Abstract
The invention discloses a method for rapidly preparing an iron-carbon composite film catalytic material by laser assistance, 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 for two times to obtain a quartz tube loaded with the iron-carbon composite film; then soaking in acid solution, then sequentially soaking in deionized water and absolute ethyl alcohol, washing to remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material. According to the invention, ferrocene is used as a carbon source and an iron source for the first time, and the iron-carbon composite film catalytic material is prepared by utilizing the laser effect. The laser preparation realizes one-step synthesis and deposition load, has simple and rapid 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 by laser assistance.
Background
In previous studies, loading nano zero-valent iron on some solid supports, such as activated carbon, not only can enhance the stability of nano zero-valent iron, but also can change some of its physical properties. The iron-carbon material is synthesized mainly by physical mixing, sintering of carbon and iron precursors. The prior art is a ball milling method (CN 110065999A, CN 112604703B), wherein ferric salt and polymer are placed in a ball mill reaction kettle and are obtained under the action of mechanical forces such as friction, collision, impact and the like; or calcining the iron-containing metal framework by heat treatment (CN 111111661A, CN109179594B, CN111112638A, CN113019420 a), or high-pressure treating the iron-containing carbon precursor (CN 105110424A, CN113499776A, CN112548095A, CN110575815A, CN113877637A, CN109626722 a). The carbon shell is used for confining the metal nano particles and protecting the metal nano particles in a small space, so that the mutual aggregation of the metal particles is prevented, the metal particles are protected from the influence of external environment, and the problem that the nano metal particles cannot be stably in the air is solved. However, these preparation processes require a large amount of organic solvents, long-time calcination or high-pressure reaction, are time-consuming and consumable, and the preparation processes of the other methods are complicated and cumbersome except that the ball milling method can be used for one-step preparation. In addition, the prepared carbon shell and 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 important to find an iron-containing precursor which is cheap and easy to obtain. Ferrocene with sandwich structure has unique molecular structure and aromatic character, and has attracted great interest in chemistry around the world in the process of organic synthesis and material preparation because of its low cost. Ferrocene molecules, which consist of two cyclopentadiene radicals with one iron atom, are often used as carbon sources in the synthesis of materials. At present, no relevant report on preparing an iron-carbon composite film catalytic material by taking ferrocene as a carbon source and an iron source through laser assistance exists.
Disclosure of Invention
The invention solves the technical problem of providing a method for rapidly preparing the iron-carbon composite film catalytic material by laser assistance, which has simple process and better repeatability.
The invention adopts the following technical proposal to solve the technical problems, and a method for rapidly preparing an iron-carbon composite film catalytic material by laser assistance is characterized by comprising the following specific steps:
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, setting the frequency to be 120-180Hz, setting the scanning speed to be 60-90mm/S, introducing auxiliary gas for 3-8min, starting a rotating motor and the laser, and performing laser scanning treatment for 5-20S;
s3, after the laser processing in the step S2 is completed, setting the power of the laser to be 2% -8% of the total power, setting the frequency to be 120-180Hz, setting the scanning speed to be 60-90mm/S, starting a rotating motor and the laser, and performing laser scanning processing for 10-30min to obtain a quartz tube of the load 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, washing to remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material.
Further defined, 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 the first time to prepare the iron-carbon composite film catalytic material. 2. The laser preparation realizes one-step synthesis and deposition load, and the process is simple and rapid 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 of the iron-carbon composite film-loaded catalytic material prepared by the invention has stable performance in a circulating advanced oxidation system, and the process method has simple operation, strong repeatability and convenient batch production, thus having very high application prospect.
Drawings
FIG. 1 is an XRD pattern of a quartz tube carrying an iron-carbon composite thin film catalytic material obtained in examples 1 to 3;
FIG. 2 is a physical diagram of a quartz tube carrying the iron-carbon composite film catalytic material obtained in examples 1 to 3;
FIG. 3 is a graph showing the performance of the iron-carbon composite film-supported catalytic material of examples 1-3 in the high-grade oxidative degradation of tetracycline hydrochloride using a quartz tube as a catalyst.
Detailed Description
The above-described matters of the present invention will be described in further detail by way of examples, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples, and all techniques realized based on the above-described matters of the present invention are within 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
Step S1, placing ferrocene in a quartz tube, introducing air at one end of the quartz tube as auxiliary gas, 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;
step S2, performing first laser treatment, namely placing a quartz tube under a 1064nm laser (the total power is 30W), setting the power of the laser to be 60% of the total power, setting the frequency to be 150Hz, setting the scanning speed to be 75mm/S, introducing auxiliary gas for 5min, starting a rotating motor and the laser, and performing laser scanning treatment for 10S;
step S3, performing laser processing for the second time, after the laser processing in the step S2 is finished, setting the power of the laser to be 5% of the total power, setting the frequency to be 150Hz, setting the scanning speed to be 75mm/S, starting a rotating motor and the laser, and performing laser scanning processing for 10min to obtain a quartz tube loaded with the iron-carbon composite film;
and S4, placing the quartz tube loaded with the iron-carbon composite film in 2M sulfuric acid solution, soaking for 10 hours at 80 ℃, then sequentially soaking in deionized water and absolute ethyl alcohol, washing to 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 9:1 into one end of the quartz tube as auxiliary gas, 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;
step S2, performing first laser treatment, namely placing a quartz tube under a 1064nm laser (the total power is 30W), setting the power of the laser to be 60% of the total power, setting the frequency to be 150Hz, setting the scanning speed to be 75mm/S, introducing auxiliary gas for 5min, starting a rotating motor and the laser, and performing laser scanning treatment for 10S;
step S3, performing laser processing for the second time, after the laser processing in the step S2 is finished, setting the power of the laser to be 5% of the total power, setting the frequency to be 150Hz, setting the scanning speed to be 75mm/S, starting a rotating motor and the laser, and performing laser scanning processing for 10min to obtain a quartz tube loaded with the iron-carbon composite film;
and S4, placing the quartz tube loaded with the iron-carbon composite film in 2M sulfuric acid solution, soaking for 10 hours at 80 ℃, then sequentially soaking in deionized water and absolute ethyl alcohol, washing to remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material.
Example 3
Step S1, placing ferrocene into a quartz tube, introducing nitrogen at one end of the quartz tube as auxiliary gas, 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;
step S2, performing first laser treatment, namely placing a quartz tube under a 1064nm laser (the total power is 30W), setting the power of the laser to be 60% of the total power, setting the frequency to be 150Hz, setting the scanning speed to be 75mm/S, introducing auxiliary gas for 5min, starting a rotating motor and the laser, and performing laser scanning treatment for 10S;
step S3, performing laser processing for the second time, after the laser processing in the step S2 is finished, setting the power of the laser to be 5% of the total power, setting the frequency to be 150Hz, setting the scanning speed to be 75mm/S, starting a rotating motor and the laser, and performing laser scanning processing for 10min to obtain a quartz tube loaded with the iron-carbon composite film;
and S4, placing the quartz tube loaded with the iron-carbon composite film in 2M sulfuric acid solution, soaking for 10 hours at 80 ℃, then sequentially soaking in deionized water and absolute ethyl alcohol, washing to remove unreacted ferrocene, and finally drying to obtain the quartz tube loaded with the iron-carbon composite film catalytic material.
While the basic principles, principal features and advantages of the present invention have been described in the foregoing examples, it will be appreciated by those skilled in the art that the present invention is not limited by the foregoing examples, but is merely illustrative of the principles of the invention, and various changes and modifications can be made without departing from the scope of the invention, which is defined by the appended claims.
Claims (3)
1. A method for rapidly preparing an iron-carbon composite film catalytic material by laser assistance is characterized by comprising the following specific steps:
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, setting the frequency to be 120-180Hz, setting the scanning speed to be 60-90mm/S, introducing auxiliary gas for 3-8min, starting a rotating motor and the laser, and performing laser scanning treatment for 5-20S;
s3, after the laser processing in the step S2 is completed, setting the power of the laser to be 2% -8% of the total power, setting the frequency to be 120-180Hz, setting the scanning speed to be 60-90mm/S, starting a rotating motor and the laser, and performing laser scanning processing for 10-30min to obtain a quartz tube of the load 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, washing to 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 by laser assistance 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 by laser assistance according to claim 1, which is characterized in that: the acidic solution is sulfuric acid solution, nitric acid solution or 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 |
|---|
| Emission spectroscopy of carbon-covered iron nanoparticles in different gas atmospheres;K. Elihn et al.;《Applied Surface Science》;第186卷;573-577 * |
| Synthesis of Bare Iron Nanoparticles from Ferrocene Hexane Solution by Femtosecond Laser Pulses;Takuya Okamoto et al.;《ChemPhysChem》;第19卷(第19期);2480-2485 * |
| 激光辐照对二茂铁掺杂单壁碳纳米管的影响;张京等;《高等学校化学学报》;第34卷(第6期);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》.2014,(第7期),正文第33页4.1.1节. * |
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