A method for improving FeSiB amorphous rib and degrading active red 195 dye

Abstract

The application discloses a method for improving FeSiB amorphous strips and degrading active red 195 dyes. 78 Si9B 13 Alloy is spun into amorphous strips; then, the original amorphous strips are treated by 80W pulse laser to form novel amorphous structure strip catalysts with nanoscale unevenness. The novel amorphous structure strip catalysts have higher reaction rates in catalytic degradation of active red 195 dye solutions than the original amorphous strips, and still have high catalytic degradation rates (k) under the condition of small surface area dosage. In addition, the novel amorphous structure catalysts with nanoscale unevenness have excellent repeatability and self-renewal characteristics. The application effectively improves the application performance of iron-based amorphous materials, makes the iron-based amorphous alloys have higher actual production value, plays a greater role of the iron-based amorphous alloys, and has wide application prospects.

Description

Technical Field

[0001] This invention belongs to the field of organic dye catalytic degradation technology, specifically relating to a method for improving Fe 78 Si9B 13 Amorphous strips, their preparation method, and a method for degrading Reactive Red 195 dye based on the amorphous strips. Background Technology

[0002] The information disclosed in this background section is intended only to enhance understanding of the overall background of the invention and is not necessarily to be construed as an admission or in any way implying that such information constitutes prior art known to those skilled in the art.

[0003] Amorphous alloys are formed by ultra-rapid solidification. During solidification, the atoms do not have enough time to arrange themselves in an orderly manner for crystallization, resulting in a solid alloy with a long-range disordered structure. The molecules (or atoms, ions) that make up the alloy do not exhibit a spatially regular periodicity, and there are no grains or grain boundaries present in crystalline alloys. These amorphous alloys possess many unique properties, and due to their excellent performance and simple processing, they have become a key focus of research and development in materials science both domestically and internationally since the 1980s. Because amorphous alloys are formed far from equilibrium, they possess high residual stress and a large number of unsaturated surface sites. Therefore, their metastable properties endow amorphous alloys with excellent catalytic degradation performance, thus showing great application potential.

[0004] With industrial development, increasing amounts of industrial wastewater are being discharged into the environment, especially dyeing and printing wastewater, causing serious environmental pollution. Amorphous alloys, due to their unique structure and properties, exhibit certain catalytic degradation activity for dye wastewater. Reactive Red 195 dye is widely used in chemical indicators, dyes, biological stains, and pharmaceuticals; direct discharge of its wastewater into the environment will cause severe pollution. Currently, research on metal catalysts for the catalytic degradation of Reactive Red 195 dye solutions is limited. The most widely studied approach is the use of FeSiB amorphous alloy catalysts for the catalytic degradation of Reactive Red 195 dye solutions; however, the catalytic degradation rate and reusability remain key factors limiting its application.

[0005] Pulsed laser processing is a complex high-temperature, transient, and nonlinear process involving the combined effects of melting and solidification, melt convection and conduction, and surface tension. Different laser energies and alloy materials all affect the processing results. Currently, there is no systematic research on laser processing technology for amorphous alloys. Developing effective control over the structure and morphology of amorphous alloys using laser processing technology is also of great significance for expanding the applications of iron-based alloys. Summary of the Invention

[0006] Therefore, in order to improve the catalytic degradation ability of FeSiB amorphous alloy system, this invention uses a nanosecond-level ultrashort pulse laser to perform pulsed laser treatment on the surface of the original FeSiB amorphous alloy. By designing a reasonable pulsed laser treatment power, the nanoscale structure of the amorphous alloy surface is specifically improved. This nanoscale non-uniform structure can not only improve the rate of catalytic degradation of Reactive Red 195 dye solution, but also effectively increase the reusability of the amorphous alloy.

[0007] Based on the above-mentioned technical effects, the present invention provides the following technical solution:

[0008] Firstly, a method to improve Fe 78 Si9B 13 The preparation method of amorphous ribbons includes the following steps: according to Fe 78 Si9B 13 The atomic ratios of Fe, Si, and B are weighed and smelted into an alloy ingot. The original Fe is then obtained by rapid cooling. 78 Si9B 13 Amorphous strips; using 70–90W power to process the original Fe... 78 Si9B 13 It is obtained by pulsed laser treatment on the surface of amorphous strips.

[0009] This invention reveals that during pulsed laser treatment with varying powers, the near-surface layer of the original amorphous strips undergoes ultra-rapid melting and solidification at the microscale. Under different pulsed laser power conditions, some atoms in the original amorphous strips gradually evolve from a loose and disordered state to a tightly packed state, forming a novel amorphous catalyst with nanoscale inhomogeneity, where nanoscale crystals and an amorphous matrix coexist. Based on this discovery, this invention investigates the power of the pulsed laser treatment. In embodiments with better results, the amorphous catalyst formed by treatment with 70–90 W power exhibits a high catalytic degradation rate and can be reused multiple times. In examples with better results, the pulsed laser treatment power is 78 W, 79 W, 80 W, 81 W, or 82 W, with 80 W being the most preferred.

[0010] The original Fe in the above preparation method 78 Si9B 13 Amorphous ribbons can be produced using conventional amorphous ribbon manufacturing processes. In one embodiment provided by this invention, the original Fe... 78 Si9B 13 The specific steps for preparing amorphous ribbons are as follows:

[0011] Fe, Si, and B with a purity of 98.8%-99.9% were selected and melted into an alloy ingot in a vacuum electric arc furnace. The alloy ingot was then heated and melted by an induction coil. The linear velocity of the copper roller was set to 3-40 m / s, and the molten liquid was sprayed onto the copper roller to obtain the original Fe. 78 Si9B 13 Amorphous stripes.

[0012] Furthermore, the vacuum degree in the aforementioned vacuum electric arc furnace is 4–6 × 10⁻⁶. -3 Pa is filled with an inert gas, such as argon.

[0013] In addition, the pulsed laser processing described in the above method is implemented using a pulsed laser, specifically a nanosecond-level ultrashort pulse laser.

[0014] Secondly, it provides improved Fe prepared by the method described in the first aspect. 78 Si9B 13 Amorphous stripes.

[0015] Thirdly, a method for the catalytic degradation of Reactive Red 195 dye is provided, comprising the following steps: adding the Fe-modifying agent described in the second aspect to the wastewater to be degraded. 78 Si9B 13 Amorphous stripes, degraded using an advanced persulfate oxidation process.

[0016] Existing advanced persulfate oxidation processes utilize UV ​​activation or the generation of sulfate and carbonate free radicals from sulfates to promote rapid dye degradation. However, Reactive Red 195 has a more complex structure than typical azo and anthraquinone dyes, making it difficult to achieve ideal degradation results using advanced oxidation processes alone. This invention introduces an improvement in Fe... 78 Si9B 13 Amorphous strips provide abundant catalytic interfaces for the above oxidation reactions, which can effectively improve the catalytic degradation rate.

[0017] Feasible persulfates include sodium persulfate and potassium persulfate, with sodium persulfate being the most commonly used. In one embodiment of the present invention, the catalytic degradation method comprises the following steps: [The text abruptly ends here, likely due to an incomplete sentence or missing information.] 78 Si9B 13 Amorphous strips and sodium persulfate are added to the wastewater to be degraded, and degradation is carried out in conjunction with ultraviolet irradiation. The concentration of sodium persulfate is preferably 1-3 mM, and the wavelength of ultraviolet light is 200-400 nm.

[0018] Fourthly, an advanced oxidation wastewater treatment apparatus is provided, the apparatus having an oxidation tank for treating wastewater containing dyes based on the method described in the third aspect.

[0019] Wastewater treatment equipment based on advanced oxidation processes is currently an important tool in wastewater treatment. The research results of this invention also provide feasible implementation methods for improving wastewater treatment devices, such as incorporating the aforementioned improved Fe... 78 Si9B 13 Amorphous strips are applied to the inner wall of oxidation tanks or laid on the surface of the stirring device in oxidation tanks, which improves the cost relatively low and also improves Fe 78 Si9B 13 Amorphous strips can continuously achieve wastewater treatment effects, reducing the frequency of equipment replacement or maintenance.

[0020] The beneficial effects of one or more of the above technical solutions are:

[0021] This invention effectively improves the application performance of iron-based amorphous materials, enabling iron-based amorphous alloys to have higher practical production value, play a greater role, and have broad application prospects. Attached Figure Description

[0022] The accompanying drawings, which form part of this invention, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an improper limitation of the invention.

[0023] Figure 1 Fe in Example 1 78 Si9B 13 XRD patterns of the strips after processing with pulsed lasers of 40W and 80W;

[0024] Figure 2 The original Fe in Example 1 78 Si9B 13 TEM characterization and corresponding SAED images of the strips after processing with pulsed lasers of 40W and 80W;

[0025] Wherein, (a) is the original Fe 78 Si9B 13 TEM image of the bands, (a1) is the original Fe 78 Si9B 13 SAED plot of the strips;

[0026] (b) is a TEM image of the strip after 40W pulsed laser treatment, and (b1) is a SAED image of the strip after 40W pulsed laser treatment.

[0027] (c) is a TEM image of the strip after 80W pulsed laser processing, (c1) is a SAED image of the strip after 80W pulsed laser processing, (c2) is a TEM image of the strip after 80W pulsed laser processing under different fields of view, and (c3) is a TEM image of the strip after 80W pulsed laser processing under different fields of view.

[0028] Figure 3 Fe in Example 1 78 Si9B 13 Verification of the effect of amorphous strips on the degradation of Reactive Red 194 dye;

[0029] Among them, (a) original Fe 78 Si9B 13 The normalized concentration C of the solution of the amorphous strip catalytic degradation of Reactive Red 195 dye after treatment with pulsed lasers of 40W and 80W was obtained. t / C0 change;

[0030] (b) Primitive Fe 78 Si9B 13 The degradation rate (k) of the amorphous strips after being treated with pulsed lasers of 40W and 80W for the catalytic degradation of Reactive Red 195 dye solution;

[0031] (c) Electron paramagnetic resonance (EPR) curves;

[0032] (d) Primitive Fe 78 Si9B 13 The efficiency of amorphous strips in generating catalytic degradation groups after being treated with an 80W pulsed laser;

[0033] Figure 4 For the original Fe 78 Si9B 13 Amorphous stripes and improved Fe 78 Si9B 13 The relationship between the number of repetitions of the catalytic degradation of Reactive Red 195 dye solution by amorphous strips and the degradation efficiency at 5 min and 20 min, respectively;

[0034] Figure 5 For the original Fe 78 Si9B 13 Amorphous stripes and improved Fe 78 Si9B 13 Changes in SEM surface morphology and elemental content of the amorphous strip catalyst during repeatability testing of reactive red 195 dye solution degradation;

[0035] Wherein, (a) is the original Fe 78 Si9B 13 SEM image of amorphous stripes;

[0036] (b) represents the original Fe 78 Si9B 13 SEM images of amorphous strips reused 5 times;

[0037] (c) represents the original Fe 78Si9B 13 SEM images of amorphous strips after 10 reuses;

[0038] (d) represents the original Fe 78 Si9B 13 SEM images of amorphous strips after 15 reuses;

[0039] (e) represents the original Fe 78 Si9B 13 SEM images of amorphous strips after 20 reuses;

[0040] (f) represents the original Fe. 78 Si9B 13 Elemental surface scans of amorphous strips after 20 repeated SEM scans, from left to right: alloy surface, Fe, Si, B, O, S elemental scan results;

[0041] (g) is the original SEM image of the strip after processing with an 80W pulsed laser;

[0042] (h) is a SEM image of the strip after 5 reuses following 80W pulsed laser processing;

[0043] (i) is a SEM image of the strip after 10 reuses following 80W pulsed laser processing;

[0044] (j) is a SEM image of the strip after 15 reuses following 80W pulsed laser processing;

[0045] (k) is a SEM image of the strip after 20 reuses following 80W pulsed laser processing;

[0046] (l) is an elemental surface scan of the strip after 20 repeated SEM scans following 80W pulsed laser processing. From left to right, the scan results are for alloy surface, Fe, Si, B, O, and S elements. Detailed Implementation

[0047] It should be noted that the following detailed descriptions are exemplary and intended to provide further illustration of the invention. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

[0048] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of exemplary embodiments according to the invention. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0049] To enable those skilled in the art to more clearly understand the technical solution of the present invention, the technical solution of the present invention will be described in detail below with reference to specific embodiments. The testing equipment information involved in the following embodiments is as follows:

[0050] Furnace type: Vacuum electric arc furnace (MAM-1Edmund Buhler).

[0051] Copper roller spinning machine type: High vacuum single roller spin quenching and spray casting system (SD500).

[0052] Magnetic stirrer type: heated magnetic stirrer (78-1).

[0053] Ultraviolet radiation equipment type: Simulated sunlight xenon lamp light source (PL-X500)

[0054] Example

[0055] In this embodiment, the focus is on improving Fe 78 Si9B 13 The processing technology and catalytic activity of amorphous ribbons were investigated: 1. Improving Fe 78 Si9B 13 Preparation of amorphous strips

[0056] (1) Fe, Si, and B with a purity range of 98.8 wt.%-99.9 wt.% were weighed according to their atomic ratio, and then the mass was measured under a vacuum of 5 × 10⁻⁶. -3 Fe was smelted in a vacuum arc furnace filled with argon gas to produce 5g of Fe. 78 Si9B 13 Alloy ingots;

[0057] (2) Fe 78 Si9B 13 The alloy ingot was placed in a quartz tube and heated and melted using an induction coil. When the linear velocity of the copper roller was 36 m / s, the already molten Fe... 78 Si9B 13 The alloy is sprayed onto a copper roller to obtain the original Fe. 78 Si9B 13 Amorphous strips;

[0058] (3) Using nanosecond-level ultrashort pulse lasers at power levels of 40W and 80W respectively, the original Fe was subjected to irradiation. 78 Si9B 13 Pulsed laser treatment of the surface of amorphous strips yields improved Fe 78 Si9B 13 Amorphous stripes.

[0059] 2. Degradation of Reactive Red 195 dye

[0060] (1) Prepare a Reactive Red 195 dye solution with a concentration of 100 mg / L and a sodium persulfate concentration of 2 mM in a 500 mL volumetric flask using deionized water;

[0061] (2) Pour 100 mL of the prepared Reactive Red 195 dye solution into a 250 mL reaction vessel, and then add the Fe... 78 Si9B 13 The amorphous ribbon was cut into 1.5cm lengths, and 50mg of the amorphous ribbon was weighed and added to a reaction vessel containing a Reactive Red 195 dye solution. The temperature was controlled at 25℃, accompanied by ultraviolet radiation and magnetic stirring.

[0062] (3) At regular intervals, 3 mL of Reactive Red 195 dye solution was drawn from the beaker using a disposable syringe and the catalytic degradation was detected using a UV-Vis spectrophotometer to determine the different types of Fe. 78 Si9B 13 The catalytic degradation effect of amorphous strips on Reactive Red 195 dye solution.

[0063] This embodiment first uses X-ray diffraction (XRD) analysis to verify the original Fe... 78 Si9B 13 The strips exhibit an amorphous structure, and XRD results after treatment with pulsed lasers of varying powers show only a single diffuse scattering peak, indicating that the Fe treated with pulsed lasers... 78 Si9B 13 The near-surface layer of the strips also exhibits an amorphous structure. Figure 1 (Note: Nanocrystals are too small to be detected by XRD.)

[0064] To more intuitively observe the changes in the near-surface nanoscale structure of the strip during pulsed laser treatment with different powers, this embodiment presents the changes through transmission electron microscopy (TEM). First, the original Fe... 78 Si9B 13 The high-resolution images of the amorphous stripes show a uniform, disordered atomic structure, and selected area electron diffraction (SAED) reveals very standard amorphous diffraction halos. Figure 2 Secondly, after treatment with a 40W pulsed laser, the near-surface layer atoms of the strip gradually evolved into a nanocrystal-like structure, and the SAED image showed nanocrystal rings of the (200) crystal plane of α-Fe. Finally, after treatment with an 80W pulsed laser, the near-surface layer atoms of the strip evolved into a novel amorphous structure with very obvious nanocrystals and amorphous matrix coexisting, exhibiting nanoscale inhomogeneity, and the SAED image simultaneously showed nanocrystal rings of the (200), (110), and (220) crystal planes of α-Fe.

[0065] During the catalytic degradation reaction, the catalytic degradation rate (k) of the novel amorphous strip with nanoscale inhomogeneity after treatment with an 80W pulsed laser was much higher than that of the original uniform amorphous strip. Figure 3 Furthermore, statistical analysis revealed that the novel amorphous catalyst with nanoscale inhomogeneity prepared in this embodiment, compared to other amorphous alloys, crystalline alloys, and oxide catalysts, still exhibits a high catalytic degradation rate (k) even with a very small surface area. The statistical results are shown in Table 1 below.

[0066] Table 1 Improvement of Fe 78 Si9B 13 Statistical comparison of surface area and catalytic degradation rate (k) of amorphous strips (80W) with other amorphous alloys, crystalline alloys and oxide catalysts.

[0067]

[0068]

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[0095] This is related to the fact that novel amorphous catalysts with nanoscale inhomogeneity can improve the rate of generation of catalytically degradable radicals. Therefore, the hydroxyl radicals (·OH) and sulfate radicals (SO4) generated during the reaction were qualitatively and quantitatively analyzed by electron paramagnetic resonance (EPR). - The sum of the results showed that the novel amorphous catalyst with nanoscale inhomogeneity generated catalytic degradation groups at a higher rate than the original uniform amorphous strip catalyst. Analysis of the results indicates that the nanoscale structure of this novel amorphous catalyst with nanoscale inhomogeneity is more conducive to the chemical reaction, i.e., the rapid generation of catalytic degradation groups. Furthermore, in the reusability test, the novel amorphous catalyst with nanoscale inhomogeneity prepared in this embodiment showed better reusability efficiency than the original uniform amorphous strip catalyst. Figure 4 ).from Figure 4 The results show that improving Fe 78 Si9B 13 The amorphous strip (80W) showed an improved catalytic degradation efficiency again after 18 reuses. To investigate the reason for this phenomenon, this example focuses on the original Fe...78 Si9B 13 Amorphous stripes and improved Fe 78 Si9B 13 The SEM surface morphology and elemental composition changes of the amorphous (80W) strip catalyst during the repeatability test of the catalytic degradation of Reactive Red 195 dye solution were measured. The results are as follows: Figure 5 As shown, improving Fe 78 Si9B 13 The amorphous strip (80W) surface catalyst exhibits the ability to automatically detach the oxide layer after repeated use, exposing a fresh substrate, which can restore the catalytic degradation rate and has significant and unique application prospects.

[0096] Example 2

[0097] In this embodiment, an improved Fe 78 Si9B 13 The preparation method of amorphous ribbons and the degradation method of Reactive Red 195 include the following parts:

[0098] 1. Improve Fe 78 Si9B 13 Preparation of amorphous strips

[0099] (1) Fe, Si, and B with a purity range of 98.8 wt.%-99.9 wt.% were weighed according to their atomic ratio, and then the mass was measured under a vacuum of 5 × 10⁻⁶. -3 Pa and argon-filled vacuum arc furnace smelting into Fe 78 Si9B 13 Alloy ingots;

[0100] (2) Fe 78 Si9B 13 The alloy ingot was placed in a quartz tube and heated and melted using an induction coil. When the linear velocity of the copper roller was 36 m / s, the already molten Fe... 78 Si9B 13 The alloy is sprayed onto a copper roller to obtain the original Fe. 78 Si9B 13 Amorphous strips;

[0101] (3) Using a nanosecond-level ultrashort pulse laser at a power of 80W to irradiate pristine Fe 78 Si9B 13 Pulsed laser treatment of the surface of amorphous strips yields improved Fe 78 Si9B 13 Amorphous stripes.

[0102] 2. Degradation of Reactive Red 195 dye

[0103] The above-mentioned Fe-improving agents were added to the wastewater to be treated. 78 Si9B 13 Amorphous stripes and sodium persulfate enable the concentration of sodium persulfate in the wastewater to reach 2 mM, improving the wastewater's interaction with Fe... 78 Si9B 13 The amorphous ribbon was added at a ratio of 100 mL: 50 mg; under ultraviolet light irradiation and with stirring, degradation was carried out, and the degradation was completed in 20 minutes.

[0104] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for the catalytic degradation of Reactive Red 195 dye, characterized in that, The steps include: adding Fe to the wastewater to be degraded. 78 Si9B 13 Amorphous strips, degraded using an advanced persulfate oxidation process; The improvement of Fe 78 Si9B 13 The preparation method of amorphous ribbons includes the following steps: selecting Fe, Si, and B with a purity of 98.8 wt.%-99.9 wt.% and melting them into an alloy ingot in a vacuum arc furnace; heating and melting the alloy ingot through an induction coil; setting the linear velocity of the copper roller to 3~40 m / s; and spraying the molten liquid onto the copper roller to obtain the original Fe. 78 Si9B 13 Amorphous strips; using 70~90W power to process raw Fe 78 Si9B 13 The amorphous strip surface is obtained by pulsed laser treatment. The improvement of Fe 78 Si9B 13 Amorphous stripes form nanoscale crystals and amorphous substrates, resulting in nanoscale inhomogeneous amorphous structures. Fe with nanoscale inhomogeneity 78 Si9B 13 Amorphous strips can improve the rate of generating catalytic degradation groups. After repeated use, the oxide layer automatically peels off, allowing the catalytic degradation rate to recover.

2. The catalytic degradation method for Reactive Red 195 dye as described in claim 1, characterized in that, The processing power of the pulsed laser is 78W, 79W, 80W, 81W or 82W.

3. The catalytic degradation method for Reactive Red 195 dye as described in claim 1, characterized in that, The vacuum degree in the vacuum electric arc furnace is 4~6×10⁻⁶. -3 Pa is filled with inert gas.

4. The catalytic degradation method for Reactive Red 195 dye as described in claim 1, characterized in that, The pulsed laser processing is achieved using a nanosecond-level ultrashort pulse laser.

5. The catalytic degradation method for Reactive Red 195 dye as described in claim 1, characterized in that, The persulfate is selected from sodium persulfate and potassium persulfate.

6. The catalytic degradation method for Reactive Red 195 dye as described in claim 5, characterized in that, The catalytic degradation method comprises the following steps: [The steps are described in the original text, which is incomplete and likely refers to a specific process involving Fe...] 78 Si9B 13 Amorphous strips and sodium persulfate are added to the wastewater to be degraded, and degradation is carried out in conjunction with ultraviolet irradiation. The concentration of sodium persulfate is 1~3mM, and the wavelength of ultraviolet light is 200~400nm.

7. An advanced oxidation wastewater treatment device, characterized in that, The apparatus has an oxidation tank that treats wastewater containing dyes according to the method of any one of claims 1-6.

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