Method for preparing magnetic micro-nano robot cluster through industrial iron mud pyrolysis
By preparing magnetic micro-nano robot clusters and using industrial iron sludge as raw material, the problem of high synthesis cost of micro-nano robot clusters is solved, and efficient and economical pollutant treatment and resource utilization are achieved.
Patent Information
- Application Number
- CN202510266213.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-07
- Publication Date
- 2025-08-05
AI Technical Summary
The synthesis process of micro-nano robot clusters is complex, which increases the industrial processing cost of actual products and thus increases the operating cost of water treatment processes.
Using industrial iron sludge as raw material, magnetic micro-nano robot clusters are prepared through steps such as concentration, dehydration, drying, crushing, screening, pyrolysis and magnetic collection, including calcination and freeze-drying treatment under a nitrogen atmosphere.
The resource utilization of industrial iron sludge has been realized, raw material and energy consumption has been reduced, and a high-active and controllable magnetic micro-nano robot cluster has been prepared, which has improved the efficiency of pollutant adsorption and degradation, and has the ability to accurately control and remote operation.
Smart Images
Figure CN120432289A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a method for preparing a magnetic micro-nano robot cluster, and belongs to the technical field of resource recycling of industrial iron sludge. Background Art
[0002] Over the past 15 years, with the rapid development of micro- and nanoscience, micro- and nanorobots, as an emerging interdisciplinary research field, have garnered widespread attention from researchers both domestically and internationally. Micro- and nanorobots are functional devices that utilize external physical or chemical fields at the micro- and nanoscale to convert environmental energy into mechanical energy, enabling autonomous motion. Micro- and nanorobots can be categorized by their actuation method: external physical field drive, chemical fuel drive, microbial drive, and hybrid drive. Physical field drive involves the active application of external physical fields, such as light, heat, electricity, magnetism, and ultrasound, to achieve autonomous control of the micro- and nanorobot. Due to their miniature structure and controllable autonomous motion, micro- and nanorobots exhibit significant application potential in environmental monitoring and remediation, targeted drug delivery, and minimally invasive surgery. In water remediation, micro- and nanorobots have been used as carrier materials in various processes, including adsorption, photocatalysis, and Fenton reaction, to remove heavy metals and recalcitrant organic pollutants such as microplastics and antibiotics. However, limited research exists on the preparation of micro- and nanorobots from solid waste. Therefore, the preparation of magnetic micro- and nanorobots from industrial iron sludge presents significant research potential. The limited activation effect of a single, dispersed micro-nanobot can hinder pollutant removal efficiency to a certain extent. Furthermore, precise movement control is difficult to achieve in a dispersed state. Forming a large number of micro-nanobots into a swarm with collective behavior can effectively address these issues. However, the complex synthesis process of micro-nanobot clusters increases the processing cost of actual product industrialization, thereby increasing the operating costs of water treatment processes. Therefore, it is imperative to seek efficient, green, and low-cost micro-nanobot cluster materials.
[0003] Iron is the fourth most abundant metallic element in the Earth's crust, after oxygen, silicon, and aluminum. It often occurs in nature as compounds. Iron and iron-based materials are widely used in advanced oxidation processes and other environmental water pollution remediation applications due to their high activation efficiency, relative nontoxicity, environmental friendliness, and low cost. Iron-based materials also possess excellent magnetic properties and are often used as the core of micro- and nanorobots, enabling precise control and remote operation under magnetic fields. Therefore, preparing iron-rich industrial sludge into micro- and nanorobot swarms not only mitigates the harm and resource waste caused by traditional sludge disposal methods to aquatic ecosystems, providing a viable solution for the green and environmentally friendly treatment of iron-rich industrial sludge, but also fully utilizes the resource properties of iron-rich industrial sludge to achieve resource utilization, creating low-cost, highly active, and controllable iron-based micro- and nanorobot swarms, saving raw material and synthesis costs. Furthermore, micro- and nanorobot technology can be fully utilized to efficiently adsorb or degrade pollutants, ultimately achieving more efficient, economical, and sustainable environmental pollution control. Summary of the Invention
[0004] In order to solve the problem that the complex synthesis process of micro-nano robot clusters increases the processing cost of actual product industrialization, thereby increasing the operating cost of the water treatment process, the present invention proposes a method for preparing magnetic micro-nano robot clusters by pyrolysis of industrial iron sludge.
[0005] The technical solution adopted by the present invention to solve the above problems is: the steps of the present invention include: Step 1: Concentrating and dehydrating the industrial iron-containing sludge to obtain a dehydrated sample; Step 2: Place the dehydrated sample in a blast drying oven and dry it to a constant weight, then grind it and pass it through a standard sieve to obtain a dry sludge sample; Step 3: Place the dry sludge sample in a crucible and place it in a vacuum atmosphere tubular resistance furnace and calcine under a nitrogen atmosphere at a heating rate of 10°C / min. After the temperature rises to a set temperature of 700-900°C, calcine at high temperature and then cool naturally to obtain an iron sludge-based biochar sample; Step 4: Use a magnet to collect the iron mud-based biochar sample in a directionally manner, wash it with deionized water and anhydrous ethanol, and then freeze-dry it to obtain an iron mud-based magnetic micro-nano robot cluster.
[0006] Furthermore, the industrial iron-containing sludge in step 1 is an iron-rich industrial sludge raw material obtained by biochemical treatment of industrial wastewater.
[0007] Furthermore, the water content of the dehydrated sludge sample in step 1 is 70%.
[0008] Furthermore, in step 2, the temperature of the blast drying oven is 105°C ± 5°C.
[0009] Furthermore, after grinding in step 2, the sludge was passed through a 200-mesh standard sieve to obtain a micro-nano dry sludge sample.
[0010] Furthermore, in step 3, the high-temperature calcination time is 2 hours after the tubular resistance furnace reaches the target temperature.
[0011] Furthermore, the sample after washing in step 4 was freeze-dried for 24 hours.
[0012] The beneficial effects of the present invention are: 1. The present invention can effectively transform industrial iron-containing sludge into magnetic micro-nano robot clusters, thereby realizing resource utilization of iron-rich industrial sludge. Through the pyrolysis and calcination process, it not only reduces the negative impact of sludge disposal on the water environment, but also avoids the resource waste and secondary pollution problems caused by traditional disposal methods such as landfill or incineration, meeting the requirements of green and environmentally friendly treatment. 2. This invention uses low-cost industrial sludge as raw material to produce highly active, controllable magnetic micro-nanorobot clusters through a simple pyrolysis and calcination process. Compared with traditional micro-nanorobot synthesis methods, the use of solid waste (industrial iron sludge) to prepare micro-nanorobots not only reduces raw material procurement costs but also reduces energy consumption during the synthesis process, thereby improving the cost-effectiveness and sustainability of the preparation process. 3. The magnetic micro-nano robot clusters prepared by the pyrolysis process of the present invention have excellent magnetic properties and a large specific surface area. These magnetic micro-nano robot clusters can efficiently adsorb and degrade harmful substances in water. They are particularly effective in environmental pollution control applications such as wastewater treatment and heavy metal removal, improving the efficiency and cost-effectiveness of sewage treatment processes. 4. The magnetic micro-nano robot clusters prepared by the present invention can be precisely controlled and remotely operated through an external magnetic field; the high magnetism of such micro-nano robot clusters gives them broad application potential in fields such as medicine and environmental remediation, especially through magnetic operation, which can achieve more precise and efficient pollutant degradation and targeted removal. BRIEF DESCRIPTION OF THE DRAWINGS
[0013] Figure 1 This is a comparison of the hysteresis loops of the iron mud-based magnetic micro-nano robot cluster and the unpyrolyzed dry sludge sample; Figure 2 This is a scanning electron microscope image of an iron mud-based magnetic micro-nano robot cluster; Figure 3 This is the energy spectrum of the iron mud-based magnetic micro-nano robot cluster; Figure 4 is a scanning electron microscope image of the unpyrolyzed dry sludge sample. DETAILED DESCRIPTION
[0014] Specific implementation method 1: Figures 1 to 4 As shown, a method for preparing a magnetic micro-nano robot cluster by pyrolysis of industrial iron sludge comprises the following steps: Step 1: Concentrating and dehydrating the industrial iron-containing sludge to obtain a dehydrated sample; Industrial iron-containing sludge is the iron-rich industrial sludge raw material obtained after biochemical treatment of industrial wastewater; The moisture content of the dewatered sludge sample was 70%; Step 2: Place the dehydrated sample in a blast drying oven and dry it to a constant weight, then grind it and pass it through a standard sieve to obtain a dry sludge sample; The temperature of the blast drying oven is 105℃±5℃; After grinding, the sample was passed through a 200-mesh standard sieve to obtain a micro-nanoscale dry sludge sample; Step 3: Place the dry sludge sample in a crucible and place it in a vacuum atmosphere tubular resistance furnace and calcine under a nitrogen atmosphere at a heating rate of 10°C / min. After the temperature rises to a set temperature of 700-900°C, calcine at high temperature and then cool naturally to obtain an iron sludge-based biochar sample; The high-temperature calcination time is 2 hours after the tubular resistance furnace reaches the target temperature; Step 4: Use a magnet to collect the iron mud-based biochar sample in a directionally manner, wash it with deionized water and anhydrous ethanol, and then freeze-dry it for 24 hours to obtain an iron mud-based magnetic micro-nano robot cluster.
[0015] Example Example 1 The industrial iron-containing sludge is concentrated and dehydrated to obtain a sludge dehydrated sample; The dehydrated sludge sample was placed in a forced air drying oven and dried at 105°C ± 5°C to a constant weight, then crushed in a grinder and further ground in a mortar, and sieved through 200 mesh to obtain a dry sludge sample; The vacuum atmosphere tubular resistance furnace was purged with nitrogen at a flow rate of 100 mL / min for 40 min, and then 5.0 g of dry sludge sample was weighed and placed in a crucible. The crucible was placed in a vacuum atmosphere tubular resistance furnace and calcined under nitrogen atmosphere at a heating rate of 10 °C / min. After the temperature was raised to the set temperature (800 °C), it was calcined at high temperature for 2 h and then naturally cooled to obtain an iron sludge-based biochar sample. The iron mud-based biochar samples were collected using a magnet, washed with deionized water and anhydrous ethanol, and then freeze-dried for 24 hours to obtain an iron mud-based magnetic micro-nanorobot cluster (MMG-800).
[0016] The magnetic properties of the MMG-800 prepared in this example and the dry sludge sample without pyrolysis were measured using a vibrating sample magnetometer. Figure 1 This is a comparison diagram of hysteresis loops. Figure 1It can be clearly seen that the magnetic properties of MMG-800 are significantly higher than those of the non-pyrolyzed dry sludge sample. MMG-800 has excellent magnetic properties and can be precisely controlled and remotely operated through an external magnetic field.
[0017] Example 2 The industrial iron-containing sludge is concentrated and dehydrated to obtain a sludge dehydrated sample; The dehydrated sludge sample was placed in a forced air drying oven and dried at 105°C ± 5°C to a constant weight, then crushed in a grinder and further ground in a mortar, and sieved through 200 mesh to obtain a dry sludge sample; The vacuum atmosphere tubular resistance furnace was purged with nitrogen at a flow rate of 100 mL / min for 40 min, and then 5.0 g of dry sludge sample was weighed and placed in a crucible. The crucible was placed in a vacuum atmosphere tubular resistance furnace and calcined under nitrogen atmosphere at a heating rate of 10 °C / min. After the temperature rose to the set temperature (900 °C), it was calcined at high temperature for 2 h and then naturally cooled to obtain an iron sludge-based biochar sample. The iron mud-based biochar samples were collected using a magnet, washed with deionized water and anhydrous ethanol, and then freeze-dried for 24 hours to obtain an iron mud-based magnetic micro-nanorobot cluster (MMG-900).
[0018] The iron mud-based magnetic micro-nano robot clusters prepared in Example 1 and Example 2 were observed using SEM-EDS. Figure 2 This is a scanning electron microscope image of an iron mud-based magnetic micro-nano robot cluster. Figure 3 This is the energy spectrum of the iron mud-based magnetic micro-nano robot cluster. Figure 2 It can be clearly seen that the surface structure of MMG-800 and MMG-900 is rough and porous, with obvious pore structure and high porosity and specific surface area. Figure 3 It can be clearly seen that the inner and outer surfaces of MMG-800 and MMG-900 are rich in active nano-iron particles, which serve as catalytic reaction sites and provide strong magnetism.
[0019] The dry sludge samples that were not pyrolyzed were observed. Figure 4 This is a scanning electron microscope image of the unpyrolyzed dry sludge sample. It can be seen from the image that the surface of the unpyrolyzed dry sludge sample is relatively smooth and there is almost no attachment.
[0020] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Although the present invention has been disclosed as a preferred embodiment as above, it is not intended to limit the present invention. Any technician familiar with the present profession can make some changes or modifications to equivalent embodiments of equivalent changes using the technical content disclosed above without departing from the scope of the technical solution of the present invention. However, any simple modification, equivalent replacement and improvement of the above embodiments made according to the technical essence of the present invention, within the spirit and principles of the present invention, without departing from the content of the technical solution of the present invention, shall still fall within the scope of protection of the technical solution of the present invention.
Claims
1. A method for preparing magnetic micro-nano robot clusters by pyrolysis of industrial iron sludge, characterized in that: The specific steps include: Step 1: Concentrating and dehydrating the industrial iron-containing sludge to obtain a dehydrated sample; Step 2: Place the dehydrated sample in a blast drying oven and dry it to a constant weight, then grind it and pass it through a standard sieve to obtain a dry sludge sample; Step 3: Place the dry sludge sample in a crucible and place it in a vacuum atmosphere tubular resistance furnace and calcine under a nitrogen atmosphere at a heating rate of 10°C / min. After the temperature rises to a set temperature of 700-900°C, calcine at high temperature and then cool naturally to obtain an iron sludge-based biochar sample; Step 4: Use a magnet to collect the iron mud-based biochar sample in a directionally manner, wash it with deionized water and anhydrous ethanol, and then freeze-dry it to obtain an iron mud-based magnetic micro-nano robot cluster.
2. The method for preparing magnetic micro-nano robot clusters by pyrolysis of industrial iron sludge according to claim 1, characterized in that: The industrial iron-containing sludge in step 1 is an iron-rich industrial sludge raw material obtained after biochemical treatment of industrial wastewater.
3. The method for preparing magnetic micro-nano robot clusters by pyrolysis of industrial iron sludge according to claim 1, characterized in that: The moisture content of the dehydrated sludge sample in step 1 is 70%.
4. The method for preparing magnetic micro-nano robot clusters by pyrolysis of industrial iron sludge according to claim 1, characterized in that: In step 2, the temperature of the blast drying oven is 105°C ± 5°C.
5. The method for preparing magnetic micro-nano robot clusters by pyrolysis of industrial iron sludge according to claim 1, characterized in that: After grinding in step 2, the sludge was passed through a 200-mesh standard sieve to obtain a micro-nanoscale dry sludge sample.
6. The method for preparing magnetic micro-nano robot clusters by pyrolysis of industrial iron sludge according to claim 1, characterized in that: In step 3, the high-temperature calcination time is 2 hours after the tubular resistance furnace reaches the target temperature.
7. The method for preparing magnetic micro-nano robot clusters by pyrolysis of industrial iron sludge according to claim 1, characterized in that: After washing in step 4, the samples were freeze-dried for 24 hours.