A method for preparing a water treatment agent and its dynamic temperature control system

Abstract

A method for preparing a water treatment agent and its dynamic temperature control system are disclosed. The method comprises a substrate material, an adsorbent material, and a magnetic material to form a water treatment agent with a core-shell structure. The substrate material is cellulose, including microcrystalline cellulose, microfiber cellulose, cellulose nanofibers, cellulose nanocrystals, and biochar fiber. The adsorbent material is a hydroxide adsorbent, including aluminum hydroxide, magnesium hydroxide, iron hydroxide, and calcium hydroxide. The magnetic material includes γ-ferric oxide, iron(II,III) oxide, and nickel-zinc ferrite. The method for preparing the water treatment agent and its dynamic temperature control system of this invention, by combining the substrate material, adsorbent material, and magnetic material into a water treatment agent with a core-shell structure, not only exhibits excellent heavy metal ion removal performance but also allows for the separation of precipitates from the water body using an external magnetic field, without generating secondary pollution.

Description

Technical Field

[0001] This invention belongs to the field of water treatment agent technology, specifically relating to a method for preparing a water treatment agent and a dynamic temperature control system used in the preparation method of the water treatment agent. Background Technology

[0002] Water pollution is one of the most serious environmental problems, and industrial water pollution is a significant part of it. Industrial wastewater contains large amounts of heavy metal ions, which, through the food chain, ultimately threaten human health. Therefore, finding economical, effective, and convenient methods to remove heavy metal ions from industrial wastewater is urgently needed.

[0003] Adsorption methods have stood out among numerous water treatment methods due to their simplicity and high removal efficiency. Exploring the use of highly efficient adsorbents in industrial wastewater treatment is of practical significance. Currently, many adsorbents with advantages such as being environmentally friendly, abundant, and low in preparation cost are available on the market, including Mg(OH)2-type adsorbents. However, a drawback of these adsorbents is that after wastewater treatment, the resulting heavy metal precipitates still remain in the water body, increasing the risk of further water pollution.

[0004] To address this issue, this invention employs a loading method to obtain a magnetic water treatment agent, ensuring efficient removal of heavy metal ions and rapid separation from the solution. After water treatment is completed, the agent is placed in a magnetic field, which can carry heavy metal precipitates and separate them from the water.

[0005] Furthermore, hydrothermal treatment is a crucial step in the preparation of water treatment agents, and the precision of temperature control significantly impacts the quality of the agent. Therefore, this invention also designs a dynamic temperature control system for precisely controlling the temperature during the preparation of water treatment agents. Summary of the Invention

[0006] Purpose of the invention: In order to overcome the above shortcomings, the purpose of this invention is to provide a method for preparing a water treatment agent and its dynamic temperature control system. The design is reasonable. By using the above preparation method and dynamic temperature control system, the substrate material, adsorbent material and magnetic material are combined to form a water treatment agent with a core-shell structure. It not only has excellent heavy metal ion removal performance, but also can separate the precipitate from the water with the help of an external magnetic field, without generating secondary pollution, and has broad application prospects.

[0007] The objective of this invention is achieved through the following technical solution:

[0008] A method for preparing a water treatment agent involves combining a substrate material, an adsorbent material, and a magnetic material to form a water treatment agent with a core-shell structure. The substrate material is cellulose, including microcrystalline cellulose, microfiber cellulose, cellulose nanofibers, cellulose nanocrystals, and biochar fiber. The adsorbent material is a hydroxide adsorbent, including aluminum hydroxide, magnesium hydroxide, iron hydroxide, and calcium hydroxide. The magnetic material includes iron(II,III) oxide, γ-ferric oxide, and nickel-zinc ferrite.

[0009] The method for preparing the water treatment agent described in this invention involves combining a substrate material, an adsorbent material, and a magnetic material to form a water treatment agent with a core-shell structure. The substrate material is cellulose, which is rich in functional groups such as -OH, providing convenient conditions for binding various substances. An adsorbent such as a hydroxide adsorbent is loaded onto the cellulose. When the hydroxide adsorbent precipitates heavy metals, the resulting heavy metal hydroxides interact with the cellulose, causing the heavy metal precipitate to adhere to the cellulose. The magnetic material imparts magnetism to the water treatment agent. After water treatment, the agent is placed in a magnetic field, whereby the cellulose, under the influence of the magnetic material, carries the magnetic material and the heavy metal precipitate away from the water, effectively preventing secondary pollution of the water.

[0010] Cellulose includes, but is not limited to, microcrystalline cellulose (MCC), microfiber cellulose (MFC), cellulose nanofibers (CNF), cellulose nanocrystals (CNC), and biochar fiber. All of these materials possess excellent physicochemical properties such as high specific surface area, high mechanical strength, biodegradability, and biocompatibility, and are rich in functional groups such as -OH.

[0011] The adsorbents include, but are not limited to, aluminum hydroxide (Al(OH)3), magnesium hydroxide (Mg(OH)2), iron hydroxide (Fe(OH)3), and calcium hydroxide (Ca(OH)2). These materials are inexpensive, environmentally friendly, and highly efficient at removing heavy metals.

[0012] The magnetic materials include, but are not limited to, iron(III) oxide (Fe3O4), γ-ferric oxide (γ-Fe2O3), and nickel-zinc ferrite (Ni-Zn ferrite). These materials all possess excellent magnetic properties and relatively stable chemical properties. When combined with the substrate and adsorbent materials, they can achieve rapid separation under the influence of a magnetic field, thus separating the water treatment agent from the water.

[0013] Furthermore, in the above-mentioned method for preparing the water treatment agent, the mass ratio of the substrate material, the adsorbent material, and the magnetic material in the water treatment agent is 1-10:1-10:1-10.

[0014] The mass ratio of the substrate material, adsorbent material, and magnetic material in the water treatment agent is selected according to actual needs.

[0015] Furthermore, the preparation method of the above-mentioned water treatment agent specifically includes the following steps:

[0016] S1: The substrate material is uniformly dispersed in the solvent, and then the metal salt used to synthesize the magnetic material is added to obtain mixed solution one;

[0017] S2: The mixed solution is transferred to a reactor for hydrothermal treatment. After hydrothermal treatment, it is cooled to room temperature, centrifuged, washed, and dried to obtain the substrate material / magnetic material.

[0018] S3: The substrate material / magnetic material is uniformly dispersed in a solvent, and then a solution containing metal ions as an adsorbent hydroxide and sodium hydroxide as a precipitant are added simultaneously to obtain mixed solution two;

[0019] S4: The mixed solution is transferred to a reactor for hydrothermal treatment. After hydrothermal treatment, it is filtered, washed, and dried to obtain the substrate material / magnetic material / adsorbent material, i.e., the water treatment agent.

[0020] In the presence of a substrate material, magnetic materials and adsorbent materials are generated in situ on the surface of the substrate material, constructing a ternary composite material of substrate material / magnetic material / adsorbent material. The three components in the water treatment agent play different roles in the wastewater treatment process, and have the functions of efficiently removing heavy metal ions and quickly separating them from the solution.

[0021] Furthermore, in the above-mentioned method for preparing the water treatment agent, the dispersion is performed using ultrasonic dispersion.

[0022] To prevent aggregation, ultrasonic dispersion is used. Ultrasound can break the agglomeration forces between substances, allowing them to be uniformly dispersed in the solvent, which is beneficial for loading on the substrate material.

[0023] Furthermore, in the above-mentioned method for preparing the water treatment agent, step S1 also involves adding a silane coupling agent and a sodium acetate solution.

[0024] For magnetic materials such as iron(III) oxide, γ-ferric oxide, and nickel-zinc ferrite, the surface may contain active functional groups such as hydroxyl groups. To better bond with the substrate and adsorbent materials, silane coupling agents are used to modify the surface of the magnetic materials, introducing specific organic functional groups to enhance the chemical bonding and physical adsorption capacity with the substrate. The addition of sodium acetate can trigger a series of chemical reactions, causing a change in the solution color. This color change often indicates the progress of the reaction and the formation of new substances. When the solution color changes significantly, the mixed solution is transferred to a reaction vessel for hydrothermal treatment.

[0025] Furthermore, in the above-mentioned method for preparing the water treatment agent, the substrate material is microcrystalline cellulose, the adsorbent material is aluminum hydroxide, and the magnetic material is γ-ferric oxide.

[0026] Microcrystalline cellulose has a stable structure and can provide a good loading platform. Al(OH)3 has the effect of adsorption and precipitation of various heavy metal ions. The magnetic properties of γ-Fe2O3 enable the treated water treatment agent to be efficiently separated in a magnetic field.

[0027] Furthermore, in the above-mentioned method for preparing the water treatment agent, the substrate material is cellulose nanofiber, the adsorbent material is magnesium hydroxide, and the magnetic material is iron(III) oxide.

[0028] Cellulose nanofibers possess a large specific surface area and abundant functional groups, enabling them to effectively load magnesium hydroxide and iron oxide. Magnesium hydroxide can precipitate heavy metal ions in water, and after treatment, it can be easily separated from the water body under the magnetic effect of iron oxide.

[0029] Furthermore, in the above-mentioned method for preparing the water treatment agent, the substrate material is biochar fiber, the adsorbent material is ferric hydroxide, and the magnetic material is nickel-zinc ferrite.

[0030] Biochar fiber contains abundant porous structures and functional groups, which is beneficial for the loading of ferric hydroxide. Ferric hydroxide has a good adsorption effect on heavy metal ions, and the magnetic properties of nickel-zinc ferrite can achieve the separation of water treatment agents from water, avoiding secondary pollution.

[0031] This invention also relates to a dynamic temperature control system for the preparation method of the water treatment agent. The dynamic temperature control system includes a temperature sensor, an A / D module, and a microcontroller. The dynamic temperature control system adopts a fuzzy RBF neural network PID intelligent control algorithm. Several temperature sensors are installed inside the reactor. The temperature data collected by the several temperature sensors is converted into digital signals by the A / D module and transmitted to the microcontroller. The microcontroller calculates the real-time temperature from the received digital signals and finally controls the temperature of the heating device of the reactor through the fuzzy RBF neural network PID intelligent control algorithm.

[0032] Hydrothermal treatment is a crucial step in the preparation of water treatment agents, and the accuracy of temperature control significantly impacts the quality of the agent. Temperature control is easily affected by factors such as the external environment, heating method, equipment / container size, and temperature transfer medium. Therefore, this invention designs a dynamic temperature control system using a fuzzy RBF neural network PID intelligent control algorithm. Compared to traditional algorithms, this system not only exhibits better dynamic response performance but also demonstrates superior step response and robustness, meeting diverse temperature control requirements with a temperature error fluctuating within ±0.2℃.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] (1) The preparation method of the water treatment agent disclosed in this invention is reasonably designed and prepares a water treatment agent with a core-shell structure, which has a good synergistic effect. It not only has excellent heavy metal ion removal performance, but also can separate the heavy metal salts precipitated by the external magnetic field from the water body, thereby solving the problem of secondary pollution of water body.

[0035] (2) The water treatment agent preparation method disclosed in this invention generates magnetic materials and adsorbent materials in situ on the surface of the substrate material. The generated adsorbent materials and magnetic materials have a close connection with the substrate material. Since they are generated directly on the surface of the substrate material, the distribution of materials is more uniform, which is conducive to the formation of a stable core-shell structure.

[0036] (3) The dynamic temperature control system proposed in this invention for the preparation method of water treatment agent adopts the fuzzy RBF neural network PID intelligent control algorithm. Compared with the traditional algorithm, it not only has better performance in dynamic response, but also has better step and robustness of the system. It can meet the needs of different temperature control, and the temperature error fluctuates within ±0.2℃, which can ensure the quality of water treatment agent. Attached Figure Description

[0037] Figure 1 This is a diagram illustrating the architecture of the fuzzy RBF neural network PID intelligent control system of the dynamic temperature control system in Embodiment 2 of the present invention. Detailed Implementation

[0038] The following will be attached Figure 1 The technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with Embodiments 1 and 2. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present invention.

[0039] Example 1 below provides a method for preparing a water treatment agent.

[0040] Example 1

[0041] The preparation method of the water treatment agent in Example 1 is as follows:

[0042] S1: Add the dried substrate material (which may be microcrystalline cellulose, cellulose nanofibers, or biochar fiber) to a solvent (which may be an alcohol solvent, water, or ether solvent), and then perform ultrasonic dispersion until the substrate material is uniformly dispersed in the solvent, providing a uniform reaction environment for subsequent reactions.

[0043] S2: Add the metal salt (FeCl3, the iron salt corresponding to Fe2O3, or nickel salt, zinc salt, and iron salt in appropriate proportions corresponding to nickel-zinc ferrite) for synthesizing magnetic materials (such as iron(II,III) oxide, γ-Fe2O3, or nickel-zinc ferrite) to the above uniformly dispersed substrate material solution. After it is completely dissolved, add the silane coupling agent. The silane coupling agent can stabilize the reaction system and enhance the connection with the substrate material. Add sodium acetate solution dropwise until the solution color changes significantly to obtain mixed solution one. Transfer mixed solution one to a reactor for hydrothermal treatment (150-250℃, 10-12 h). Under high temperature and high pressure conditions, promote the synthesis of magnetic materials and load them onto the substrate material. After hydrothermal treatment, cool to room temperature, centrifuge to separate the solid product, wash to remove impurities, and dry to obtain pure substrate material / magnetic material.

[0044] S3: The obtained substrate material / magnetic material is uniformly dispersed in a solvent (which can be an alcohol solvent, water, or ether solvent), and then a solution containing metal ions of hydroxide adsorbent (which can be MgCl2, AlCl3, FeCl3, etc.) and a precipitant (which can be sodium hydroxide) are added simultaneously. The pH is adjusted to 10-11 to create an alkaline environment for the generation of hydroxide adsorbent, resulting in mixed solution two.

[0045] S4: Transfer the mixed solution to a reactor for hydrothermal treatment (80-100℃, 3-6h). After hydrothermal treatment, filter to separate the solid product, wash to remove impurities, and dry to obtain pure substrate material / magnetic material / adsorbent material (the mass ratio of substrate material / magnetic material / adsorbent material is 1-10:1-10:1-10, and the ratio is adjusted according to actual needs), i.e., water treatment agent.

[0046] A magnetic water treatment agent with a core-shell layered structure of substrate material / magnetic material / adsorbent material is prepared by in-situ generation. When the hydroxide adsorbent adsorbs heavy metals in wastewater, the heavy metal precipitate formed interacts with the cellulose substrate material and adheres to the cellulose. The magnetic material imparts magnetism to the water treatment agent. After water treatment, the agent is placed in a magnetic field, and the cellulose can separate the heavy metal precipitate from the water under the action of the magnetic material without causing secondary pollution.

[0047] Example 2 below provides a dynamic temperature control system for use in the preparation method of water treatment agents.

[0048] Example 2

[0049] Multiple temperature sensors (contact temperature sensors, PT1000 resistance temperature sensors with an accuracy of one-thousandth, which effectively mitigate system errors) are installed inside the hydrothermal treatment reactor. The temperature data collected by the multiple temperature sensors is converted into digital signals by an A / D module and transmitted to the microcontroller. The microcontroller calculates the real-time temperature from the received digital signals and finally controls the temperature of the reactor's heating device through a fuzzy RBF neural network PID intelligent control algorithm.

[0050] Specifically, such as Figure 1 As shown, the fuzzy RBF neural network PID intelligent control algorithm of this invention adopts a control strategy that combines superimposed fuzzy control and RBF neural network. Its structure is a control system with two inputs and three outputs of a neural network. By transmitting the system-generated deviation e and deviation change ec signals to the fuzzy RBF neural network controller, the fuzzy RBF neural network controller adjusts the three PID output parameters through online self-tuning, thereby achieving the ideal control effect on the controlled object.

[0051] This dynamic temperature control system adopts a fuzzy RBF neural network PID intelligent control algorithm. Compared with traditional algorithms, it not only has better performance in dynamic response, but also better system step and robustness, which can meet the needs of different temperature control, with temperature error fluctuating within ±0.2℃.

[0052] This invention has many specific applications, and the above description is only a preferred embodiment. It should be noted that the above embodiments are for illustrative purposes only and are not intended to limit the scope of protection of this invention. For those skilled in the art, several improvements can be made without departing from the principle of this invention, and these improvements should also be considered within the scope of protection of this invention.

Claims

1. A method for preparing a water treatment agent, characterized in that, A water treatment agent with a core-shell structure is created by combining a substrate material, an adsorbent material, and a magnetic material. In the water treatment agent, the mass ratio of the substrate material, the adsorbent material, and the magnetic material is 1-10:1-10:1-10; The preparation method includes the following steps: S1: The substrate material is uniformly dispersed in the solvent, and then the metal salt used to synthesize the magnetic material is added to obtain mixed solution one; S2: The mixed solution is transferred to a reactor for hydrothermal treatment at 150-250°C. After hydrothermal treatment, it is cooled to room temperature, centrifuged, washed, and dried to obtain the substrate material / magnetic material. S3: The substrate material / magnetic material is uniformly dispersed in a solvent, and then a solution containing metal ions as an adsorbent hydroxide and sodium hydroxide as a precipitant are added simultaneously to obtain mixed solution two; S4: The mixed solution is transferred to a reactor for hydrothermal treatment at 80-100°C. After hydrothermal treatment, it is filtered, washed, and dried to obtain the substrate material / magnetic material / adsorbent material, i.e., the water treatment agent. When adding magnetic material to S1, silane coupling agent and sodium acetate solution are also added. The substrate material is microcrystalline cellulose, the adsorbent material is aluminum hydroxide, and the magnetic material is γ-ferric oxide; or, the substrate material is cellulose nanofiber, the adsorbent material is magnesium hydroxide, and the magnetic material is iron(III) oxide; or, the substrate material is biochar fiber, the adsorbent material is iron hydroxide, and the magnetic material is nickel-zinc ferrite.

2. The method for preparing the water treatment agent according to claim 1, characterized in that, The dispersion is performed using ultrasonic dispersion.

3. A dynamic temperature control system for the preparation method of the water treatment agent as described in any one of claims 1-2, characterized in that, The dynamic temperature control system includes temperature sensors, an A / D module, and a microcontroller. The system employs a fuzzy RBF neural network PID intelligent control algorithm. Several temperature sensors are installed inside the reactor. These sensors collect temperature data, which is converted into digital signals by the A / D module and transmitted to the microcontroller. The microcontroller calculates the real-time temperature from the received digital signals and ultimately controls the temperature of the reactor's heating device using the fuzzy RBF neural network PID intelligent control algorithm.

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