Preparation equipment and preparation method of nano-silver modified porous air purification material

Abstract

The invention discloses air purification material preparation equipment, and particularly relates to nano-silver modified porous air purification material preparation equipment and a preparation method thereof.The equipment comprises a rotary liquid membrane reactor, a nano-silver modified porous air purification material preparation device and a nano-silver modified porous air purification material preparation method, and the rotary liquid membrane reactor ensures uniform distribution of silver ions and optimization of reduction reaction by means of the rotary liquid membrane principle; the constant-temperature water bath kettle is used for providing a stable temperature control environment and controlling the temperature of a reaction system so as to ensure that the reaction is carried out stably; the centrifugal machine is used for separating solid and liquid generated after the reaction and collecting the silver modified molecular sieve; the vacuum drying box is used for efficiently drying materials and removing moisture and other volatile substances; the muffle furnace is used for carrying out thermal activation treatment on the silver modified molecular sieve so as to remove potential organic substances and enhance the pore structure of the material; and the solution preparation device is used for ensuring the accuracy of solution preparation and ensuring the controllability and consistency of reaction.

Description

Technical Field

[0001] The invention relates to the technical field of preparation equipment, and in particular to a preparation equipment for a nano-silver modified porous air purification material and a preparation method thereof. Background Art

[0002] The presence of harmful gases (such as formaldehyde, benzene, ammonia, etc.) and microorganisms (such as bacteria and viruses) in indoor and outdoor air poses a major threat to human health. Porous materials are widely used in the field of air purification due to their unique characteristics such as large specific surface area and rich pore structure. In recent years, by loading nanosilver particles on the surface of porous materials, not only can their adsorption performance be further improved, but also excellent antibacterial and catalytic activity can be given, which has become a research hotspot. However, the traditional preparation process has problems such as low efficiency, uneven particle distribution, and environmental pollution. It is urgent to develop an efficient, environmentally friendly, and stable preparation method and corresponding equipment to meet the application needs of high-performance air purification materials. Summary of the invention

[0003] In order to solve the problems existing in the above-mentioned prior art, the present invention provides a nano-silver modified porous air purification material preparation device and a preparation method thereof to solve the current technical problems.

[0004] The technical solution adopted by the present invention to solve its technical problem is: The present invention provides a nano-silver modified porous air purification material preparation device and a preparation method thereof, comprising: Rotating liquid film reactor: This equipment uses the principle of rotating liquid film to ensure the uniform distribution of silver ions and the optimization of their reduction reaction; Constant temperature water bath: used to provide a stable temperature control environment, control the temperature of the reaction system, and ensure the smooth progress of the reaction; Centrifuge: used to separate the solid and liquid produced after the reaction and collect the silver-modified molecular sieve; Vacuum drying oven: used to efficiently dry materials and remove moisture and other volatile substances; Muffle furnace: used for thermal activation of silver-modified molecular sieves to remove potential organic matter and enhance the pore structure of the material; Liquid preparation device: ensure the accuracy of solution preparation and guarantee the controllability and consistency of the reaction; pH meter and temperature sensor: used to monitor the pH value and reaction temperature of the solution in real time to ensure accurate control of reaction conditions.

[0005] Preferably, the outlet of the liquid preparation device is connected to the reaction container through a pipeline, and the liquid preparation device is also provided with a pH meter.

[0006] Preferably, a rotating liquid film reactor is not connected to the outlet of the constant temperature water bath, and the reaction liquid flows into the inlet of the centrifuge after passing through the rotating liquid film reactor.

[0007] Preferably, the centrifuge is located downstream of the rotating liquid film reactor and is used to separate the solid and liquid after the reaction. The outlet of the centrifuge is connected to a collecting tank for collecting the precipitate of the silver-modified molecular sieve.

[0008] Preferably, the precipitate is dried in a vacuum drying oven, and the inlet of the vacuum drying oven is connected to the collecting tank.

[0009] Preferably, the outlet of the vacuum drying oven is connected to a muffle furnace.

[0010] The beneficial effects of the present invention are: Optimization design of equipment system: An integrated equipment system is proposed, which forms a set of efficient and continuous nano-silver modified porous air purification material preparation equipment through the reasonable connection of rotating liquid film reactor, constant temperature water bath, centrifuge, vacuum drying oven, muffle furnace and other equipment. The system realizes efficient collaboration between various equipment, simplifies complex operation processes, and improves production efficiency and product consistency.

[0011] Application of rotating liquid film reaction technology: A uniform reaction environment is formed by rotating the liquid film to avoid the agglomeration of silver particles, while achieving precise distribution and effective loading of silver nanoparticles in the pores of the molecular sieve. This method significantly improves the performance of the material, such as antibacterial properties and adsorption capacity.

[0012] Accurate parameter control and monitoring: By integrating pH meter, temperature sensor and UV-Vis spectrometer, key parameters of the reaction process (such as temperature, pH value, reduction degree of silver ions, etc.) are monitored and feedback controlled in real time. The accuracy and consistency of reaction conditions are ensured, effectively avoiding the problem of unstable product performance caused by parameter fluctuations.

[0013] Modular design, easy to expand and apply: The equipment adopts modular design, and the equipment function can be adjusted or upgraded according to needs. For example, different types of reactors can be replaced or added to prepare other multifunctional modified molecular sieve materials, laying the foundation for further industrial promotion.

[0014] Universality and economy: The preparation method and equipment design of the present invention have strong universality, not only applicable to 13X molecular sieve, but also applicable to other porous materials (such as activated carbon, silica gel, etc.). The process and equipment use common chemical reagents and experimental instruments, with low cost, simple operation, and significant economic benefits and industrialization potential. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] The above aspects and advantages of the present invention will become apparent and easily understood from the description of the embodiments in conjunction with the following drawings, in which: Figure 1 It is a schematic diagram of a device for preparing a nano-silver modified porous air purification material according to an embodiment of the present invention. DETAILED DESCRIPTION

[0016] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0017] A nano-silver modified porous air purification material preparation device, comprising: Solution preparation and stirring system: Liquid preparation device: This device is located on one side of the experimental table and is responsible for accurately preparing the solution required for the reaction (such as silver nitrate solution, sodium borohydride solution, etc.), or using a related solution storage tank instead. Its outlet is connected to the reaction vessel of the constant temperature water bath through a pipe. This ensures the consistency of the amount and time of solution added each time, avoiding errors caused by human operation.

[0018] During the liquid dissolution process, the liquid dispensing device is connected to a pH meter to monitor the pH of the solution in real time. When the device flows the solution into the agitator or reaction vessel, the temperature sensor will continuously monitor the temperature in the water bath to ensure that the temperature is within the required range (60°C~70°C) to prevent the reaction from being affected by excessively high or low temperatures.

[0019] Impregnation and reduction reaction process: Rotating liquid film reactor: This equipment is located at the outlet of the constant temperature water bath. Inside the rotating liquid film reactor, the stirring and rotating action ensures the uniform distribution of silver ions and optimizes their reduction reaction. The speed control system of the equipment cooperates with the constant temperature water bath through the temperature sensor to ensure the stability of the temperature control system. After the reaction liquid passes through the rotating liquid film reactor, it will flow into the centrifuge inlet.

[0020] Centrifuge: The centrifuge is located downstream of the rotating liquid film reactor and is used to separate the solid and liquid after the reaction. The outlet of the centrifuge is connected to a collection tank for collecting the precipitation of the silver-modified molecular sieve. After the centrifuge is operated, the reaction liquid is separated from the solid, and the solid precipitation will be further washed.

[0021] Cleaning and drying process: The washed solid precipitate is transported to the vacuum drying oven through a pipeline. During this process, the precipitate will be dried under vacuum conditions. The inlet of the vacuum drying oven is connected to the collection tank to ensure that the precipitate can be transferred to the drying oven and the drying effect will not be affected by air humidity. When the vacuum drying oven is in operation, the internal temperature and vacuum degree are continuously monitored through the temperature control system and pressure sensor to ensure that the temperature is controlled at 100°C~110°C and maintain an appropriate vacuum degree to accelerate the drying process.

[0022] Heat activation treatment: After being completely dried, the silver-modified molecular sieve will be transferred to the muffle furnace for further thermal activation treatment. The inlet of the muffle furnace is connected to the outlet of the vacuum drying oven, and the material is transferred smoothly by a conveyor belt or manually. The temperature and atmosphere in the muffle furnace are controlled by its internal temperature control system and gas flow controller, and are maintained in the range of 300°C~350°C, ensuring that the pore structure of the molecular sieve is optimized and potential organic matter is removed.

[0023] Final product collection and storage: The heat-activated silver-modified molecular sieve will be delivered to the collection container by an automatic conveying system, or manually collected and stored in a dry container as needed. The storage container has good sealing properties to avoid the influence of air humidity and impurities to ensure the stable performance of the final product.

[0024] Data monitoring and control: The pH meter and temperature sensor are connected to multiple devices to monitor the pH value of the solution and the temperature during the reaction in real time. The results of the pH meter monitoring are fed back to the operator through the digital display, and the temperature sensor is directly connected to the constant temperature water bath, rotating liquid film reactor and vacuum drying oven to ensure accurate temperature control. In addition, the data of all devices can be synchronously transmitted to the operating platform through the control system to ensure the automation and accuracy of the reaction.

[0025] Through the close connection and reasonable configuration of the above-mentioned equipment, each reaction step can proceed smoothly, ensuring the efficient preparation of silver-modified molecular sieves and the optimization of final performance.

[0026] In particular, all the devices thereon can adopt existing devices, and the present application optimizes the system composed of these devices.

[0027] A method for preparing a nano-silver modified porous air purification material preparation device, comprising: Raw materials and equipment preparation: raw material: 13X molecular sieve (or other porous materials, such as activated carbon, silica gel, etc.): As a base adsorption material, 13X molecular sieve has a large specific surface area (about 1000 m² / g) and excellent pore structure, which is suitable for adsorbing harmful substances in the air.

[0028] Silver nitrate: used as a silver source to form nanosilver particles through a reduction reaction, enhancing the antibacterial and catalytic properties of the material.

[0029] Sodium borohydride: As a reducing agent, it has strong reducing properties and can reduce silver ions to silver nanoparticles.

[0030] Deionized water: used to dissolve silver nitrate and other solvents in chemical reactions to ensure the purity of the solution.

[0031] equipment: Rotating liquid film reactor: This equipment uses the principle of rotating liquid film to ensure the uniform distribution of silver ions and the optimization of their reduction reaction.

[0032] Constant temperature water bath: used to provide a stable temperature control environment, control the temperature of the reaction system, and ensure the smooth progress of the reaction.

[0033] Centrifuge: used to separate the solid and liquid produced after the reaction and collect the silver-modified molecular sieve.

[0034] Vacuum drying oven: used to efficiently dry materials and remove moisture and other volatile substances.

[0035] Muffle furnace: used for thermal activation of silver-modified molecular sieves to remove potential organic matter and enhance the pore structure of the material.

[0036] Automatic liquid preparation device: ensure the accuracy of solution preparation and guarantee the controllability and consistency of the reaction.

[0037] pH meter and temperature sensor: used to monitor the pH value and reaction temperature of the solution in real time to ensure accurate control of reaction conditions.

[0038] (1) Solution preparation and pretreatment: Solution A Preparation: Accurately weigh 10 g of 13X molecular sieve, add it to 100 mL of deionized water, and stir it at 300 rpm using a stirrer to ensure that the molecular sieve is completely dispersed.

[0039] The stirring duration is 1 hour, until there is no visible particulate matter in the solution, and a uniform suspension is obtained, namely solution A. At this time, the pore structure of the molecular sieve has been penetrated by water and is ready for the adsorption of silver ions.

[0040] Solution B Preparation: Accurately weigh 4 g of silver nitrate, add it to 100 mL of deionized water, and stir until the silver nitrate is completely dissolved.

[0041] At this time, the concentration of solution B is 0.1 mol·L - ¹, providing sufficient silver source for the subsequent reduction of silver ions.

[0042] (2) Impregnation and reduction reaction: Silver ion impregnation: Mix solution A and solution B in a 1:1 volume ratio and pour them into a 250 mL beaker.

[0043] The beaker used as a reaction container was placed in a constant temperature water bath, the temperature was adjusted to 60°C~70°C, and the stirring rate was maintained at 200 rpm. The reaction was carried out for 2.5 hours to ensure that the silver ions completely penetrated into the pores of the molecular sieve.

[0044] During this process, observe the transparency of the reaction solution regularly. If the reaction is sufficient, the solution should remain clear and transparent, with no silver precipitation visible to the naked eye.

[0045] In situ reduction reaction: Prepare 0.1 mol·L - ¹ of sodium borohydride solution, accurately take 5 mL for later use.

[0046] Under stirring conditions, the sodium borohydride solution was slowly added dropwise to the silver ion impregnation system, and the dropping rate was controlled at 0.5 mL / min to ensure uniform reaction.

[0047] The reduction reaction temperature was set at 70°C to 80°C, and the uniformity of the reaction solution was maintained by a rotating liquid film reactor. The reaction time was 2 hours to ensure that the silver ions were completely reduced to silver nanoparticles and the silver particles were evenly distributed.

[0048] Reaction process monitoring: During the reduction reaction, the pH value and temperature of the reaction solution are monitored in real time to ensure that the pH is between 8.5 and 9.5. A pH value that is too low may affect the reduction efficiency of silver ions, while a pH value that is too high may cause the agglomeration of silver particles.

[0049] UV-Vis spectroscopy is used to detect the progress of silver ion reduction, and the characteristic absorption peak of silver nanoparticles is usually visible at a wavelength of 400-450 nm.

[0050] (3) Post-processing and cleaning: Centrifugation and washing: After the reaction is completed, centrifuge at 8000 rpm for 10 minutes to separate the reaction solution from the solid precipitate. The precipitate is the silver-modified molecular sieve, and the reaction solution needs to be discarded in time.

[0051] The collected solid precipitate was repeatedly washed with 500 mL of deionized water for 3-4 times until the pH value of the washing solution reached 7-8, ensuring that all reaction by-products, such as unreduced silver ions or excess reducing agent, were removed.

[0052] Vacuum drying: Transfer the washed precipitate to a vacuum drying oven and dry it at 100°C~110°C for 8 hours. During the drying process, ensure that the vacuum degree is maintained at 0.005 MPa to accelerate water evaporation and prevent the material from getting wet.

[0053] After drying is complete, check the appearance of the material to ensure that there is no visible moisture remaining and the material should be loose and free of lumps.

[0054] Heat activation treatment: The dried silver-modified molecular sieve was transferred to a muffle furnace and subjected to a thermal activation treatment at 300°C to 350°C for hours.

[0055] During the thermal activation process, potential organic matter and incompletely reacted chemicals are removed, while the pore structure of the molecular sieve is optimized and its adsorption performance is increased. This process can further enhance the stability of silver particles on the pore wall of the molecular sieve.

[0056] (4) Optimization and characterization of silver nanoparticle distribution (optional step): Optimization of Nanosilver Distribution: The particle size and distribution of silver particles were characterized using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). By optimizing the reaction conditions, the particle size of the silver particles was ensured to be between 5 and 10 nm, and the silver particles were evenly distributed on the surface and pores of the molecular sieve.

[0057] The chemical state of silver can be analyzed by X-ray photoelectron spectroscopy (XPS), confirming that the silver is in a metallic state rather than an oxidized state.

[0058] Particle size and distribution control: According to the SEM and TEM results, the temperature, reducing agent concentration and dropping rate of the reduction reaction were appropriately adjusted to ensure that the silver particles would not agglomerate and maintain a small particle size.

[0059] Compare the effects of different temperatures, concentrations and stirring rates on the distribution of silver particles and select the most suitable conditions.

[0060] (5) Finished product processing and storage: Storage of final product: After cleaning, drying and heat activation, the silver-modified molecular sieve is collected and stored in a dry container. The humidity of the storage environment should be controlled at 5% to 50% to avoid oxidation or hydrolysis of the silver particles.

[0061] The storage temperature should be kept at 20°C~25°C, avoiding direct sunlight and high temperature environment to prevent inactivation or decomposition of silver particles.

[0062] Application performance evaluation: The final silver-modified molecular sieve was tested for adsorption and catalytic performance. The specific surface area and pore volume were measured by N2 adsorption-desorption experiments to evaluate the gas adsorption capacity of the material.

[0063] Use an air purification test device to evaluate the performance of the silver-modified material in removing harmful gases (such as formaldehyde, ammonia, etc.) and antibacterial properties. The test results should show that the material has good air purification effect and antibacterial activity.

[0064] Special: Silver nitrate solution and sodium borohydride solution must be prepared and used immediately to avoid solution ineffectiveness.

[0065] The control of temperature, pH value and stirring rate during the reaction is crucial. Too high or too low temperature may affect the silver reduction efficiency and the pore structure of the molecular sieve.

[0066] Silver nitrate and sodium borohydride are somewhat corrosive, so protective equipment such as gloves and goggles must be worn during operation.

[0067] During the reaction, avoid exposing the solution to strong light for a long time to prevent decomposition reaction.

[0068] When disposing of waste liquid and waste, they must be disposed of in strict accordance with environmental protection requirements to prevent silver ions or harmful chemicals from polluting the environment.

[0069] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A nano-silver modified porous air purification material preparation device and preparation method thereof, characterized in that: include: Rotating liquid film reactor: using the principle of rotating liquid film to ensure uniform distribution of silver ions and optimization of their reduction reaction; Constant temperature water bath: used to provide a stable temperature control environment, control the temperature of the reaction system, and ensure the smooth progress of the reaction; Centrifuge: used to separate the solid and liquid produced after the reaction and collect the silver-modified molecular sieve; Vacuum drying oven: used to efficiently dry materials and remove moisture and other volatile substances; Muffle furnace: used for thermal activation of silver-modified molecular sieves to remove potential organic matter and enhance the pore structure of the material; Liquid preparation device: ensure the accuracy of solution preparation and guarantee the controllability and consistency of the reaction; pH meter and temperature sensor: used to monitor the pH value and reaction temperature of the solution in real time to ensure accurate control of reaction conditions.

2. The nano-silver modified porous air purification material preparation device and preparation method thereof according to claim 1, characterized in that: The outlet of the liquid preparation device is connected to the reaction container through a pipeline, and a pH meter is also arranged on the liquid preparation device.

3. The nano-silver modified porous air purification material preparation device and preparation method thereof according to claim 2, characterized in that: The outlet of the constant temperature water bath is not connected to a rotating liquid film reactor, and the reaction liquid flows into the inlet of the centrifuge after passing through the rotating liquid film reactor.

4. The nano-silver modified porous air purification material preparation device and preparation method thereof according to claim 3, characterized in that: The centrifuge is located downstream of the rotating liquid film reactor and is used to separate the solid and the liquid after the reaction. The outlet of the centrifuge is connected to a collecting tank for collecting the precipitation of the silver-modified molecular sieve.

5. The nano-silver modified porous air purification material preparation device and preparation method thereof according to claim 4, characterized in that: The precipitate is dried in a vacuum drying oven, and the inlet of the vacuum drying oven is connected to the collecting tank.

6. The nano-silver modified porous air purification material preparation device and preparation method thereof according to claim 5, characterized in that: The outlet of the vacuum drying box is connected to the muffle furnace.

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