Pretreatment device and method for nanometer material slurry

Abstract

The invention relates to the technical field of material preparation and pretreatment, and discloses a pretreatment device for nano material slurry, comprising: a treatment container for accommodating to-be-treated slurry; the mechanical dispersion module acts on the slurry in the processing container and provides a mechanical shearing effect; the sound energy dispersion module is coupled with the processing container and is used for applying ultrasonic energy into the slurry; the vacuum module is communicated with the internal space of the treatment container and is used for establishing and maintaining a negative pressure environment in the slurry treatment process; and the control module is configured to automatically control starting, stopping, working parameters and time sequences of the mechanical dispersion module, the sound energy dispersion module and the vacuum module according to a preset process program so as to enable the three modules to work cooperatively. According to the method, secondary agglomeration and overheat denaturation of the slurry caused by overhigh energy can be avoided while initial soft agglomeration of the nano powder can be effectively broken, so that the high-solid-content slurry with high uniformity and stability is obtained.

Description

Technical Field

[0001] This invention relates to the field of material preparation and pretreatment technology, specifically to a vacuum stirring degassing and dispersion device and its working method for nanomaterial slurries (such as nano-glass slurries, nano-ceramic slurries, etc.) with high solid content, easy agglomeration and high viscosity. Background Technology

[0002] In precision manufacturing (such as photopolymer 3D printing and tape casting), slurries prepared using high-solids-content nanoparticles (such as nanoglass, nanoceramics, and nanometals) are key raw materials for obtaining products with high density and high optical or mechanical properties. However, a series of technical challenges exist in the pretreatment and mixing process of such slurries, which traditional mixing devices struggle to effectively address: 1. Nanoparticles are difficult to disperse efficiently and persistently: Due to the huge specific surface area and high surface energy of nanoparticles, they are very easy to form soft agglomerates that are difficult to completely break down under the action of van der Waals forces. Although traditional high-speed shear stirring or high-frequency ultrasound can temporarily break the agglomerates, the energy is often too high, which can cause violent collisions and temperature rises in local areas. This may lead to "secondary agglomeration" or change the rheological properties of the slurry, ultimately resulting in micro-defects inside the molded parts, affecting their light transmittance, strength or uniformity. 2. Powder escape and blockage during vacuum degassing: When high-viscosity nano slurry is vacuum degassed, the bubbles inside the slurry may carry away ultrafine powder. The filters used in traditional vacuum systems usually have large pore sizes (>0.5μm) and cannot effectively intercept submicron and nano-sized powders, causing powder to enter the vacuum pump, resulting in equipment wear or contamination, or rapid blockage of the filter element, increasing maintenance costs and downtime.

[0003] Therefore, there is an urgent need for a pretreatment device specifically designed for high-solids-content nanomaterial slurries, capable of achieving efficient and low-damage dispersion and reliable anti-clogging vacuum degassing, thereby meeting the stringent requirements of high-performance products for slurry uniformity, purity, and batch stability. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of existing technologies and provide a pretreatment device and method for nanomaterial slurries. It aims to achieve high-quality, high-efficiency, and low-maintenance pretreatment of slurries through a systematic structural design that collaboratively solves problems such as nanopowder agglomeration, vacuum system blockage, equipment inner wall residue, and high control complexity.

[0005] The present invention provides a pretreatment device for nanomaterial slurries, comprising: A processing container used to hold the slurry to be processed; The mechanical dispersing module acts on the slurry within the processing container, providing mechanical shearing action; An acoustic energy dispersing module, coupled to the processing container, is used to apply ultrasonic energy into the slurry; A vacuum module, connected to the internal space of the processing container, is used to establish and maintain a negative pressure environment during the slurry processing; The control module is configured to automatically control the start-up, shutdown, working parameters, and timing of the mechanical dispersion module, acoustic energy dispersion module, and vacuum module according to a preset process procedure, so that the three work together. The processing container is a stainless steel mixing tank with a jacketed structure. The mechanical dispersion module is a low-shear dual-propeller agitator driven by a servo motor. The acoustic dispersion module consists of multiple sets of low-frequency ultrasonic transducers welded to the outside of the bottom of the mixing tank. The vacuum module includes a vacuum pump and a nano-level anti-clogging filter connected to the front end. The control module is a PLC control cabinet with an integrated preset process parameter library. The three modules work together in a programmed manner to achieve integrated dispersion and degassing of the slurry.

[0006] As a further optimization of the present invention, the vacuum module includes a vacuum generating component and a filter unit disposed on the air inlet path of the vacuum generating component, wherein the rated filtration accuracy of the filter unit is sufficient to intercept solid particles in the slurry. The vacuum generating component is a three-stage rotary vane vacuum pump, and the filtration unit is a nano-level anti-clogging filter. Its filter element is made of PTFE membrane and glass fiber composite material with a pore size ≤0.2μm, which can effectively intercept submicron and nano-sized powders, prevent them from entering the vacuum pump and causing wear and contamination, and ensure the long-term stable operation of the system.

[0007] As a further optimization of the present invention, the filter unit is equipped with a cleaning component, which is configured to apply a reverse fluid impact to the filter unit to remove particulate matter adhering to its surface. The cleaning component is a nitrogen backflushing component, which is connected to the filter unit. When the pressure difference across the filter exceeds a set threshold such as 0.02MPa, the PLC controls the backflushing valve to open and use nitrogen at a pressure of 0.3MPa to backflush the filter element, automatically removing the powder adhering to the surface, restoring its filtration capacity, and significantly extending the service life of the filter element.

[0008] As a further optimization of the present invention, at least a portion of the inner surface of the processing container is provided with a surface energy modification layer to reduce the adhesion of solid components in the slurry to its surface. The entire inner wall and bottom guide cone of the processing container (mixing tank) are coated with a SiO2-based superhydrophobic nano-coating. The coating is 30-50nm thick and has a static water contact angle of ≥150°. This coating can greatly reduce the adhesion of nanoparticles to the inner wall and, in conjunction with the subsequent cleaning process, effectively prevent cross-contamination.

[0009] As a further optimization of the present invention, the processing container is provided with a sandwich structure, and a temperature control medium can flow through the sandwich structure to adjust the temperature of the slurry in the processing container; The outer layer of the processing container is a high-precision temperature control sleeve, and the inner layer can circulate heat transfer oil and other temperature control media to achieve precise temperature control (such as 25-50℃, with an accuracy of ±0.2℃). This design ensures that the slurry temperature is stable during the processing and prevents viscosity changes and agglomeration caused by temperature rise.

[0010] As a further optimization of the present invention, the acoustic energy dispersing module is configured to output ultrasonic waves with a frequency range of 15kHz to 50kHz, and its output power can be adjusted in at least two stages according to the preset process procedure. The acoustic energy dispersion module is an ultrasonic transducer with a frequency of 18-30kHz. The control module performs segmented power control according to a preset program: for example, the first stage uses a high power (e.g., 120W) mode to efficiently break up the initial agglomerates; the second stage switches to a low power (e.g., 80W) mode to maintain the dispersion state and prevent secondary agglomeration.

[0011] As a further optimization of the present invention, the mechanical dispersion module includes a stirrer driven by a motor, the structure of which is designed to disperse the slurry in less than 100 seconds within a predetermined speed range. -1 The shear rate; The mechanical dispersion module includes a low-shear twin-propeller agitator driven by a servo motor. The impeller blades have an arc-shaped design, and the servo motor speed is adjustable within the range of 30-200 r / min. The preset speed (e.g., 75 r / min) corresponds to a macroscopic shear rate of approximately 20 s. -1 This low-shear design promotes overall slurry circulation while avoiding secondary particle agglomeration or slurry rheological damage caused by excessive shear.

[0012] As a further optimization of the present invention, a cleaning module is also included, which is configured to spray cleaning fluid into the processing container and execute an automatic cleaning process under the control of the control module. The cleaning module includes a high-pressure micro-mist spray head, a cleaning agent / hot water supply unit, an ultrasonic auxiliary module, and a drying unit. Under PLC control, it can automatically perform the entire cleaning process, including hot cleaning liquid atomization spraying, ultrasonic-assisted peeling, hot air drying, and nitrogen purging, to ensure thorough removal of nanoscale residues and meet the cleanliness requirements for batch switching.

[0013] A pretreatment method for nanomaterial slurry, using the aforementioned pretreatment apparatus, includes the following steps: Step 1: Inject the predetermined amount of slurry into the processing container; Step 2: Call the preset process program through the control module; Step 3: Under the control of the process program, perform the following operations sequentially or simultaneously: start the vacuum module to establish a negative pressure environment, and start the mechanical dispersion module and the acoustic dispersion module to perform synergistic dispersion treatment of the slurry; Step 4: After processing, drain the slurry; The method is as follows: First, the high solids content nano slurry is injected into the mixing tank. The matching preset process program (such as the "30nm quartz powder-optical lens" program) is selected through the PLC touch screen. After starting, the system automatically performs the coordinated operation of vacuuming, temperature control, low shear stirring and ultrasonic dispersion according to the program. The processing usually includes at least two stages to take into account both efficient agglomeration breaking and stable anti-reagglomeration. After the processing is completed, the slurry is discharged smoothly under a micro-vacuum state.

[0014] As a further optimization of the present invention, the slurry is a high solids content slurry, wherein the median particle size D50 of the solid components is less than 500 nm, and the solid components include nanoparticles of glass, ceramics, metals or their composites; the preset process procedure is selected based at least on the type and particle size of the solid components. The slurry is a high-solids-content nano-slurry with a solid content of ≥53% and a solid component D50 <500nm, such as nano-glass slurry for 3D printing. The PLC control module has a "nano-glass powder parameter library" pre-stored. For nano-powders of different materials (quartz, high borosilicate, etc.) and different particle sizes, it presets optimized process parameter combinations including stirring speed, ultrasonic segmented power curve, temperature, time, etc. Users only need to select the corresponding program to achieve customized and highly reproducible preprocessing.

[0015] The pretreatment apparatus and method for nanomaterial slurries proposed in this invention have the following beneficial effects: (i) Through the synergistic effect of low-shear mechanical stirring and ultrasonic dispersion within a specific frequency range, the initial soft agglomeration of nanoparticles can be effectively broken down while avoiding secondary agglomeration and slurry overheating and denaturation caused by excessive energy, thereby obtaining a highly uniform and stable high-solids slurry, laying a solid foundation for subsequent molding processes. (ii) The high-precision filter combined with the reverse airflow cleaning design can effectively intercept nano-sized powders, prevent them from entering the vacuum pump, significantly extend the service life of the filter element and the vacuum pump, reduce frequent maintenance and downtime caused by blockage, and ensure production continuity. (iii) The low surface energy coating on the inner wall of the mixing container physically reduces the adhesion of nanoparticles. Combined with a dedicated high temperature and high pressure micro-mist cleaning and auxiliary peeling (such as ultrasonic) process, it can efficiently and thoroughly remove nanoscale residues, ensure the purity between different batches and different formulations of slurry pretreatment, and ensure the consistency of product performance. (iv) The pre-programmed automatic control system allows operators to select the process formula for the corresponding material type and the device can automatically complete the entire process from vacuuming, temperature control, segmented stirring / ultrasound to cleaning. This reduces the reliance on operator experience, reduces human error, improves process reproducibility and production efficiency, and avoids the use of complex online sensors, thus reducing system cost and failure rate. (v) By adjusting the preset process parameter library, this device can be adapted to the pretreatment requirements of different types (such as quartz glass, high borosilicate glass, functional ceramics), different particle sizes and solid contents of nano slurries, and has good process flexibility and scalability.

[0016] Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the overall structure of the pretreatment device for nanomaterial slurry provided by the present invention; Figure 2 This is a schematic diagram of the structure of the filter unit provided by the present invention; Figure 3 This is a partial cross-sectional schematic diagram of the coating on the bottom wall of the mixing tank provided by the present invention.

[0018] In the diagram: 1. Mixing tank; 2. Low-shear twin propellers; 3. Servo motor; 4. Discharge port; 5. Three-stage rotary vane vacuum pump; 6. Nanoscale anti-clogging filter; 7. PLC control cabinet; 8. Filter element; 9. Nitrogen backflush pipeline connector; 10. Differential pressure sensor; 11. SiO2-based superhydrophobic nano-coating. Detailed Implementation

[0019] Embodiments of the present invention are described in detail below. Examples of these embodiments are illustrated in the accompanying drawings, wherein the same or similar symbols denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.

[0020] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "over," and "on top" of the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.

[0021] This invention provides a pretreatment apparatus and method for nanomaterial slurries, aiming to systematically solve the problems of soft agglomeration, vacuum system blockage, and equipment cleaning during the pretreatment process.

[0022] Example: Pretreatment of silica nano-slurry with a solid content of 53% as an example like Figure 1 and Figure 2 As shown, this device mainly includes the following subsystems, which are physically connected to the circuits via pipes and logically controlled by a PLC control cabinet: (1) Low-shear segmented dispersion system, including A double-layered SUS316L stainless steel mixing tank 1, with an inner volume of 10L (which can be designed to be 5-20L as needed), is used to hold slurry. The entire inner wall of the mixing tank 1, including the bottom, is coated with a SiO2-based superhydrophobic nano-coating 11. The coating thickness is 30-50 nm, the surface roughness Ra≤0.1 μm, and the static water contact angle≥150°. The bottom of the tank is designed as a 45° inclined low-shear guide cone (not shown separately in the figure, located at the bottom of the tank), replacing the traditional U-shaped bottom. The cone surface is also coated with a SiO2-based superhydrophobic nano-coating 11 to eliminate dead flow angles and promote gentle circulation of the slurry. The outer layer of the mixing tank 1 is a high-precision temperature control jacket, and heat transfer oil can be circulated in its jacket. The temperature control range is 25-50℃, and the temperature control accuracy is ±0.2℃. In this example, it is set to 30℃. The tank top is equipped with a feed inlet with a sealed cap and an observation window, and the tank bottom is equipped with a discharge outlet 4 with heat tracing and a ball valve; It also includes a low-shear twin propeller 2, driven by a servo motor 3, which is vertically mounted at the center of the mixing tank 1; The blade edges are designed with rounded edges to provide low shear force. Specifically, the upper blade rotates clockwise, with a diameter designed to be 60% of the inner diameter of the mixing tank and a pitch of 1.2 times the diameter of the upper blade. The lower blade rotates counterclockwise, with a diameter of 50% of the inner diameter of the tank and a pitch of 1.2 times the diameter of the lower blade. This design can create an upper and lower convection circulation inside the tank. The servo motor 3's speed can be steplessly adjusted within the range of 30-200 r / min. In this example, it is preset to 75 r / min, which corresponds to a macroscopic shear rate of approximately 20 s for the slurry. -1 ; The blade body is made of SUS316L and coated with a polyimide wear-resistant coating. It also includes low-frequency ultrasonic transducers, a total of 4 sets, which are welded and coupled to the outside of the bottom of the mixing tank at equal intervals of 90° around the circumference. The working frequency is 18-30kHz. In this example, the center frequency is set to 25kHz. Segmented power control is adopted, and the power is adjustable from 60-150W.

[0023] (2) Nanoscale vacuum anti-blocking system, including Three-stage rotary vane vacuum pump 5, ultimate vacuum degree ≤ -0.0995MPa, pumping speed ≥ 30L / min, connected via pipeline; The nano-level anti-clogging filter 6 is connected in series at the front end of the air inlet of the three-stage rotary vane vacuum pump 5. Its filter element 8 is made of PTFE membrane and glass fiber composite material with a pore size ≤0.2μm. The surface of the filter element 8 is additionally coated with a layer of SiO2 nano powder coating. The top of the filter is also equipped with a differential pressure sensor 10. An airflow distributor (not shown in the figure) is installed inside the air extraction port at the top of the mixing tank 1. It has a porous spherical structure with a pore diameter of about 1 mm, which enables the airflow to pass through the slurry liquid surface evenly and smoothly, avoiding the formation of local high-speed airflow that entrains nanoparticles. Nitrogen backflush device (not shown in the figure): connected to the nitrogen backflush pipeline connector 9 at the lower side of the nano-level anti-clogging filter 6, storing 0.3MPa of nitrogen, and controlled by PLC; The connection sequence is as follows: agitator exhaust port → airflow distributor → nano-level anti-clogging filter → three-stage rotary vane vacuum pump → atmosphere.

[0024] (3) Nanoscale anti-adhesion cleaning system, including Four high-pressure micro-mist spray heads are installed on the inner side of the top of the mixing tank 1. The spray pressure is 0.6-0.8MPa, which can produce fine mist with a diameter of 5-10μm. Cleaning agent supply unit: stores nano-level special cleaning agent, which is an aqueous solution containing 0.5%-1% silane coupling agent (such as KH-550); Hot water supply unit: can provide hot water at 85-90℃; Ultrasonic auxiliary module: can generate 15kHz, approximately 50W fixed power ultrasonic waves for auxiliary cleaning; Drying unit: includes a hot air generator (80℃) and a nitrogen source with 99.99% purity.

[0025] (4) Automatic control system, including PLC control cabinet 7 is the core control unit, equipped with a 10-inch touch screen. The PLC has a "nano glass powder parameter library" pre-stored, which presets fixed process parameter combinations for nano glass powder of different materials (such as quartz, high borosilicate) and particle sizes, including: stirring speed, ultrasonic frequency / power curve (segmented setting), temperature control, total stirring time, cleaning process parameters, etc. The sensors mainly include a vacuum sensor inside the tank (used only for display and monitoring, and not involved in closed-loop regulation), a filter differential pressure sensor, and a temperature sensor for the temperature control sleeve, and do not rely on an online viscometer or particle size analyzer.

[0026] The above slurry formula is as follows: The detailed workflow and methods are as follows: Step 1: Slurry Injection and Initial Preparation The prepared slurry is injected from the top inlet of the mixing tank using a peristaltic pump at a speed of 10 rpm. The filling volume should be controlled at 60% of the tank volume (i.e., 6L) to avoid overfilling and splashing during stirring; During the injection process, the PLC controls the vacuum pump to start at low power to maintain a "micro-vacuum" environment (approximately -0.02MPa) inside the tank. This weak evacuation action, in conjunction with the airflow distributor, can smoothly remove the air bubbles entrained during injection, reducing the initial gas content from 3.2% to approximately 2.5%.

[0027] Step 2: Parameter Calling and System Sequential Startup The operator enters the parameter library on the PLC touch screen and selects a preset program that matches the current slurry, such as the "30nm quartz powder - optical lens" program. After clicking "Start", the PLC will automatically execute the following fixed logical sequence: First, start the three-stage rotary vane vacuum pump, delay for 5 seconds to establish a high vacuum, and the vacuum sensor shows that the pressure continues to drop. Send a command to the temperature control sleeve to start the heating cycle to the preset 30℃ (feedback signal after constant temperature). The servo motor of the low-shear dual propeller is started, and the speed is steadily increased to the preset 75r / min, with a 3-second delay to avoid instantaneous load; Start the low-frequency ultrasonic transducer and immediately enter the first stage of high-power mode, with the power set to 120W.

[0028] Step 3: Segmented Coordinated Control of the Preprocessing Process 1) First stage (0-12 minutes): Efficiently breaking up group reunions During this stage, the ultrasonic waves operate at high power (120W), creating a strong cavitation effect, which is specifically designed to break up initially existing chain-like / flocculent soft agglomerates (1-5μm in size) in the slurry. The low-shear stirring paddle (75r / min) operates synchronously, forming a gentle overall circulation, which quickly carries the agglomerates that have been locally broken up by the ultrasonic waves away from the vibration source area, promotes global homogenization, and assists in heat diffusion. The vacuum pump operates continuously, and the vacuum level inside the tank is stably maintained within the set range of -0.099 to -0.0995 MPa. As air bubbles are continuously extracted from the slurry, the gas content continues to decrease. The temperature control sleeve precisely controls the temperature at 30±0.2℃, avoiding temperature fluctuations in the slurry caused by heat generated by ultrasound and stirring, thereby preventing abnormal viscosity changes; Through the observation window, it can be seen that the slurry gradually changes from an initial slightly turbid state with flocculent matter to a uniform and transparent fluid state within 8-10 minutes. The differential pressure sensor showed that the pressure difference across the filter slowly rose to approximately 0.008 MPa, far below the alarm threshold of 0.02 MPa; 2) Second stage (12-30 minutes): Stabilize and prevent secondary re-aggregation At the 12th minute, the PLC automatically executes the program switch: reducing the power of the ultrasonic transducer from 120W to 80W. During this stage, the ultrasonic waves operate in low-power mode, with enough energy to suppress the re-aggregation of dispersed nanoparticles due to van der Waals forces (secondary agglomeration), but without generating excessive local disturbances. The agitator (75 r / min) and vacuum pump continued to operate stably, and the temperature control remained unchanged; The main purpose of this stage is to homogenize and stabilize the slurry and to deeply degas it, so that the slurry viscosity is stabilized at about 7200 cP (due to the viscosity decrease caused by uniform dispersion, rather than shear thinning). The vacuum level remained stable with fluctuations ≤ ±0.0005MPa, the filter differential pressure remained stable in the range of 0.010-0.012MPa, and the system did not trigger backflushing. 3) Vacuum anti-blocking logic monitoring Throughout the 30-minute processing, the differential pressure sensor collected data every 10 minutes. In this example, the pressure difference remained below 0.02 MPa, so the nitrogen backflushing device was not activated. Anti-clogging logic description: If the pressure difference is >0.02MPa during a certain operation, the PLC will automatically trigger the nitrogen backflush valve to open and backflush the filter at a pressure of 0.3MPa for 10 seconds. If the pressure difference returns to <0.02MPa after backflush, the operation will continue. If it is still >0.02MPa, the touch screen will issue a "filter replacement warning" signal, but the already set stirring process will not be interrupted.

[0029] Step 4: Processing Completed and Slurry Discharge After the preset total duration of 30 minutes is reached, the PLC will automatically stop the machine in sequence: First, turn off the ultrasonic transducer, then turn off the vacuum pump, but maintain a micro-vacuum of about -0.05MPa inside the tank through valve control to prevent air from rushing in and impacting the slurry surface. Then turn off the stirring paddle servo motor. Subsequently, the PLC controls the opening of the heat-insulating ball valve at the bottom of the tank. The outlet is equipped with heat tracing, and the temperature is maintained at 30°C to prevent the high-viscosity slurry from cooling down, thickening, and clogging at the outlet. Under the influence of gravity and a slight positive pressure (relative to the atmosphere) inside the tank, the slurry flows out at a uniform speed and smoothly, without stratification or blockage. The final slurry has an air content of ≤0.2% and a soft agglomeration dispersion efficiency of ≥95%.

[0030] Step 5: Batch-to-batch cleaning process (to prevent cross-contamination) After the slurry is discharged, if it is necessary to replace the next batch (especially slurry of different materials or colors), a standard cleaning procedure must be performed. The operator clicks "Automatic Cleaning" on the PLC interface. 1) Hot cleaning fluid spraying and assisted peeling The PLC automatically opens the valve and injects 15L of hot water at 85-90℃ into the tank. At the same time, it pumps in 300mL of nano-grade special cleaning agent containing 0.5%-1% silane coupling agent (KH-550) according to the ratio. Activate the high-pressure micro-mist spray head to atomize the hot cleaning liquid and spray it onto the tank wall at a pressure of 0.7MPa for physical rinsing; At the same time, the low-shear stirring paddle is started to run at a low speed (e.g., 30r / min), and the 15kHz ultrasonic auxiliary module (50W fixed power) is started. The ultrasonic and mechanical stirring work together to allow the cleaning fluid to penetrate and destroy the bonding force between the possible nano-adsorption membrane and the superhydrophobic coating of the tank wall. 2) Discharge and drying After mixing and cleaning for 15 minutes, drain the waste liquid; Turn on the hot air dryer and blow 80℃ hot air into the can for 8 minutes to evaporate most of the moisture. After the hot air is finished, switch to high-purity nitrogen to purge for 5 minutes to further dry the residual moisture and create an inert environment to prevent the nanoparticles from oxidizing or re-adsorbing. 3) Residue verification After drying, wipe the tank wall and the surface of the guide cone with a clean, lint-free cloth; Weigh or analyze the composition of the cleanroom wipes; In this example, the measured residual quartz powder mass was only 0.08g, which meets the system's cleanliness standard of ≤0.1g, allowing for the pretreatment of the next batch of slurry.

[0031] Through the above specific implementation methods, this device achieves fully automated and efficient processing of high solids content nanoglass slurry from feeding, parameterized collaborative processing, anti-clogging monitoring to thorough cleaning, effectively ensuring slurry quality and batch stability.

[0032] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A pretreatment apparatus for nanomaterial slurry, characterized in that, include: A processing container used to hold the slurry to be processed; The mechanical dispersing module acts on the slurry within the processing container, providing mechanical shearing action; An acoustic energy dispersing module, coupled to the processing container, is used to apply ultrasonic energy into the slurry; A vacuum module, connected to the internal space of the processing container, is used to establish and maintain a negative pressure environment during the slurry processing; The control module is configured to automatically control the start-up, shutdown, working parameters, and timing of the mechanical dispersion module, acoustic energy dispersion module, and vacuum module according to a preset process procedure, so that the three work together.

2. The pretreatment apparatus for nanomaterial slurry according to claim 1, characterized in that, The vacuum module includes a vacuum generating component and a filter unit disposed on the air inlet path of the vacuum generating component. The rated filtration accuracy of the filter unit is sufficient to intercept solid particles in the slurry.

3. The pretreatment apparatus for nanomaterial slurry according to claim 2, characterized in that, The filtration unit is equipped with a cleaning component configured to apply a reverse fluid impact to the filtration unit to remove particulate matter adhering to its surface.

4. The pretreatment apparatus for nanomaterial slurry according to claim 1, characterized in that, The processing container has at least a portion of its inner surface with a surface energy modification layer to reduce the adhesion of solid components in the slurry to its surface.

5. The pretreatment apparatus for nanomaterial slurry according to claim 1, characterized in that, The processing container is provided with a sandwich structure, within which a temperature control medium can circulate to regulate the temperature of the slurry inside the processing container.

6. The pretreatment apparatus for nanomaterial slurry according to claim 1, characterized in that, The acoustic energy dispersion module is configured to output ultrasonic waves with a frequency range of 15kHz to 50kHz, and its output power can be adjusted in at least two stages according to the preset process procedure.

7. The pretreatment apparatus for nanomaterial slurry according to claim 1, characterized in that, The mechanical dispersion module includes a motor-driven agitator, the agitator being designed to disperse the slurry in less than 100 seconds within a predetermined speed range. -1 The shear rate.

8. The pretreatment apparatus for nanomaterial slurry according to any one of claims 1 to 7, characterized in that, It also includes a cleaning module configured to spray cleaning fluid into the treatment container and to perform an automatic cleaning process under the control of the control module.

9. A pretreatment method for nanomaterial slurry, using the pretreatment apparatus as described in any one of claims 1 to 8, characterized in that, Includes the following steps: Step 1: Inject the predetermined amount of slurry into the processing container; Step 2: Call the preset process program through the control module; Step 3: Under the control of the process program, perform the following operations sequentially or simultaneously: start the vacuum module to establish a negative pressure environment, and start the mechanical dispersion module and the acoustic dispersion module to perform synergistic dispersion treatment of the slurry; Step 4: After processing, drain the slurry.

10. The pretreatment method for nanomaterial slurry according to claim 9, characterized in that, The slurry is a high solids content slurry, wherein the median particle size D50 of the solid components is less than 500 nm, and the solid components include nanoparticles of glass, ceramics, metals or their composites; the preset process procedure is selected based at least on the type and particle size of the solid components.

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