A uniform dispersion preparation process of a low-energy-consumption TBC-toluene composite system

Abstract

The present application relates to the field of chemical engineering and process technology, and particularly relates to a low-energy-consumption TBC-toluene composite system uniform dispersion preparation process. The process is controlled by a DCS system, first detects the toluene moisture and TBC particle size and matches parameters, adopts a segmented feeding method to first feed 50%-60% toluene as a base material to form a rotating liquid film, TBC is pre-dispersed by gradient wetting through DCS control atomization spraying, and is mixed by stirring-ultrasonic synergy under normal temperature and pressure. The parameters are dynamically adjusted in combination with energy consumption and dispersion degree double index, the stirring rate is simultaneously fine-tuned to correct the density deviation, and after mixing, the content, appearance, density, color and other indexes are detected, the qualified products are dynamically weighed and packaged, and the unqualified products are processed according to the procedure. The process has significantly reduced energy consumption, greatly improved product dispersion uniformity and long-term stability, is suitable for different concentration ranges, has strong compatibility, and is suitable for industrial scale production.

Description

Technical Field

[0001] This invention relates to the field of chemical engineering and process technology, and in particular to a low-energy TBC-toluene composite system uniform dispersion preparation process. Background Technology

[0002] tert-Butylcatechol (TBC), as a high-performance polymerization inhibitor and antioxidant, is widely used in petrochemical, rubber processing, and polymer synthesis fields due to its excellent solubility and stability in toluene solutions. It is a key auxiliary material for ensuring continuous and stable production processes and improving product quality. However, with the increasing demands for green and low-carbon production and product consistency in industrial production, the preparation process of TBC-toluene solutions faces even greater technical challenges.

[0003] Currently, the commonly used TBC-toluene solution preparation process in the industry is the "direct feeding of solid TBC + mechanical stirring and mixing" mode. This involves first synthesizing solid TBC through a Friedel-Crafts alkylation reaction, then adding the solid TBC and toluene to a mixing vessel in a preset ratio, and finally mixing and dissolving them through mechanical stirring alone. However, this traditional process has significant technical drawbacks: Firstly, solid TBC particles exhibit strong van der Waals forces, and upon direct addition to toluene, they easily agglomerate rapidly, forming blocky or flocculent agglomerates. The shear force of mechanical stirring alone is insufficient to effectively break up these small agglomerates, resulting in uneven dispersion of TBC in toluene. This leads to problems such as locally high concentrations and excessive density fluctuations in the final product, severely impacting its polymerization inhibition and antioxidant effects in subsequent applications. Secondly, to improve dispersion, existing processes often employ methods such as extending stirring time and increasing stirring rate, resulting in high energy consumption. Conventional processes can consume over 10 kWh / ton, and the stirring parameters are fixed, unable to be dynamically adjusted according to fluctuations in raw material characteristics, resulting in significant ineffective energy consumption.

[0004] Furthermore, traditional processes lack real-time and targeted quality control: During raw material acceptance, key indicators such as TBC particle size and toluene moisture content are not accurately detected and matched. Moisture forms a liquid film on the surface of TBC particles, hindering dissolution, and large TBC particles are further aggravated by uneven dispersion due to the difficulty of wetting. During mixing, manual sampling at regular intervals is used to test indicators such as density and concentration, resulting in a delayed response to quality issues such as density deviations. This typically requires adding raw materials or rework, reducing production efficiency and further increasing energy consumption and production costs. Simultaneously, existing processes do not consider physical losses during production; the TBC feeding ratio is set based on theoretical values, easily leading to substandard final product concentration and poor batch stability.

[0005] While some improvement schemes attempt to enhance dispersion by adding chemical dispersants or introducing complex mixing equipment, the addition of chemical dispersants may affect product purity, and modifications to complex equipment require alterations to the existing process flow, resulting in poor compatibility and high costs, making widespread adoption in industrial production difficult. Therefore, developing a TBC-toluene composite system preparation process that requires no additional chemical reagents, does not alter the core process flow, and simultaneously achieves low energy consumption, high dispersion uniformity, and high process stability has become a pressing technical challenge for the industry. Summary of the Invention

[0006] The purpose of this invention is to overcome the shortcomings of the existing technology and to propose a low-energy TBC-toluene composite system uniform dispersion preparation process.

[0007] To achieve the above objectives, this invention provides a low-energy-consumption TBC-toluene composite system uniform dispersion preparation process, comprising the following steps: (1) Equipment pretreatment and raw material pre-matching: Open the manhole of the mixing tank to check the integrity of the equipment, close the bottom valve, verify that the reducer is normal, and then seal the mixing tank; test the moisture content of the raw toluene and the particle size distribution of the solid TBC. Enter the test data into the DCS system, and the DCS will automatically match the subsequent feeding rate and mixing parameters according to the particle size of TBC. Because the moisture in toluene forms a liquid film on the surface of TBC particles, hindering direct contact between TBC and toluene, the dissolution rate decreases and the probability of particle agglomeration increases. Higher energy input is required to break up the agglomeration. Therefore, a standard of ≤0.05% moisture content is set. If this standard is exceeded, water is removed by molecular sieve adsorption to ensure dissolution efficiency from the source. Furthermore, the particle size of TBC directly determines its wetting difficulty and dispersion load. Large TBC particles (100-150μm) have a small specific surface area, requiring stronger liquid film encapsulation and higher dispersion load during wetting. To prevent material aggregation, the DCS automatically increases the atomization feeding pressure to 0.3-0.4 MPa and adjusts the toluene base material ratio to 60% of the raw toluene, thereby enhancing the wetting effect through more sufficient liquid film coverage. Small TBC particles (≤100μm) have a large specific surface area and are easy to wet. If high pressure and a high base material ratio are still used, it will result in energy and solvent waste. Therefore, a lower atomization pressure and a raw toluene ratio of 50% of the base material are matched to achieve on-demand adaptation and lay the foundation for subsequent low-energy mixing. (2) Gradient wetting-pre-dispersion coupled feeding: Turn on the feed pump and add 50%-60% of the raw material toluene as the base material to the mixing vessel according to the ratio through the proton flow meter. Start low-speed stirring at 40-50 r / min to form a rotating liquid film. Spray the solid TBC evenly onto the surface of the liquid film through the atomizing feeding device. After the atomizing feeding is completed, add the remaining raw material toluene through the proton flow meter to maintain the normal temperature and pressure environment. During the feeding process, TBC is a solid particle. If it is directly added to toluene, the van der Waals forces between the particles will cause it to agglomerate rapidly, forming difficult-to-disperse lumpy agglomerates. Subsequent high-intensity stirring or long-term ultrasonication is required to break it up, which is extremely energy-intensive and has limited effect. This process uses a coupling method of rotating liquid film and atomized feeding. First, a portion of the toluene forms a continuous rotating liquid film. The surface tension of the liquid is used to wrap the atomized TBC particles, achieving gradient wetting. Each TBC particle can fully contact the toluene, breaking the agglomeration forces between particles and completing pre-dispersion. When the remaining raw material toluene is added later, the pre-dispersed TBC particles are already in a monodisperse or micro-agglomerate state, which can be quickly dissolved and dispersed without additional high energy input. At the same time, the TBC spraying rate is matched with the stirring rate of the toluene base material, avoiding the liquid film not being able to wrap the particles in time due to spraying too fast, or the energy wasted due to spraying too slow. This further enhances the pre-dispersion effect and reduces the energy consumption of subsequent mixing processes. (3) Dynamic response stirring-ultrasonic synergistic mixing: Start the reducer to increase the stirring rate to 80-100 r / min, and turn on the built-in ultrasonic transducer after 5 min; The DCS system detects the particle size distribution variation coefficient CV and energy consumption data of the system through an online laser particle size analyzer and energy consumption detection module, and automatically adjusts the stirring rate, ultrasonic power and working cycle according to the CV and energy consumption data, and controls the total mixing time to 40-50 min; This step utilizes a synergistic system of macroscopic circulation and microscopic agglomeration breaking through agitation and ultrasound. The agitation employs a slanted-blade turbine (45° inclination, distance from the bottom of the vessel to 1 / 3 of the vessel's inner diameter). This structure maximizes turbulence intensity, driving the material to circulate throughout the vessel and avoiding uneven dispersion caused by local dead zones. Four ultrasound transducers are evenly distributed circumferentially along the inner wall of the vessel (radiation angle 60°), their radiation area covering the core area of ​​the agitation turbulence. Ultrasound generates microbubbles through cavitation, and the impact force released when these bubbles burst can break up TBC micro-agglomerates (a scale that conventional agitation cannot effectively address). Under the synergistic effect of both, the dispersion efficiency is significantly improved compared to agitation or ultrasound alone, and energy consumption is significantly reduced for the same dispersion effect. The 5-minute delay in starting the ultrasound is to allow the agitation to complete the macroscopic mixing of the material first, avoiding the waste of ultrasound energy in the pure toluene region due to initial solid-liquid separation, further improving energy utilization efficiency. The principle of dynamic parameter adjustment lies in "supplying energy on demand and avoiding ineffective consumption": the CV value directly reflects the uniformity of dispersion, and the energy consumption data reflects the energy utilization efficiency. The DCS system achieves real-time monitoring and rapid response through CV sampling once every 10 seconds and energy consumption sampling once every 5 seconds. When energy consumption is normal and dispersion meets the standard, the initial parameters are maintained to avoid excessive energy consumption. When energy consumption exceeds the standard but dispersion meets the standard, the ultrasonic interval time is extended or the working time is shortened because dispersion has met the requirements at this time, and continuous high energy input is ineffective consumption. The total energy consumption is reduced by "reducing the duration of energy input". When dispersion is insufficient but energy consumption is normal, the ultrasonic interval time is shortened or the ultrasonic power is increased to prioritize the dispersion effect. Energy consumption is optimized after the CV meets the standard. When energy consumption exceeds the standard and dispersion is insufficient, the initial parameters are restored and the stirring rate is increased to quickly repair the dispersion effect. Then, energy consumption is gradually reduced to avoid the dispersion effect deteriorating due to blindly reducing energy consumption, thus achieving a dynamic balance between dispersion effect and energy consumption. (4) Process quality monitoring: During the mixing process, the DCS system uses an online density meter to monitor the density deviation when it exceeds 0.002 g / cm³. 3 At the same time, it automatically maintains density stability by fine-tuning the stirring rate; The TBC-toluene system is a physical mixture. The total proportion was controlled by a proton flow meter during the feeding stage. Therefore, the density deviation is not a problem with the raw material ratio, but rather due to uneven local dispersion of TBC in toluene. The TBC density is approximately 1.049 g / cm³. 3 The concentration was much higher than that of toluene (approximately 0.865 g / cm³). 3 The density is higher when TBC is enriched in certain areas and lower when TBC is scarce in others. The stirring rate directly determines the turbulence intensity and material diffusion efficiency. When the density is high, increasing the stirring rate by 3-5 r / min can enhance the shear flow's breaking effect on locally rich agglomerates and accelerate the diffusion of TBC to low-concentration areas, eliminating the concentration gradient. When the density is low, if insufficient stirring intensity prevents TBC from circulating to the area, increasing the stirring rate by 1-5 r / min can enhance material circulation and ensure uniform TBC distribution. If excessive stirring causes TBC to splash and adhere to the inner wall of the mixing vessel (without participating in mixing), decreasing the stirring rate by 1-5 r / min can reduce turbulent splashing and allow the adhered TBC to fall back into the material and participate in mixing. Thus, without changing the raw material ratio or increasing additional energy consumption, local uneven dispersion can be eliminated by optimizing the fluid motion state, maintaining stable density, and avoiding energy loss and efficiency reduction caused by rework or refueling. (5) Sampling and testing and qualified packaging: After mixing, samples are taken to test the content, appearance, density and color index. After passing the test, the samples are dynamically weighed and packaged through the automatic filling system to obtain TBC-toluene solution. Non-conforming products are handled according to the non-conforming product control procedure. Sampling and testing also include dynamic stability testing, using accelerated aging at 50℃ for 72 hours. This is because high temperatures accelerate molecular motion; if TBC is not uniformly dispersed, it is more likely to aggregate or settle under high temperatures, leading to density changes. This process, through pre-dispersion, synergistic mixing, and dynamic control, ensures that TBC forms a molecular-level dispersion in toluene. In this state, the interaction between TBC molecules and toluene molecules is stable, making them less prone to aggregation or sedimentation due to changes in ambient temperature. Therefore, it meets the requirement of a density change rate ≤0.1%, ensuring the stability of the product during actual storage and use. The TBC feed ratio is 0.5% higher than the theoretical value to compensate for physical losses during production (such as adhering to equipment during feeding, consumption during sampling and testing, and pipeline residues during discharging), ensuring that the final product concentration accurately meets the standards, avoiding low concentrations due to losses, reducing rework rates, and indirectly reducing energy consumption.

[0008] Preferably, the standard for detecting the moisture content of toluene in (1) is ≤0.05%. When the moisture content of toluene exceeds 0.05%, the DCS system automatically triggers the toluene pretreatment process, removes excess moisture through a molecular sieve adsorption device, and then puts it into the mixing tank.

[0009] Preferably, in step (1), the logic of the DCS automatically matching the subsequent feeding rate and mixing parameters according to the TBC particle size is as follows: when the TBC particle size is 100-150μm, the atomization feeding pressure is automatically increased to 0.3-0.4MPa, and the toluene base material feeding ratio is adjusted to 60% of the raw toluene; when the TBC particle size is ≤100μm, the atomization feeding pressure is 0.2-0.3MPa, and the toluene base material feeding ratio is 50% of the raw toluene.

[0010] Preferably, the atomizing particle size of the atomizing feeding device in (2) is 50-80μm, and the TBC spraying rate is controlled at 0.5-1.0kg / min.

[0011] Preferably, in step (3), four ultrasonic transducers are evenly distributed along the circumference of the inner wall of the mixing vessel. The radiation angle of each transducer is 60°. The installation position of the ultrasonic transducer works in synergy with the stirring blade. The ultrasonic radiation area covers the turbulent core area of ​​the stirring blade. The ultrasonic frequency is 25-35kHz, the initial power is 300-500W, and the initial working cycle is 30s with a 10s interval.

[0012] Preferably, the sampling frequency of the online laser particle size analyzer in (3) is 1 time / 10s, and the sampling frequency of the energy consumption monitoring module is 1 time / 5s.

[0013] Preferably, the logic for automatically adjusting the stirring rate, ultrasonic power, and working cycle based on CV and energy consumption data in (3) is as follows: The DCS system uses an online laser particle size analyzer to detect the coefficient of variation (CV) of the system's particle size distribution. Simultaneously, it uses an energy consumption monitoring module to collect the instantaneous power consumption of the ultrasonic transducer and stirring motor, converting this into comprehensive energy consumption per unit time. It also presets energy consumption threshold ranges: normal threshold ≤ 7.5 kWh / ton·h, warning threshold 7.5-8.0 kWh / ton·h, and exceedance threshold > 8.0 kWh / ton·h, with the dispersion constraint index CV ≤ 3%. ① When energy consumption ≤ 7.5 kWh / ton·h and CV ≤ 3%, maintain the initial ultrasonic working cycle; ② When 7.5 kWh / ton·h < energy consumption ≤ 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 30 seconds of operation and 15 seconds of rest. If the energy consumption is still ≥ 7.5 kWh / ton·h after 10 minutes, further adjust the ultrasonic working cycle to 25 seconds of operation and 15 seconds of rest. ③ When energy consumption > 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 20 seconds of operation and 20 seconds of rest. If the energy consumption still exceeds the limit after 5 minutes, then simultaneously fine-tune the stirring rate to reduce it by 5 r / min. ④ When the energy consumption is ≤7.5kwh / ton·h but CV>3%, adjust the ultrasonic working cycle to 30s working and 5s intermittent. If CV is still >3% after 10min, increase the ultrasonic power to 550W. ⑤ When energy consumption > 8.0 kWh / ton·h and CV > 3%, first restore the initial ultrasonic working cycle and increase the stirring rate by 10 r / min. After CV ≤ 3%, gradually optimize energy consumption according to the logic in ②.

[0014] Preferably, in step (3), the stirring blade is an inclined turbine blade with an inclination angle of 45° and a distance of 1 / 3 of the inner diameter of the mixing vessel from the bottom of the mixing vessel.

[0015] Preferably, the fine-tuning of the stirring rate in (4) refers to increasing the stirring rate by 3-5 r / min when the density is too high, and increasing or decreasing the stirring rate by 1-5 r / min when the density is too low, until the density returns to normal.

[0016] Preferably, the sampling and testing in (5) further includes dynamic stability testing: the sample is placed in an environment of 50°C for accelerated aging for 72 hours, and the density change rate is detected to be ≤0.1%.

[0017] Preferably, the concentration of the TBC-toluene solution in (5) is 10%-30%, the ratio of TBC to toluene is adjusted by linear interpolation, the total ratio of the two is always kept at 100%, and the ratio of TBC is always higher than the theoretical value of 0.5%.

[0018] The beneficial effects of this invention are: 1. This invention reduces mixing energy consumption from the source through a synergistic design of "raw material pre-matching - pre-dispersion - dynamic parameter adjustment". Raw material pre-matching adapts process parameters according to TBC particle size and toluene moisture content as needed, avoiding energy waste; gradient wetting pre-dispersion breaks up TBC particle agglomeration in advance, reducing the energy load of subsequent mixing; the dynamic response stirring-ultrasound synergistic system adjusts parameters in real time based on energy consumption and dispersion status, avoiding ineffective energy input, while the ultrasonic hysteresis activation design further improves energy utilization. The overall process achieves significant energy savings without the need for additional high-energy-consuming equipment, aligning with the green and low-carbon development needs of industrial production.

[0019] 2. This invention completely solves the problem of uneven dispersion caused by TBC particle agglomeration through the dual guarantee of gradient wetting-pre-dispersion coupled feeding and stirring-ultrasonic synergistic mixing. Atomized feeding ensures that TBC particles are uniformly sprayed onto the surface of the rotating toluene liquid film, achieving sufficient wetting and pre-dispersion; stirring provides macroscopic turbulent circulation, and ultrasound breaks up micro-agglomerates through cavitation effect. The synergistic effect of these two methods achieves molecular-level dispersion of TBC in toluene. The product has no local concentration deviation, uniform density distribution, and can stably perform its application properties such as polymerization inhibition and antioxidant properties, effectively avoiding subsequent production quality fluctuations caused by uneven dispersion.

[0020] 3. This invention establishes a full-process online monitoring and real-time control system, capturing changes in process status in real time through equipment such as online densitometers and laser particle size analyzers. When density deviations or insufficient dispersion are detected, the DCS system automatically fine-tunes the stirring rate and ultrasonic parameters to quickly correct quality problems without manual intervention or rework, significantly shortening production response time. Simultaneously, the TBC feed surplus design compensates for physical losses during production, ensuring accurate product concentration, significantly improving production efficiency and batch pass rate, and reducing production costs and resource waste.

[0021] 4. This invention retains the core process flow of existing "equipment inspection-feeding-mixing-testing-packaging," and achieves technological upgrades only by optimizing the technical logic and parameter control methods of each process. It requires no changes to the production line layout or the addition of complex equipment, resulting in low modification costs, strong compatibility, and direct application to existing industrial production lines. The process can be flexibly adapted to the preparation of TBC-toluene solutions within different concentration ranges. By adjusting the feeding ratio through linear interpolation, it meets the application needs of different industries, possessing strong industrial promotion value and practicality.

[0022] 5. This invention ensures stable product performance during long-term storage and use through the construction of a molecular-level dispersion state and a dynamic stability testing mechanism. The synergistic effect of pre-dispersion, synergistic mixing, and dynamic regulation enables TBC molecules and toluene molecules to form stable interactions, making them less prone to aggregation, stratification, or sedimentation even at high temperatures. The product meets long-term storage requirements without the need for additional stabilizers, effectively extending shelf life, reducing quality risks for users, and improving application experience and reliability. Attached Figure Description

[0023] Figure 1 This is a process diagram for the production of TBC-toluene solution according to the present invention. Detailed Implementation

[0024] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments.

[0025] Example 1: A low-energy-consumption process for the uniform dispersion preparation of a 10% TBC-toluene composite system, specifically including the following steps: Raw materials: 10.5% solid TBC, particle size 90μm; 89.5% toluene, moisture content 0.04%. (1) Equipment pretreatment and raw material pre-matching: Open the manhole of the mixing vessel to check the integrity of the equipment, close the bottom valve, verify that the reducer is normal, and then seal the mixing vessel; enter the raw material toluene moisture content detection data and TBC particle size distribution detection data into the DCS system, and the DCS will automatically increase the atomization feeding pressure to 0.25MPa according to the TBC particle size, and adjust the toluene bottom material input ratio to 50% of the raw material toluene; (2) Gradient wetting-pre-dispersion coupled feeding: Turn on the feed pump and feed 50% of the raw material toluene into the mixing vessel as the base material through the proton flow meter. Start low-speed stirring at 40 r / min to form a rotating liquid film. Spray solid TBC evenly onto the surface of the liquid film at 0.5 kg / min through the atomizing feeding device. After the atomizing feeding is completed, add the remaining raw material toluene through the proton flow meter to maintain the normal temperature and pressure environment. (3) Dynamic response stirring-ultrasonic synergistic mixing: Start the reducer to increase the stirring speed to 80 r / min, and after 5 min, turn on the built-in ultrasonic transducer in the mixing vessel (ultrasonic frequency 25 kHz, initial power 300 W, initial working cycle of 30 s and 10 s interval); The DCS system uses an online laser particle size analyzer (sampling frequency of 1 time / 10 s) and an energy consumption detection module (sampling frequency of 1 time / 5 s) to detect the particle size distribution variation coefficient CV and energy consumption data of the system. Based on the CV and energy consumption data: ① When energy consumption ≤ 7.5 kWh / ton·h and CV ≤ 3%, maintain the initial ultrasonic working cycle; ② When 7.5 kWh / ton·h < energy consumption ≤ 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 30 seconds of operation and 15 seconds of rest. If the energy consumption is still ≥ 7.5 kWh / ton·h after 10 minutes, further adjust the ultrasonic working cycle to 25 seconds of operation and 15 seconds of rest. ③ When energy consumption > 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 20 seconds of operation and 20 seconds of rest. If the energy consumption still exceeds the limit after 5 minutes, then simultaneously fine-tune the stirring rate to reduce it by 5 r / min. ④ When the energy consumption is ≤7.5kwh / ton·h but CV>3%, adjust the ultrasonic working cycle to 30s working and 5s intermittent. If CV is still >3% after 10min, increase the ultrasonic power to 550W. ⑤ When energy consumption > 8.0 kWh / ton·h and CV > 3%, first restore the initial ultrasonic working cycle and increase the stirring rate by 10 r / min. After CV ≤ 3%, gradually optimize energy consumption according to the logic in ②. Automatically adjust the stirring rate, ultrasonic power and working cycle, and control the total mixing time to 40 min. (4) Process quality monitoring: During the mixing process, the DCS system uses an online density meter to monitor the density deviation when it exceeds 0.002 g / cm³. 3 When the density is too high, the stirring speed is increased by 3-5 r / min; when the density is too low, the stirring speed is increased or decreased by 1-5 r / min until the density returns to normal. (5) Sampling and testing and qualified packaging: After mixing, samples are taken to test the content, appearance, density and color index. After passing the test, the samples are dynamically weighed and packaged through the automatic filling system to obtain 10% TBC-toluene solution. Non-conforming products are handled according to the non-conforming product control procedure.

[0026] Example 2: A low-energy-consumption preparation process for the uniform dispersion of a 20% TBC-toluene composite system, specifically including the following steps: Raw materials: 20.5% solid TBC, particle size 110μm; 79.5% toluene, moisture content 0.03%. (1) Equipment pretreatment and raw material pre-matching: Open the manhole of the mixing vessel to check the integrity of the equipment, close the bottom valve, verify that the reducer is normal, and then seal the mixing vessel; enter the raw material toluene moisture content detection data and TBC particle size distribution detection data into the DCS system, and the DCS will automatically increase the atomization feeding pressure to 0.35MPa according to the TBC particle size, and adjust the toluene bottom material input ratio to 60% of the raw material toluene; (2) Gradient wetting-pre-dispersion coupled feeding: Turn on the feed pump and feed 60% of the raw material toluene into the mixing vessel as the base material through the proton flow meter. Start low-speed stirring at 45 r / min to form a rotating liquid film. Spray solid TBC evenly onto the surface of the liquid film at 0.8 kg / min through the atomizing feeding device. After the atomizing feeding is completed, add the remaining raw material toluene through the proton flow meter to maintain the normal temperature and pressure environment. (3) Dynamic response stirring-ultrasonic synergistic mixing: Start the reducer to increase the stirring speed to 90 r / min, and after 5 min, turn on the built-in ultrasonic transducer in the mixing vessel (ultrasonic frequency 30 kHz, initial power 400 W, initial working cycle of 30 s and 10 s interval); The DCS system uses an online laser particle size analyzer (sampling frequency of 1 time / 10 s) and an energy consumption detection module (sampling frequency of 1 time / 5 s) to detect the coefficient of variation (CV) of the particle size distribution and energy consumption data of the system. Based on the CV and energy consumption data: ① When energy consumption ≤ 7.5 kWh / ton·h and CV ≤ 3%, maintain the initial ultrasonic working cycle; ② When 7.5 kWh / ton·h < energy consumption ≤ 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 30 seconds of operation and 15 seconds of rest. If the energy consumption is still ≥ 7.5 kWh / ton·h after 10 minutes, further adjust the ultrasonic working cycle to 25 seconds of operation and 15 seconds of rest. ③ When energy consumption > 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 20 seconds of operation and 20 seconds of rest. If the energy consumption still exceeds the limit after 5 minutes, then simultaneously fine-tune the stirring rate to reduce it by 5 r / min. ④ When the energy consumption is ≤7.5kwh / ton·h but CV>3%, adjust the ultrasonic working cycle to 30s working and 5s intermittent. If CV is still >3% after 10min, increase the ultrasonic power to 550W. ⑤ When energy consumption > 8.0 kWh / ton·h and CV > 3%, first restore the initial ultrasonic working cycle and increase the stirring rate by 10 r / min. After CV ≤ 3%, gradually optimize energy consumption according to the logic in ②. Automatically adjust the stirring rate, ultrasonic power and working cycle, and control the total mixing time to 44 min. (4) Process quality monitoring: During the mixing process, the DCS system uses an online density meter to monitor the density deviation when it exceeds 0.002 g / cm³. 3 When the density is too high, the stirring speed is increased by 3-5 r / min; when the density is too low, the stirring speed is increased or decreased by 1-5 r / min until the density returns to normal. (5) Sampling and testing and qualified packaging: After mixing, samples are taken to test the content, appearance, density and color index. After passing the test, the samples are dynamically weighed and packaged through the automatic filling system to obtain 20% TBC-toluene solution. Non-conforming products are handled according to the non-conforming product control procedure.

[0027] Example 3: A low-energy-consumption process for the uniform dispersion preparation of a 10% TBC-toluene composite system, specifically including the following steps: Raw materials: 30.5% solid TBC, particle size 120μm; 69.5% toluene, moisture content 0.03%. (1) Equipment pretreatment and raw material pre-matching: Open the manhole of the mixing vessel to check the integrity of the equipment, close the bottom valve, verify that the reducer is normal, and then seal the mixing vessel; enter the raw material toluene moisture content detection data and TBC particle size distribution detection data into the DCS system, and the DCS will automatically increase the atomization feeding pressure to 0.35MPa according to the TBC particle size, and adjust the toluene bottom material input ratio to 50% of the raw material toluene; (2) Gradient wetting-pre-dispersion coupled feeding: Turn on the feed pump and feed 60% of the raw material toluene into the mixing vessel as the base material through the proton flow meter. Start low-speed stirring at 50 r / min to form a rotating liquid film. Spray solid TBC evenly onto the surface of the liquid film at 1.0 kg / min through the atomizing feeding device. After the atomizing feeding is completed, add the remaining raw material toluene through the proton flow meter to maintain the normal temperature and pressure environment. (3) Dynamic response stirring-ultrasonic synergistic mixing: Start the reducer to increase the stirring speed to 100r / min, and after 5min, turn on the built-in ultrasonic transducer of the mixing vessel (ultrasonic frequency 35kHz, initial power 500W, initial working cycle of 30s working and 10s intermittent); The DCS system detects the particle size distribution variation coefficient CV and energy consumption data of the system through an online laser particle size analyzer (sampling frequency of 1 time / 10s) and an energy consumption detection module (sampling frequency of 1 time / 5s). Based on the CV and energy consumption data: ① When energy consumption ≤ 7.5 kWh / ton·h and CV ≤ 3%, maintain the initial ultrasonic working cycle; ② When 7.5 kWh / ton·h < energy consumption ≤ 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 30 seconds of operation and 15 seconds of rest. If the energy consumption is still ≥ 7.5 kWh / ton·h after 10 minutes, further adjust the ultrasonic working cycle to 25 seconds of operation and 15 seconds of rest. ③ When energy consumption > 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 20 seconds of operation and 20 seconds of rest. If the energy consumption still exceeds the limit after 5 minutes, then simultaneously fine-tune the stirring rate to reduce it by 5 r / min. ④ When the energy consumption is ≤7.5kwh / ton·h but CV>3%, adjust the ultrasonic working cycle to 30s working and 5s intermittent. If CV is still >3% after 10min, increase the ultrasonic power to 550W. ⑤ When energy consumption > 8.0 kWh / ton·h and CV > 3%, first restore the initial ultrasonic working cycle and increase the stirring rate by 10 r / min. After CV ≤ 3%, gradually optimize energy consumption according to the logic in ②. Automatically adjust the stirring rate, ultrasonic power and working cycle, and control the total mixing time to 50 min. (4) Process quality monitoring: During the mixing process, the DCS system uses an online density meter to monitor the density deviation when it exceeds 0.002 g / cm³. 3 When the density is too high, the stirring speed is increased by 3-5 r / min; when the density is too low, the stirring speed is increased or decreased by 1-5 r / min until the density returns to normal. (5) Sampling and testing and qualified packaging: After mixing, samples are taken to test the content, appearance, density and color index. After passing the test, the samples are dynamically weighed and packaged through an automatic filling system to obtain a 30% TBC-toluene solution. Non-conforming products are handled according to the non-conforming product control procedure.

[0028] Comparative Example: A process for uniformly dispersing a TBC-toluene composite system, specifically including the following steps: Raw materials: 30.5% solid TBC, particle size 120μm; 70.5% toluene, moisture content 0.03%. (1) Equipment pretreatment: Open the manhole of the mixing vessel to check the integrity of the equipment, close the bottom valve, verify that the reducer is normal, and then seal the mixing vessel; do not test the toluene moisture content and TBC particle size distribution, and do not pre-match the DCS system; (2) Direct feeding: Turn on the feed pump and feed all the toluene into the mixing tank through the proton flow meter. Pour the solid TBC directly into the mixing tank. There is no atomization feeding device and no gradient wetting-pre-dispersion stage. Start the low-speed stirring at 50r / min and maintain the normal temperature and pressure environment. (3) Single mechanical stirring and mixing: Start the reducer to fix the stirring rate at 100r / min, do not turn on the ultrasonic transducer, do not use the online laser particle size analyzer and energy consumption monitoring module, do not dynamically adjust any parameters, and extend the total mixing time to 60min; (4) Manual quality monitoring: During the mixing process, the density is measured manually every 15 minutes. When the density deviation is >0.002 g / cm³, the density is measured. 3 In such cases, corrections are made by adding toluene or TBC. (5) Sampling, testing and packaging: After mixing, samples are taken to test the content, appearance, density and color index; after passing the test, the samples are dynamically weighed and packaged through an automatic filling system to obtain a 30% TBC-toluene solution. Non-conforming products are handled according to the non-conforming product control procedure.

[0029] Performance testing: 1. Particle Size Variation Coefficient (CV) Test: A Malvern laser particle size analyzer (model: Mastersizer 3000) was used to test the dispersion uniformity of the TBC-toluene systems in Examples 1-3 and the comparative example. In the examples, following the online detection logic set in the process, the laser particle size analyzer collected particle size distribution data of the mixing system in real time at a frequency of 1 time / 10 seconds. From the start of stirring-ultrasonic co-mixing until the end of mixing, at least 240 sets of valid data were recorded. The particle size variation coefficient (CV) of each set of data was calculated using the instrument's built-in software, and the average value of all data was taken as the final result. For the comparative example, which lacked an online detection module, manual sampling was used. Every 20 minutes, one sample was taken from different areas (upper, middle, and lower layers) of the mixing vessel, for a total of 3 samples per sampling. A total of 3 samplings were performed during the mixing process. Each sample was placed in the laser particle size analyzer for offline detection, and the CV value of each sample was calculated. The average value of 9 samples was taken as the final CV value of the comparative example. The experimental results are shown in Table 1.

[0030] 2. Process Unit Consumption Test: A high-precision power meter (accuracy class 0.5) was used to measure the total energy consumption during the production process of Examples 1-3 and the comparative example. The test scope covered the entire preparation process. For the examples, the instantaneous power consumption of the stirring motor and ultrasonic transducer was recorded separately (sampling frequency 1 time / 5s), while for the comparative example, only the instantaneous power consumption of the stirring motor was recorded. After production, the total power consumption (unit: kWh) was calculated, and combined with the actual mass of TBC-toluene solution produced (unit: tons), the process unit consumption (unit: kWh / ton) was calculated. For the examples, the fluctuation and final average value of energy consumption during dynamic parameter adjustment were calculated, while the average energy consumption under a fixed stirring rate was calculated for the comparative example. The experimental results are shown in Table 1.

[0031] 3. Density deviation test: An online density meter was used (measurement accuracy ±0.0001 g / cm³). 3 The system density during the mixing process of Examples 1-3 was monitored in real time, with the monitoring frequency consistent with the process. Density data was recorded throughout the entire mixing process, from start to finish. The absolute value of the difference between all density data and the target density during the mixing process was taken as the density deviation result for each example. An offline density meter (accuracy ±0.0001 g / cm³) was used for the comparative example. 3Samples were taken from different areas of the mixing vessel according to the manual sampling cycle (every 20 minutes), the sample density was detected and compared with the corresponding target density, the density deviation of each sampling was recorded, and the maximum value of all deviation values ​​was taken as the density deviation result of the comparative example. The experimental results are shown in Table 1.

[0032] 4. Dynamic Stability Test: Dynamic stability testing was performed only on the qualified products from Examples 1-3 and the comparative examples. Three parallel samples were taken from each group, with each parallel sample containing 500 mL. After sealing, the samples were placed in a 50℃ constant temperature aging chamber for accelerated aging for 72 hours. During aging, sample shaking or temperature fluctuations were avoided. After aging, the samples were cooled to room temperature. The dynamic stability was measured with an accuracy of ±0.0001 g / cm³. 3 The density of the samples before and after aging was measured by a densitometer. The density change rate of each parallel sample was calculated (density change rate = |density after aging - density before aging| / density before aging × 100%). The average value of the three parallel samples was taken as the final dynamic stability result. The results of the example and the comparative example were observed to see whether stratification or precipitation occurred after high-temperature aging. The experimental results are shown in Table 1.

[0033] Table 1 Performance Test Results Performance Analysis: As shown in Table 1, the particle size variation coefficient (CV) of Examples 1-3 was controlled between 2.3% and 2.8%, and showed a slight increasing trend with increasing TBC concentration, meeting the process setting constraint of CV ≤ 3%. In contrast, the CV value of the comparative example was as high as 5.7%, more than twice that of the examples, indicating a significant difference in dispersion uniformity. This difference stems from the core difference in process design: the examples used a "gradient wetting-pre-dispersion coupled feeding" method, where solid TBC was uniformly sprayed onto the surface of a rotating toluene liquid film after passing through an atomizing feeding device, breaking the particle agglomeration force at the source. Combined with the "stirring-ultrasonic synergistic mixing" system, the full-bottle turbulent circulation brought by the inclined blade turbine propeller and the microscopic de-agglomeration effect of ultrasonic cavitation complement each other. With the dynamic control logic of the DCS system adjusting parameters in real time according to the CV value, the TBC particles were ensured to achieve molecular-level dispersion in toluene. In contrast, the lack of a pre-dispersion stage resulted in the formation of blocky agglomerates after TBC was directly fed in. Simple mechanical stirring was insufficient to break up the tiny agglomerates, and there was no dynamic adjustment mechanism. Even with the mixing time extended to 60 minutes, there was still significant local uneven dispersion, which ultimately resulted in a significantly higher CV value.

[0034] Energy consumption data shows that the process energy consumption of Examples 1-3 is between 6.2-6.9 kWh / ton, which is 33%-39% lower than the 10.3 kWh / ton of the comparative example, demonstrating a significant advantage in low energy consumption. The energy consumption optimization of the examples is not simply a reduction in parameters, but rather based on the core logic of "on-demand energy supply": the pre-dispersion stage keeps TBC particles in a monodisperse or micro-aggregate state, significantly reducing the energy load of subsequent mixing; the ultrasonic transducer starts stirring 5 minutes later to avoid energy waste caused by initial solid-liquid separation; the DCS system collects data in real time through the energy consumption monitoring module. When energy consumption exceeds the standard but dispersion meets the standard, ineffective energy consumption is reduced by extending the ultrasonic interval and shortening the working time; when dispersion is insufficient, parameters are appropriately increased to ensure the effect, achieving a dynamic balance between energy consumption and dispersion effect. The comparative example, lacking pre-dispersion and dynamic energy consumption optimization mechanisms, requires long-term fixed-rate stirring to overcome agglomeration resistance, resulting in persistently high energy consumption due to continuous high-load operation. This highlights the innovative improvement in energy utilization efficiency of the present invention.

[0035] The density deviation data directly reflects the effectiveness of process quality control: the density deviation in Examples 1-3 was only 0.001-0.002 g / cm³. 3 It fully meets the process specification of ≤0.002g / cm³. 3 Requirements; however, the density deviation of the comparative example reached 0.008 g / cm³. 3 The density difference between TBC and toluene is four times that of the previous example, with significant fluctuations in process quality. This result is attributed to the online monitoring and real-time control design of the previous example: TBC and toluene have a large density difference; the density deviation is essentially due to localized uneven dispersion leading to TBC enrichment or depletion. The previous example uses an online density meter to capture density changes in real time. When the deviation exceeds a threshold, the DCS system automatically fine-tunes the stirring rate. When the density is too high, the rate is increased to enhance shear diffusion; when the density is too low, the rate is adjusted as needed to optimize material circulation and quickly eliminate concentration gradients. In contrast, the comparative example relies on manual sampling and replenishment every 15 minutes, which has a significant lag and cannot correct localized uneven dispersion in real time. Furthermore, single stirring cannot completely eliminate density fluctuations caused by agglomeration, resulting in poor process quality stability.

[0036] Dynamic stability tests showed that the density change rate of Examples 1-3 was only 0.03%-0.07%, and they remained uniform and transparent after high-temperature aging, without stratification or precipitation. The density change rate of the comparative example was 0.32%, with slight stratification and fine sedimentation at the bottom, indicating a significant difference in long-term stability. The superior stability of the examples stems from the construction of a molecular-level dispersion: the synergistic effect of pre-dispersion, stirring-ultrasonic mixing, and dynamic parameter adjustment allows TBC molecules to form a stable interaction with toluene molecules, preventing aggregation or sedimentation even under the harsh conditions of accelerated aging at 50°C for 72 hours. The comparative example, due to uneven dispersion, contained incompletely broken micro-agglomerates. The high-temperature environment accelerated molecular motion and agglomerate aggregation, ultimately leading to stratification, precipitation, and a surge in density change rate, demonstrating the technical value of the process in ensuring the long-term reliability of the product.

[0037] Based on comprehensive performance indicators, the process of this invention, through an integrated technical system of "raw material pre-matching - gradient wetting pre-dispersion - dynamic response stirring - ultrasonic synergy - process quality monitoring," achieves a synergistic improvement in dispersion uniformity, low energy consumption, process stability, and dynamic stability. In the examples, within a TBC concentration range of 10%-30%, the CV value remained ≤2.8%, energy consumption ≤6.9 kWh / ton, and density deviation ≤0.002 g / cm³. 3 It exhibits excellent performance with a density change rate of ≤0.07%, and compared with traditional processes (comparative example), it improves dispersion uniformity by more than 50%, reduces energy consumption by more than 33%, improves process stability by more than 75%, and improves dynamic stability by more than 78%.

[0038] 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 low-energy-consumption TBC-toluene composite system uniform dispersion preparation process, characterized in that, Includes the following steps: (1) Equipment pretreatment and raw material pre-matching: Open the manhole of the mixing tank to check the integrity of the equipment, close the bottom valve, verify that the reducer is normal, and then seal the mixing tank; test the moisture content of the raw toluene and the particle size distribution of solid p-tert-butylcatechol (TBC). Enter the test data into the DCS system, and the DCS will automatically match the subsequent feeding rate and mixing parameters according to the TBC particle size. (2) Gradient wetting-pre-dispersion coupled feeding: Turn on the feed pump and add 50%-60% of the raw material toluene as the base material to the mixing vessel according to the ratio through the proton flow meter. Start low-speed stirring at 40-50 r / min to form a rotating liquid film. Spray the solid TBC evenly onto the surface of the liquid film through the atomizing feeding device. After the atomizing feeding is completed, add the remaining raw material toluene through the proton flow meter to maintain the normal temperature and pressure environment. (3) Dynamic response stirring-ultrasonic synergistic mixing: Start the reducer to increase the stirring speed of the stirring blades in the mixing vessel to 80-100 r / min, and turn on the built-in ultrasonic transducer after 5 min; The DCS system detects the particle size distribution variation coefficient CV and energy consumption data of the system through an online laser particle size analyzer and energy consumption detection module, and automatically adjusts the stirring speed, ultrasonic power and working cycle according to the CV and energy consumption data, and controls the total mixing time to 40-50 min; (4) Process quality monitoring: During the mixing process, the DCS system uses an online density meter to monitor the density deviation when it exceeds 0.002 g / cm³. 3 At the same time, it automatically maintains density stability by fine-tuning the stirring rate; (5) Sampling and testing and qualified packaging: After mixing, samples are taken to test the content, appearance, density and color index. After passing the test, the samples are dynamically weighed and packaged through an automatic filling system to obtain TBC-toluene solution. Non-conforming products are handled according to the non-conforming product control procedure.

2. The uniform dispersion preparation process of the low-energy TBC-toluene composite system according to claim 1, characterized in that, The standard for detecting the moisture content of toluene in (1) is ≤0.05%. When the moisture content of toluene exceeds 0.05%, the DCS system automatically triggers the toluene pretreatment process, removes excess moisture through a molecular sieve adsorption device, and then puts it into the mixing tank.

3. The uniform dispersion preparation process of the low-energy TBC-toluene composite system according to claim 1, characterized in that, The logic of DCS automatically matching subsequent feeding rate and mixing parameters according to TBC particle size in (1) is as follows: when TBC particle size is 100-150μm, the atomization feeding pressure is automatically increased to 0.3-0.4MPa, and the toluene base material feeding ratio is adjusted to 60% of the raw toluene; when TBC particle size is ≤100μm, the atomization feeding pressure is 0.2-0.3MPa, and the toluene base material feeding ratio is 50% of the raw toluene.

4. The uniform dispersion preparation process of the low-energy TBC-toluene composite system according to claim 1, characterized in that, The atomizing particle size of the atomizing feeding device in (2) is 50-80μm, and the TBC spraying rate is controlled at 0.5-1.0kg / min.

5. The uniform dispersion preparation process of the low-energy TBC-toluene composite system according to claim 1, characterized in that, In (3), four ultrasonic transducers are evenly distributed along the circumference of the inner wall of the mixing vessel. The radiation angle of each transducer is 60°. The installation position of the ultrasonic transducer works in synergy with the stirring blade. The ultrasonic radiation area covers the turbulent core area of ​​the stirring blade. The ultrasonic frequency is 25-35kHz, the initial power is 300-500W, and the initial working cycle is 30s with a 10s interval. The sampling frequency of the online laser particle size analyzer is 1 time / 10s, and the sampling frequency of the energy consumption monitoring module is 1 time / 5s.

6. The uniform dispersion preparation process of the low-energy TBC-toluene composite system according to claim 1, characterized in that, The logic in (3) for automatically adjusting the stirring rate, ultrasonic power, and working cycle based on CV and energy consumption data is as follows: The DCS system uses an online laser particle size analyzer to detect the coefficient of variation (CV) of the system's particle size distribution. Simultaneously, it uses an energy consumption monitoring module to collect the instantaneous power consumption of the ultrasonic transducer and stirring motor, converting this into comprehensive energy consumption per unit time. It also presets energy consumption threshold ranges: normal threshold ≤ 7.5 kWh / ton·h, warning threshold 7.5-8.0 kWh / ton·h, and exceedance threshold > 8.0 kWh / ton·h, with the dispersion constraint index CV ≤ 3%. ① When energy consumption ≤ 7.5 kWh / ton·h and CV ≤ 3%, maintain the initial ultrasonic working cycle; ② When 7.5 kWh / ton·h < energy consumption ≤ 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 30 seconds of operation and 15 seconds of rest. If the energy consumption is still ≥ 7.5 kWh / ton·h after 10 minutes, further adjust the ultrasonic working cycle to 25 seconds of operation and 15 seconds of rest. ③ When energy consumption > 8.0 kWh / ton·h and CV ≤ 3%, adjust the ultrasonic working cycle to 20 seconds of operation and 20 seconds of rest. If the energy consumption still exceeds the limit after 5 minutes, then simultaneously fine-tune the stirring rate to reduce it by 5 r / min. ④ When the energy consumption is ≤7.5kwh / ton·h but CV>3%, adjust the ultrasonic working cycle to 30s working and 5s intermittent. If CV is still >3% after 10min, increase the ultrasonic power to 550W. ⑤ When energy consumption > 8.0 kWh / ton·h and CV > 3%, first restore the initial ultrasonic working cycle and increase the stirring rate by 10 r / min. After CV ≤ 3%, gradually optimize energy consumption according to the logic in ②.

7. The uniform dispersion preparation process of the low-energy TBC-toluene composite system according to claim 1, characterized in that, In (3), the stirring blade is an inclined turbine blade with an inclination angle of 45° and a distance of 1 / 3 of the inner diameter of the mixing vessel from the bottom of the mixing vessel.

8. The uniform dispersion preparation process of the low-energy TBC-toluene composite system according to claim 1, characterized in that, The fine-tuning of the stirring rate in (4) refers to increasing the stirring rate by 3-5 r / min when the density is too high, and increasing or decreasing the stirring rate by 1-5 r / min when the density is too low, until the density returns to normal.

9. The uniform dispersion preparation process of the low-energy TBC-toluene composite system according to claim 1, characterized in that, The sampling and testing in (5) also includes dynamic stability testing: the sample is placed in an environment of 50°C for accelerated aging for 72 hours, and the density change rate is detected to be ≤0.1%.

10. The uniform dispersion preparation process of the low-energy TBC-toluene composite system according to claim 1, characterized in that, The concentration of the TBC-toluene solution in (5) is 10%-30%, and the ratio of TBC to toluene is adjusted by linear interpolation. The total ratio of the two is always kept at 100%, and the ratio of TBC is always higher than the theoretical value of 0.5%.

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