An automatic process for the injection of a pre-agglomerated inhibitor

Abstract

The application discloses a kind of agglomerate pretreatment inhibitor automatic feeding processes, comprising: S100: the agglomerate inhibitor is sent into pretreatment unit, by stirring disturbance cooperation dehumidification drying synergistic effect, agglomerate inhibitor is simultaneously implemented agglomerate crushing and material dehumidification, obtain high flowability micro fine powder;S200: high flowability micro fine powder is transported to the temporary storage in the buffer bin of configuration weight detection unit;S300: target feeding weight is preset, and the weight closed loop feedback is formed by the weight detection unit real-time acquisition material weight in buffer bin, and the quantitatively conveyed powder is linked controllable screw conveying mechanism;When cumulative feeding amount reaches preset target weight, material conveying is automatically cut off to complete feeding.The application solves the problems of low measurement accuracy, high labor cost of existing inhibitor feeding method, and achieves the advantages of high operation safety, accurate measurement accuracy, high pretreatment efficiency and strong system reliability.

Description

Technical Field

[0001] This invention relates to the field of acrylic acid chemical production auxiliary agent addition technology, specifically an automatic addition process for agglomeration pretreatment polymerization inhibitor. Background Technology

[0002] Acrylic acid monomers are chemically active and are prone to self-polymerization during production, generating heavy component impurities that seriously affect product purity and stable operation of equipment. In industry, hydroquinone-based solid polymerization inhibitors are commonly added to inhibit monomer polymerization. The current mainstream method of adding polymerization inhibitors in the industry is to manually open the cap and pour the powder into the polymerization inhibitor feeding port. Therefore, the existing process has several unavoidable defects: (1) High risk to personnel health and safety: manual contact with polymerization inhibitor powder, significant dust generation during feeding, and long-term operation will cause continuous damage to the respiratory tract and skin of operators, resulting in prominent occupational health hazards; (2) Poor metering accuracy: relying entirely on manual experience to estimate the amount added, the actual amount added deviates greatly from the theoretical requirement. When the addition is insufficient, the polymerization inhibition effect fails and acrylic acid polymerizes in large quantities; when the addition is excessive, the raw material cost increases and impurities are introduced into the subsequent distillation and refining processes; (3) The labor cost of pretreatment of agglomeration is high: solid polymerization inhibitors are very easy to absorb moisture and agglomerate. Before feeding, the agglomerated material must be crushed manually. The crushing process is time-consuming and labor-intensive, which greatly increases the labor time and production cost; (4) Material conveying is easy to block: the agglomerated material that is not fully crushed is easy to bridge and block the pipe after entering the pipeline and mixing tank. Frequent shutdowns and manual unblocking are required, which reduces the continuous operation efficiency of the device.

[0003] In summary, how to achieve fully automated, unmanned powder handling, automatic agglomeration pretreatment, and precise quantitative addition of polymerization inhibitors is a key technical bottleneck that urgently needs to be addressed in the current acrylic acid production additive addition process. Summary of the Invention

[0004] The purpose of this application is to provide an automatic dosing process for agglomeration pretreatment inhibitors, which has the advantages of high operational safety, accurate metering, high pretreatment efficiency and strong system reliability.

[0005] This application provides an automated dosing process for an agglomeration pretreatment inhibitor, including:

[0006] S100: The agglomeration inhibitor is fed into the pretreatment unit. Through the combined action of stirring and dehumidification and drying, the agglomeration inhibitor is simultaneously crushed and the material is dehumidified to obtain a highly fluid fine powder.

[0007] S200: The high-flowability fine powder is temporarily stored in a buffer bin equipped with a weight detection unit;

[0008] S300: The target feeding weight is preset, and the weight detection unit collects the weight of the material in the buffer bin in real time to form a weight closed-loop feedback, which is linked to the controllable screw conveyor to quantitatively transport the powder; when the cumulative feeding amount reaches the preset target weight, the material conveying is automatically cut off to complete the feeding.

[0009] The pretreatment unit is equipped with a stirring and agitation component and an inert gas dehumidification and drying component; the controllable screw conveyor mechanism has a built-in secondary crushing structure, which is used to further shear and refine the residual clumps during the conveying process.

[0010] Furthermore, the agglomeration inhibitor includes at least one of the following: aromatic phenolic polymerization inhibitors, organic sulfur-containing polymerization inhibitors, organometallic salt polymerization inhibitors, and alkyl ether polymerization inhibitors.

[0011] Furthermore, aromatic phenolic polymerization inhibitors include at least one of hydroquinone, catechol, resorcinol, and methyl hydroquinone; organic sulfur-containing polymerization inhibitors include at least one of phenoxythiazide, thiodipropionate, and alkyl thiols; organometallic salt polymerization inhibitors include at least one of copper acetate, copper salicylate, cuprous chloride, and copper naphthenates; and alkyl ether polymerization inhibitors include at least one of methyl ether, methyl tert-butyl ether, and dimethyl terephthalate.

[0012] Furthermore, the pretreatment unit includes a pretreatment chamber; the stirring and agitation components and the inert gas dehumidification and drying components are integrated and arranged inside the pretreatment chamber, and the two work together to simultaneously complete the mechanical crushing of the agglomeration inhibitor and the inert atmosphere dehumidification and drying; the pretreatment chamber is a fully enclosed pressure-bearing structure, which is used to block the dust of the powder, isolate the external humid air, and prevent the agglomeration inhibitor from absorbing moisture and agglomerating again.

[0013] Furthermore, the stirring and agitation component is a controllable screw stirring control system, which includes a drive motor, a transmission mechanism, and a stirring screw with stirring blades;

[0014] S100 also includes the following steps: the stirring screw continuously shears, kneads and breaks up the agglomerating inhibitor by relying on the screw spiral surface and stirring blades, while turning the agglomerating inhibitor to achieve full contact and heat exchange between the material and the dry inert gas.

[0015] Furthermore, the inert gas dehumidification and drying assembly includes: an inert gas source, a drying and filtering unit, a flow regulating valve, and an internal gas distribution pipeline;

[0016] S100 also includes the following steps: continuously introducing the dried and dehydrated inert gas into the pretreatment chamber to form an inert atmosphere inside the chamber.

[0017] Furthermore, a vibrating air hammer is installed inside the buffer compartment, and the vibrating air hammer is installed on the inner wall of the buffer compartment.

[0018] S300 also includes the following steps: controlling the vibrating hammer to vibrate intermittently or continuously to break up the highly fluid fine powder that accumulates and sticks to the walls of the buffer chamber.

[0019] Furthermore, the controllable screw conveyor mechanism is a metering screw, which is connected to the discharge port of the buffer bin;

[0020] The S300 also includes the following steps: the blades of the metering screw quantitatively push high-flowability fine powder, and the conveying speed of the metering screw is controlled in a closed loop according to the real-time weight feedback signal from the weight detection unit.

[0021] Furthermore, the secondary crushing structure consists of shearing and crushing teeth installed on the metering screw shaft, with multiple sets of shearing and crushing teeth distributed along the axial direction of the metering screw and rotating synchronously with the metering screw.

[0022] S300 also includes the following steps: shearing and grinding the residual trace amounts of agglomerated material after pretreatment on the high-flowability fine powder conveying path to make the powder output uniform and smooth.

[0023] Furthermore, a linkage control ball valve is installed at the discharge end of the metering screw;

[0024] S300 also includes the following steps: when the cumulative discharge reaches the preset addition weight, the metering screw is simultaneously shut down and the linkage control ball valve is closed to block the gravity flow of powder.

[0025] One or more technical solutions provided in this application have at least the following technical effects or advantages:

[0026] (1) This application achieves the synergistic effect of agglomeration crushing and dehumidification drying through an automatic pretreatment unit, and accurately controls the amount of feed by relying on weight closed-loop feedback. It has the advantages of high operational safety, accurate metering, high pretreatment efficiency and strong system reliability.

[0027] (2) The process of this application obtains fine and free-flowing powder through agglomeration pretreatment. After adding the polymerization inhibitor solution, it can ensure the stability of the polymerization inhibitor content in the system and is not easy to cause blockage in the feeding system.

[0028] (3) The process of this application adds the polymerization inhibitor to the polymerization inhibitor mixing tank through a metering screw, which can make the addition of the polymerization inhibitor more stable, and the metering screw has high precision in discharging the polymerization inhibitor, which can effectively prevent the misoperation of manual feeding.

[0029] (4) The process of this application can prevent the "dust" phenomenon during the addition of the polymerization inhibitor by designing a buffer chamber and a pretreatment chamber;

[0030] (5) In the process of this application, the pretreatment and the addition of the polymerization inhibitor can be mechanized and automated, which can effectively reduce labor costs. Attached Figure Description

[0031] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0032] Figure 1 A schematic diagram of an automatic dosing process for an agglomeration pretreatment inhibitor provided in this application;

[0033] Explanation of reference numerals in the attached figures:

[0034] 1-Tractor; 2-Pretreatment chamber; 3-Inert gas dehumidification and drying assembly; 4-Stirring and agitation assembly; 5-Buffer chamber; 6-Vibrating air hammer; 7-Controllable screw conveyor mechanism; 8-Weight detection unit; 9-Inhibitor mixing tank. Detailed Implementation

[0035] The technical solutions in the embodiments of this application are described clearly and completely below. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.

[0036] It should be noted that the terms "first," "second," etc., used in the specification and claims of this application are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of this application described herein can be implemented in orders other than those described herein. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion; for example, a process, method, system, product, or server that comprises a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or modules not explicitly listed or inherent to such processes, methods, products, or devices.

[0037] In traditional acrylic acid production, the addition of solid polymerization inhibitors relies on manual operation, which has several drawbacks. First, manual contact with the inhibitor powder easily generates dust, posing a threat to the health of operators. Second, manual metering has low accuracy, leading to large deviations in the amount of inhibitor added, affecting the inhibition effect or increasing costs. Third, solid polymerization inhibitors are prone to absorbing moisture and clumping, requiring time-consuming and labor-intensive manual crushing pretreatment. Furthermore, insufficiently crushed clumped material can easily clog pipelines during transportation, reducing production efficiency.

[0038] To address this issue, this application proposes an automatic dosing process for agglomeration inhibitors in pretreatment. By feeding the agglomeration inhibitor into a pretreatment unit, the process utilizes agitation combined with dehumidification and drying to simultaneously break up agglomerates and dehumidify the material, resulting in highly fluid fine powder. The powder is then temporarily stored in a buffer chamber equipped with a weight detection unit. A preset target dosing weight is established, and the weight detection unit collects material weight data in real time, forming a closed-loop feedback loop. This triggers a controllable screw conveyor mechanism to quantitatively deliver the powder. When the cumulative dosing reaches the preset target weight, the material conveying is automatically cut off. The pretreatment unit includes agitation components and an inert gas dehumidification and drying component; the controllable screw conveyor mechanism incorporates a secondary crushing structure to further shear and refine any remaining agglomerates during transport.

[0039] For ease of understanding, the following explains some key terms in this embodiment:

[0040] Agglomeration inhibitors refer to materials that, during storage or transportation, cause particles to agglomerate and form larger lumps due to factors such as moisture absorption and pressure.

[0041] A pretreatment unit refers to the equipment or area used for the preliminary treatment of agglomeration inhibitors. Its main function is to improve the physical state of the material so that it is suitable for subsequent automated conveying and dosing.

[0042] A stirring and agitation component refers to a device installed inside a pretreatment unit that applies force to materials through mechanical movement to achieve material agitation, dispersion, and physical crushing.

[0043] An inert gas dehumidification and drying assembly refers to a device used to provide dry inert gas to a pretreatment unit to reduce the moisture content of materials and maintain a low-humidity environment.

[0044] High-flowability fine powder refers to powdery materials that, after pretreatment, have small particle size, good dispersibility, are not prone to agglomeration, and can flow smoothly under gravity or mechanical action.

[0045] A weight detection unit refers to a sensor or weighing system used to monitor the weight of materials in a buffer bin in real time, and its output signal can be used to control the feeding process.

[0046] A buffer container is a container used for the temporary storage of pre-processed, highly fluid fine powders. Its design aims to ensure the continuity and stability of material supply.

[0047] A controllable screw conveyor is a conveying device that propels materials forward by rotating screw blades, and its conveying speed and flow rate can be adjusted according to control signals.

[0048] Secondary crushing structure refers to a device integrated inside a controllable screw conveyor mechanism, used to further shear and refine any trace residual lumps that may exist during material conveying.

[0049] This application provides an automated dosing process for an inhibitor in the pretreatment of agglomeration, the specific implementation of which is as follows:

[0050] First, the agglomeration inhibitor is fed into the pretreatment unit. This pretreatment unit is equipped with a stirring and agitation component and an inert gas dehumidification and drying component. The agglomeration inhibitor can be fed into the pretreatment unit via a simple conveying device (overhead crane). Inside the pretreatment unit, the stirring and agitation component can be a rotating shaft with simple blades, which agitates and initially breaks down the material through low-speed rotation. The dehumidification and drying component can be a simple heater, which, in conjunction with a fan, heats outside air and blows it into the pretreatment unit to remove moisture from the material. Through the synergistic effect of stirring and agitation combined with dehumidification and drying, the agglomeration inhibitor is simultaneously broken down and the material is dehumidified, resulting in a highly free-flowing fine powder.

[0051] Next, the aforementioned highly fluid fine powder is temporarily stored in a buffer hopper equipped with a weight detection unit. After pretreatment, the highly fluid fine powder can be conveyed to the buffer hopper via pneumatic conveying, mechanical conveying, or gravity flow. Weighing sensors can be installed at the bottom or on the supporting structure of the buffer hopper as weight detection units to monitor the total weight of the material inside. The buffer hopper can be designed as a simple conical hopper to promote gravity flow of the material.

[0052] Secondly, a target feeding weight is preset, and a weight detection unit collects real-time weight data from the buffer silo to form a closed-loop weight feedback, which in turn triggers a controllable screw conveyor to quantitatively deliver the powder. Before feeding, the operator can input the desired target feeding weight on the control system. The weight detection unit continuously sends real-time weight data from the buffer silo to the control system. Based on this data, the control system calculates the amount of material already added. The controllable screw conveyor can be a screw conveyor with a fixed rotation speed, and the feeding amount is approximated by controlling its running time. When the cumulative feeding amount reaches the preset target weight, the control system issues a command to automatically cut off the material conveying, completing the feeding process.

[0053] In addition, the controllable screw conveyor mechanism incorporates a secondary crushing structure to further shear and refine any residual clumps during transport. This secondary crushing structure can be simple fixed blades or screens that physically block and shear any small clumps that may be present as the material passes through, further ensuring smooth powder conveying.

[0054] The automated dosing process for pretreatment polymerization inhibitors in this application effectively solves the problems of high labor intensity and health hazards associated with traditional manual crushing by integrating stirring and dehumidification functions. Simultaneously, closed-loop feedback control using a weight detection unit achieves precise quantitative dosing of the polymerization inhibitor, avoiding ineffective inhibition or increased costs due to inaccurate measurement. The built-in secondary crushing structure further ensures smooth material transport, fundamentally eliminating the risk of pipeline blockage and significantly improving the automation, closed-loop system, and precision of the acrylic acid production additive dosing process.

[0055] In some of the solutions mentioned above in this application, an automatic dosing process for pretreatment of agglomeration inhibitors was proposed to achieve crushing, dehumidification and precise quantitative dosing of powder. However, in actual industrial production, the agglomeration mechanism, hygroscopic characteristics and physical forms of different chemical inhibitors are significantly different. If only a general pretreatment process is used, it is difficult to achieve the optimal crushing and dehumidification effect for specific chemical types, resulting in some special inhibitors still having agglomeration residues or incomplete dehumidification during the treatment process.

[0056] In this regard, this application further clarifies the scope of the agglomeration inhibitor, which includes at least one of aromatic phenolic inhibitors, organic sulfur-containing inhibitors, organometallic salt inhibitors, and alkyl ether inhibitors.

[0057] Specifically, agglomeration inhibitors are polymerization inhibitors that are prone to agglomeration and solidification into lumps during storage, transportation, or use. These inhibitors typically possess hygroscopic properties, are easily oxidized, or have specific crystal structures, causing them to lose fluidity under certain conditions, thus affecting subsequent dosing processes. The main function of these inhibitors is to suppress monomer self-polymerization during the polymerization reaction, ensuring product purity and stable operation of the equipment.

[0058] Aromatic phenolic polymerization inhibitors are a class of aromatic compounds containing phenolic hydroxyl groups in their molecular structure. They typically act as free radical scavengers, interrupting the growth of polymerization chains by reacting with free radicals, thereby inhibiting polymerization. Agglomeration of these inhibitors may be related to factors such as oxidation, polymerization, or hygroscopicity. Besides hydroquinone, catechol, resorcinol, and methylhydroquinone, they can also include, for example, tert-butylhydroquinone and 2,6-di-tert-butyl-4-methylphenol.

[0059] Organic sulfur-containing polymerization inhibitors are organic compounds containing sulfur atoms in their molecular structure. Their polymerization inhibition mechanism may involve free radical transfer, chain termination, or reaction with reactive intermediates. The agglomeration of these inhibitors is often closely related to their hygroscopicity or chemical stability. Besides phenothiazines, thiodipropionates, and alkyl thiols, they can also be, for example, dithiocarbamates and thiourea derivatives.

[0060] Organometallic salt polymerization inhibitors are a class of salt compounds formed by metal ions and organic ligands. They typically inhibit polymerization reactions by forming complexes with free radicals or active monomers. Agglomeration of these inhibitors may be related to factors such as crystal water, hygroscopicity, or the deliquescent nature of the salt. Besides copper acetate, copper salicylate, cuprous chloride, and copper naphthenate salts, they can also include, for example, copper stearate and copper acetylacetonate.

[0061] Alkyl ether polymerization inhibitors are compounds whose molecular structure contains alkyl ether bonds. Their polymerization inhibition may be achieved by altering monomer activity, affecting free radical lifetime, or acting as a solvent to dilute monomer concentration. Agglomeration of these inhibitors may be related to low-temperature curing, moisture absorption, or reactions with other components. Besides methyl ether, methyl tert-butyl ether, and dimethyl terephthalate, they can also be, for example, ethylene glycol dimethyl ether and diethylene glycol dimethyl ether.

[0062] By clearly defining the specific chemical categories of the agglomeration inhibitors, the pretreatment process of this application can optimize and adjust parameters according to the characteristics of different materials. For example, for aromatic phenolic inhibitors, they can be crushed under a closed inert atmosphere based on their easy oxidation, while adjusting the intensity of stirring to avoid excessive shearing leading to local overheating; for organic sulfur-containing inhibitors and organometallic salt inhibitors, since they usually have strong hygroscopicity, the dehumidification efficiency and flow rate of the inert gas dehumidification and drying components can be increased accordingly to ensure that the material remains in a dry environment during the crushing process and effectively prevent secondary moisture absorption and agglomeration; for alkyl ether inhibitors, the speed of the stirring screw and the blade design can be adjusted according to their physical form and viscosity characteristics to achieve optimal crushing and flowability. This targeted approach ensures that all types of agglomeration inhibitors can be efficiently crushed and thoroughly dehumidified in the pretreatment unit, ultimately yielding highly fluid fine powder. This addresses the root cause of problems such as poor pretreatment results, agglomeration residue, or incomplete dehumidification due to differences in material properties, significantly improving the versatility and reliability of the entire automatic dosing process.

[0063] In some of the embodiments described above in this application, an automatic dosing process for agglomeration inhibitors is proposed. However, in actual industrial applications, there are many types of agglomeration inhibitors with different chemical properties. Different types of agglomeration inhibitors have significant differences in moisture absorption and agglomeration characteristics, physical morphology, and chemical stability. If only a general processing technology is used, it is difficult to achieve precise crushing and dehumidification effects for agglomeration inhibitors with specific chemical components. This may result in agglomeration residues or changes in material properties when processing specific agglomeration inhibitors.

[0064] In this regard, this application further clarifies the specific types of the agglomeration inhibitors, wherein the aromatic phenolic inhibitors include at least one of hydroquinone, catechol, resorcinol, and methyl hydroquinone; the organic sulfur-containing inhibitors include at least one of phenoxythiazide, thiodipropionate, and alkyl thiols; the organometallic salt inhibitors include at least one of copper acetate, copper salicylate, cuprous chloride, and copper naphthenates; and the alkyl ether inhibitors include at least one of methyl ether, methyl tert-butyl ether, and dimethyl terephthalate.

[0065] Specifically, aromatic phenolic polymerization inhibitors are a class of organic compounds containing hydroxyl groups directly attached to the aromatic ring. They inhibit polymerization by capturing free radicals, but are generally susceptible to oxidation and moisture, leading to agglomeration. Besides hydroquinone, catechol, resorcinol, and methylhydroquinone, this category may also include tert-butylhydroquinone or 4-methoxyphenol. Organic sulfur-containing polymerization inhibitors are organic compounds containing sulfur atoms. They function through chain transfer or free radical capture mechanisms, and their thermal stability and reactivity may differ from phenolic polymerization inhibitors. Besides phenthiazides, thiodipropionates, and alkyl thiols, this category may also include dodecyl mercaptan or various thiosulfates. Organometallic salt polymerization inhibitors are compounds formed by metal ions and organic ligands. They are commonly used to inhibit polymerization and sometimes also act as oxygen scavengers or catalysts for inhibitor regeneration. These substances often have strong hygroscopic properties. Besides copper acetate, copper salicylate, cuprous chloride, and copper naphthenates, this category may also include copper acetylacetonate or copper stearate. Alkyl ether polymerization inhibitors are organic compounds containing ether bonds (RO-R'), where R and R' are alkyl groups. These inhibitors can act as depressants or synergists, and their physical properties (such as melting point and hygroscopicity) need to be considered during pretreatment. Besides dimethyl ether, methyl tert-butyl ether, and dimethyl terephthalate, this category may also include diethyl ether (which is a solid under certain conditions) or various polyether compounds.

[0066] Through the above technical solutions, this application clarifies the applicable material range of the process by refining the specific chemical composition of the polymerization inhibitors, thus providing a basis for targeted optimization of pretreatment parameters. By classifying polymerization inhibitors into aromatic phenols, organic sulfur-containing inhibitors, organometallic salts, and alkyl ethers, the process system can match the corresponding stirring intensity, dehumidification parameters, and crushing force according to the physicochemical properties of different types of materials. Specifically, the clarification of aromatic phenolic polymerization inhibitors helps to effectively protect them from oxidation and agglomeration during pretreatment using an inert gas atmosphere; the classification of organic sulfur-containing polymerization inhibitors considers their stability at specific temperatures, ensuring that they do not deteriorate due to local overheating during stirring and disturbance; the enumeration of organometallic salt polymerization inhibitors addresses their potential hygroscopicity, ensuring that the dehumidification and drying components maintain optimal drying efficiency through classified management; and the clarification of alkyl ether polymerization inhibitors further improves the applicability of the process. This precise definition of material properties allows for more targeted synergistic effects of subsequent mechanical crushing and dehumidification, effectively avoiding incomplete crushing or insufficient dehumidification caused by differences in material properties. It ensures that all types of polymerization inhibitors meet the standards for high-flowability fine powder before addition, thereby guaranteeing the stability and reliability of the automatic addition process from the source.

[0067] In some of the embodiments described above in this application, a pretreatment unit is proposed to break up and dehumidify the agglomeration inhibitor. However, in actual industrial applications, if the pretreatment unit is not designed properly, it can easily lead to secondary moisture absorption and agglomeration of the material during the processing. Furthermore, the dust generated during the processing of the powder will not only pollute the environment but also cause material loss and health risks to the operators, making it difficult to effectively guarantee the efficiency and safety of the pretreatment.

[0068] In response, this application proposes an automatic dosing process for the aforementioned pretreatment inhibitor for agglomeration, wherein the pretreatment unit includes a pretreatment chamber; a stirring and agitation component and an inert gas dehumidification and drying component are integrated and arranged inside the pretreatment chamber, and the two work together to simultaneously complete the mechanical crushing and inert atmosphere dehumidification and drying of the agglomeration inhibitor; the pretreatment chamber is a fully enclosed pressure-bearing structure to block dust from the powder, isolate external humid air, and prevent the inhibitor from absorbing moisture and agglomerating again.

[0069] Specifically, the pretreatment chamber is a sealed container used to hold the agglomeration inhibitor to be treated, providing physical space for the mechanical crushing and inert atmosphere dehumidification and drying of the inhibitor. The pretreatment chamber can be a cylindrical or square container with an anti-stick treatment on its internal surface to reduce material adhesion. Furthermore, the pretreatment chamber can be designed with a conical bottom to facilitate smooth material discharge and can be equipped with observation windows and access ports for easy operation and maintenance.

[0070] The integrated arrangement of the agitation and inert gas dehumidification drying components within the pretreatment chamber means that these components are tightly installed within the chamber's interior space, forming a compact processing system. This integration aims to ensure that materials come into immediate contact with the drying medium during crushing, avoiding the risks of material retention and secondary agglomeration associated with step-by-step processing. Specifically, the main structure of the agitation component (e.g., a shaft or propeller with agitator blades) can be mounted together with the inert gas dehumidification drying component (e.g., a gas distribution device, such as a perforated plate or nozzle array) on the central axis or side wall of the pretreatment chamber, resulting in a high degree of overlap between the agitation and gas distribution areas. Alternatively, the drive portion of the agitation component can be located outside the chamber, while its working parts extend into the chamber, with the inlet and gas distribution device of the inert gas dehumidification drying component directly fixed inside the chamber, ensuring uniform gas coverage of the agitation area.

[0071] The coordinated operation of these two components, simultaneously completing the mechanical crushing and inert atmosphere dehumidification and drying of the agglomeration inhibitor, means that the stirring and agitation components and the inert gas dehumidification and drying components start simultaneously and work in coordination under the control system. Simultaneous mechanical crushing and inert atmosphere dehumidification and drying means that while the agglomeration inhibitor is being mechanically crushed, the drying inert gas continuously acts on the material, removing moisture. For example, through the central control system, when the pretreatment unit starts, the motor driving the stirring and agitation components and the flow regulating valve of the inert gas dehumidification and drying components can simultaneously receive commands and begin operation, ensuring that the crushing and dehumidification processes are synchronized. Furthermore, sensors can be installed to monitor the humidity or material status in the pretreatment chamber in real time, and the rotation speed of the stirring and agitation components and the gas supply of the inert gas dehumidification and drying components can be dynamically adjusted based on feedback signals to optimize the crushing and dehumidification effects.

[0072] The pretreatment chamber is a fully enclosed pressure-bearing structure, meaning it is designed and manufactured to be completely sealed, effectively preventing the exchange of substances between the internal materials and the external environment, and capable of withstanding certain internal or external pressures. Specifically, the chamber body, inlet, outlet, and all connecting components are rigorously sealed using gaskets, flange connections, or welding to ensure no leakage, and are constructed with high-strength materials to withstand the pressure of the internal inert gas. Alternatively, the pretreatment chamber can be equipped with pressure sensors and safety valves to monitor and control the internal pressure, ensuring safety during closed-loop operation, while its structural design must comply with relevant pressure vessel standards.

[0073] The fully enclosed pressure-bearing structure is used to block dust from the powder and isolate it from external humid air, preventing the polymerization inhibitor from absorbing moisture and clumping again. This functional description emphasizes its role in environmental protection, material protection, and process stability. Blocking dust from the powder means preventing fine powder from escaping into the environment during processing; isolating it from external humid air means preventing high-humidity air from entering the chamber, thus avoiding the polymerization inhibitor from reabsorbing moisture and clumping. Through the airtight design, a relatively independent microenvironment is formed inside the chamber. Fine particles generated during the mixing and crushing process are confined within the chamber, preventing leakage and dust pollution; simultaneously, water vapor from the outside air cannot enter, ensuring a consistently dry environment inside the chamber. Furthermore, maintaining a slightly positive pressure inert gas environment inside the chamber enhances the isolation effect against external humid air, effectively preventing backflow of external air even when the inlet and outlet are briefly opened, thereby minimizing the risk of the polymerization inhibitor absorbing moisture and clumping again.

[0074] Through the aforementioned technical solution, the stirring and agitation components and the inert gas dehumidification and drying components are integrated and arranged inside the pretreatment chamber, enabling them to operate in tandem. This achieves simultaneous mechanical crushing of the agglomeration inhibitor and inert atmosphere dehumidification and drying. This integrated and synchronized processing method allows the material to be immediately exposed to a dry inert gas environment while being crushed, effectively avoiding the risks of material retention and secondary moisture absorption and agglomeration that may occur with traditional step-by-step processing, significantly improving pretreatment efficiency. Furthermore, the pretreatment chamber adopts a fully enclosed pressure-bearing structure, physically preventing dust leakage generated during the crushing process, greatly improving the operating environment, reducing occupational health risks for personnel, and minimizing material loss. Simultaneously, this enclosed structure effectively isolates external humid air from entering the chamber, eliminating the potential for the inhibitor to agglomerate due to re-absorbing moisture during processing. This ensures the quality stability of the highly fluid fine powder after pretreatment, providing a reliable material basis for subsequent precise quantitative dosing, thereby comprehensively improving the safety, efficiency, and material quality of the inhibitor dosing process.

[0075] In some of the embodiments described above in this application, a stirring and agitation component is proposed to break up agglomerated inhibitors. However, in actual operation, if only simple stirring is used, it is difficult to ensure that the agglomerated inhibitors achieve efficient breaking up and sufficient heat exchange in a dry inert gas atmosphere, resulting in incomplete material breaking up or uneven drying, which in turn affects the flowability and metering accuracy of subsequent feeding.

[0076] In this regard, this application further proposes that the stirring and disturbance component is a controllable screw stirring control system, which includes a drive motor, a transmission mechanism, and a stirring screw with stirring blades; S100 also includes the following steps: the stirring screw continuously shears, kneads and breaks up the agglomerating inhibitor by relying on the screw helical surface and stirring blades, while turning the agglomerating inhibitor to achieve full contact and heat exchange between the material and the dry inert gas.

[0077] Specifically, a controllable screw agitation control system is a mechanical device capable of precisely controlling the screw's rotation speed, direction of rotation, and agitation intensity. Its core lies in applying mechanical force to the material through the screw's rotational motion, achieving material crushing, mixing, and conveying. By introducing a "controllable" characteristic, this system allows for dynamic adjustments to the crushing and agitation process of agglomeration inhibitors based on material conditions and process requirements, thereby optimizing pretreatment results. For example, the system can employ a variable frequency motor drive, with the output frequency of the frequency converter adjusted via a PLC (Programmable Logic Controller) or DCS (Distributed Control System) to achieve stepless speed control of the screw. Alternatively, a servo motor drive can be used, coupled with a high-precision encoder for position and speed feedback, to achieve precise control of the screw agitation process, including forward and reverse rotation, intermittent operation, and switching between different speed ranges.

[0078] The drive motor in a screw agitation control system is the core component providing mechanical power, responsible for driving the entire system and converting electrical energy into mechanical energy to power the rotation of the agitating screw. For example, an AC asynchronous motor can be used, which is simple in structure, reliable in operation, and can be speed-regulated with a frequency converter; alternatively, a DC motor or servo motor can be used to provide a wider speed range and higher control precision. The transmission mechanism is responsible for transmitting the power from the drive motor to the agitating screw and typically acts as a speed reducer and torque amplifier to meet the torque requirements of the agitating screw when breaking up agglomerated materials. Common transmission mechanisms include gear reducers, which achieve speed reduction through gear meshing with different gear ratios; alternatively, chain drives or belt drives can be used, with a gearbox to achieve power transmission and torque amplification. The agitating screw with agitating blades is the actuator that directly contacts and breaks up and agitates the agglomerating inhibitor. Its helical surface is designed to push the material, while the additional agitating blades enhance the shearing and kneading action, improving crushing efficiency and material mixing uniformity. For example, the mixing screw can adopt a single screw structure, with its helical surface integrally formed or welded to the mixing blades. The blade shape can be designed as a paddle, scraper, or tooth to adapt to the crushing requirements of different materials. Alternatively, a twin screw structure can be adopted, with two screws meshing and rotating to provide stronger shearing force and mixing effect. The mixing blades can be designed to be staggered or arranged in the same direction.

[0079] In step S100, the agitating screw continuously shears, kneads, and breaks down the agglomerating inhibitor using its helical surface and agitating blades. Simultaneously, the agitation of the inhibitor ensures thorough contact and heat exchange between the material and the dry inert gas. This step effectively decomposes the agglomerating inhibitor into smaller particles through the pushing action of the screw's helical surface and the shearing and kneading action of the agitating blades, solving the material agglomeration problem. Furthermore, the screw's tumbling action continuously moves and renews the surface of the material within the pretreatment chamber, maximizing the contact area and time between the material and the dry inert gas, significantly improving the efficiency and uniformity of dehumidification and drying. For example, in actual operation, the intensity and duration of shearing and kneading can be adjusted by controlling the screw's rotation speed and running time to accommodate inhibitors with varying degrees of agglomeration. For severely agglomerated materials, a lower rotation speed can be used for initial crushing, gradually increasing the speed for finer processing. Additionally, optimizing the angle and number of agitating blades, as well as the screw pitch design, can enhance the material's agitation effect and contact efficiency with the dry inert gas. For example, using a variable pitch screw or setting different shaped stirring blades at different positions on the screw can achieve a more uniform material distribution and gas contact while crushing.

[0080] By introducing a controllable screw agitation control system, the above technical solution organically combines mechanical crushing with material tumbling, achieving efficient pretreatment of agglomeration inhibitors. The drive motor and transmission mechanism rotate a screw with agitation blades, applying continuous shearing and kneading forces to the agglomerated material using the screw's spiral surface and the blades. This effectively breaks down large pieces of inhibitor into fine powder, solving the conveying blockage problem caused by material agglomeration. Simultaneously, the tumbling action of the screw continuously changes the position of the agglomeration inhibitor within the pretreatment chamber, ensuring sufficient contact and heat exchange between the material and the introduced dry inert gas, significantly improving the efficiency and uniformity of dehumidification and drying. This method of coordinating mechanical crushing and material tumbling not only ensures the flowability of the powder but also lays a solid material foundation for subsequent precise quantitative dosing by optimizing the contact state between the material and the drying medium. The pretreatment unit is a fully enclosed pressure-bearing structure designed to block dust from the powder, isolate it from external humid air, and prevent the inhibitor from absorbing moisture and agglomerating. The controllable screw agitation control system efficiently completes crushing and drying in a closed environment, further ensuring the quality of the powder and the safety of the operators. It avoids the health risks and environmental pollution caused by manual contact with the powder, while also improving the level of automation and feeding accuracy.

[0081] In some of the embodiments described above in this application, a pretreatment unit is proposed to crush and dehumidify the agglomeration inhibitor to obtain a highly fluid powder. However, in the actual pretreatment process, if the environment inside the pretreatment chamber is not properly controlled, the material is very likely to reabsorb moisture from the air during the crushing process, resulting in repeated agglomeration and affecting the subsequent quantitative conveying accuracy and the stability of the device operation.

[0082] In response, this application further proposes an inert gas dehumidification and drying assembly, which includes an inert gas source, a drying and filtering unit, a flow regulating valve, and an in-chamber gas distribution pipeline; and in step S100, the dried and dehydrated inert gas is continuously introduced into the pretreatment chamber to form an inert atmosphere inside the chamber.

[0083] Specifically, the inert gas source provides a stable supply of inert gas, such as from high-pressure inert gas cylinders, vaporized liquid inert gas storage tanks, or inert gas prepared on-site by air separation equipment. The drying and filtration unit performs deep dehydration and impurity filtration on the inert gas to ensure that the gas entering the pretreatment chamber has extremely low water content and high purity. This unit can be implemented using various methods, such as adsorption dryers (e.g., molecular sieves, activated alumina), refrigerated dryers, or membrane separation technology. The flow control valve precisely controls the inert gas flow rate to maintain the required dry atmosphere and pressure inside the pretreatment chamber. This valve can be a manual regulating valve, an electrically or pneumatically controlled proportional regulating valve, or even a mass flow controller for finer flow control. The gas distribution pipeline within the chamber is responsible for evenly distributing the dried inert gas throughout the pretreatment chamber, ensuring that the material fully contacts the dried inert gas during crushing and tumbling. The gas distribution pipeline can be designed as a porous pipe, nozzle array, or diffuser to optimize gas distribution. By continuously introducing the dried and dehydrated inert gas into the pretreatment chamber, the humid air inside the chamber can be effectively replaced, and a continuous inert atmosphere can be formed inside the chamber. This fundamentally solves the technical problem of the polymerization inhibitor absorbing moisture and clumping due to contact with humid air during the crushing process.

[0084] Through the above technical solution, this application constructs a controlled inert atmosphere environment inside the pretreatment chamber by introducing an inert gas dehumidification and drying component. The inert gas source provides a stable gas supply, and after deep dehydration treatment by the drying and filtration unit, ensures that the gas entering the chamber has extremely low moisture content, providing a dry physical environment for the agglomeration inhibitor. The flow regulating valve allows operators to precisely control the inert gas flow rate according to the actual processing requirements of the material, maintaining the optimal dry atmosphere inside the chamber. The design of the gas distribution pipeline within the chamber ensures that the dried inert gas is evenly distributed inside the pretreatment chamber, allowing the material to fully contact and exchange heat with the dry inert gas during the continuous shearing, kneading, crushing, and tumbling process of the stirring and agitation components, achieving simultaneous dehumidification. By continuously introducing dry inert gas, not only can the humid air inside the chamber be effectively replaced, but a continuous inert atmosphere can also be formed inside the chamber, effectively isolating the material from the influence of the external environment, thereby preventing the agglomeration inhibitor from re-agglomerating due to secondary moisture absorption during the crushing process. This ensures that the pre-treated high-flowability fine powder can maintain its dry state, laying a solid foundation for subsequent precise quantitative addition and significantly improving the stability and reliability of the entire addition process.

[0085] In some of the embodiments described above in this application, it is proposed to break up and dehumidify the agglomerated polymerization inhibitor through a pretreatment unit and temporarily store it in a buffer bin to achieve quantitative addition. However, in actual operation, due to the hygroscopic properties of the polymerization inhibitor powder, even after pretreatment, it is still easy to cause secondary adhesion or bridging phenomena when it is piled up in the buffer bin for a long time or affected by the environment, resulting in a decrease in material flowability and thus affecting the stability and continuity of subsequent metering and conveying.

[0086] In response, this application further proposes to install a vibrating air hammer inside the buffer chamber, with the vibrating air hammer installed on the inner wall of the buffer chamber; and to control the vibrating air hammer to vibrate intermittently or continuously to break up the highly fluid fine powder that accumulates and sticks to the walls of the buffer chamber.

[0087] Specifically, a vibratory hammer is a device that uses mechanical vibration energy to improve the flowability of powder materials. It can be a pneumatic vibrator, which uses compressed air to drive an internal piston or ball bearing to generate high-frequency vibration, offering advantages such as simple structure and good explosion-proof performance; or an electric vibrator, which uses a motor to drive an eccentric block to generate rotational vibration, featuring adjustable vibration intensity and high control precision. Both vibrators can transmit vibration energy to the silo wall, thereby acting on the material. The vibratory hammer is installed on the inner wall of the buffer silo to ensure that vibration energy acts efficiently and directly on the material on the inner wall of the silo, and is transmitted through the silo wall to the material accumulated inside, effectively disrupting material adhesion and bridging structures. One installation method involves welding or bolting the base of the vibratory hammer directly to the outer wall of the buffer silo, allowing vibration to be transmitted through the silo wall; another method uses flexible connectors, such as elastic gaskets or shock-absorbing brackets, to install the vibratory hammer on the outside of the buffer silo, optimizing vibration transmission efficiency and reducing stress concentration on the silo structure. The vibratory hammer is located at the bottom of the buffer silo and has no tilt angle. To flexibly adjust the vibration mode according to the actual flow state of the material and the feeding requirements, thereby achieving optimal dispersing effect and energy consumption balance, this application controls the vibrating hammer to vibrate intermittently or continuously. This can be controlled by a programmable logic controller (PLC) integrated into the automatic control system, which automatically switches the working mode of the vibrating hammer according to a preset program, time interval, or feedback signals from material level sensors, pressure sensors, etc.; alternatively, it can be manually set and adjusted by the operator on the control interface. Through the above vibration control, highly fluid fine powders that have accumulated and adhered to the walls of the buffer silo can be dispersed. The mechanical vibration generated by the vibrating hammer causes relative movement between the silo wall and the material, thereby breaking the binding force between material particles and eliminating bridging; at the same time, the vibration can also cause material particles adhering to the silo wall to fall off, preventing adhesion and ensuring that the material can be smoothly discharged from the outlet of the buffer silo and enter the subsequent conveying mechanism.

[0088] By adding a vibrating hammer to the buffer silo and installing it on the silo wall, the above technical solution effectively solves the problem of secondary adhesion and bridging of pre-treated high-flowability fine powders caused by prolonged accumulation or environmental influences within the buffer silo. By controlling the vibrating hammer to vibrate intermittently or continuously, the resulting mechanical disturbances continuously disrupt the bridging structure of the material and peel off the powder adhering to the silo wall, thus ensuring the material maintains good flowability. This not only ensures smooth and continuous discharge of material from the buffer silo, avoiding interruptions in feeding due to material blockage, but also, in conjunction with the closed-loop feedback of the weight detection unit and the quantitative conveying function of the controllable screw conveyor, further improves the accuracy and stability of the feeding metering. This significantly enhances the reliability of the entire automatic polymerization inhibitor dosing process, effectively avoiding manual intervention and reducing production risks and operating costs.

[0089] Furthermore, this application employs an integrated anti-clogging material design that combines pre-treatment crushing and drying in the pre-treatment chamber with a vibrating air hammer on the outer wall of the chamber. This significantly simplifies the fluidization structure at the bottom of the buffer chamber and may even eliminate the need for a fluidizer. After the material is agitated by a screw in the pretreatment chamber and simultaneously dehumidified and crushed by inert nitrogen, the resulting fine powder of the polymerization inhibitor has high dryness, uniform particle dispersion, sufficient particle gaps, and significantly improved overall flowability. The periodic wall vibration of the vibrating air hammer alone can eliminate the problems of powder sticking to the walls and bridging in the chamber. There is no need to add an additional fluidizer to supply fluidizing gas for auxiliary feeding, simplifying the entire equipment piping configuration, reducing hardware investment and nitrogen consumption, and reducing the risk of powder leakage and moisture backflow in the pipeline.

[0090] In some of the solutions mentioned above in this application, a feeding method is proposed that temporarily stores powder in a buffer bin and uses a weight detection unit for closed-loop feedback. However, in the actual powder conveying process, if there is a lack of a targeted quantitative conveying mechanism and a precise feedback adjustment mechanism, it is easy to cause problems such as flow fluctuation, inaccurate metering or unstable conveying during the feeding process, which in turn affects the accuracy and continuity of the polymerization inhibitor addition.

[0091] In this regard, this application further proposes that the controllable screw conveyor mechanism is a metering screw, which is connected to the discharge port of the buffer bin; S300 also includes the following steps: the blades of the metering screw quantitatively push high-flowability fine powder, and the conveying speed of the metering screw is controlled in a closed loop according to the real-time weight feedback signal of the weight detection unit.

[0092] The controllable screw conveyor mechanism specifically refers to a metering screw. A metering screw is a device that uses screw rotation to push material from the inlet to the outlet and precisely controls the conveying volume. A metering screw typically consists of a screw body, a drive motor, and a reducer. Its key feature is the precise control over the screw's geometry (such as pitch and thread depth) and rotational speed, thereby achieving accurate metering of the powder conveyed. Besides the common single-screw structure, a twin-screw structure can also be used to improve conveying stability or handle specific materials.

[0093] The connection between the metering screw and the outlet of the buffer hopper is designed to ensure a smooth and continuous flow of material from the buffer hopper into the metering screw, preventing material accumulation, bridging, or leakage at the connection point, and ensuring the stability and airtightness of the conveying process. The connection can be achieved through flange connections, flexible connectors, or by designing the metering screw's inlet as part of the buffer hopper's outlet. For example, a tapered transition section can be used to tightly connect the buffer hopper's outlet to the metering screw's inlet, or a seamless connection can be achieved using sealing gaskets and fasteners.

[0094] The blades of the metering screw quantitatively deliver highly flowable fine powders. Through their rotational motion, the blades exert a forced pushing effect on the powder, ensuring it is conveyed at a stable volumetric flow rate. This overcomes the instability that may arise from the powder's inherent flowability, achieving precise metering. The blades of the metering screw can be continuous helical blades or segmented blades, and their shape, pitch, and blade thickness are optimized according to the characteristics of the powder being conveyed (such as density, particle size, and flowability). For example, for highly flowable powders, blades with a smaller pitch can be used to improve metering accuracy; for easily adhering powders, the blade surface can undergo special treatment.

[0095] The conveying speed of the metering screw is controlled in a closed loop based on the real-time weight feedback signal from the weight detection unit. This closed-loop control system typically includes a weight sensor (such as a weighing module), a controller (such as a PLC or DCS), a frequency converter, and a drive motor. The weight sensor transmits the real-time weight signal to the controller, which calculates the required screw speed according to a preset algorithm (such as PID control) and adjusts the speed of the drive motor through the frequency converter, thereby changing the conveying rate of the metering screw.

[0096] Through the above technical solution, the controllable screw conveyor mechanism is specifically implemented as a metering screw, which is tightly connected to the outlet of the buffer bin, ensuring the continuity and stability of high-flowability fine powder from the buffer bin to the conveying stage. The blades of the metering screw forcefully and quantitatively push the powder, effectively overcoming the problem of uneven flow caused by gravity or flowability differences in the powder during the conveying process. Furthermore, by linking the conveying speed of the metering screw with the real-time weight feedback signal of the weight detection unit in a closed loop, the system can dynamically and in real time adjust the screw speed according to the achievement of the target feeding weight, thereby achieving precise correction and control of the flow rate during the feeding process. This closed-loop control mechanism not only ensures the accuracy of the feeding amount, but also further improves the stability of powder conveying through the mechanical forced conveying characteristics of the screw, effectively solving the problem of fluctuation in the polymerization inhibitor effect caused by metering deviation and unstable conveying in traditional feeding methods, and significantly improving the accuracy and continuity of polymerization inhibitor addition.

[0097] In some of the embodiments described above in this application, a controllable screw conveyor mechanism is proposed for quantitative conveying of powder. However, in the actual conveying process, even after crushing and dehumidification by the pretreatment unit, the powder may still generate a small amount of secondary agglomeration in the conveying path due to environmental fluctuations or material characteristics, resulting in increased conveying resistance, uneven discharge, or even blockage of the pipeline, affecting the overall accuracy and continuity of feeding.

[0098] In response, this application further proposes that, in order to effectively solve the above problems, the secondary crushing structure is a shearing crushing tooth set on the metering screw body, and multiple sets of shearing crushing teeth are distributed along the axial direction of the metering screw and rotate synchronously with the metering screw; S300 also includes the following steps: shearing and grinding the residual micro-agglomerated material after pretreatment on the high-flowability fine powder conveying path, so that the powder is discharged uniformly and smoothly.

[0099] Specifically, shearing and crushing teeth are mechanical structures used to shear and grind materials. They can be designed as blade-like structures with sharp edges, toothed structures with serrated edges, or protrusions with specific geometries to apply shearing and grinding forces as the material passes through. Their function is to further refine any small agglomerates that may form during conveying, ensuring the uniformity and flowability of the powder. Multiple sets of shearing and crushing teeth are distributed along the axial direction of the metering screw, meaning these teeth are not concentrated at a single point but arranged along the length of the metering screw. This distribution ensures that the material is continuously subjected to shearing and grinding throughout its journey from the feed end to the discharge end of the metering screw. For example, they can be arranged in an evenly spaced spiral pattern or with locally denser arrangements based on areas prone to agglomeration. This design aims to provide continuous crushing effects and prevent the material from forming larger agglomerates again during conveying. The shearing and crushing teeth rotate synchronously with the metering screw, indicating that these teeth are an integral part of the metering screw or rigidly connected to it and rotate together with the metering screw. This synchronous rotation mechanism enables the crushing teeth to actively shear and grind the material while it is being conveyed, utilizing the driving force of the metering screw. For example, the shearing crushing teeth can be directly cast or welded to the rod of the metering screw, or fixed to the screw via key connections, ensuring that they maintain the same rotational speed and trajectory as the screw. Shearing and grinding the residual trace agglomerates in the high-flowability fine powder conveying path refers to the physical treatment of small agglomerates that were not completely eliminated during pretreatment or that reformed during conveying, using the shearing crushing teeth during the powder conveying process of the metering screw. The shearing action separates the agglomerates through the cutting force of the blades or teeth, while the grinding action further refines the agglomerates through friction and compression. This process aims to further homogenize the particle size of the material and eliminate potential clogging risks. Ensuring uniform and smooth powder output means that, through the aforementioned shearing and grinding refining actions, the powder output from the metering screw maintains a high degree of consistency and stability in particle size, density, and flow rate, avoiding problems such as intermittent clogging, flow fluctuations, or material bridging. This is crucial for accurate subsequent feeding, ensuring the continuity and accuracy of the feeding process.

[0100] Through the above technical solution, the secondary crushing structure, namely the shearing crushing teeth, is directly set on the rod of the metering screw, and is distributed axially and rotates synchronously with the metering screw, thereby constructing a dynamic secondary crushing mechanism during the powder conveying process. This mechanism can continuously shear and grind the residual trace agglomerated materials after pretreatment or the agglomerated materials that reform during conveying. This effectively solves the problems of increased conveying resistance, uneven discharge, and even pipeline blockage caused by trace secondary agglomeration of powder in the conveying path. In view of this, this application ensures the uniformity and smoothness of highly fluid fine powder throughout the conveying process, significantly improves the operational reliability and feeding accuracy of the controllable screw conveyor mechanism, and thus ensures the stability and accuracy of the quantitative powder conveying based on weight closed-loop feedback in step S300, avoiding the impact of poor material conveying on the continuity and accuracy of overall feeding.

[0101] In some of the solutions described above in this application, a metering screw is proposed for quantitative conveying of powder. However, when the metering screw stops conveying, due to the fluidity of the powder, the powder remaining in the conveying pipeline is prone to flow under gravity, resulting in the actual amount added exceeding the preset target weight and causing deviation in the feeding accuracy.

[0102] In response, this application further proposes that a linkage-controlled ball valve be installed at the discharge end of the metering screw. A linkage-controlled ball valve is a valve that controls the flow of fluid by rotating a ball, characterized by its operation being synchronized with the action of another mechanism (in this case, the metering screw). This linkage-controlled ball valve can be implemented in various ways. For example, it can be configured with an electric actuator, receiving start / stop signals from the metering screw through a control system to synchronously drive the valve to open or close; alternatively, it can be configured with a pneumatic actuator, controlling the air source through a solenoid valve to achieve linkage operation with the metering screw; or, it can be directly coupled to the opening and closing action of the ball valve with the stopping action of the metering screw through a mechanical linkage or gear mechanism. Its main function is to provide a physical barrier when the metering screw stops conveying, completely cutting off the flow path of the powder.

[0103] In practical implementation, when the cumulative discharge reaches the preset addition weight, the metering screw is simultaneously shut down and the interlocking control ball valve is closed to prevent the powder from flowing out by gravity. "Simultaneously shutting down the metering screw and closing the interlocking control ball valve" means that when the target addition weight is reached, the stopping of the metering screw and the closing of the ball valve occur almost simultaneously, minimizing any additional powder outflow due to inertia or gravity. This synchronous control can be achieved in various ways. For example, a programmable logic controller (PLC) can be used to receive real-time feedback signals from the weight detection unit. When the cumulative addition reaches the preset value, the PLC simultaneously sends stop / close commands to the driver of the metering screw and the actuator of the interlocking control ball valve. Alternatively, a distributed control system (DCS) can be used for integrated control to achieve a higher level of synchronization and coordination. For simpler systems, even relay logic circuits can be used to achieve synchronous control of the metering screw and the ball valve. This synchronous operation can effectively block the free flow of powder, that is, prevent the powder from continuing to flow out of the outlet after the metering screw stops due to its own fluidity, gravity or residual pressure in the pipeline, thus preventing the dosage from exceeding the standard.

[0104] Through the above technical solution, as the metering screw completes its quantitative conveying task and shuts down, the linkage control ball valve simultaneously closes, completely cutting off the flow path of the powder by utilizing the sealing effect of the physical valve. This dual blocking mechanism effectively prevents overfeeding caused by powder gravity flow, ensuring the accuracy of the feeding process and strictly controlling the feeding amount within the preset target range. It avoids metering errors caused by residual material gravity flow, thereby significantly improving the control accuracy and stability of the overall feeding process.

[0105] The hydrogen storage material of this application is described below with specific experiments and experimental data:

[0106] Example 1:

[0107] In an acrylic acid production plant A, hydroquinone-based solid polymerization inhibitors need to be added to the acrylic acid monomers to inhibit monomer self-polymerization. Traditional manual addition methods present problems such as operator health risks, inaccurate metering, time-consuming clumping treatment, and material conveyor blockages. To address these issues, plant A introduced an automated dosing process for the pre-treatment polymerization inhibitor to prevent clumping.

[0108] The process begins by feeding the bagged hydroquinone polymerization inhibitor into a fully enclosed, pressure-bearing pretreatment chamber. This chamber integrates a stirring and agitation component and an inert gas dehumidification and drying component. The stirring and agitation component is a controllable screw agitation control system, comprising a drive motor, transmission mechanism, and a stirring screw with agitator blades. The inert gas dehumidification and drying component consists of an inert gas source, a drying and filtration unit, a flow control valve, and internal gas distribution piping.

[0109] In step S100 of the process, after the agglomerating inhibitor enters the pretreatment chamber, the drive motor rotates the stirring screw. The stirring screw, relying on its helical surface and stirring blades, continuously shears, kneads, and breaks down the agglomerating inhibitor from large crystals into fine powder. Simultaneously, the tumbling action of the stirring screw ensures the material moves freely within the chamber, allowing for thorough contact and heat exchange with the drying inert gas. The inert gas dehumidification and drying assembly continuously introduces dehydrated inert gas (e.g., nitrogen) processed by the drying and filtration unit into the pretreatment chamber through a flow regulating valve, creating an inert atmosphere within the chamber. This inert atmosphere not only effectively isolates the material from external humid air, preventing secondary moisture absorption and agglomeration of the inhibitor, but also works in conjunction with the stirring and agitation assembly to dehumidify and dry the material. Through the synergistic effect of stirring and agitation and dehumidification, the agglomerating inhibitor is simultaneously broken up and the material is dehumidified, ultimately yielding highly fluid fine powder. Compared to the traditional method of manually breaking up lumpy materials, this step automates the pretreatment of lumps, significantly reducing labor costs and the workload of operators. Furthermore, the pretreatment time for the S100 is controlled within 25 minutes.

[0110] Subsequently, in step S200, these highly fluid fine powders are transported through a closed conveying pipeline to a buffer chamber equipped with a weight detection unit for temporary storage. A vibrating air hammer is installed on the inner wall of the buffer chamber.

[0111] In step S300, the operator pre-sets a target feed weight of 30 kg in the control system. The weight detection unit collects the weight of the material in the buffer silo in real time and feeds the weight signal back to the control system, forming a closed-loop weight feedback. When the weight of the material in the buffer silo changes, the control system, based on the preset target feed weight and the real-time weight feedback signal, activates the controllable screw conveyor mechanism for quantitative conveying. This controllable screw conveyor mechanism is a metering screw, whose outlet is connected to the outlet of the buffer silo. The blades of the metering screw quantitatively push the highly fluid fine powder, and its conveying speed is controlled in a closed loop according to the real-time weight feedback signal from the weight detection unit to ensure the accuracy of the feed. The metering screw is connected to the polymerization inhibitor mixing tank. Compared with the traditional method of estimating the dosage based on manual experience, this closed-loop weight feedback control system achieves precise quantitative addition of the polymerization inhibitor, avoiding the problems of under- or over-dosing.

[0112] Furthermore, the metering screw incorporates a secondary crushing structure, meaning that multiple sets of shearing and crushing teeth are installed on the screw shaft. These teeth are distributed along the axial direction of the metering screw and rotate synchronously with it. During powder conveying, these shearing and crushing teeth further shear and grind any trace amounts of agglomerated material that may remain after pretreatment, ensuring uniform and smooth powder discharge. This effectively avoids bridging and blockage problems that may occur if insufficiently crushed agglomerated material enters subsequent pipelines or mixing tanks, thus improving the continuous operation efficiency of the unit.

[0113] To prevent powder from accumulating or sticking to the walls of the buffer silo, the control system controls the vibrating hammer installed on the inner wall of the buffer silo to vibrate intermittently or continuously, breaking up the accumulated or sticking high-flow-rate fine powder and ensuring smooth powder feeding.

[0114] When the cumulative dosage reaches the preset target weight (30 kg), the control system will automatically cut off the material conveying, completing the feeding process. Specifically, the discharge end of the metering screw is equipped with a linkage control ball valve. When the cumulative discharge reaches the preset dosage weight, the control system will simultaneously shut down the metering screw and close the linkage control ball valve to prevent the powder from flowing by gravity, further ensuring the accuracy of feeding and the safety of the system.

[0115] Through the above process, Factory A has achieved unmanned powder addition of the polymerization inhibitor, automatic completion of agglomeration pretreatment and precise quantitative addition, effectively solving technical problems such as high personnel health and safety risks, poor material metering accuracy, high labor costs for agglomeration pretreatment and easy blockage of material conveying, and improving the automation level and safety of the production process.

[0116] Example 2:

[0117] The experimental steps were the same as in Example 1, but the S100 pretreatment time was controlled to be 20 min.

[0118] Example 3:

[0119] The experimental steps were the same as in Example 1, but the S100 pretreatment time was controlled to be 15 min.

[0120] Example 4:

[0121] The experimental steps were the same as in Example 1, but the S100 pretreatment time was controlled to be 10 min.

[0122] Example 5:

[0123] The experimental steps were the same as in Example 1, but the S100 pretreatment time was controlled to be 5 minutes.

[0124] Example 6:

[0125] The experimental procedure was the same as in Example 1, except that the agglomerated copper acetate polymerization inhibitor was sent into the pretreatment chamber.

[0126] Example 7:

[0127] The experimental procedure was the same as in Example 2, except that the agglomerated copper acetate polymerization inhibitor was sent into the pretreatment chamber.

[0128] Example 8:

[0129] The experimental procedure was the same as in Example 3, except that the agglomerated copper acetate polymerization inhibitor was sent into the pretreatment chamber.

[0130] Example 9:

[0131] The experimental procedure was the same as in Example 4, except that the agglomerated copper acetate polymerization inhibitor was sent into the pretreatment chamber.

[0132] Example 10:

[0133] The experimental procedure was the same as in Example 5, except that the agglomerated copper acetate polymerization inhibitor was sent into the pretreatment chamber.

[0134] Example 11:

[0135] The experimental procedure was the same as in Example 1, except that the agglomerated phenthiazide polymerization inhibitor was sent into the pretreatment chamber.

[0136] Example 12:

[0137] The experimental procedure was the same as in Example 2, except that the agglomerated phenthiazide polymerization inhibitor was sent into the pretreatment chamber.

[0138] Example 13:

[0139] The experimental procedure was the same as in Example 3, except that the agglomerated phenthiazide polymerization inhibitor was sent into the pretreatment chamber.

[0140] Example 14:

[0141] The experimental procedure was the same as in Example 4, except that the agglomerated phenthiazide polymerization inhibitor was sent into the pretreatment chamber.

[0142] Example 15:

[0143] The experimental procedure was the same as in Example 5, except that the agglomerated phenthiazide polymerization inhibitor was sent into the pretreatment chamber.

[0144] Example 16:

[0145] The experimental procedure was the same as in Example 1, except that the agglomerated copper salt polymerization inhibitor was sent into the pretreatment chamber.

[0146] Example 17:

[0147] The experimental procedure was the same as in Example 2, except that the agglomerated copper salt polymerization inhibitor was sent into the pretreatment chamber.

[0148] Example 18:

[0149] The experimental procedure was the same as in Example 3, except that the agglomerated copper salt polymerization inhibitor was sent into the pretreatment chamber.

[0150] Example 19:

[0151] The experimental procedure was the same as in Example 4, except that the agglomerated copper salt polymerization inhibitor was sent into the pretreatment chamber.

[0152] Example 20:

[0153] The experimental procedure was the same as in Example 5, except that the agglomerated copper salt polymerization inhibitor was sent into the pretreatment chamber.

[0154] Example 21:

[0155] The experimental procedure was the same as in Example 1, except that the agglomerated methyl ether polymerization inhibitor was sent into the pretreatment chamber.

[0156] Example 22:

[0157] The experimental procedure was the same as in Example 2, except that the agglomerated methyl ether polymerization inhibitor was sent into the pretreatment chamber.

[0158] Example 23:

[0159] The experimental procedure was the same as in Example 3, except that the agglomerated methyl ether polymerization inhibitor was sent into the pretreatment chamber.

[0160] Example 24:

[0161] The experimental procedure was the same as in Example 4, except that the agglomerated methyl ether polymerization inhibitor was sent into the pretreatment chamber.

[0162] Example 25:

[0163] The experimental procedure was the same as in Example 5, except that the agglomerated methyl ether polymerization inhibitor was sent into the pretreatment chamber.

[0164] Comparative Example 1:

[0165] The experimental steps are the same as in Example 1, but the S100 pretreatment time is controlled to be 0 min.

[0166] Comparative Example 2:

[0167] The experimental procedure was the same as that of Comparative Example 1, but the agglomerated copper acetate polymerization inhibitor was sent into the pretreatment chamber.

[0168] Comparative Example 3:

[0169] The experimental procedure was the same as that of Comparative Example 1, but the agglomerated phenthiazide polymerization inhibitor was sent into the pretreatment chamber.

[0170] Comparative Example 4:

[0171] The experimental procedure was the same as that of Comparative Example 1, but the agglomerated copper salt polymerization inhibitor was sent into the pretreatment chamber.

[0172] Comparative Example 5:

[0173] The experimental procedure was the same as that of Comparative Example 1, but the agglomerated methyl ether polymerization inhibitor was sent into the pretreatment chamber.

[0174] The agglomeration state of the powder and the actual weight of the output inhibitor were observed in Examples 1-25 and Comparative Examples 1-5, and the results are shown in Table 1.

[0175] Table 1

[0176]

[0177] The data above shows that, under no pretreatment conditions (Comparative Examples 1-5), all types of polymerization inhibitors exhibit significant agglomeration. The raw agglomerated materials, without crushing and dehumidification drying, show severe particle aggregation and extremely poor flowability, making them highly susceptible to bridging and blockage in buffer bins and metering screws, thus hindering continuous automated conveying. Under 5-minute pretreatment conditions (Examples 5, 10, 15, 20, 25), only a few low-agglomeration-prone polymerization inhibitors (copper salts, methyl ether) retain only minor agglomerates; hydroquinone and copper acetate still exhibit large agglomerates, while phenthiazide exhibits smaller agglomerates. Insufficient crushing and drying results in inadequate powder flowability and a continued risk of blockage. Under 10-minute pretreatment conditions (Examples 4, 9, 14, 19, 24), methyl ether and copper salts achieve complete agglomeration-free operation; hydroquinone and copper acetate still retain varying degrees of agglomeration, while phenthiazide retains only trace amounts of minor agglomerates. For hygroscopic phenolic and copper salt raw materials, the 10-minute pretreatment time is insufficient for crushing. Under a 15-minute pretreatment condition (Examples 3, 8, 13, 18, 23), hydroquinone, phenothiazine, copper salts, and methyl ether all four polymerization inhibitors completely eliminated agglomeration, resulting in uniform fine powder. Only copper acetate still exhibited small agglomerates, and the crushing and drying effect basically met the requirements for continuous conveying. Under a 20-minute pretreatment condition (Examples 2, 7, 12, 17, 22), hydroquinone, phenothiazine, copper salts, and methyl ether showed no agglomeration. Copper acetate only retained trace amounts of tiny agglomerates, and the flowability of all materials was significantly improved. The material could be smoothly fed using the vibrating hammer in the buffer silo without the need for an additional fluidizer. Under a 25-minute pretreatment condition (Examples 1, 6, 11, 16, and 21), all five polymerization inhibitors used in the experiment achieved complete crushing and drying. The discharged powder was free of any agglomeration, with uniform particle dispersion, sufficient gaps, and excellent flowability. This eliminated the problems of buffer bridging and metering screw blockage at the source, making it suitable for long-term continuous and stable automated feeding conditions. This is the optimal general pretreatment time for this process at a target dosage of 30 kg. In summary, as the pretreatment time increases, the degree of agglomeration dissolution of various polymerization inhibitors gradually improves. Different types of polymerization inhibitors have different moisture absorption and agglomeration characteristics, requiring different pretreatment times to meet the standards. The longest pretreatment time required is only 25 minutes to cover all tested polymerization inhibitors, achieving the preparation of agglomerate-free fine powder, replacing the traditional manual crushing process.

[0178] The data above also shows that the actual output weight range for all groups was 29.8 kg to 30.5 kg, with an overall measurement deviation of less than 1%. Even in the comparative example with no pretreatment and severe material agglomeration, the quantitative feeding structure of this application, featuring "closed-loop feedback of the weighing sensor, a metering screw with shearing and crushing teeth, and an end-linked ball valve," still maintained high measurement accuracy. In the example with sufficient pretreatment (15 min to 25 min), the actual feeding weight stably fell within the range of 29.9 to 30.2 kg, with even smaller measurement fluctuations and optimal feeding accuracy. This demonstrates that the weight closed-loop automatic control metering system of this application is not affected by the slight degree of material agglomeration and can stably achieve accurate quantitative feeding, completely solving the defects of traditional manual feeding that relies on experience estimation and has large deviations in feeding amount.

[0179] It should be noted that the order of the embodiments described above is merely for descriptive purposes and does not represent the superiority or inferiority of the embodiments. Furthermore, specific embodiments have been described above. Other embodiments are within the scope of the appended claims. In some cases, the actions or steps described in the claims can be performed in a different order than those in the embodiments and still achieve the desired results. Additionally, in some implementations, multitasking and parallel processing are possible or may be advantageous.

[0180] The above description is only a preferred embodiment of this application and is not intended to limit this application. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.

[0181] This specification is merely an illustrative description of this application and is intended to cover any and all modifications, variations, combinations, or equivalents within the scope of this application. Clearly, those skilled in the art can make various alterations and modifications to this application without departing from its scope. Therefore, if such modifications and modifications fall within the scope of this application and its equivalents, this application intends to include such modifications and modifications.

Claims

1. An automatic dosing process for an inhibitor to pretreat agglomeration, characterized in that, include: S100: The agglomeration inhibitor is fed into the pretreatment unit. Through the combined action of stirring and dehumidification, the agglomeration inhibitor is simultaneously crushed and the material is dehumidified to obtain a highly fluid fine powder. S200: The highly fluid fine powder is temporarily stored in a buffer chamber equipped with a weight detection unit; S300: The target feeding weight is preset, and the weight detection unit collects the weight of the material in the buffer bin in real time to form a weight closed-loop feedback, which is linked to the controllable screw conveyor to quantitatively transport the powder; when the cumulative feeding amount reaches the preset target weight, the material conveying is automatically cut off to complete the feeding. The pretreatment unit is equipped with a stirring and agitation component and an inert gas dehumidification and drying component; the controllable screw conveyor mechanism has a built-in secondary crushing structure for further shearing and refining residual clumps during the conveying process.

2. The automatic dosing process for the pretreatment inhibitor of agglomeration as described in claim 1, characterized in that, The agglomeration inhibitor includes at least one of the following: aromatic phenolic polymerization inhibitors, organic sulfur-containing polymerization inhibitors, organometallic salt polymerization inhibitors, and alkyl ether polymerization inhibitors.

3. The automatic dosing process for the agglomeration pretreatment inhibitor as described in claim 2, characterized in that, The aromatic phenolic polymerization inhibitors include at least one of hydroquinone, catechol, resorcinol, and methyl hydroquinone; the organic sulfur-containing polymerization inhibitors include at least one of phenoxythiazide, thiodipropionate, and alkyl thiols; the organometallic salt polymerization inhibitors include at least one of copper acetate, copper salicylate, cuprous chloride, and copper naphthenates; and the alkyl ether polymerization inhibitors include at least one of methyl ether, methyl tert-butyl ether, and dimethyl terephthalate.

4. The automatic dosing process for the pretreatment inhibitor of agglomeration as described in any one of claims 1-3, characterized in that, The pretreatment unit includes a pretreatment chamber; the stirring and agitation component and the inert gas dehumidification and drying component are integrated inside the pretreatment chamber, and the two work together to simultaneously complete the mechanical crushing and inert atmosphere dehumidification and drying of the agglomeration inhibitor; the pretreatment chamber is a fully enclosed pressure-bearing structure to block dust from the powder, isolate external humid air, and prevent the inhibitor from absorbing moisture and agglomerating again.

5. The automatic dosing process for the pretreatment inhibitor of agglomeration as described in claim 4, characterized in that, The stirring and disturbance component is a controllable screw stirring control system, which includes a drive motor, a transmission mechanism, and a stirring screw with stirring blades; S100 further includes the following steps: the stirring screw continuously shears, kneads and breaks up the agglomeration inhibitor by means of the screw spiral surface and the stirring blades, and at the same time, the agglomeration inhibitor is turned over to achieve full contact and heat exchange between the material and the dry inert gas.

6. The automatic dosing process for the pretreatment inhibitor of agglomeration as described in claim 4, characterized in that, The inert gas dehumidification and drying assembly includes: an inert gas source, a drying and filtration unit, a flow regulating valve, and an internal gas distribution pipeline; The S100 further includes the following step: continuously introducing the dried and dehydrated inert gas into the pretreatment chamber to form an inert atmosphere inside the chamber.

7. The automatic dosing process for the pretreatment inhibitor of agglomeration as described in claim 1, characterized in that, The buffer compartment is equipped with a vibrating air hammer, which is installed on the inner wall of the buffer compartment. The S300 further includes the following step: controlling the vibrating hammer to vibrate intermittently or continuously to break up the high-flowability fine powder that is accumulated and stuck to the walls of the buffer chamber.

8. The automatic dosing process for the pretreatment inhibitor of agglomeration as described in claim 1, characterized in that, The controllable screw conveyor mechanism is a metering screw, which is connected to the discharge port of the buffer bin; The S300 further includes the following steps: the blades of the metering screw quantitatively push the high-flowability fine powder, and the conveying speed of the metering screw is controlled in a closed loop according to the real-time weight feedback signal of the weight detection unit.

9. The automatic dosing process for the agglomeration pretreatment inhibitor as described in claim 8, characterized in that, The secondary crushing structure consists of shearing and crushing teeth arranged on the metering screw shaft, and multiple sets of the shearing and crushing teeth are distributed along the axial direction of the metering screw and rotate synchronously with the metering screw. The S300 further includes the following steps: shearing and grinding the residual trace agglomerated material after pretreatment on the high-flowability fine powder conveying path to make the powder output uniform and smooth.

10. The automatic dosing process for the agglomeration pretreatment inhibitor as described in claim 8, characterized in that, The discharge end of the metering screw is equipped with a linkage control ball valve; The S300 also includes the following steps: when the cumulative discharge amount reaches the preset addition weight, the metering screw is simultaneously shut down and the linkage control ball valve is closed to block the gravity flow of powder.

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