Hydride arsenic reactor feed control method, device, equipment and storage medium

Abstract

The application provides a hydrogen arsenide reaction kettle feeding control method and device, equipment and storage medium, and belongs to the technical field of hydrogen arsenide reaction. The method comprises the following steps: determining an initial feeding mode of raw materials in the initial stage of reaction based on the volume of the reaction kettle and an expected reaction molar ratio; the raw materials comprise zinc arsenide and dilute sulfuric acid; the expected reaction molar ratio is an expected molar ratio between the zinc arsenide and the dilute sulfuric acid; in response to a pressure change rate in the reaction kettle being less than a preset change rate value, switching the initial feeding mode to a uniform feeding mode of the raw materials in the middle stage of reaction; and in response to a generation rate of hydrogen arsenide being lower than a preset generation rate value, switching the uniform feeding mode to a final feeding mode of the raw materials in the late stage of reaction. The hydrogen arsenide reaction kettle feeding control method and device, equipment and storage medium provided by the application can accurately grasp the feeding time and feeding speed of the reaction kettle.

Description

Technical Field

[0001] This application belongs to the field of arsine reaction technology, and more specifically, relates to a method, apparatus, equipment, and storage medium for controlling the feeding of an arsine reactor. Background Technology

[0002] In semiconductor manufacturing, solar cell production, and other fields, arsine is a key electronic gas, and the efficiency and safety of its preparation process are crucial. Traditional methods for controlling the feed of arsine reactors often fail to achieve precise control of the reaction process, resulting in low reaction efficiency and poor raw material utilization. For example, during the reaction, the inability to accurately control the timing and rate of feed can easily lead to large pressure fluctuations within the reactor, affecting the formation rate and purity of arsine. Inappropriate feed control can also trigger side reactions, further reducing product quality. Summary of the Invention

[0003] The purpose of this application is to provide a method, apparatus, equipment, and storage medium for controlling the feeding of an arsine reactor, so as to accurately control the timing and speed of feeding into the reactor.

[0004] A first aspect of this application provides a method for controlling the feed of an arsine reactor, comprising:

[0005] The initial feed pattern of the raw materials in the initial stage of the reaction is determined based on the volume of the reactor and the desired reaction molar ratio; the raw materials include zinc arsenide and dilute sulfuric acid; the desired reaction molar ratio is the desired molar ratio between zinc arsenide and dilute sulfuric acid;

[0006] In response to the pressure change rate inside the reactor being less than the preset change rate value, the initial feeding mode is switched to the uniform feeding mode of raw materials in the middle of the reaction.

[0007] In response to the arsine generation rate being lower than the preset generation rate value, the uniform feed mode is switched to the final feed mode for the raw materials at the end of the reaction.

[0008] The feed rates corresponding to the initial feed mode, uniform feed mode and final feed mode decrease sequentially. The feed rates include the feed rate of zinc arsenide and the feed rate of dilute sulfuric acid.

[0009] A second aspect of this application provides an arsine reactor feed control device, comprising:

[0010] The initial feed module is used to determine the initial feed mode of the raw materials in the initial stage of the reaction based on the volume of the reactor and the desired reaction molar ratio; the raw materials include zinc arsenide and dilute sulfuric acid; the desired reaction molar ratio is the desired molar ratio between zinc arsenide and dilute sulfuric acid;

[0011] The uniform feed module is used to switch the initial feed mode to the uniform feed mode of raw materials in the middle of the reaction when the pressure change rate in the reactor is less than the preset change rate value.

[0012] The final feed module is used to switch from uniform feed mode to final feed mode for raw materials at the end of the reaction when the arsine generation rate is lower than the preset generation rate value.

[0013] The feed rates corresponding to the initial feed mode, uniform feed mode and final feed mode decrease sequentially. The feed rates include the feed rate of zinc arsenide and the feed rate of dilute sulfuric acid.

[0014] A third aspect of this application provides an electronic device, including a memory, a processor, and a computer program stored in the memory and running on the processor, wherein the processor executes the computer program to implement the steps of the above-described arsine reactor feed control method.

[0015] A fourth aspect of this application provides a computer-readable storage medium storing a computer program that, when executed by a processor, implements the steps of the above-described arsine reactor feed control method.

[0016] The beneficial effects of the arsine reactor feed control method, apparatus, equipment, and storage medium provided in this application embodiment are as follows: Firstly, this application embodiment determines the initial feed mode based on the reactor volume and the desired molar ratio of zinc arsenide to dilute sulfuric acid. This quickly establishes a stoichiometric raw material system, avoiding reaction lag and sudden pressure changes caused by imbalances in the initial feed ratio or improper feed rate, thus laying the foundation for efficient reaction start-up. Secondly, when the pressure change rate is less than a preset value, it switches to a uniform feed mode with a lower rate than the initial mode. This design matches the stable consumption rate in the middle of the reaction, dynamically balancing raw material replenishment and consumption, solving the problem of large pressure fluctuations caused by improper feed rate in traditional methods, reducing the impact on the arsine generation rate and purity, and lowering the risk of side reactions. Finally, when the arsine generation rate is lower than a preset value, it switches to a final feed mode with a further reduced rate. This allows for precise control of low-flow-rate feed based on the remaining raw material at the end of the reaction, avoiding raw material residue or waste caused by the inability to determine the endpoint in traditional methods, and improving raw material utilization. Therefore, the embodiments of this application can achieve precise control of the timing and speed of feeding into the reactor by using a phased and precise switching and gradient rate reduction method, thereby improving reaction efficiency, product purity and raw material utilization, and ensuring safe and stable reaction. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of this application, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 A schematic flowchart of an arsine reactor feed control method provided in an embodiment of this application;

[0019] Figure 2 This is a structural block diagram of an arsine reactor feed control device provided in an embodiment of this application;

[0020] Figure 3 This is a schematic block diagram of an electronic device provided in an embodiment of this application. Detailed Implementation

[0021] In the following description, specific details such as particular system architectures and techniques are set forth for illustrative purposes and not for limitation, in order to provide a thorough understanding of the embodiments of this application. However, those skilled in the art will understand that this application may also be implemented in other embodiments without these specific details. In other instances, detailed descriptions of well-known systems, apparatuses, circuits, and methods have been omitted so as not to obscure the description of this application with unnecessary detail.

[0022] To make the objectives, technical solutions, and advantages of this application clearer, the following description will be provided in conjunction with the accompanying drawings and specific embodiments.

[0023] In one embodiment of this application, the chemical reaction equation for hydrogen arsine is provided;

[0024] The chemical reaction equation is:

[0025]

[0026] in, Indicates zinc arsenide, This indicates dilute sulfuric acid. It represents arsine. This indicates that arsine is in gaseous form. This indicates zinc sulfate.

[0027] In this embodiment, as shown in the equation, 1 mole of zinc arsenide reacts with 3 moles of dilute sulfuric acid to produce 2 moles of hydrogen arsine (…). (released in gaseous form) and 3 moles of zinc sulfate ( Whether it's ensuring the molar ratio of zinc arsenide to dilute sulfuric acid meets the reaction requirements in the initial feed mode, or adjusting the feed rate in subsequent stages to maintain reaction stability, the 1:3 raw material ratio determined by this equation must be used as a benchmark. This ensures that the reaction proceeds according to the predetermined stoichiometry, providing theoretical chemical support for precisely controlling the arsine generation rate and pressure changes within the reactor, ensuring that the reaction proceeds efficiently, stably, and safely.

[0028] In this embodiment, the feed control of the reactor during the preparation of arsine is divided into three modes: initial feed mode, uniform feed mode, and final feed mode. The feed rates corresponding to the initial feed mode, uniform feed mode, and final feed mode decrease sequentially, and the feed rates include the feed rates of zinc arsenide and dilute sulfuric acid.

[0029] Please refer to Figure 1 , Figure 1 This is a flowchart illustrating a method for controlling the feed of an arsine reactor according to an embodiment of this application. The method can be executed by electronic equipment and may include:

[0030] S101: Determine the initial feed mode of the raw materials in the initial stage of the reaction based on the volume of the reactor and the desired reaction molar ratio; the raw materials include zinc arsenide and dilute sulfuric acid; the desired reaction molar ratio is the desired molar ratio between zinc arsenide and dilute sulfuric acid.

[0031] In this embodiment, the desired reaction molar ratio refers to zinc arsenide ( ) and dilute sulfuric acid ( According to the chemical reaction equation ( The target value is set at the required 1:3 ratio.

[0032] In the initial feeding stage, it is necessary to strictly control the feeding rate of zinc arsenide and dilute sulfuric acid. By adjusting the feeding amount and rate of both, the reaction can be kept in a state of stable pressure change and appropriate raw material ratio at the beginning stage. This avoids sudden pressure changes or raw material ratio imbalance caused by improper initial feeding, which would affect the subsequent arsine generation efficiency and reaction safety.

[0033] In this embodiment, the total amount of raw materials required for the initial stage can be calculated based on the reactor volume. According to the effective volume of the reactor and the preset initial reaction concentration (such as the initial concentration of dilute sulfuric acid), the amount of raw materials required to achieve the desired molar ratio is determined. and The total molar quantity; based on the set initial feeding time (e.g., 5-10 minutes), the total molar quantity is converted into the feeding rate ( In terms of mass flow rate (kg / min), (Measured by volumetric flow rate in L / min), ensuring that the two feedstocks are fed synchronously at a molar ratio of 1:3; the initial feed mode is used during the reaction start-up stage, where precise control of the feed rates of the two feedstocks is used to quickly establish a reaction system conforming to this molar ratio, while avoiding a sudden pressure rise due to excessively fast feed or a reaction lag due to excessively slow feed. The initial feed rate needs to be higher than that in the intermediate and final stages, with the aim of quickly bringing the reaction system to the critical start-up state and shortening the reaction lag time. For example, if the reactor volume is 100L, the desired initial stage... If the concentration is 2 mol / L, then The total demand is 200 mol, corresponding to The required amount is approximately 66.7 mol (at a 1:3 molar ratio). If the initial feed time is set to 10 minutes, then... The initial feed rate is 20 mol / min. The flow rate was 6.67 mol / min.

[0034] S102: In response to the pressure change rate inside the reactor being less than the preset change rate value, the initial feeding mode is switched to the uniform feeding mode of raw materials in the middle of the reaction.

[0035] In this embodiment, after the initial feeding rate is relatively high, the arsine in the reactor ( As the amount of gas generated gradually increases, the pressure change rate (pressure increment per unit time) will experience a process of rapid increase followed by gradual stabilization. When the pressure change rate drops below the preset value, it indicates that the reaction has entered a stable stage, at which point it is necessary to switch to a uniform feed mode to match the reaction consumption rate.

[0036] In this embodiment, the consumption rate of the intermediate reaction is calculated based on the reaction kinetic model to ensure... and The feed molar ratio should always be maintained at 1:3; the uniform feed rate should be lower than the initial feed rate, for example, in the initial stage. The feed rate is 10L / min, which may be reduced to 5L / min in the middle stage to avoid pressure fluctuations or side reactions caused by excessive raw materials and to ensure reaction stability.

[0037] In this embodiment, the uniform feed mode is set based on the stability of the reaction state. Under the premise of stable pressure changes, maintaining a constant feed rate for zinc arsenide and dilute sulfuric acid can sustain the continuous and stable reaction. Uniform feed allows the feed rate to remain relatively balanced with the reaction consumption rate, ensuring that the generation of arsine is within a stable rate range, avoiding large pressure changes caused by fluctuations in the feed rate, and guaranteeing the continuity and stability of the reaction in the middle stage.

[0038] In this embodiment, a preset initial feeding time is established. Before the preset initial feeding time is reached, even if the pressure change rate is less than the preset value, the initial feeding mode continues to be maintained to ensure that the initial raw material input is completed according to the predetermined amount, establishing a stable foundation for the reaction. When the preset initial feeding time is reached, if the pressure change rate in the reactor is not less than the preset change rate value, the feeding rate in the initial feeding mode is reduced (while maintaining the 1:3 molar ratio of zinc arsenide to dilute sulfuric acid) to avoid a sudden pressure increase that could lead to safety risks. If the pressure change rate remains stable but does not drop below the preset value, the current initial feeding rate is maintained until the pressure change rate is less than the preset change rate value, at which point the feed mode is switched to uniform feeding mode. During this process, the raw material concentration and the arsine generation rate are monitored simultaneously to ensure that no abnormal fluctuations occur in the reaction system.

[0039] S103: In response to the arsine generation rate being lower than the preset generation rate value, the uniform feed mode is switched to the final feed mode for the raw materials at the end of the reaction.

[0040] In this embodiment, as the reaction proceeds, the effective raw material in the reactor gradually decreases. The generation rate will gradually decrease. When the generation rate is lower than the preset value (such as 20% of the initial peak), it indicates that the reaction is nearing its end point and it is necessary to switch to the final feed mode to minimize raw material waste.

[0041] In this embodiment, after detecting that the arsine generation rate is lower than the preset generation rate value, the system automatically switches to the final feed mode. The feed rate in the final feed mode is determined based on the amount of raw material remaining in the reactor (which can be calculated by the difference between the previous feed rate and the reaction consumption) and the estimated remaining reaction time (which can be estimated based on historical data or real-time reaction rate). The raw material is slowly replenished at a low flow rate to ensure that the remaining raw material is completely reacted. Finally, the feed is stopped when the raw material is exhausted, thus completing the entire reaction process.

[0042] In this embodiment, the remaining amount in the reactor can be calculated by accumulating the difference between the initial feed amount and the reaction consumption. and The molar amount is determined by the desired molar ratio of 1:3 to determine the total final feed volume; the final feed rate must be lower than the intermediate uniform rate, for example, the intermediate feed rate... The feed rate is 5 L / min, which can be reduced to 1-2 L / min in the final stage to ensure complete reaction of the remaining raw materials; when detected... When the production rate approaches zero, stop feeding to avoid excessive raw material residue affecting product purity.

[0043] As can be seen from the above, this embodiment determines the initial feed mode based on the reactor volume and the desired molar ratio of zinc arsenide to dilute sulfuric acid. This allows for the rapid establishment of a stoichiometric feed system, avoiding reaction lag and sudden pressure changes caused by imbalances in the initial feed ratio or improper feed rate, thus laying the foundation for efficient reaction start-up. Secondly, when the pressure change rate is less than a preset value, the system switches to a uniform feed mode at a lower rate than the initial mode. This design matches the stable consumption rate during the reaction, dynamically balancing feed replenishment and consumption, solving the problem of large pressure fluctuations caused by improper feed rates in traditional methods, reducing the impact on the arsine generation rate and purity, and lowering the risk of side reactions. Finally, when the arsine generation rate is lower than a preset value, the system switches to a final feed mode with a further reduced rate. This allows for precise control of the low-flow-rate feed based on the remaining feed at the end of the reaction, avoiding feed residue or waste caused by the inability to determine the endpoint in traditional methods, and improving feed utilization. Therefore, this embodiment, through precise phased switching and gradient rate reduction, can achieve precise control of the timing and rate of feed into the reactor, improving reaction efficiency, product purity, and feed utilization, and ensuring safe and stable reaction.

[0044] In one embodiment of this application, the method further includes:

[0045] The feed rate of the raw materials during the mid-reaction phase was determined based on the reaction kinetics model of zinc arsenide and dilute sulfuric acid;

[0046] The feed rate of raw materials at the end of the reaction is determined based on the target remaining amount of raw materials. The target remaining amount of raw materials is the remaining amount of dilute sulfuric acid and zinc arsenide when the pressure change rate inside the reactor is detected to be less than the preset change rate value.

[0047] In this embodiment, the reaction kinetic model for zinc arsenide and dilute sulfuric acid is as follows:

[0048] in, Indicates the reaction rate. Represents the reaction rate constant. Indicates the concentration of zinc arsenide. The concentration of dilute sulfuric acid is given, m represents the reaction order of zinc arsenide, and n represents the reaction order of dilute sulfuric acid.

[0049] In this embodiment, the intermediate stage of the reaction begins when the pressure change rate is less than a preset value. At this point, the feed rate needs to be dynamically calculated using a model to maintain reaction stability. In the model, the relationship between the reaction rate and the reactant concentration is determined by the reaction order m and n (for example, if both m and n are 1, the reaction rate is linearly related to the concentrations of the two raw materials). Combining the 1:3 molar ratio in the chemical reaction equation, the consumption rates of zinc arsenide and dilute sulfuric acid can be derived through the model, thereby determining the feed rates of both and ensuring a precise match between the raw material replenishment rate and the reaction consumption rate.

[0050] In this embodiment, the feed rate at the end of the reaction is determined based on a target remaining amount, which refers to the amount of zinc arsenide and dilute sulfuric acid remaining in the reactor when the pressure change rate first falls below a preset value (i.e., at the beginning of the intermediate stage). and The chemical reaction equation requires the two substances to react completely in a 1:3 molar ratio to maximize the production of the target product. If any raw material is in excess, it will not only cause waste, but may also trigger side reactions due to the reaction of excess raw material with products or impurities. At the beginning of the intermediate stage, the remaining raw material has shifted from rapid fluctuations in the initial stage to stable consumption. The amount of remaining raw material accurately reflects the matching amount that needs to be replenished later. Using this remaining amount as a benchmark, combined with a 1:3 molar ratio, the total feed amount at the end can be calculated to ensure that the replenished raw material reacts exactly with the remaining raw material, avoiding the problem of over- or under-replenishment.

[0051] When the pressure change rate is detected to meet the target, the molar amounts of unreacted zinc arsenide and dilute sulfuric acid at this time (i.e., the target remaining amount) are recorded simultaneously. After entering the final stage, based on the target remaining amount and combined with the 1:3 molar ratio of the chemical reaction equation, the total amount of raw materials to be added is calculated (to ensure that the remaining raw materials react completely). According to the estimated final stage reaction time (based on historical data or real-time generation rate), the total amount to be added is converted into the final stage feed rate, and this rate must be lower than the intermediate uniform rate. Feed is carried out slowly at a low flow rate until the target remaining amount is exhausted.

[0052] For example, if the remaining zinc arsenide is 0.1 moles, then 0.3 moles of dilute sulfuric acid should be added at a constant rate in a 1:3 ratio until the raw material is exhausted. Precise control of the remaining amount avoids the waste of raw materials or increased side reactions caused by blind feeding in traditional methods, ensuring that the reaction is completed efficiently in the final stage.

[0053] As can be seen from the above, in the uniform feed mode, the feed rate is determined based on the reaction kinetic model, which can accurately match the reaction consumption and maintain a stable reaction state. The final feed mode is based on a fixed feed rate according to the remaining amount of raw materials, which avoids waste. The combination of these two methods improves the accuracy of feed control, ensures efficient and stable reaction, and increases the utilization rate of raw materials.

[0054] In one embodiment of this application, the feed rate of the raw materials during the intermediate stage of the reaction is determined based on a reaction kinetic model of zinc arsenide and dilute sulfuric acid, including:

[0055] The reaction kinetic model is derived from the reaction rate constant and mass transfer efficiency correction coefficient corresponding to the chemical reaction equation of hydrogen arsenide; the mass transfer efficiency is the degree of effective mass transfer between zinc arsenide and dilute sulfuric acid.

[0056] In the arsine reaction, zinc arsenide is added to the reactor in the form of solid particles. The contact efficiency between zinc arsenide and dilute sulfuric acid directly affects the reaction rate. However, the traditional model does not take into account the problems of particle sedimentation and uneven acid diffusion.

[0057] In this embodiment, when the particle diameter increases or the stirring speed decreases, the mass transfer efficiency correction coefficient decreases, correcting the actual situation of a low reaction rate and resolving the calculation deviation caused by the assumption of complete mixing in the reaction kinetic model.

[0058] In one embodiment of this application, a reaction kinetic model is obtained based on the reaction rate constant and mass transfer efficiency correction coefficient corresponding to the chemical reaction equation of arsine, including:

[0059] The reaction kinetic model is derived based on the first formula;

[0060] The first formula is:

[0061]

[0062] in, Indicates the reaction rate. Represents the reaction rate constant. This represents the mass transfer efficiency correction factor. Indicates the concentration of zinc arsenide. The concentration of dilute sulfuric acid is given, m represents the reaction order of zinc arsenide, and n represents the reaction order of dilute sulfuric acid.

[0063] In this embodiment, For chemical kinetics, traditional rate equations only consider the effect of concentration on the reaction rate, but cannot describe the mass transfer resistance at the solid-liquid interface. A mass transfer efficiency correction coefficient is introduced as the mass transfer efficiency correction term. (0< ≤1), consider mass transfer limitations caused by uneven sedimentation and diffusion of zinc arsenide particles. For example, when stirring is insufficient, Reduce and automatically correct the predicted reaction rate.

[0064] Since zinc arsenide exists in the form of solid particles, its contact efficiency with dilute sulfuric acid is affected by factors such as particle sedimentation and uneven acid diffusion. Traditional rate equations only consider the effect of concentration on the reaction and cannot reflect these mass transfer limitations. Therefore, this embodiment introduces a mass transfer efficiency correction coefficient η.

[0065] In one embodiment of this application, the method further includes:

[0066] The reaction rate constant is determined based on the second formula;

[0067] The second formula is:

[0068]

[0069] in, Represents the reaction rate constant. Indicates pre-exponential factor, R represents the activation energy for the main reaction of zinc arsenide with dilute sulfuric acid to produce hydrogen arsine, R represents the gas constant, and T represents the temperature inside the reactor.

[0070] In this embodiment, the introduction of the second formula addresses the effect of temperature on the reaction rate, and the activation energy for the main reaction of zinc arsenide with dilute sulfuric acid to produce hydrogen arsine is determined. Reflecting the main reaction ( +3 2 +3 The energy barrier Ea. The higher the Ea, the more significant the effect of temperature on the reaction rate. Pre-exponential factor. The effective collision frequency of reactant molecules can be determined experimentally.

[0071] In one embodiment of this application, the method further includes:

[0072] The mass transfer efficiency correction coefficient is determined based on the third formula.

[0073] The mass transfer efficiency correction factor is:

[0074]

[0075] in, This represents the mass transfer efficiency correction factor. The system characteristic constants (which can be determined experimentally, with values ​​ranging from 0.02 to 0.05, and are used to reflect specific properties of the arsine reaction system); Indicates the particle diameter of zinc arsenide (measured value, ranging from 80 to 100 mesh). This indicates the viscosity of an acid solution (referring to the magnitude of internal friction experienced by a liquid like dilute sulfuric acid when it flows). In the arsine reaction, acid viscosity affects its fluidity and diffusion capacity. Acids with lower viscosity flow better and diffuse more smoothly. The surface of solid particles is beneficial for improving mass transfer efficiency; high-viscosity acids have poor fluidity, hinder diffusion, and thus reduce mass transfer efficiency. (The chance of contact with dilute sulfuric acid, thus affecting the reaction process). express The stirring speed when mixing solid particles with dilute sulfuric acid directly affects the mixing effect of the solid and liquid phases: the higher the speed, the greater the stirring intensity. Better particle dispersion in acid reduces particle sedimentation and promotes acid diffusion to the particle surface, thereby improving mass transfer efficiency; conversely, if the rotational speed is too low (N decreases), the denominator in the formula increases. The decrease in value reflects the inhibitory effect of particle sedimentation and uneven acid diffusion on mass transfer efficiency.

[0076] In this embodiment, mass transfer efficiency refers to the efficiency during the arsine reaction. The effectiveness of mass transfer between solid particles and dilute sulfuric acid. In the reaction, only when... For the reaction to proceed smoothly, the surface of the solid particles must be in full contact with the dilute sulfuric acid. High mass transfer efficiency means that the two reactants can contact and interact efficiently, allowing the reaction to proceed more completely and rapidly; conversely, low mass transfer efficiency leads to insufficient contact between the reactants, resulting in a decreased reaction rate and affecting the reaction outcome. For example... Particle sedimentation and uneven acid diffusion can both reduce mass transfer efficiency. The mass transfer efficiency correction factor... This effect can be used to characterize the actual reaction rate more accurately.

[0077] In this embodiment, the mass transfer efficiency correction coefficient It is a dimensionless parameter (value 0 < ≤1), used to quantify the impact of mass transfer efficiency on the reaction. Therefore, in practical applications, the terms in the third formula can be normalized to convert them into dimensionless form to eliminate the interference of physical quantity units, making the formula applicable to reaction systems of different scales.

[0078] As can be seen from the above, this embodiment solves the problem of uneven contact between solid particles and liquid by using a mass transfer efficiency correction coefficient. The reaction rate constant is adjusted in real time according to the temperature inside the reactor to avoid reaction runaway caused by temperature fluctuations.

[0079] The first molar flow rate of zinc arsenide and the second molar flow rate of dilute sulfuric acid were determined based on the reaction kinetic model.

[0080] The feed rate of zinc arsenide is determined based on the first molar flow rate, molar mass, feed density, and purity.

[0081] The feed rate of dilute sulfuric acid is determined based on the second molar flow rate and the concentration of dilute sulfuric acid.

[0082] In this embodiment, the reaction equation is as follows: and The molar ratio is 1:3, but the feed rate (unit: kg / min or L / min) cannot be directly set according to this ratio because: For solid particles, measured by mass flow rate (e.g., kg / min); For liquids, measured by volumetric flow rate (e.g., L / min). For solids... The concentration is expressed as purity (e.g., 98%); liquid The concentration is expressed as a mass fraction (e.g., 15%-20%) or a molar concentration (mol / L).

[0083] Therefore, the reaction stoichiometry needs to be converted into the actual feed rate using molar flow rates. The first molar flow rate of zinc arsenide and the second molar flow rate of dilute sulfuric acid are determined based on a reaction kinetic model.

[0084] The first mole flow rate of zinc arsenide consumed per unit time is calculated as follows:

[0085] ;

[0086] in, This indicates the first molar flow rate of zinc arsenide. V represents the reaction rate, and V represents the volume of the reaction vessel.

[0087] The second mole flow rate of dilute sulfuric acid consumed per unit time is calculated as follows:

[0088]

[0089] in, This indicates the second molar flow rate of dilute sulfuric acid.

[0090] The first molar flow rate of zinc arsenide and the second molar flow rate of dilute sulfuric acid were converted into feed rates, respectively.

[0091] The feed rate (mass flow rate) of zinc arsenide is:

[0092]

[0093] in, This indicates the feed rate of zinc arsenide. This indicates the molar mass of zinc arsenide (approximately 284.11 g / mol). This indicates the feed density of zinc arsenide (kg / L, taken as 2.5-3.0 kg / L). This indicates the purity of zinc arsenide (e.g., 98%).

[0094] The feed rate (volume flow rate) of dilute sulfuric acid is:

[0095]

[0096] in, This indicates the feed rate of dilute sulfuric acid. This indicates the concentration of dilute sulfuric acid (which can be calculated from the density, molar mass, and mass fraction of dilute sulfuric acid, such as 2.3 mol / L).

[0097] For example, assume that the reaction kinetic model calculates r = 0.05 mol / (L·min), the reactor volume V = 100 L, the sulfuric acid mass fraction is 20%, and the zinc arsenide purity is 98%.

[0098] Calculate molar flow rate: =0.05 100 = 5 mol / min; =3 5 = 15 mol / min.

[0099] Feeding speed: kg / min.

[0100] Feeding speed: L / min.

[0101] As can be seen from the above, this embodiment solves the calculation errors caused by neglecting particle sedimentation and uneven acid diffusion in traditional models by introducing a mass transfer efficiency correction coefficient. It dynamically corrects the reaction rate using parameters such as particle diameter and stirring speed. Furthermore, by incorporating the effect of temperature into the second formula, it accurately reflects the impact of temperature fluctuations on the reaction. Based on the reaction stoichiometry and material characteristics, it converts the molar flow rate into the actual feed rate, achieving precise solid-liquid feed ratios. This allows for real-time adaptation to changes in reaction conditions, preventing reaction runaway, improving feedstock utilization and reaction stability, and providing reliable technical support for the efficient and safe production of arsine.

[0102] In one embodiment of this application, the method further includes:

[0103] Based on the rate of change of raw material purity, the preset rate of change value is adjusted to obtain a new preset rate of change value;

[0104] The desired reaction concentration is the concentration at which the rate of pressure change inside the reactor is less than the new preset rate of change, and the molar ratio of zinc arsenide to dilute sulfuric acid is satisfied.

[0105] In this embodiment, the rate of change in raw material purity refers to the degree to which the purity of the reaction raw materials (such as zinc arsenide or dilute sulfuric acid) changes over time or batch (for example, the purity of a certain batch of raw materials decreases by 5% / hour compared to the standard value, or the purity fluctuation range between different batches is 3%). The purity of raw materials directly affects the reaction efficiency, and thus affects the pressure change inside the reactor.

[0106] The preset rate of change is a pre-defined reasonable range of pressure variation within the reactor over time. The rate of pressure change is a key indicator of the reaction state; an excessively fast reaction rate will cause a sudden pressure surge (exceeding the safe range), while an excessively slow rate will result in an incomplete reaction.

[0107] In this embodiment, the purity change of the raw materials is monitored in real time or periodically during the reaction process. For example, if the purity of the raw materials decreases due to prolonged storage time (the purity change rate is negative), or if the purity fluctuates due to batch differences (the change rate is the fluctuation value), the change rate data needs to be recorded.

[0108] Based on the change rate of raw material purity, the initial preset change rate value is corrected to obtain a new preset change rate value.

[0109] For example, if the purity of the raw materials decreases (the rate of change in purity is negative), the reactivity decreases, the reaction rate at the same concentration will be slower, and the pressure rise rate will be lower than the initial preset value. In this case, the preset rate of change value needs to be reduced (for example, from 0.1 MPa / hour to 0.08 MPa / hour) to avoid misjudging the reaction as abnormal due to the actual pressure change rate appearing too low. Conversely, if the purity of the raw materials increases (the rate of change is positive), the reaction is more vigorous, and the pressure may rise sharply. The preset rate of change value needs to be increased (for example, from 0.1 MPa / hour to 0.12 MPa / hour) to ensure that the reaction pressure does not exceed the safe threshold.

[0110] The final new preset rate of change value is a dynamic control threshold that adapts to the current purity state of the raw materials.

[0111] As can be seen from the above, this embodiment dynamically adjusts the preset pressure change rate by changing the purity of the raw materials, making the determination of the desired reaction concentration more suitable for the actual state of the raw materials. This ensures that the pressure change is within a safe range and that the raw material molar ratio is compliant, reducing reaction runaway or inefficiency caused by purity fluctuations, and improving control flexibility and reaction stability.

[0112] In one embodiment of this application, the method further includes:

[0113] Based on the deviation between the real-time purity value of arsine in the reactor and the preset purity threshold, the feed rate adjustment coefficient of each stage is dynamically corrected.

[0114] Each stage includes the initial reaction phase, the middle reaction phase, and the final reaction phase;

[0115] The adjustment coefficient is used to finely adjust the feed rates of zinc arsenide and dilute sulfuric acid proportionally while maintaining the desired reaction molar ratio, and the adjustment coefficient is negatively correlated with the purity deviation.

[0116] In this embodiment, the purity of hydrogen arsine at the reactor outlet (e.g., purity value P, in %) can be monitored in real time using an online gas chromatograph throughout the entire reaction process (initial, intermediate, and final stages). This purity is then compared with a preset purity threshold (e.g., 99.99%, set according to product requirements) to calculate the purity deviation. P:

[0117] P = Preset purity threshold - Real-time purity value P;

[0118] when When P>0, it indicates that the real-time purity is below the threshold, and there is a purity deviation; when When P≤0, it indicates that the real-time purity meets the standard and no adjustment coefficient needs to be corrected.

[0119] Adjustment coefficient (denoted as) ,0< ≤1) Used to finely adjust the feed rates of zinc arsenide and dilute sulfuric acid proportionally based on the basic feed rates at each stage, while always maintaining the desired reaction molar ratio of 1:3 between the two. With purity deviation The negative correlation of P is shown in Table 1 below:

[0120]

[0121] In this embodiment, when An increase in P (resulting in increased purity deviation) Accordingly reduce the feed rate to ensure a proportional decrease, thereby reducing the intensity of local reactions and suppressing side reactions; when P decreases (purity increases). It gradually recovered to 1.0.

[0122] In the initial stage of the reaction, the initial basic feed rate of zinc arsenide and dilute sulfuric acid is calculated based on the volume of the reactor and the desired reaction molar ratio of 1:3 (this process is consistent with the logic of claim 1 and S101). Then, an adjustment coefficient is determined based on the real-time monitored purity deviation, and the initial basic feed rate is adjusted proportionally.

[0123] The adjusted zinc arsenide feed rate = initial base feed rate × adjustment coefficient;

[0124] The adjusted dilute sulfuric acid feed rate = initial base feed rate × adjustment coefficient.

[0125] For example, if the initial calculated basic feed rate for zinc arsenide is 1.5 kg / min and for dilute sulfuric acid is 10 L / min, and the purity deviation is 0.03% (corresponding to an adjustment coefficient of 0.95), after fine-tuning, the feed rates for both are 1.425 kg / min and 9.5 L / min, respectively, while still maintaining a 1:3 molar ratio. This fine-tuning can avoid side reactions (such as the generation of impurity gases) caused by excessively high local concentrations of raw materials in the initial stage, ensuring purity while rapidly establishing the reaction system.

[0126] After entering the middle stage of the reaction, the basic uniform feed rate for both raw materials is first determined based on the reaction kinetic model. Then, the basic uniform feed rate is adjusted proportionally according to the adjustment coefficient corresponding to the real-time purity deviation.

[0127] The adjusted zinc arsenide feed rate = uniform base feed rate × adjustment coefficient;

[0128] The fine-tuned dilute sulfuric acid feed rate = uniform base feed rate × adjustment coefficient.

[0129] For example, if the basic constant feed rate of zinc arsenide calculated based on the reaction kinetic model is 0.8 kg / min and the dilute sulfuric acid is 5 L / min, when the purity deviation is 0.08% (corresponding to an adjustment coefficient of 0.90), the fine-tuned feed rates are 0.72 kg / min and 4.5 L / min, respectively, while maintaining the same molar ratio. This can address potential mass transfer inconsistencies during the intermediate stage (such as violent local reactions caused by zinc arsenide particle sedimentation) by reducing the feed rate to suppress side reactions and maintain stable purity.

[0130] At the end of the reaction, the baseline feed rate is first calculated based on the target remaining amount of raw materials recorded at the beginning of the intermediate stage. Then, an adjustment coefficient is determined by combining this with the real-time purity deviation, and the baseline feed rate is adjusted proportionally.

[0131] The adjusted zinc arsenide feed rate = final base feed rate × adjustment coefficient;

[0132] The adjusted dilute sulfuric acid feed rate = final base feed rate × adjustment coefficient.

[0133] For example, if the initial feed rate for zinc arsenide at the end of the process, calculated based on the target remaining amount, is 0.2 kg / min, and the feed rate for dilute sulfuric acid is 1.2 L / min, then when the purity deviation is 0.02% (corresponding to an adjustment coefficient of 0.95), the adjusted rates are 0.19 kg / min and 1.14 L / min, respectively, while maintaining the same molar ratio. This avoids secondary reactions caused by residual raw materials at the end of the process (such as the reaction of excess dilute sulfuric acid with the product), ensuring that the final product purity meets the standards.

[0134] As can be seen from the above, controlling the timing and speed of feeding by pressure change rate and generation rate may result in stable reaction but substandard product purity (e.g., trace impurities generated by side reactions). This embodiment establishes closed-loop control through real-time purity monitoring. When the purity of arsine is detected to be below a threshold (e.g., due to side reactions caused by excessively high local concentrations), the feed rates of the two raw materials are automatically reduced proportionally (maintaining a 1:3 molar ratio) to reduce the intensity of local reactions and suppress side reactions. When the purity recovers above the threshold, the original feed rate is gradually restored. This further achieves precise control over product quality and improves the overall reliability of the process.

[0135] In one embodiment of this application, the method further includes:

[0136] Acquire normal fluctuation data of arsine gas flow rate during historical feeding process, and establish a flow fluctuation characteristic baseline based on the normal fluctuation data. The flow fluctuation characteristic baseline includes a preset range of frequency, amplitude and duration of normal arsine gas flow rate fluctuation during historical feeding process.

[0137] Anomaly detection thresholds are determined based on the baseline characteristics of flow fluctuations. These thresholds include frequency anomaly thresholds, amplitude anomaly thresholds, and duration anomaly thresholds.

[0138] The system calculates the comprehensive deviation between the flow fluctuation characteristics and the baseline of the flow fluctuation characteristics under the current feeding mode in real time. When the comprehensive deviation exceeds the anomaly judgment threshold more than the preset number of times, a feeding anomaly warning is triggered.

[0139] In response to abnormal feeding warnings, an emergency feeding adjustment mechanism is automatically activated.

[0140] The emergency feed adjustment mechanism includes: reducing the current feed rate of zinc arsenide and dilute sulfuric acid based on the first preset adjustment step size, increasing the stirring speed based on the second preset adjustment step size, until the overall deviation is less than or equal to the abnormal judgment threshold, and then restoring the current feed mode.

[0141] In this embodiment, arsine gas flow data of the same type of reactor, the same batch of raw materials, and the same reaction stage within the past 3 months can be collected. Historical data under abnormal operating conditions such as abnormal raw material purity (e.g., zinc arsenide purity is less than 95%) and equipment failure (e.g., abnormal noise from the stirring motor) should be excluded to ensure data representativeness.

[0142] For each batch of historical data, the number of times the flow rate deviates from the average value within a unit of time (e.g., the number of fluctuations within 1 minute) is counted. After removing the maximum and minimum values, the average value is taken to determine the normal fluctuation frequency range for each stage. Using the average flow rate of each batch of data as a benchmark, the maximum deviation value of a single fluctuation is calculated, and the 95th percentile of the amplitude for each batch is calculated to determine the normal fluctuation amplitude range. The duration of a single fluctuation from deviation from the average value to regression to the average value is counted, and the median of each batch of data is taken to determine the normal fluctuation duration range. The preset ranges of frequency, amplitude, and duration corresponding to each reaction stage are entered into the database to form a phased flow fluctuation characteristic baseline.

[0143] In this embodiment, based on the upper limit of the characteristic baseline of each stage and combined with the reaction safety requirements (such as pressure fluctuation not exceeding 0.1 MPa), an anomaly judgment threshold is set by statistical methods to ensure that the threshold can both avoid false triggering of warnings and timely capture of true anomalies.

[0144] The frequency anomaly threshold can be set to 1.5 times the upper limit of the normal fluctuation frequency range for the corresponding stage. When the real-time fluctuation frequency exceeds this value, it is judged as a frequency anomaly.

[0145] The amplitude abnormality threshold can be set to twice the upper limit of the normal fluctuation amplitude range for the corresponding stage. When the real-time fluctuation amplitude exceeds this range, it is judged as an amplitude abnormality.

[0146] The abnormal duration threshold can be set to 1.5 times the upper limit of the normal fluctuation duration range for the corresponding stage. When the duration of a single fluctuation exceeds this value, it is judged as an abnormal duration.

[0147] The overall deviation is calculated using a weighted summation formula, which is as follows:

[0148] Overall deviation = (real-time frequency / frequency anomaly threshold) × 0.3 + (real-time amplitude absolute value / amplitude anomaly threshold) × 0.5 + (real-time duration / duration anomaly threshold) × 0.2.

[0149] Here, 0.3, 0.5, and 0.2 all represent weights, which can be set based on experience.

[0150] In this embodiment, the real-time fluctuation frequency, real-time amplitude (maximum flow deviation in the current minute), and real-time duration (longest single fluctuation duration in the current minute) of the current stage can be automatically calculated every minute, and a preliminary comparison can be made with the characteristic baseline of the corresponding stage.

[0151] The current comprehensive deviation is calculated in real time according to the above comprehensive deviation formula. If the deviation is greater than 1 (i.e., the anomaly judgment threshold, since all parameters in the formula use the threshold as the denominator, deviation = 1 exactly reaches the upper limit of the threshold), then one over-threshold event is recorded. The preset number of times is set to 3. When the control system detects 3 consecutive deviations > 1, it immediately triggers a feeding anomaly warning and displays the anomaly type (such as "amplitude exceeds threshold" or "duration exceeds threshold") on the control system interface to facilitate the operator's judgment.

[0152] The first preset adjustment step size can be set based on the initial feed rate of each stage to ensure that the rate reduction does not cause the reaction to be interrupted, while also quickly suppressing abnormal fluctuations. For example: in the initial stage, the dilute sulfuric acid feed rate is 10L / min, and the step size is set to 1L / min; in the uniform stage, the feed rate is 5L / min, and the step size is set to 0.5L / min; in the final stage, the feed rate is 2L / min, and the step size is set to 0.2L / min. In addition, the zinc arsenide and dilute sulfuric acid are always reduced synchronously at a molar ratio of 1:3 (e.g., when the dilute sulfuric acid rate is reduced by 1L / min, the zinc arsenide rate is reduced from 1.45kg / min to 1.21kg / min according to the molar ratio).

[0153] The second preset adjustment step size can be set based on the current stirring speed to avoid particle breakage or energy waste caused by excessive speed. For example, when the current speed is 50 r / s, the step size is set to 5 r / s; when the speed is 30 r / s, the step size is set to 3 r / s), and the maximum speed does not exceed 90% of the rated speed of the equipment (e.g., when the rated speed is 80 r / s, the upper limit is set to 72 r / s).

[0154] After triggering the warning, this embodiment can automatically send a speed reduction command to the feed pump (adjusted according to the first step length) and a speed increase command to the stirring motor (adjusted according to the second step length). The deviation is recalculated every 30 seconds to determine if it is still greater than 1. When the deviation is ≤1 (i.e., the frequency, amplitude, and duration have all returned to the normal range), the adjustment stops, and the current feed speed and stirring speed are maintained for 5 minutes. After confirming that the flow fluctuation is stable, the feed mode before the warning was triggered is automatically restored (e.g., from the uniform feed speed after the emergency speed reduction to the original uniform feed speed), avoiding frequent switching that could cause reaction fluctuations.

[0155] If the deviation is still greater than 1 after 5 consecutive adjustments, this embodiment can automatically upgrade the warning to an equipment shutdown warning, and at the same time shut down the feed pump, reduce the stirring speed to the minimum value, and trigger an audible and visual alarm to prompt the operator to check on-site.

[0156] As can be seen from the above, this embodiment, by establishing a baseline for the characteristic fluctuations of arsine gas flow rate and multi-dimensional anomaly judgment thresholds, combined with comprehensive deviation monitoring and continuous threshold exceeding judgment, can accurately identify feed anomalies and avoid the problems of delayed or misjudged anomaly responses in traditional control. After triggering an early warning, the feed rates of zinc arsenide and dilute sulfuric acid are simultaneously reduced by a fixed step size while the stirring speed is increased, which can quickly suppress abnormal flow fluctuations and prevent risks such as sudden changes in reactor pressure and increased side reactions caused by improper feeding. In conjunction with the staged feeding mode, it further enhances the stability and safety of the reaction process, reduces raw material waste, ensures the efficiency and purity of arsine generation, and improves the overall controllability and reliability of the process.

[0157] Corresponding to the arsine reactor feed control method in the above embodiment, Figure 2 This is a structural block diagram of an arsine reactor feed control device according to an embodiment of this application. For ease of explanation, only the parts relevant to the embodiment of this application are shown. References Figure 2 The arsine reactor feed control device 20 includes: an initial feed module 21, a uniform feed module 22, and a final feed module 23.

[0158] The initial feed module 21 is used to determine the initial feed mode of the raw materials in the initial stage of the reaction based on the volume of the reactor and the desired reaction molar ratio; the raw materials include zinc arsenide and dilute sulfuric acid; the desired reaction molar ratio is the desired molar ratio between zinc arsenide and dilute sulfuric acid;

[0159] The uniform feed module 22 is used to switch the initial feed mode to the uniform feed mode of raw materials in the middle stage of the reaction when the pressure change rate in the reactor is less than the preset change rate value.

[0160] The final feed module 23 is used to switch the uniform feed mode to the final feed mode of the raw materials at the end of the reaction in response to the arsine generation rate being lower than the preset generation rate value.

[0161] The feed rates corresponding to the initial feed mode, uniform feed mode and final feed mode decrease sequentially. The feed rates include the feed rate of zinc arsenide and the feed rate of dilute sulfuric acid.

[0162] In one embodiment of this application, the uniform feed module 22 is specifically used for:

[0163] The feed rate of the raw materials during the mid-reaction phase was determined based on the reaction kinetics model of zinc arsenide and dilute sulfuric acid;

[0164] The final feeding module 23 is specifically used for:

[0165] The feed rate of raw materials at the end of the reaction is determined based on the target remaining amount of raw materials. The target remaining amount of raw materials is the remaining amount of dilute sulfuric acid and zinc arsenide when the pressure change rate inside the reactor is detected to be less than the preset change rate value.

[0166] In one embodiment of this application, the uniform feeding module 22 is further used for:

[0167] The reaction kinetic model is derived from the reaction rate constant and mass transfer efficiency correction coefficient corresponding to the chemical reaction equation of hydrogen arsenide; the mass transfer efficiency is the degree of effective mass transfer between zinc arsenide and dilute sulfuric acid.

[0168] The first molar flow rate of zinc arsenide and the second molar flow rate of dilute sulfuric acid were determined based on the reaction kinetic model.

[0169] The feed rate of zinc arsenide is determined based on the first molar flow rate, molar mass, feed density, and purity.

[0170] The feed rate of dilute sulfuric acid is determined based on the second molar flow rate and the concentration of dilute sulfuric acid.

[0171] In one embodiment of this application, the uniform feeding module 22 is further used for:

[0172] The reaction kinetic model is derived based on the first formula;

[0173] The first formula is:

[0174]

[0175] in, Indicates the reaction rate. Represents the reaction rate constant. This represents the mass transfer efficiency correction factor. Indicates the concentration of zinc arsenide. The concentration of dilute sulfuric acid is given, m represents the reaction order of zinc arsenide, and n represents the reaction order of dilute sulfuric acid.

[0176] In one embodiment of this application, the uniform feeding module 22 is further used for:

[0177] The reaction rate constant is determined based on the second formula;

[0178] The second formula is:

[0179]

[0180] in, Represents the reaction rate constant. Indicates pre-exponential factor, R represents the activation energy for the main reaction of zinc arsenide with dilute sulfuric acid to produce hydrogen arsine, R represents the gas constant, and T represents the temperature inside the reactor.

[0181] In one embodiment of this application, the arsine reactor feed control device 20 further includes: a first adjustment module; the first adjustment module is specifically used for:

[0182] Based on the rate of change of raw material purity, the preset rate of change value is adjusted to obtain a new preset rate of change value;

[0183] Among them, in response to the pressure change rate inside the reactor being less than a preset change rate value, the initial feeding mode is switched to a uniform feeding mode for raw materials in the middle stage of the reaction, including:

[0184] In response to the pressure change rate inside the reactor being less than the new preset change rate value, the initial feeding mode is switched to the uniform feeding mode of raw materials in the middle of the reaction.

[0185] In one embodiment of this application, the arsine reactor feed control device 20 further includes: a second adjustment module; the second adjustment module is specifically used for:

[0186] Based on the deviation between the real-time purity value of arsine in the reactor and the preset purity threshold, the feed rate adjustment coefficient of each stage is dynamically corrected.

[0187] Each stage includes the initial reaction phase, the middle reaction phase, and the final reaction phase;

[0188] The adjustment coefficient is used to finely adjust the feed rates of zinc arsenide and dilute sulfuric acid proportionally while maintaining the desired reaction molar ratio, and the adjustment coefficient is negatively correlated with the purity deviation.

[0189] See Figure 3 , Figure 3 This is a schematic block diagram of an electronic device provided according to an embodiment of this application. Figure 3 The electronic device 300 in this embodiment may include one or more processors 301, one or more input devices 302, one or more output devices 303, and one or more memories 304. The processors 301, input devices 302, output devices 303, and memories 304 communicate with each other via a communication bus 305. The memories 304 store computer programs, including program instructions. The processors 301 execute the program instructions stored in the memories 304. Specifically, the processors 301 are configured to invoke the program instructions to perform the functions of the modules in the aforementioned device embodiments, for example... Figure 2 The functions of the initial feeding module 21, the uniform feeding module 22, and the final feeding module 23 are shown.

[0190] It should be understood that, in the embodiments of this application, the processor 301 may be a central processing unit (CPU), or it may be other general-purpose processors, digital signal processors (DSPs), application-specific integrated circuits (ASICs), field-programmable gate arrays (FPGAs), or other programmable logic devices, discrete gate or transistor logic devices, discrete hardware components, etc. The general-purpose processor may be a microprocessor or any conventional processor.

[0191] Input device 302 may include a touchpad, a fingerprint sensor (for collecting the user's fingerprint information and fingerprint orientation information), a microphone, etc., and output device 303 may include a display (LCD, etc.), a speaker, etc.

[0192] The memory 304 may include read-only memory and random access memory, and provides instructions and data to the processor 301. A portion of the memory 304 may also include non-volatile random access memory. For example, the memory 304 may also store information such as chemical reaction equations, a first formula, and then a second formula.

[0193] In specific implementations, the processor 301, input device 302, and output device 303 described in the embodiments of this application can execute the implementation method described in the arsine reactor feeding control method provided in the embodiments of this application, or they can execute the implementation method of the electronic device described in the embodiments of this application, which will not be repeated here.

[0194] In another embodiment of this application, a computer-readable storage medium is provided. This computer-readable storage medium stores a computer program, which includes program instructions. When executed by a processor, the program instructions implement all or part of the processes in the methods described above. Alternatively, the computer program can instruct related hardware to complete the process. The computer program can be stored in a computer-readable storage medium, and when executed by a processor, it can implement the steps of the various method embodiments described above. The computer program includes computer program code, which can be in the form of source code, object code, executable files, or certain intermediate forms. The computer-readable medium can include any entity or device capable of carrying computer program code, a recording medium, a USB flash drive, a portable hard drive, a magnetic disk, an optical disk, a computer memory, a read-only memory (ROM), a random access memory (RAM), an electrical carrier signal, a telecommunication signal, and a software distribution medium, etc.

[0195] The computer-readable storage medium can be an internal storage unit of the electronic device in any of the foregoing embodiments, such as a hard disk or memory of the electronic device. The computer-readable storage medium can also be an external storage device of the electronic device, such as a plug-in hard disk, smart media card (SMC), secure digital card (SD), flash card, etc., equipped on the electronic device. Furthermore, the computer-readable storage medium can include both internal and external storage units of the electronic device. The computer-readable storage medium is used to store computer programs and other programs and data required by the electronic device. The computer-readable storage medium can also be used to temporarily store data that has been output or will be output.

[0196] Those skilled in the art will recognize that the units and algorithm steps of the various examples described in conjunction with the embodiments disclosed herein can be implemented in electronic hardware, computer software, or a combination of both. To clearly illustrate the interchangeability of hardware and software, the components and steps of the various examples have been generally described in terms of functionality in the foregoing description. Whether these functions are implemented in hardware or software depends on the specific application and design constraints of the technical solution. Those skilled in the art can use different methods to implement the described functions for each specific application, but such implementations should not be considered beyond the scope of this application.

[0197] Those skilled in the art will clearly understand that, for the sake of convenience and brevity, the specific working process of the electronic devices and units described above can be referred to the corresponding process in the foregoing method embodiments, and will not be repeated here.

[0198] In the several embodiments provided in this application, it should be understood that the disclosed electronic devices and methods can be implemented in other ways. For example, the device embodiments described above are merely illustrative; for instance, the division of units is only a logical functional division, and in actual implementation, there may be other division methods. For example, multiple modules may be combined or integrated into another system, or some features may be ignored or not executed. Furthermore, the couplings or direct couplings or communication connections shown or discussed may be indirect couplings or communication connections through some interfaces or units, or they may be electrical, mechanical, or other forms of connection.

[0199] The units described as separate components may or may not be physically separate. The components shown as units may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the units can be selected to achieve the purpose of the embodiments of this application, depending on actual needs.

[0200] Furthermore, the functional modules in the various embodiments of this application can be integrated into one processing unit, or each module can exist physically separately, or two or more modules can be integrated into one unit. The integrated unit can be implemented in hardware or as a software functional unit.

[0201] The above are merely specific embodiments of this application, but the scope of protection of this application is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope disclosed in this application, and these modifications or substitutions should all be covered within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. A method for controlling the feed of a hydrogen arsenide reactor, characterized in that, The method comprises the following steps: determining an initial feeding mode of raw materials at the initial stage of the reaction based on the volume of the reactor and a desired reaction molar ratio; the raw materials include zinc arsenide and dilute sulfuric acid; the desired reaction molar ratio is a desired molar ratio between the zinc arsenide and the dilute sulfuric acid; switching the initial feeding mode to a uniform feeding mode of raw materials at the middle stage of the reaction in response to a pressure change rate in the reactor being less than a preset change rate value; switching the uniform feeding mode to a final feeding mode of raw materials at the end stage of the reaction in response to a generation rate of arsine being lower than a preset generation rate value; the feeding speeds corresponding to the initial feeding mode, the uniform feeding mode and the final feeding mode decrease in turn, and the feeding speeds include a feeding speed of the zinc arsenide and a feeding speed of the dilute sulfuric acid; The method further comprises the following steps: determining a feeding speed of raw materials at the middle stage of the reaction based on a reaction kinetics model of zinc arsenide and dilute sulfuric acid; wherein the reaction kinetics model is obtained based on a reaction rate constant corresponding to a chemical reaction equation of arsine and a mass transfer efficiency correction coefficient; the mass transfer efficiency is an effective degree of mass transfer between zinc arsenide and dilute sulfuric acid; determining a first molar flow of zinc arsenide and a second molar flow of dilute sulfuric acid based on the reaction kinetics model; determining the feeding speed of the zinc arsenide based on the first molar flow, molar mass, feeding density and purity of the zinc arsenide; determining the feeding speed of the dilute sulfuric acid based on the second molar flow and the concentration of the dilute sulfuric acid; determining a feeding speed of raw materials at the end stage of the reaction based on a target residual amount of the raw materials; the target residual amount of the raw materials is a residual amount of the dilute sulfuric acid and a residual amount of the zinc arsenide when it is detected that the pressure change rate in the reactor is less than the preset change rate value.

2. The arsine reactor feed control method of claim 1, wherein, The reaction kinetics model obtained based on the reaction rate constant corresponding to the chemical reaction equation of arsine and the mass transfer efficiency correction coefficient comprises the following steps: obtaining the reaction kinetics model based on a first formula; the first formula is: wherein, represents the reaction rate, represents the reaction rate constant, represents the mass transfer efficiency correction coefficient, represents the concentration of zinc arsenide, represents the concentration of dilute sulfuric acid, m represents the reaction order of zinc arsenide, and n represents the reaction order of dilute sulfuric acid.

3. The arsine reactor feed control method of claim 2, wherein, The method further comprises the following steps: determining the reaction rate constant based on a second formula; the second formula is: wherein, represents a reaction rate constant, represents a pre-exponential factor, represents an activation energy of the main reaction of zinc arsenide with dilute sulfuric acid to produce arsine, R represents a gas constant, and T represents a temperature in a reaction vessel.

4. The arsine reactor feed control method of claim 1, wherein, The method further comprises the following steps: adjusting the preset change rate value based on a change rate of the purity of the raw materials to obtain a new preset change rate value; wherein the step of switching the initial feeding mode to the uniform feeding mode of raw materials at the middle stage of the reaction in response to the pressure change rate in the reactor being less than the preset change rate value comprises the following step: switching the initial feeding mode to the uniform feeding mode of raw materials at the middle stage of the reaction in response to the pressure change rate in the reactor being less than the new preset change rate value.

5. The arsine reactor feed control method of claim 1 wherein, The method further comprises the following steps: dynamically correcting an adjustment coefficient of the feeding speed at each stage based on a deviation between a real-time purity value of arsine in the reactor and a preset purity threshold value; the stages include the initial stage, the middle stage and the end stage of the reaction; the adjustment coefficient is used to proportionally fine-tune the feeding speeds of the zinc arsenide and the dilute sulfuric acid while maintaining the desired reaction molar ratio, and the adjustment coefficient is negatively correlated with the purity deviation.

6. A control device for carrying out the control method of the feed of a hydrogen arsenide reactor according to any one of claims 1 to 5, characterized in that, The method comprises the following steps: An initial feeding module is configured to determine an initial feeding mode of raw materials at the beginning of a reaction based on a volume of a reactor and a desired reaction molar ratio between zinc arsenide and dilute sulfuric acid; A constant feeding module is configured to switch the initial feeding mode to a constant feeding mode of raw materials at a middle stage of the reaction in response to a pressure change rate in the reactor being less than a preset change rate value; The constant feeding module is specifically configured to: determine a feeding speed of the raw materials at the middle stage of the reaction based on a reaction kinetics model of the zinc arsenide and the dilute sulfuric acid; and The constant feeding module is specifically configured to: obtain the reaction kinetics model based on a reaction rate constant and a mass transfer efficiency correction coefficient corresponding to a chemical reaction equation of the arsine; the mass transfer efficiency is an effective degree of mass transfer between the zinc arsenide and the dilute sulfuric acid; determine a first molar flow of the zinc arsenide and a second molar flow of the dilute sulfuric acid based on the reaction kinetics model; determine the feeding speed of the zinc arsenide based on the first molar flow, a molar mass, a feeding density and a purity of the zinc arsenide; determine the feeding speed of the dilute sulfuric acid based on the second molar flow and a concentration of the dilute sulfuric acid; A final feeding module is configured to switch the constant feeding mode to a final feeding mode of raw materials at an end stage of the reaction in response to a generation rate of the arsine being less than a preset generation rate value; The final feeding module is specifically configured to: determine a feeding speed of the raw materials at the end stage of the reaction based on a target residual amount of the raw materials, the target residual amount of the raw materials being a residual amount of the dilute sulfuric acid and a residual amount of the zinc arsenide when the pressure change rate in the reactor is detected to be less than the preset change rate value; 7. An electronic device comprising a memory, a processor, and a computer program stored in the memory and running on the processor, characterized in that, The feeding speeds corresponding to the initial feeding mode, the constant feeding mode and the final feeding mode decrease in sequence, and the feeding speeds include the feeding speed of the zinc arsenide and the feeding speed of the dilute sulfuric acid.

8. A computer-readable storage medium storing a computer program, the computer-readable storage medium comprising: The processor executes the computer program to implement the steps of the method according to any one of claims 1 to 5. The computer program is executed by the processor to implement the steps of the method according to any one of claims 1 to 5.

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