Continuous production equipment of antimony mercaptide

Abstract

The invention provides continuous antimony mercaptide production equipment, and relates to the technical field of antimony mercaptide production, the continuous antimony mercaptide production equipment comprises a feeding machine, a mixing kettle is mounted on one side of the feeding machine, a first reaction kettle is placed on one side of the mixing kettle, a second reaction kettle is placed on one side of the first reaction kettle, and a first cooling kettle is placed on one side of the second reaction kettle; a second cooling kettle is placed on one side of the first cooling kettle, a plate-and-frame filter is placed on one side of the second cooling kettle, a storage tank is placed on one side of the plate-and-frame filter, and the antimony mercaptide continuous production equipment and process have the primary advantage that the product quality is greatly improved. Through the fine control means shown in the embodiment 3 and the embodiment 4, in the feeding link of the mixing kettle, by means of cooperative work of a pressure sensor, a raw material component spectrum analyzer and a miniature image recognition sensor, a PID control algorithm and a multiple linear regression algorithm are used, and the feeding speed of the mixing kettle is improved. Accurate and stable raw material feeding pressure and ultra-accurate proportioning feeding are achieved.

Description

Technical Field

[0001] The invention relates to the technical field of antimony mercaptide production, in particular to continuous production equipment for antimony mercaptide. Background Art

[0002] Antimony mercaptide occupies a very critical position in the field of material stabilization. As a stabilizer with excellent performance, its unique chemical structure gives it a series of remarkable excellent properties. In terms of initial coloring performance, antimony mercaptide performs extremely well. Compared with many traditional stabilizers, it can more effectively inhibit color changes and degradation in the initial stage of material processing, allowing the material to maintain a good color appearance in the early stage. This is of great importance for some application scenarios with strict color requirements, such as high-quality plastic products, exquisite rubber products, etc.

[0003] At present, the main production process of antimony thiolate mostly adopts batch-by-batch intermittent production method. Under this traditional intermittent production mode, the production process of each batch is relatively independent. From the input of raw materials, the control of reaction conditions to the output of the final product, it is difficult to achieve high consistency and stability in each link. Since there are inevitably some subtle differences in the operation of each batch, such as the weighing error of raw materials, the fluctuation of reaction time and temperature, and the incomplete stirring effect, these factors accumulate and lead to large differences in the final product between batches. This difference between batches is not only reflected in the physical and chemical properties of the product, such as purity, color, stability, etc., but may also affect its performance in practical applications, making it difficult to reliably guarantee the quality of the product.

[0004] At the same time, intermittent production requires a lot of manpower to operate and monitor each batch of production. From the preparation of raw materials, the start and stop of equipment, the adjustment of parameters during the reaction process to the subsequent processing of the product, all require direct human participation. This not only increases labor costs, but also further aggravates the instability of product quality due to the limitations of manual operation and inevitable human errors. In addition, the large number of on-site operators makes the operating environment of the production site more complex and chaotic, which is prone to safety accidents and poses great safety hazards. For example, leakage may occur during the handling and addition of raw materials, and improper operation during the reaction may lead to safety issues such as pressure out of control.

[0005] Therefore, a continuous production equipment of antimony mercaptides is needed to solve the above problems. Summary of the invention

[0006] Technical issues solved

[0007] In view of the shortcomings of the prior art, the present invention provides a continuous production device for antimony mercaptides, which solves the problems in the above background technology.

[0008] Technical Solution

[0009] To achieve the above objectives, the present invention is implemented through the following technical scheme: a continuous production equipment of antimony mercaptides, including a feeder, a mixing kettle is installed on one side of the feeder, a first reactor is placed on one side of the mixing kettle, a second reactor is placed on one side of the first reactor, a first cooling kettle is placed on one side of the second reactor, a second cooling kettle is placed on one side of the first cooling kettle, a plate and frame filter is placed on one side of the second cooling kettle, and a storage tank is placed on one side of the plate and frame filter.

[0010] Preferably, sight glasses are installed between the feeder, the mixing kettle, the first reactor, the second reactor, the first cooling kettle, the second cooling kettle, the plate and frame filter and the storage tank.

[0011] Preferably, a feeder interface is provided on one side of the top of the mixing kettle, a connecting pipe is installed between the feeder interface and the feeder, a stirring motor is installed in the middle of the top of the mixing kettle, the first reaction kettle, the second reaction kettle, the first cooling kettle and the second cooling kettle, and the bottom end of the stirring motor is transmission-connected with a stirring shaft.

[0012] Preferably, a feed inlet is provided on the other side of the top of the mixing kettle, and there are two groups of feed inlets on the other side of the top of the mixing kettle. A regulating valve is installed at the top of the feed inlet, and a flow meter is installed at the bottom of the feed inlet.

[0013] Preferably, a temperature sensor is installed on one side of the top of the first reaction kettle, the second reaction kettle, the first cooling kettle and the second cooling kettle.

[0014] Preferably, a vacuum gauge is installed on one side of the top of the first reactor and the second reactor close to the temperature sensor, a vacuum device is installed on the other side of the top of the first reactor and the second reactor, and a vacuum regulating valve is installed in the middle of the vacuum device.

[0015] Preferably, a temperature control medium inlet is installed on the top of the outer side of the first reactor, the second reactor, the first cooling kettle and the second cooling kettle, and an inlet regulating valve is installed in the middle of the temperature control medium inlet; a temperature control device is installed on the bottom of the outer side of the first reactor, the second reactor, the first cooling kettle and the second cooling kettle, and a temperature control medium outlet is included in the temperature control device, and an outlet regulating valve is installed in the middle of the temperature control medium outlet.

[0016] Preferably, the outlet of the feeder is connected to the mixing kettle, and the feed is directly fed into the mixing kettle through the feeder; the mixing kettle, the first reactor, the second reactor, the first cooling kettle and the second cooling kettle are connected in sequence through an overflow pipe; the cooling kettle is connected to the feed port of a plate and frame filter; the outlet of the plate and frame filter is connected to a storage tank; the first reactor and the second reactor are sandwich reactors, and a medium is passed into the interlayer for heating; the first reactor and the second reactor are both provided with vacuum lines; the first cooling kettle and the second cooling kettle are sandwich reactors, and a medium is passed into the interlayer for cooling.

[0017] Preferably, the process flow of the overall continuous production equipment is:

[0018] Sp1: First, the raw materials are transported to the mixing kettle through the connecting pipe by the feeder, and the feed amount of other raw materials is accurately controlled by the regulating valve and flow meter at the feed inlet. The stirring shaft is driven by the stirring motor in the mixing kettle for stirring and mixing;

[0019] Sp2: The mixed materials flow into the first reactor through the overflow pipe, the first reactor is evacuated through the vacuum device and the vacuum regulating valve, and the temperature of the medium in the interlayer is controlled by the temperature control medium inlet, the inlet regulating valve, the temperature control medium outlet and the outlet regulating valve to adjust the reaction temperature, so that the materials react in the first reactor;

[0020] Sp3: The reacted material flows into the second reactor through the overflow pipe, and the vacuum and temperature control operations in the first reactor are repeated for further reaction;

[0021] Sp4: After the reaction is completed, the material flows into the first cooling kettle, and the temperature is lowered by controlling the cooling medium introduced into the interlayer;

[0022] Sp5: The cooled material flows into the second cooling kettle for secondary cooling;

[0023] Sp6: After the cooled material is filtered through the plate and frame filter, the filtrate flows into the storage tank for storage. During the entire production process, the material status and production status are observed through the sight glasses between the equipment.

[0024] Beneficial Effects

[0025] The present invention provides a continuous production device for antimony mercaptide, which has the following beneficial effects:

[0026] The primary benefit of the continuous production equipment and process of antimony mercaptides of the present invention is the substantial improvement of product quality. Through the refined control means shown in Examples 3 and 4, in the mixing kettle feeding link, with the help of the coordinated work of pressure sensors, raw material component spectrometers and micro-image recognition sensors, the PID control algorithm and the multivariate linear regression algorithm are used to achieve the precise stability of the raw material feeding pressure and the ultra-precise proportioning feeding. This ensures the uniformity and accuracy of the reaction materials from the source, and greatly reduces the product quality fluctuations caused by raw material differences. In the reactor stage, whether it is the intelligent stable control of the vacuum degree or the intelligent temperature control based on the neural network algorithm, it ensures that the reaction conditions can be maintained in an ideal state at every moment, effectively avoiding the adverse effects of temperature mutations, vacuum instability and other factors on the reaction process and product quality. In the cooling stage, precise flow metering, intelligent refrigeration power adjustment and temperature uniformity control are used to make the product cooling process smooth and uniform, further improving the stability of the product's physical and chemical properties, such as higher purity, more uniform and lasting color, and greater stability. This makes the product more competitive in the market and can better meet the stringent requirements of various high-end application scenarios for product quality consistency and stability.

[0027] The continuous production equipment in the present invention is effective in reducing production costs. From the perspective of labor costs, traditional intermittent production requires a lot of manual operation and monitoring for each batch, and the manpower investment is huge. The present invention greatly reduces the dependence on on-site operators through automated and intelligent production process design, such as automated connection between various devices, automatic adjustment of production parameters by intelligent algorithms, and remote monitoring operations in the central control room. During the entire production process, except for the necessary equipment maintenance and inspection personnel, most operations can be completed by the intelligent control system, thereby greatly reducing labor cost expenditures. At the same time, due to the improved stability of product quality and the reduction of batch differences, material waste caused by unqualified products is reduced, and the utilization rate of raw materials is improved.

[0028] 3. In terms of safety, compared with intermittent production, the continuous production equipment of the present invention reduces manual on-site intervention and reduces the risk of safety accidents caused by human operating errors. For example, in the process of adding raw materials, the precise automatic feeding system avoids the risk of leakage caused by manual handling and adding raw materials; in the reaction process, the intelligent pressure, temperature and vacuum control can effectively prevent dangerous situations such as excessive pressure and explosion caused by uncontrolled reaction conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is the overall structure diagram of the present invention;

[0030] Figure 2 It is the structural diagram of the mixing kettle of the present invention;

[0031] Figure 3 It is a structural diagram of the first reaction kettle and the second reaction kettle of the present invention;

[0032] Figure 4 It is a structural diagram of the first cooling kettle and the second cooling kettle of the present invention;

[0033] Figure 5 A flow chart is generated for the continuation of the present invention.

[0034] Among them: 1. Feeder; 2. Mixing kettle; 21. Feed inlet; 211. Regulating valve; 212. Flow meter; 22. Connecting pipe; 23. Feeder interface; 24. Stirring motor; 25. Stirring shaft; 3. First reactor; 31. Temperature control device; 311. Temperature control medium inlet; 312. Temperature control medium outlet; 313. Inlet regulating valve; 314. Outlet regulating valve; 32. Vacuum device; 321. Vacuum gauge; 322. Vacuum regulating valve; 33. Temperature sensor; 4. Second reactor; 5. First cooling kettle; 6. Second cooling kettle; 7. Plate and frame filter; 8. Storage tank; 9. Sight glass. DETAILED DESCRIPTION

[0035] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Specific embodiment one:

[0037] like Figure 1-5As shown, a continuous production equipment of antimony mercaptide comprises a feeder 1, a mixing kettle 2 is installed on one side of the feeder 1, a first reactor 3 is placed on one side of the mixing kettle 2, a second reactor 4 is placed on one side of the first reactor 3, a first cooling kettle 5 is placed on one side of the second reactor 4, a second cooling kettle 6 is placed on one side of the first cooling kettle 5, a plate-frame filter 7 is placed on one side of the second cooling kettle 6, a storage tank 8 is placed on one side of the plate-frame filter 7, a sight glass 9 is installed between the feeder 1, the mixing kettle 2, the first reactor 3, the second reactor 4, the first cooling kettle 5, the second cooling kettle 6, the plate-frame filter 7 and the storage tank 8, and a top side of the mixing kettle 2 is provided with a A feeder interface 23, a connecting pipe 22 is installed between the feeder interface 23 and the feeder 1, a stirring motor 24 is installed in the middle of the top of the mixing kettle 2, the first reactor 3, the second reactor 4, the first cooling kettle 5 and the second cooling kettle 6, the bottom end of the stirring motor 24 is transmission-connected with a stirring shaft 25, a feed port 21 is provided on the other side of the top of the mixing kettle 2, there are two groups of feed ports 21 on the other side of the top of the mixing kettle 2, a regulating valve 211 is installed on the top of the feed port 21, a flow meter 212 is installed on the bottom of the feed port 21, and a temperature sensor 33 is installed on one side of the top of the first reactor 3, the second reactor 4, the first cooling kettle 5 and the second cooling kettle 6.

[0038] A vacuum gauge 321 is installed on one side of the top of the first reactor 3 and the second reactor 4 near the temperature sensor 33 , a vacuum device 32 is installed on the other side of the top of the first reactor 3 and the second reactor 4 , and a vacuum regulating valve 322 is installed in the middle of the vacuum device 32 .

[0039] A temperature control medium inlet 311 is installed on the top of the outer side of the first reactor 3, the second reactor 4, the first cooling kettle 5 and the second cooling kettle 6, and an inlet regulating valve 313 is installed in the middle of the temperature control medium inlet 311. A temperature control device 31 is installed on the bottom of the outer side of the first reactor 3, the second reactor 4, the first cooling kettle 5 and the second cooling kettle 6, which includes a temperature control medium outlet 312, and an outlet regulating valve 314 is installed in the middle of the temperature control medium outlet 312.

[0040] The outlet of the feeder 1 is connected to the mixing kettle 2, and the feed is directly fed into the mixing kettle 2 through the feeder 1. The mixing kettle 2, the first reactor 3, the second reactor 4, the first cooling kettle 5 and the second cooling kettle 6 are connected in sequence through an overflow pipe. The cooling kettle 6 is connected to the feed port 21 of the plate and frame filter 7, and the outlet of the plate and frame filter 7 is connected to the storage tank 8. The first reactor 3 and the second reactor 4 are sandwich reactors, and the medium is passed into the interlayer for heating. The first reactor 3 and the second reactor 4 are both provided with vacuum pipelines. The first cooling kettle 5 and the second cooling kettle 6 are sandwich reactors, and the medium is passed into the interlayer for cooling.

[0041] The process flow of the overall continuous production equipment is:

[0042] Sp1: First, the raw materials are transported to the mixing kettle 2 through the connecting pipe 22 by the feeder 1, and the feeding amount of other raw materials is accurately controlled by the regulating valve 211 and the flow meter 212 at the feed inlet 21, and the stirring shaft 25 is driven by the stirring motor 24 to stir and mix in the mixing kettle 2;

[0043] Sp2: The mixed materials flow into the first reactor 3 through the overflow pipe, and the first reactor 3 is evacuated by the vacuum device 32 and the vacuum regulating valve 322. The temperature of the medium in the interlayer is controlled by the temperature control medium inlet 311, the inlet regulating valve 313, the temperature control medium outlet 312 and the outlet regulating valve 314 to adjust the reaction temperature, so that the materials react in the first reactor 3;

[0044] Sp3: The reacted material flows into the second reactor 4 through the overflow pipe, and the vacuum and temperature control operations in the first reactor 3 are repeated for further reaction;

[0045] Sp4: After the reaction is completed, the material flows into the first cooling kettle 5, and the temperature is reduced by controlling the cooling medium introduced into the interlayer;

[0046] Sp5: The cooled material flows into the second cooling kettle 6 for secondary cooling;

[0047] Sp6: After the cooled material is filtered by the plate and frame filter 7, the filtrate flows into the storage tank 8 for storage. During the entire production process, the material state and production status are observed through the sight glass 9 between each equipment. Specific embodiment 2:

[0049] like Figure 1-5 As shown, the continuous production equipment of antimony mercaptides in the present invention mainly includes a feeder 1, a mixing kettle 2, two reactors, two cooling kettles, a plate and frame filter 7 and a storage tank 8. The discharge port of the feeder 1 is connected to the feed port 21 of the first reactor 3, the mixing kettle 2, the two reactors and the two cooling kettles are connected in sequence through an overflow pipeline, and the last cooling kettle is connected to the feed port 21 of the plate and frame filter 7. The finished antimony mercaptides obtained after the plate and frame filter 7 enters the storage tank 8.

[0050] A regulating valve 211 is installed on a feed port 21 on the mixing kettle 2, and a regulating valve 211 and a flow meter 212 are installed on the feed port 21. The two reactors are sandwich reactors, and steam, heat transfer oil and other media can be introduced to heat the materials in the reactors. There are vacuum pipelines on both reactors. The two cooling kettles are sandwich reactors, and cold water, liquid nitrogen and other media can be introduced into the interlayer to cool the materials in the kettles. The plate and frame filter 7 is used to filter the antimony mercaptan material, and the storage tank 8 is used to store the antimony mercaptan material. The feeder 1 is connected to the mixing kettle 2 and all overflow pipes, including the plate and frame filter 7 and the cooling kettle and the storage tank 8. The pipeline is equipped with a sight glass 9 for observing the material situation. The mixing kettle 2, the two reactors and the two cooling kettles are equipped with motors connected to the kettle for stirring, driving the stirring to mix the materials.

[0051] The invention discloses a continuous production equipment for antimony thiolate. Antimony trioxide and mercapto ester are uniformly mixed in a mixing kettle 2 according to a proportion, and a catalyst is added dropwise at the same time. Then the mixed materials overflow into a first reactor for temperature reaction, and the temperature is controlled at 60-70°C. At the same time, vacuum is started, and the vacuum pressure is -0.08--0.09MPa. Then the materials overflow into a second reactor for temperature reaction, and the temperature is controlled at 90-120°C. Since the vacuum pipeline is connected in parallel with the first reactor, the vacuum pressure in the reactor is -0.085--0.095MPa. Then the materials overflow into a first cooling kettle for cooling, and the temperature is controlled at 70-90°C. Then the materials overflow into a second cooling kettle for cooling, and the temperature is controlled at 30-50°C. A crude antimony thiolate product is obtained. The crude product is filtered in a plate-frame filter 7 to obtain an antimony thiolate finished product, which is then filtered in a storage tank 8.

[0052] The automatic and continuous production of the present invention reduces the frequent manual operation in intermittent production, reduces the occurrence of misoperation, reduces the waste of materials, and also reduces the number of operators on site, saving labor costs. The final product has small performance differences and high stability. Therefore, it is more suitable for large-scale industrial production and more conducive to market competition.

[0053] The flow meter 212 and the regulating valve 211 control the feed, and the plate and frame filter 7 filters the coarse product. Specific embodiment three:

[0055] like Figure 1-5As shown, in-depth intelligent control is achieved in the feed control of the mixing kettle 2. In addition to installing the regulating valve 211 and the flowmeter 212 at the feed port 21, a pressure sensor, a raw material component spectrometer and a micro-image recognition sensor are added. The feed pressure is monitored in real time by the pressure sensor. Once the pressure deviates from the preset stable interval, the control system immediately starts the PID control algorithm according to the pressure deviation to adjust the opening of the regulating valve 211. The specific process is that the control system first calculates the deviation between the pressure setting value and the current pressure measurement value, multiplies the deviation by the proportional coefficient to obtain the proportional term adjustment amount, and at the same time, the deviation is integrated and multiplied by the integral coefficient to obtain the integral term adjustment amount. The role of the integral term is to eliminate the steady-state error of the system. Even if the pressure deviation persists for a period of time, the integral term can gradually accumulate the adjustment amount to make the pressure return to the set value. In addition, the rate of change of the pressure deviation is differentiated and multiplied by the differential coefficient to obtain the differential term adjustment amount. The differential term can be adjusted in advance according to the speed of the pressure change. For example, when the pressure rises or falls rapidly, the differential term can quickly give a large adjustment amount to suppress the sudden change of pressure. The final opening adjustment of the regulating valve 211 is determined by comprehensively adjusting the proportional term, the integral term and the differential term, thereby ensuring the stability of the feed pressure and guaranteeing high-precision control of the feed amount.

[0056] The raw material component spectrometer can emit a multi-band spectrum to perform a fast, non-destructive and accurate component analysis of the raw materials entering the mixing kettle 2, and transmit the spectral data to the central control system. The micro-image recognition sensor identifies and analyzes the appearance characteristics of the raw materials such as particle morphology and color, such as judging the uniformity of the particles, whether there is agglomeration phenomenon, etc., and converts the image data into characteristic parameters and transmits them to the control system. Based on these multi-dimensional data information, the control system uses a multivariate linear regression algorithm combined with a preset raw material ratio model to accurately calculate the optimal opening adjustment value of the regulating valve 211, so as to achieve ultra-precise proportioning of raw materials. The implementation steps of the multivariate linear regression algorithm are as follows: First, a large amount of historical feeding data is collected, including spectral analysis data, image feature parameters and corresponding optimal opening data of the regulating valve, as a training data set, and then, using the principle of least squares method, the regression coefficient is continuously adjusted so that the sum of squares of the error between the predicted regulating valve opening value calculated according to the independent variables (spectral analysis data, image feature parameters, etc.) in the training data set and the actual optimal opening value is minimized. After sufficient training, the final regression coefficient is determined. In the actual feeding process, the opening adjustment value of the regulating valve 211 is calculated through the constructed multivariate linear regression model based on the new spectral analysis data and image feature parameters, thereby achieving precise feeding control.

[0057] At the same time, during the stirring process of the mixing kettle 2, the stirring motor 24 adopts vector frequency conversion speed control and combines with intelligent stirring algorithm. According to different raw material ratios and mixing stages, as well as the material mixing uniformity information fed back by the sensor, the speed of the stirring motor 24 is accurately adjusted. For example, a lower speed is used in the initial mixing stage to prevent local uneven reactions caused by splashing of raw materials and excessive mixing; in the middle of mixing, the speed is automatically adjusted according to the viscosity change of the material to ensure that the material can be fully stirred under different viscosity conditions; in the later stage of mixing, the speed is appropriately increased to ensure that the raw materials are fully and evenly mixed. In addition, the stirring shaft 25 adopts a special propeller blade design, and the surface of the blade is coated with anti-corrosion and wear-resistant coatings to improve the stirring efficiency and equipment life.

[0058] In the reactor stage, the vacuum device 32 is optimized. In addition to the vacuum regulating valve 322, an automatic vacuum compensation system and an intelligent vacuum monitoring module are added. When the vacuum drops due to material volatilization or other reasons during the reaction, the intelligent vacuum monitoring module quickly detects the change and transmits the signal to the automatic vacuum compensation system. The system automatically starts to replenish the vacuum, so that the reaction is always carried out in a stable vacuum environment, improving the consistency of the reaction and product quality. In addition, a microwave heating auxiliary device is installed inside the reactor. On the basis of conventional interlayer heating, microwave heating can be started in time according to the reaction requirements, so that the material molecules can vibrate rapidly to generate heat and accelerate the reaction process. It is especially suitable for some special raw material combinations that require rapid heating to initiate the reaction, and the power and time of microwave heating can be precisely controlled to further improve the refinement of the reaction. Specific embodiment four:

[0060] like Figure 1-5 As shown: All-round refinement and innovation are carried out in the temperature control link. High-precision temperature probes and flow sensors are installed respectively for the temperature control medium inlet 311 and the temperature control medium outlet 312 of the first reactor 3 and the second reactor 4 to monitor the temperature change and flow data of the inlet and outlet media in real time.

[0061] According to these data, an intelligent temperature control algorithm based on artificial intelligence is used to coordinately control the inlet regulating valve 313 and the outlet regulating valve 314. The intelligent temperature control algorithm is constructed based on a neural network algorithm. First, a large amount of temperature and flow data during the operation of the reactor and the corresponding regulating valve opening control data are collected as training samples. The input layer of the neural network contains the temperature and flow data collected by the temperature probe and the flow sensor. The middle layer extracts features and performs complex nonlinear mapping processing on the data through multiple neurons, and the output layer gives the opening adjustment suggestions of the inlet regulating valve 313 and the outlet regulating valve 314. During the training process, the weights and thresholds of the neural network are continuously adjusted through the back propagation algorithm, so that the regulating valve opening adjustment suggestions output by the network can make the temperature in the reactor quickly and accurately reach the set value and remain stable during the reaction process. During the heating process, not only can the temperature in the reactor be accurately controlled within the set range, but the heating rate can also be dynamically adjusted according to the reaction process to avoid the influence of temperature mutation on the reaction. At the same time, the temperature distribution sensor network inside the reactor is used to monitor the temperature differences at different locations in the reactor in real time. By adjusting the inlet and outlet flow rates and temperature of the temperature control medium, the temperature uniformity in the reactor is controlled, reducing product quality fluctuations caused by local temperature differences.

[0062] In terms of the cooling kettle, the interlayer cooling medium flow of the first cooling kettle 5 and the second cooling kettle 6 is accurately measured by an electromagnetic flowmeter, and is linked to the cooling medium inlet regulating valve for control. According to the cooling requirements, the flow of the cooling medium is accurately adjusted to achieve more accurate temperature gradient cooling. In addition, the cooling medium adopts a circulating refrigeration system, which is equipped with an efficient heat exchanger and an intelligent refrigeration power adjustment module. During the cooling process, the heat exchanger can quickly transfer the heat of the material in the cooling kettle to the cooling medium, and the intelligent refrigeration power adjustment module dynamically adjusts the refrigeration power according to the temperature change of the cooling medium and the cooling requirements of the material. The specific algorithm is as follows: first, the target temperature curve for material cooling is set, and the intelligent refrigeration power adjustment module monitors the current temperature of the cooling medium in real time, and compares it with the target temperature curve to calculate the temperature deviation. Then, according to the size and change trend of the temperature deviation, the fuzzy control algorithm is used to determine the adjustment range of the refrigeration power. The fuzzy control algorithm establishes a fuzzy rule table by defining fuzzy sets of temperature deviation and deviation change rate. For example, when the temperature deviation is large and the deviation change rate is fast, a larger refrigeration power adjustment amount is output; when the temperature deviation is small and the deviation change rate is slow, a smaller refrigeration power adjustment amount is output. In this way, energy-saving and efficient cooling operation is achieved. In addition, a turbulent device is installed in the cooling kettle to improve the heat exchange efficiency and further accelerate the cooling speed by changing the flow pattern of the cooling medium.

[0063] A pre-filtering device is added before the plate-and-frame filter 7, which uses multiple layers of filter screens with different apertures and an electrostatic adsorption unit. The cooled antimony mercaptan crude product is first preliminarily filtered to remove larger particle impurities. The electrostatic adsorption unit can adsorb some tiny charged impurity particles, reduce the workload of the plate-and-frame filter 7, extend its service life, and improve the filtration efficiency and product purity. During the entire production process, the viewing mirror 9 between each device is connected to a high-definition camera, and the camera data is transmitted to the central control system. The operator can clearly observe the material status remotely in the central control room, realize remote monitoring and operation, further reduce manual on-site intervention, and improve the automation and refinement level of production. Specific embodiment five:

[0065] like Figure 1-5 As shown: The core formula of the algorithm used in the above embodiment is as follows:

[0066] 1. PID control algorithm:

[0067] formula:

[0068] Where u(t): control output of the regulating valve, i.e., a signal for adjusting the opening of the regulating valve 211; K P : Proportional coefficient, which determines the response degree of the proportional term to the deviation, and its size affects the response speed and stability of the system; e(t): The deviation between the pressure setting value and the actual measured value, e(t) = P set -P actual (t), where P set is the preset pressure value, P actual (t) is the actual pressure value measured at time t.

[0069] K I : Integral coefficient. The integral term is used to eliminate the steady-state error of the system. By integrating the deviation, even if the deviation is small but persists, the adjustment amount can be gradually accumulated to return the pressure to the set value.

[0070] K D : Differential coefficient, the differential term is adjusted in advance according to the speed of pressure change. Indicates the rate of change of pressure deviation. When the pressure changes rapidly, the differential term can quickly give a larger adjustment amount to suppress the sudden change of pressure.

[0071] 2. Multiple Linear Regression Algorithm:

[0072] Formula: y=β0+β1x1+β2x2+…+β n x n +∈

[0073] y: regulating valve opening adjustment value, that is, the opening adjustment amount of the regulating valve 211; β0, β1, ..., βn : Regression coefficient, determined by training data; β0 is a constant term, β1 to β n The weight coefficients corresponding to different independent variables (such as spectral analysis data, image characteristic parameters, etc.) reflect the influence of the independent variable on the opening of the regulating valve.

[0074] x1,x2,…,x n : Independent variables, including spectral analysis data and image feature parameters. For example, x1 can be the spectral intensity value of a specific frequency band of the raw material component spectrometer, and x2 can be the average particle size detected by the micro image recognition sensor.

[0075] ∈: Random error term, used to represent the error caused by some unpredictable factors in actual situations. During the training process, the principle of least squares is used to make minimum, where m is the number of training data, y i is the actual control valve opening value in the i-th training data, It is the predicted control valve opening value in the i-th training data calculated by the regression model. By continuously adjusting β0, β1, …, β n to achieve this goal.

[0076] 3. Neural network algorithm (for intelligent temperature control):

[0077] Neural network structure:

[0078] Input layer: Contains the temperature collected by the temperature probe and flow sensor (set as T in and T out Respectively represent the inlet and outlet temperatures of the temperature control medium, F in and F out Indicates data such as the inlet and outlet flow of the temperature control medium).

[0079] Middle layer: Multiple neurons, which extract features and perform nonlinear mapping on input data through complex connections and activation functions (such as Sigmoid function, ReLU function, etc.). The connection weights between specific neurons (set as w ij represents the connection weight b from the i-th input neuron to the j-th intermediate neuron j represents the bias of the j-th interneuron) is determined during the training process.

[0080] Output layer: Give the inlet regulating valve 313 (set as V in ) and outlet regulating valve 314 (set to V out ) opening adjustment suggestions.

[0081] Back propagation algorithm during training:

[0082] Calculate the loss function: Use mean square error (MSE) as the loss function, the formula is:

[0083]

[0084] Where q is the number of training samples, V in, and V out, is the inlet and outlet control valve opening adjustment suggestion output by the neural network in the kth training sample, and is the actual optimal inlet and outlet control valve opening value corresponding to the kth training sample.

[0085] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the statement "comprising a reference structure" do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0086] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A continuous production device for antimony mercaptide, comprising a feeder (1), characterized in that: A mixing kettle (2) is installed on one side of the feeder (1), a first reactor (3) is placed on one side of the mixing kettle (2), a second reactor (4) is placed on one side of the first reactor (3), a first cooling kettle (5) is placed on one side of the second reactor (4), a second cooling kettle (6) is placed on one side of the first cooling kettle (5), a plate and frame filter (7) is placed on one side of the second cooling kettle (6), and a storage tank (8) is placed on one side of the plate and frame filter (7).

2. The continuous production equipment of antimony mercaptide according to claim 1, characterized in that: Sight glasses (9) are installed between the feeder (1), the mixing kettle (2), the first reaction kettle (3), the second reaction kettle (4), the first cooling kettle (5), the second cooling kettle (6), the plate and frame filter (7) and the storage tank (8).

3. The continuous production equipment of antimony mercaptide according to claim 2, characterized in that: A feeder interface (23) is provided on one side of the top of the mixing kettle (2), a connecting pipe (22) is installed between the feeder interface (23) and the feeder (1), a stirring motor (24) is installed in the middle of the top of the mixing kettle (2), the first reaction kettle (3), the second reaction kettle (4), the first cooling kettle (5) and the second cooling kettle (6), and the bottom end of the stirring motor (24) is drivingly connected to a stirring shaft (25).

4. The continuous production equipment of antimony mercaptide according to claim 3, characterized in that: A feed port (21) is provided on the other side of the top of the mixing kettle (2), and there are two groups of feed ports (21) on the other side of the top of the mixing kettle (2). A regulating valve (211) is installed at the top of the feed port (21), and a flow meter (212) is installed at the bottom of the feed port (21).

5. The continuous production equipment of antimony mercaptide according to claim 4, characterized in that: A temperature sensor (33) is installed on one side of the top of the first reaction kettle (3), the second reaction kettle (4), the first cooling kettle (5) and the second cooling kettle (6).

6. The continuous production equipment of antimony mercaptide according to claim 5, characterized in that: A vacuum gauge (321) is installed on one side of the top of the first reaction kettle (3) and the second reaction kettle (4) close to the temperature sensor (33), a vacuum device (32) is installed on the other side of the top of the first reaction kettle (3) and the second reaction kettle (4), and a vacuum regulating valve (322) is installed in the middle of the vacuum device (32).

7. The continuous production equipment of antimony mercaptide according to claim 6, characterized in that: A temperature control medium inlet (311) is installed at the top of the outer side of the first reaction kettle (3), the second reaction kettle (4), the first cooling kettle (5) and the second cooling kettle (6), and an inlet regulating valve (313) is installed in the middle of the temperature control medium inlet (311). A temperature control device (31) is installed at the bottom of the outer side of the first reaction kettle (3), the second reaction kettle (4), the first cooling kettle (5) and the second cooling kettle (6), and a temperature control medium outlet (312) is included in the temperature control device (31), and an outlet regulating valve (314) is installed in the middle of the temperature control medium outlet (312).

8. The continuous production equipment of antimony mercaptide according to claim 7, characterized in that: The outlet of the feeder (1) is connected to the mixing kettle (2), and the feed is directly fed into the mixing kettle (2) through the feeder (1). The mixing kettle (2), the first reactor (3), the second reactor (4), the first cooling kettle (5) and the second cooling kettle (6) are connected in sequence through an overflow pipe. The second cooling kettle (6) is connected to the feed port (21) of the plate and frame filter (7). The outlet of the plate and frame filter (7) is connected to the storage tank (8). The first reactor (3) and the second reactor (4) are sandwich reactors, and a medium is passed into the sandwich for heating. The first reactor (3) and the second reactor (4) are both provided with vacuum lines. The first cooling kettle (5) and the second cooling kettle (6) are sandwich reactors, and a medium is passed into the sandwich for cooling.

9. The continuous production equipment of antimony mercaptide according to claim 8, characterized in that: The process flow of the overall continuous production equipment is as follows: Sp1: First, the raw materials are transported to the mixing kettle (2) through the connecting pipe (22) by the feeder (1), and the feed amount of other raw materials is accurately controlled by the regulating valve (211) and the flow meter (212) at the feed inlet (21), and the stirring shaft (25) is driven by the stirring motor (24) to stir and mix in the mixing kettle (2); Sp2: The mixed materials flow into the first reaction kettle (3) through the overflow pipe, and the first reaction kettle (3) is evacuated through the vacuum device (32) and the vacuum regulating valve (322), and the temperature of the medium in the interlayer is controlled by the temperature control medium inlet (311), the inlet regulating valve (313), the temperature control medium outlet (312) and the outlet regulating valve (314) to adjust the reaction temperature, so that the materials react in the first reaction kettle (3); Sp3: The reacted material flows into the second reactor (4) through the overflow pipe, and the vacuum and temperature control operations in the first reactor (3) are repeated for further reaction; Sp4: After the reaction is completed, the material flows into the first cooling kettle (5), and the temperature is reduced by controlling the cooling medium introduced into the interlayer; Sp5: The cooled material flows into the second cooling kettle (6) for secondary cooling; Sp6: After the cooled material is filtered by the plate and frame filter (7), the filtrate flows into the storage tank (8) for storage. During the entire production process, the material state and production status are observed through the sight glass (9) between each device.

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