Reaction device for continuously producing thiothiazole intermediate and use method of reaction device

Abstract

The invention relates to the technical field of production of thiothiazole intermediates, in particular to a reaction device for continuously producing thiothiazole intermediates and a using method of the reaction device, and the reaction device is characterized by comprising a liquid-liquid reaction module which comprises a plurality of tubular reactors; the raw material conveying module is used for conveying reaction raw materials to the corresponding tubular reactors; the feeding control module is used for controlling the feeding sequence and feeding parameters of the reaction raw materials; the detection module is used for detecting the in-tube temperature and the in-tube air pressure of each tubular reactor and the in-tube liquid phase image of each tubular reactor; the data analysis module is used for determining the reaction degree of each tubular reactor and judging whether to adjust the feeding sequence and / or feeding parameters of the reaction raw materials; and the temperature adjusting module is used for determining a temperature adjusting mode of each tubular reactor. The continuous production of the thiothiazole intermediate 3-chloro-4-oxo-1-pentanol and the ammonium dithiocarbamate aqueous solution can be realized, and the production efficiency of the thiothiazole intermediate is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of the production of thiazole intermediates, and particularly relates to a reaction device for continuously producing thiazole intermediates and a method for using the same. Background Art

[0002] 4-Methyl-5-hydroxyethylthiazole, also known as thiazole, is a colorless or yellow viscous liquid, non-volatile, non-flammable and non-explosive, non-corrosive, non-toxic, soluble in organic solvents such as ethanol, ether, benzene, chloroform, etc., and has a relatively large solubility in water, and can form a hydrochloride salt soluble in water or alcohol with hydrogen chloride. It has an unpleasant odor of thiazole compounds, but has a pleasant fragrance at extremely dilute concentrations. It is the basic structural ring that composes vitamin VB1. At the same time, 4-methyl-5-hydroxyethylthiazole is also an edible flavor. It has nutty, milky, and meaty aromas. Therefore, it is used in nutty, milky meat, bread, dairy products, and seasoning flavors, and is approved as a temporarily permitted food flavor by China's GB2706-1996. At the same time, it is also a common synthetic intermediate in the pharmaceutical industry and can also be used as an N-heterocyclic carbene catalyst to catalyze a series of organic chemical reactions.

[0003] The current domestic technical route for producing 4-methyl-5-hydroxyethylthiazole is as follows: α-acetyl-γ-butyrolactone is chlorinated to obtain α-acetyl-α-chloro-γ-butyrolactone, which is then hydrolyzed to obtain 3-chloro-4-oxo-1-pentanol. Carbon disulfide and ammonia are ammoniated to obtain ammonium dithiocarbamate. 3-chloro-4-oxo-1-pentanol and ammonium dithiocarbamate are condensed to obtain 2-mercapto-4-methyl-5-(β-hydroxyethyl)-thiazole. 2-mercapto-4-methyl-5-(β-hydroxyethyl)-thiazole is oxidized to obtain 4-methyl-5-hydroxyethylthiazole, and finally, through desolvation, rectification, etc., the finished product of 4-methyl-5-hydroxyethylthiazole is obtained. This technical route involves multiple steps and the process is relatively complex. In the current technical production, it is produced step by step intermittently, and each batch needs to go through multiple steps such as feeding, reaction, discharging, equipment cleaning, and preparation, resulting in relatively low production efficiency. Summary of the Invention

[0004] Therefore, the present invention provides a reaction device for continuously producing thiazole intermediates and a method for using the same to overcome the problem of relatively low production efficiency in the prior art.

[0005] To achieve the above object, on the one hand, the present invention provides a reaction device for continuously producing thiazole intermediates, including:

[0006] A liquid-liquid reaction module, which includes a plurality of tubular reactors for providing a place for the reaction to occur;

[0007] A raw material transportation module, which is connected to the liquid-liquid reaction module and is used to transport reaction raw materials to the corresponding tubular reactors;

[0008] A feed control module, which is connected to the raw material transportation module and is used to control the feeding sequence and feeding parameters of the reaction raw materials. Among them, the feeding parameters include the feeding speed and the feeding amount;

[0009] A detection module, which is connected to the liquid-liquid reaction module and is used to detect the temperature and air pressure inside the tubes of each tubular reactor and obtain the liquid-phase images inside each tubular reactor;

[0010] A data analysis module, which is respectively connected to the feed control module and the detection module and is used to determine the reaction degree of each tubular reactor based on the temperature change inside the tubes of each tubular reactor and the liquid-phase images, and determine whether to adjust the feeding sequence and / or feeding parameters of the reaction raw materials;

[0011] A temperature adjustment module, which is respectively connected to the liquid-liquid reaction module, the detection module and the data analysis module and is used to determine the temperature adjustment method for each tubular reactor based on the reaction degree of each tubular reactor. The temperature adjustment method includes a heating mode and a cooling mode;

[0012] Among them, the heating amount and heating rate corresponding to the heating mode are determined based on the temperature and air pressure inside the tubes of each tubular reactor, and the cooling amount and cooling rate corresponding to the cooling mode are determined based on the temperature and air pressure inside the tubes of each tubular reactor.

[0013] Further, the data analysis module determines the distribution state of the organic phase and the aqueous phase inside the tubular reactor and the distribution of bubbles in the liquid based on the liquid-phase images inside each tubular reactor.

[0014] Further, the data analysis module determines the reaction degree of each tubular reactor based on the comparison result between the temperature change situation inside the tubes of each tubular reactor and the preset temperature change situation, the distribution state of the organic phase and the aqueous phase inside each tubular reactor, and the distribution of bubbles in the liquid.

[0015] Further, the data analysis module determines whether to adjust the feeding sequence and / or feeding parameters of the reaction raw materials based on the reaction degree of each tubular reactor;

[0016] Among them, if the reaction degree of the tubular reactor meets the corresponding preset standard, the feeding sequence and feeding parameters of the reaction raw materials corresponding to the tubular reactor are not adjusted;

[0017] If the reaction degree of the tubular reactor does not meet the corresponding preset standard, the feeding sequence / feeding parameters of the reaction raw materials corresponding to the tubular reactor are adjusted.

[0018] Further, based on the determination result of adjusting the feeding parameters of the reaction raw materials, the data analysis module determines the adjustment amount of the feeding speed according to the in-tube temperature of each tubular reactor, and determines the adjustment amount of the feeding quantity according to the in-tube air pressure of each tubular reactor; based on the determination result of adjusting the feeding sequence of the reaction raw materials, the data analysis module adjusts the feeding sequence of the reaction raw materials based on a preset feeding sequence table.

[0019] Further, the data analysis module determines the corresponding in-tube temperature change curve based on the in-tube temperature of each tubular reactor, determines the corresponding current theoretical temperature based on each in-tube temperature change curve, and determines the adjustment amount of the feeding speed based on the comparison result between the current theoretical temperature and the current in-tube temperature.

[0020] Further, the data analysis module determines the adjustment amount of the feeding quantity based on the comparison result between the in-tube air pressure change condition of each tubular reactor and the preset air pressure change condition.

[0021] Further, the temperature adjustment module determines adjustment parameters based on the in-tube temperature and the in-tube air pressure of each tubular reactor, determines the heating or cooling amount based on the adjustment parameters and the set temperature, and determines the heating or cooling rate based on the adjustment parameters and the set rate.

[0022] Further, the liquid-liquid reaction module further includes:

[0023] A pipeline mixer element mechanism, which is arranged inside each tubular reactor to make the materials in the tubular reactor mix evenly;

[0024] A heat exchange mechanism, which is arranged outside each tubular reactor and is connected to the temperature adjustment module to adjust the temperature in each tubular reactor based on the determined temperature adjustment method;

[0025] A heat preservation mechanism, which is arranged outside the heat exchange mechanism to form a heat preservation environment.

[0026] On the other hand, the present invention also provides a usage method, including:

[0027] The raw material conveying module conveys each reaction raw material to the corresponding tubular reactor and mixes them evenly;

[0028] The detection module detects the in-tube temperature and the in-tube air pressure of each tubular reactor in real time and obtains the liquid-phase image in each tubular reactor;

[0029] Determine the reaction degree of each tubular reactor based on the temperature change inside the tube of each tubular reactor and the liquid-phase image, and determine the temperature adjustment method of each tubular reactor based on the reaction degree of each tubular reactor, including the heating mode and the cooling mode;

[0030] Among them, determine the heating amount and heating rate corresponding to the heating mode based on the temperature inside the tube and the air pressure inside the tube of each tubular reactor, and determine the cooling amount and cooling rate corresponding to the cooling mode based on the temperature inside the tube and the air pressure inside the tube of each tubular reactor;

[0031] Determine whether to adjust the feeding order and / or feeding parameters of the reaction raw materials based on the reaction degree of each tubular reactor;

[0032] Among them, if it is determined to be adjusted, determine the adjustment amount of the feeding speed according to the temperature inside the tube of each said tubular reactor, determine the adjustment amount of the feeding amount according to the air pressure inside the tube of each tubular reactor, and adjust the feeding order of the reaction raw materials based on the preset feeding order table.

[0033] Compared with the prior art, the beneficial effects of the present invention are as follows. The liquid-liquid reaction module of the present invention provides a reaction occurrence place by setting multiple tubular reactors, realizes continuous and multi-stage reactions, improves production efficiency, and improves reaction controllability. By setting the raw material conveying module, accurate conveying of reaction raw materials can be realized, ensuring stable supply of reaction raw materials, avoiding errors in manual feeding, and improving reaction consistency. By setting the feeding control module, the feeding order and feeding parameters can be dynamically adjusted, avoiding incomplete reactions or increased side reactions caused by improper feeding, thereby improving the production efficiency and purity of the thiazole intermediate. By setting the detection module, the temperature, air pressure and liquid-phase image inside the tubular reactor can be monitored in real time, providing a data basis for subsequent analysis. By setting the data analysis module, the reaction process can be effectively evaluated and decision-making adjustments can be made to ensure the stability and continuity of the reaction. By setting the temperature adjustment module, rapid and accurate adjustment of the reaction temperature can be realized, ensuring that the reaction proceeds at a suitable temperature and improving production efficiency.

[0034] Furthermore, the data analysis module of the present invention determines the distribution state of the organic phase and the aqueous phase inside the tubular reactor and the bubble distribution in the liquid based on the liquid-phase image inside the tubular reactor, which can provide data support for the automatic control of the production process, thereby improving production efficiency.

[0035] Furthermore, the data analysis module of the present invention determines the reaction degree of each tubular reactor based on the comparison result of the temperature change inside the tube of each tubular reactor and the preset temperature change situation, the distribution state of the organic phase and the aqueous phase inside each tubular reactor, and the bubble distribution in the liquid. Determined by multi-dimensional data fusion, it can improve the judgment accuracy, avoid misjudgment, and thereby improve production efficiency.

[0036] Furthermore, the data analysis module of the present invention determines whether to adjust the feeding order and / or feeding parameters of the reaction raw materials based on the reaction degree of the tubular reactor, ensuring the stability of the reaction and improving production efficiency. By precisely controlling the feeding order and feeding parameters, raw material waste caused by incomplete or excessive reactions can be avoided, reducing production costs.

[0037] Furthermore, the temperature adjustment module of the present invention determines the adjustment parameters based on the temperature inside the tubes and the air pressure inside the tubes of each tubular reactor, and determines the temperature increase or decrease amount based on the adjustment parameters and the set temperature, and determines the heating rate or cooling rate based on the adjustment parameters and the set rate. It can precisely control the reaction temperature, save energy. At the same time, by dynamically adjusting the temperature, the temperature inside the tubular reactor can be ensured to be in the optimal reaction conditions, further improving production efficiency.

[0038] Furthermore, the present invention sets up a pipeline mixer element mechanism, which can fully mix the reaction raw materials in the tubular reactor, ensuring more uniform contact between the reactants, thereby improving production efficiency. By setting up a heat exchange mechanism, the temperature inside each tubular reactor can be flexibly adjusted based on the determined temperature adjustment method. By setting up a heat preservation mechanism, most of the temperature can be locked inside the tubular reactor, reducing resource waste. Description of the Drawings

[0039] Figure 1 is a schematic structural diagram of the reaction device for continuously producing thiazole intermediates according to an embodiment of the present invention;

[0040] Figure 2 is a structural block diagram of the reaction device for continuously producing thiazole intermediates according to an embodiment of the present invention;

[0041] Figure 3 is a production process diagram of the thiazole intermediate 3-chloro-4-oxo-1-pentanol according to an embodiment of the present invention;

[0042] Figure 4 is a production process diagram of the aqueous solution of ammonium dithiocarbamate, the thiazole intermediate according to an embodiment of the present invention;

[0043] Figure 5 is a schematic flow diagram of the usage method of the reaction device for continuously producing thiazole intermediates according to an embodiment of the present invention;

[0044] In the figure: 1, liquid-liquid reaction module; 11, tubular reactor; 2, raw material conveying module; 21, raw material storage tank; 22, conveying pipeline; 3, feed valve; 4, heat exchange mechanism; 5, heat preservation mechanism; 6, product storage mechanism. Detailed Embodiments

[0045] To make the objectives and advantages of the present invention more clearly understood, the present invention will be further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only for explaining the present invention and are not used to limit the present invention.

[0046] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. Those skilled in the art should understand that these embodiments are only used to explain the technical principles of the present invention and do not limit the protection scope of the present invention.

[0047] It should be noted that in the description of the present invention, the terms indicating directions or positional relationships such as "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings. This is only for convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present invention.

[0048] In addition, it should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "installation", "connection", and "connection" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0049] Please refer to Figure 1 - Figure 2 as shown in Figure 1 the structural schematic diagram of the reaction device for continuously producing thiazole intermediates according to the embodiment of the present invention; Figure 2 the structural block diagram of the reaction device for continuously producing thiazole intermediates according to the embodiment of the present invention; in the figure: liquid-liquid reaction module 1, tubular reactor 11, raw material conveying module 2, raw material storage tank 21, conveying pipeline 22, feed valve 3, heat exchange mechanism 4, heat preservation mechanism 5, product storage mechanism 6; Figure 1 Only one tubular reactor is taken as an example herein, and the technical solution of the present application is not limited. The number of tubular reactors can be set according to actual needs.

[0050] The present invention provides a reaction device for continuously producing thiazole intermediates, including:

[0051] A liquid-liquid reaction module 1, which includes a plurality of tubular reactors 1 for providing a place for the reaction to occur;

[0052] A raw material conveying module 2, which is connected to the liquid-liquid reaction module 1 for conveying reaction raw materials to the corresponding tubular reactor 1;

[0053] Specifically, the raw material conveying module 2 includes a number of raw material storage tanks 21 and corresponding conveying pipelines 22. The conveying pipelines 22 are used to convey the reaction raw materials in the raw material storage tanks 21 to the corresponding tubular reactors 1.

[0054] The feeding control module is connected to the raw material conveying module 2 and is used to control the feeding sequence and feeding parameters of the reaction raw materials. Among them, the feeding parameters include the feeding speed and the feeding amount.

[0055] In implementation, the reaction device is provided with feeding valves 3 on each conveying pipeline 22. The feeding control module controls the feeding sequence and feeding parameters of the reaction raw materials by controlling the opening degree of the feeding valves 3.

[0056] The detection module is connected to the liquid-liquid reaction module 1 and is used to detect the temperature and air pressure inside the tubes of each tubular reactor 1 and obtain the liquid phase images inside each tubular reactor.

[0057] It should be noted that those skilled in the art know that any equipment and method in the prior art that can obtain the temperature, air pressure inside the tubes and liquid phase images of each tubular reactor fall within the protection scope of the present invention and will not be elaborated here.

[0058] In implementation, the detection module includes a number of temperature detection components, a number of air pressure detection components and a number of liquid phase image acquisition components. Each temperature detection component includes a number of heat-resistant temperature sensors. Each air pressure detection component includes a number of air pressure sensors. Each liquid phase image acquisition component includes a liquid phase detection device, such as an intelligent sight glass.

[0059] The data analysis module is respectively connected to the feeding control module and the detection module and is used to determine the reaction degree of each tubular reactor based on the temperature change situation inside the tubes of each tubular reactor and the liquid phase images, and determine whether to adjust the feeding sequence and / or feeding parameters of the reaction raw materials.

[0060] Specifically, the data analysis module determines the distribution state of the organic phase and the aqueous phase inside the tubular reactor and the bubble distribution situation in the liquid based on the liquid phase images inside each tubular reactor.

[0061] In implementation, based on the liquid-phase images in each tubular reactor, distribution maps of the organic phase and the aqueous phase are drawn, and based on these distribution maps of the organic phase and the aqueous phase, the distribution area of the organic phase and the distribution area of the aqueous phase are determined respectively. The distribution area of the organic phase is compared with the preset distribution area of the organic phase to determine the first comparison value, and the distribution area of the aqueous phase is compared with the preset distribution area of the aqueous phase to determine the second comparison value. A comprehensive comparison value is determined according to the first comparison value and the second comparison value. For example, if the distribution area of the organic phase is FM, the preset distribution area of the organic phase is YJ, the distribution area of the aqueous phase is SM, and the preset distribution area of the aqueous phase is YX, then the first comparison value YB = FM / YJ, the second comparison value EB = SM / YX, and the comprehensive comparison value ZB = (YB + EB) / 2. Bubbles in the liquid-phase images in each tubular reactor are detected and identified based on algorithms such as image segmentation and edge detection. Bubbles in the liquid-phase image have brightness and unique shape features, and the bubble distribution in the liquid is obtained, including the number of bubbles and the bubble diameter. The bubble distribution in the liquid is compared with the preset bubble distribution to determine the bubble comparison value. For example: the number of bubbles QS in the liquid, the bubble diameter QZ, the preset number of bubbles YS, and the preset bubble diameter YZ, then the bubble comparison value QB = sqrt((QS - YS) 2 +(QZ - YZ) 2 ), where sqrt() is the preset square root determination function.

[0062] It can be understood that actual implementers can set the preset distribution area of the organic phase and the preset distribution area of the aqueous phase based on actual situations (such as the solubility of reaction raw materials and target products, reaction conditions, product yield, feed rate, etc.) or set the preset distribution area of the organic phase and the preset distribution area of the aqueous phase based on the distribution of the organic phase and the aqueous phase in the reaction process that passed the qualification test in historical data. Actual implementers can set the preset number of bubbles and the preset bubble diameter based on actual situations or the bubble distribution in the reaction process that passed the qualification test in historical data.

[0063] The data analysis module of the present invention determines the distribution states of the organic phase and the aqueous phase in the tubular reactor and the bubble distribution in the liquid based on the liquid-phase images in the tubular reactor, and can provide data support for the automatic control of the production process, thereby improving production efficiency.

[0064] Specifically, the data analysis module determines the reaction degree of each tubular reactor based on the comparison result of the in-tube temperature change situation of each tubular reactor and the preset temperature change situation, the distribution states of the organic phase and the aqueous phase in each tubular reactor, and the bubble distribution in the liquid.

[0065] The data analysis module of the present invention determines the reaction degree of each tubular reactor based on the comparison result between the in-tube temperature change of each tubular reactor and the preset temperature change, the distribution state of the organic phase and the aqueous phase in each tubular reactor, and the bubble distribution in the liquid. By performing multi-dimensional data fusion for determination, it can improve the judgment accuracy, avoid misjudgment, and thus improve the production efficiency.

[0066] Specifically, the data analysis module determines whether to adjust the feeding order and / or feeding parameters of the reaction raw materials based on the reaction degree of each tubular reactor.

[0067] Among them, if the reaction degree of the tubular reactor meets the corresponding preset standard, the feeding order and feeding parameters of the reaction raw materials corresponding to the tubular reactor are not adjusted.

[0068] If the reaction degree of the tubular reactor does not meet the corresponding preset standard, the feeding order / feeding parameters of the reaction raw materials corresponding to the tubular reactor are adjusted.

[0069] Please refer to Figure 3 and Figure 4 as shown, Figure 3 which is the production process diagram of 3-chloro-4-oxo-1-pentanol, an intermediate of ditazole, in an embodiment of the present invention; Figure 4 which is the production process diagram of ammonium dithiocarbamate aqueous solution, an intermediate of ditazole, in an embodiment of the present invention; In a specific embodiment, a hydrochloric acid solution, α-acetyl-α-chloro-γ-butyrolactone, and a catalyst are fed into the tubular reactor. α-acetyl-α-chloro-γ-butyrolactone will undergo a hydrolysis reaction to obtain 3-chloro-4-oxo-1-pentanol and carbon dioxide. The reaction is endothermic. Since α-acetyl-α-chloro-γ-butyrolactone is insoluble in water and 3-chloro-4-oxo-1-pentanol has a relatively high solubility, the distribution state of the organic phase and the aqueous phase in the tubular reactor changes. The gas generated by the reaction changes the bubble distribution in the reaction liquid. As the reaction gradually completes during the reaction process, the reaction raw materials decrease and the products increase. The bubble distribution in the tubular reactor tends to be average and stable, and the heat absorbed by the reaction per unit time also gradually decreases.

[0070] In another specific embodiment, dimethyl carbonate solvent, carbon disulfide, a catalyst (a mixture of organic base pyridine and inorganic base sodium hydroxide solution), and ammonia water are fed into a tubular reactor. Carbon disulfide undergoes an ammoniation reaction to obtain ammonium dithiocarbamate, which is soluble in water. The reaction is exothermic. Since carbon disulfide and dimethyl carbonate have low water solubility, as the reaction proceeds, the distribution state of the organic phase and the aqueous phase in the tubular reactor changes. The corresponding preset temperature change is that the temperature increases with a small increase amplitude. As the reaction gradually completes during the reaction process, the reaction raw materials decrease and the products increase, and the density of the reaction liquid in the tubular reactor tends to be stable, and the heat released per unit time by the reaction also gradually decreases.

[0071] It can be understood that the preset standards corresponding to the tubular reactor can be set as follows: the temperature change amplitude is less than the preset change amplitude, or the comprehensive comparison value is greater than the preset comprehensive comparison threshold, or the bubble comparison value is greater than the preset bubble comparison threshold. If the reaction degree of the tubular reactor meets this preset standard, the feeding order and feeding parameters of the reaction raw materials are not adjusted; if the temperature change amplitude is not less than the preset change amplitude, the comprehensive comparison value is not greater than the preset comprehensive comparison threshold, and the bubble comparison value is not greater than the preset bubble comparison threshold, then the reaction degree of this tubular reactor does not meet this preset standard, and the feeding order and feeding parameters of the reaction raw materials are adjusted. In practice, the chemical reactions corresponding to each tubular reactor are different, and the corresponding preset standards are different. The preset standards corresponding to each tubular reactor can be set according to the actual situation, and the feeding order / feeding parameters of the reaction raw materials of the corresponding tubular reactor can be adjusted according to the comparison results.

[0072] In practice, the actual implementers can set the preset change amplitude according to the actual situation or based on the average value of the temperature change amplitudes that passed the qualification test in the historical data. Preferably, the value range of the preset change amplitude is set to 5°C to 8°C; the actual implementers can set the preset comprehensive comparison threshold according to the actual situation or based on the average value of the comprehensive comparison thresholds that passed the qualification test in the historical data. The value range of the preset comprehensive comparison threshold is set to 0.8 to 0.9. The actual implementers can set the preset bubble comparison threshold according to the actual situation or based on the average value of the bubble comparison thresholds that passed the qualification test in the historical data. Preferably, the value range of the preset bubble comparison threshold is set to 0.8 to 0.9.

[0073] Specifically, based on the determination result of adjusting the feeding parameters of the reaction raw materials, the data analysis module determines the adjustment amount of the feeding speed according to the temperature inside the tubes of each tubular reactor, and determines the adjustment amount of the feeding quantity according to the internal pressure of the tubes of each tubular reactor; based on the determination result of adjusting the feeding order of the reaction raw materials, the data analysis module adjusts the feeding order of the reaction raw materials based on a preset feeding order table.

[0074] In implementation, the actual implementers can set a preset feed sequence table based on the reaction raw materials and reaction conditions of the actual reaction.

[0075] Specifically, the data analysis module determines the corresponding in-tube temperature change curve based on the in-tube temperature of each tubular reactor, determines the corresponding current theoretical temperature based on each in-tube temperature change curve, and determines the adjustment amount of the feed rate based on the comparison result between the current theoretical temperature and the current in-tube temperature.

[0076] In implementation, an in-tube temperature change curve is plotted based on the in-tube temperature in a preset time period before the detected current time point. The in-tube temperature change curve is input into the temperature prediction model to obtain the current theoretical temperature output by the temperature prediction model. The adjustment coefficient TX is determined according to the current theoretical temperature LT and the current in-tube temperature DT detected at the current time point. The adjustment amount TV of the feed rate is determined based on the adjustment coefficient TX and the current feed rate DV. Then TX = (DT - LT) / LT, TV = TX × DV, and the adjusted feed rate is determined according to the sum of the current feed rate and the adjustment amount of the feed rate. The actual implementers can set the preset time period based on the reaction rate in the actual reaction process. Preferably, the value range of the preset time period is set to 3 min to 5 min. It should be noted that those skilled in the art know that any prediction model capable of predicting temperature in the prior art falls within the protection scope of the present invention and will not be elaborated here.

[0077] Specifically, the data analysis module determines the adjustment amount of the feed quantity based on the comparison result between the in-tube air pressure change situation of each tubular reactor and the preset air pressure change situation.

[0078] In implementation, an in-tube air pressure change curve is plotted based on the in-tube air pressure detected in a preset time period. The adjustment ratio BL is determined according to the comparison result between the preset air pressure YQ corresponding to the moment of sudden change in in-tube air pressure (which can be determined according to the slope or turning point) and the in-tube air pressure FQ. BL = FQ / YQ. The adjusted feed quantity is determined according to the product of the adjustment ratio and the current feed quantity (respectively determine the current feed quantities of all reaction raw materials corresponding to the tubular reactors to be adjusted). The actual implementers can set the preset air pressure change situation based on the air pressure change situation in the reaction process that has passed the qualification test in the historical data.

[0079] The data analysis module of the present invention determines whether to adjust the feed sequence and / or feed parameters of the reaction raw materials based on the reaction degree of the tubular reactor, ensuring the stability of the reaction and improving the production efficiency. By precisely controlling the feed sequence and feed parameters, raw material waste caused by incomplete or excessive reactions can be avoided, and the production cost can be reduced.

[0080] A temperature adjustment module, which is respectively connected to the liquid-liquid reaction module 1, the detection module and the data analysis module, and is used to determine the temperature adjustment method for each tubular reactor based on the reaction degree of each tubular reactor. The temperature adjustment method includes a heating mode and a cooling mode;

[0081] Among them, the heating amount and heating rate corresponding to the heating mode are determined based on the temperature inside the tube and the pressure inside the tube of each tubular reactor, and the cooling amount and cooling rate corresponding to the cooling mode are determined based on the temperature inside the tube and the pressure inside the tube of each tubular reactor.

[0082] Specifically, the temperature adjustment module determines adjustment parameters based on the temperature inside the tube and the pressure inside the tube of each tubular reactor, determines the heating amount or cooling amount based on the adjustment parameters and the set temperature, and determines the heating rate or cooling rate based on the adjustment parameters and the set rate.

[0083] In implementation, if the reaction degree in each tubular reactor does not meet the preset standard, the temperature of each tubular reactor is adjusted, and the corresponding temperature adjustment method is determined according to the reaction degree. Among them, if the reaction in the tubular reactor is an endothermic reaction, the corresponding temperature adjustment method is determined to be the heating mode, and the temperature inside the tubular reactor is increased by heating to provide the heat energy required for the reaction and improve the reaction efficiency; if the reaction in the tubular reactor is an exothermic reaction, the corresponding temperature adjustment method is determined to be the cooling mode, and the temperature inside the tubular reactor is decreased by cooling to take away the excess heat energy of the reaction, improve the reaction efficiency, and avoid the occurrence of side reactions.

[0084] It can be understood that data fitting is performed based on the temperature data and pressure data during the reaction process in the corresponding tubular reactor in the historical data to construct a mathematical model between the adjustment parameters, the temperature inside the tube, and the pressure inside the tube, so as to obtain an adjustment parameter model. The temperature inside the tube and the pressure inside the tube of each detected tubular reactor are input into the adjustment parameter model to obtain the adjustment parameters output by the adjustment parameter model. The actual implementer can set the set temperature and set rate based on the temperature and temperature change rate during the reaction process that passed the qualification test in the historical data. Preferably, the value range of the set temperature is set to 30°C to 50°C, and the value range of the set rate is set to 10°C / min to 20°C / min.

[0085] It should be noted that those skilled in the art know that any model in the prior art that can fit the relationship between the adjustment parameters, the temperature inside the tube, and the pressure inside the tube, such as a linear regression model, a neural network model, etc., falls within the protection scope of the present invention and will not be elaborated here.

[0086] In implementation, the amount of temperature increase or decrease is determined based on the product of the adjustment parameter and the set temperature, and the rate of temperature increase or decrease is determined based on the product of the adjustment parameter and the set rate.

[0087] The temperature adjustment module of the present invention determines the adjustment parameter based on the temperature inside the tube and the air pressure inside the tube of each tubular reactor, and determines the amount of temperature increase or decrease based on the adjustment parameter and the set temperature, and determines the rate of temperature increase or decrease based on the adjustment parameter and the set rate. It can accurately control the reaction temperature, save energy. At the same time, by dynamically adjusting the temperature, it can ensure that the temperature inside the tubular reactor is in the optimal reaction conditions, further improving the production efficiency.

[0088] Please continue to refer to Figure 1 As shown, specifically, the liquid-liquid reaction module 1 further includes:

[0089] A pipeline mixer element mechanism, which is arranged inside each of the tubular reactors to make the materials inside the tubular reactors mix evenly;

[0090] In implementation, the specific structure of the pipeline mixer element mechanism is not limited as long as it can mix the materials inside the tubular reactor. It can be understood that by setting the pipeline mixer element mechanism in the present invention, the reaction raw materials inside the tubular reactor can be fully mixed, ensuring more uniform contact between the reactants, thereby improving the production efficiency.

[0091] A heat exchange mechanism 4, which is arranged outside each of the tubular reactors and is connected to the temperature adjustment module to adjust the temperature inside each of the tubular reactors based on the determined temperature adjustment method;

[0092] In implementation, the heat exchange mechanism 4 can achieve temperature reduction and increase, and is adjusted in real time based on the temperature adjustment method determined by the temperature adjustment module. For example, when the temperature adjustment method is the heating mode, by opening the steam valve connected to the heat exchange mechanism 4 and introducing high-temperature steam into the heat exchange mechanism 4, the outside of the tubular reactor is heated to increase the temperature inside the tubular reactor; when the temperature adjustment method is the cooling mode, by opening the condensation valve connected to the heat exchange mechanism 4 and introducing low-temperature cooling water / refrigerating brine into the heat exchange mechanism 4, the outside of the tubular reactor is cooled to reduce the temperature inside the tubular reactor.

[0093] A heat preservation mechanism 5, which is arranged outside the heat exchange mechanism 4 to form a heat preservation environment.

[0094] In implementation, the heat preservation mechanism 5 provides a heat preservation environment, locking most of the temperature inside the tubular reactor. The implementation form of the heat preservation mechanism 5 can be set according to the specific application scenario, which is not limited in the present invention and will not be elaborated here.

[0095] The liquid-liquid reaction module 1 of the present invention provides a reaction site by setting up a multi-tubular reactor, realizing continuous and multi-stage reactions, improving production efficiency, and enhancing reaction controllability. By setting up the raw material conveying module 2, accurate conveyance of reaction raw materials can be achieved, ensuring stable supply of reaction raw materials, avoiding errors in manual feeding, and improving reaction consistency. By setting up the feeding control module, the feeding sequence and feeding parameters can be dynamically adjusted, avoiding incomplete reactions or increased side reactions caused by improper feeding, thereby improving the production efficiency and purity of the thiazole intermediate. By setting up the detection module, the temperature, air pressure, and liquid-phase image inside the tubular reactor can be monitored in real time, providing a data basis for subsequent analysis. By setting up the data analysis module, the reaction process can be effectively evaluated and decision-making adjustments can be made to ensure the stability and continuity of the reaction. By setting up the temperature adjustment module, rapid and accurate adjustment of the reaction temperature can be achieved, ensuring that the reaction proceeds at an appropriate temperature and improving production efficiency. The device of the present invention is used for continuously producing the thiazole intermediate 3-chloro-4-oxo-1-pentanol and aqueous ammonium dithiocarbamate solution, simplifying the operation process of production personnel, improving the quality stability of reaction products, and enhancing the production efficiency of the thiazole intermediate.

[0096] Please continue to refer to Figure 1 as shown, in the implementation, it further includes:

[0097] An exhaust gas recovery mechanism, which is connected to each tubular reactor for recovering the gas generated in the tubular reactor;

[0098] It can be understood that by setting up the exhaust gas recovery mechanism, the generated gas can be prevented from being discharged into the air to pollute the environment, and at the same time, the gas utilization rate can be improved, which is environmentally friendly.

[0099] In the implementation, it further includes a product storage mechanism 6, which is connected to each tubular reactor for receiving the products produced by the tubular reactor.

[0100] Please refer to Figure 5 as shown, which is a schematic flow chart of the usage method of the reaction device for continuously producing the thiazole intermediate in the embodiment of the present invention; the embodiment of the present invention also provides a usage method, including:

[0101] Step S1, the raw material conveying module conveys each reaction raw material to the corresponding tubular reactor and uniformly mixes them;

[0102] Step S2, the detection module detects the temperature and air pressure inside the tubes of each tubular reactor in real time and obtains the liquid-phase image inside each tubular reactor;

[0103] Step S3: Determine the reaction degree of each tubular reactor based on the temperature change inside the tube and the liquid-phase image of each tubular reactor, and determine the temperature adjustment method for each tubular reactor based on the reaction degree of each tubular reactor, including the heating mode and the cooling mode;

[0104] Among them, determine the heating amount and heating rate corresponding to the heating mode based on the temperature inside the tube and the pressure inside the tube of each tubular reactor, and determine the cooling amount and cooling rate corresponding to the cooling mode based on the temperature inside the tube and the pressure inside the tube of each tubular reactor;

[0105] Step S4: Determine whether to adjust the feeding order and / or feeding parameters of the reaction raw materials based on the reaction degree of each tubular reactor;

[0106] Among them, if it is determined to make an adjustment, determine the adjustment amount of the feeding speed according to the temperature inside the tube of each tubular reactor, determine the adjustment amount of the feeding amount according to the pressure inside the tube of each tubular reactor, and adjust the feeding order of the reaction raw materials based on the preset feeding order table.

[0107] Specifically, the usage method provided in the embodiments of the present invention can be applied to the above reaction device for continuously producing thiazole intermediates to achieve the same technical effects, which will not be elaborated here.

[0108] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

Claims

1. A reaction device for continuously producing a thiothiazole intermediate, characterized in that: include: A liquid-liquid reaction module, which includes a plurality of tubular reactors, for providing a place for the reaction to occur; A raw material delivery module, which is connected to the liquid-liquid reaction module and is used to deliver the reaction raw materials to the corresponding tubular reactor; A feed control module, which is connected to the raw material delivery module and is used to control the feed sequence and feed parameters of the reaction raw materials, wherein the feed parameters include feed speed and feed amount; A detection module, which is connected to the liquid-liquid reaction module and is used to detect the temperature and gas pressure inside each tubular reactor and obtain a liquid phase image inside each tubular reactor; A data analysis module, which is connected to the feed control module and the detection module respectively, and is used to determine the reaction degree of each tubular reactor based on the temperature change in the tube of each tubular reactor and the liquid phase image, and to determine whether to adjust the feed sequence and / or feed parameters of the reaction raw materials; a temperature adjustment module, which is connected to the liquid-liquid reaction module, the detection module and the data analysis module respectively, and is used to determine a temperature adjustment mode for each tubular reactor based on the reaction degree of each tubular reactor, wherein the temperature adjustment mode includes a temperature increase mode and a temperature decrease mode; Among them, the temperature increase amount and temperature increase rate corresponding to the heating mode are determined based on the tube temperature and tube pressure of each tubular reactor, and the temperature reduction amount and temperature reduction rate corresponding to the cooling mode are determined based on the tube temperature and tube pressure of each tubular reactor.

2. The reaction device for continuously producing thiothiazole intermediates according to claim 1, characterized in that: The data analysis module determines the distribution state of the organic phase and the aqueous phase in the tubular reactor and the distribution of bubbles in the liquid based on the liquid phase images in each tubular reactor.

3. The reaction device for continuously producing thiothiazole intermediates according to claim 2, characterized in that: The data analysis module determines the reaction degree of each tubular reactor based on the comparison results of the temperature change in the tube of each tubular reactor with the preset temperature change, the distribution state of the organic phase and the aqueous phase in each tubular reactor, and the bubble distribution in the liquid.

4. The reaction device for continuously producing thiothiazole intermediates according to claim 3, characterized in that: The data analysis module determines whether to adjust the feed sequence and / or feed parameters of the reaction raw materials based on the reaction degree of each tubular reactor; If the reaction degree of the tubular reactor meets the corresponding preset standard, the feeding sequence and feeding parameters of the reaction raw materials corresponding to the tubular reactor are not adjusted; If the reaction degree of the tubular reactor does not meet the corresponding preset standard, the feeding sequence / feeding parameters of the reaction raw materials corresponding to the tubular reactor are adjusted.

5. The reaction device for continuously producing thiothiazole intermediates according to claim 4, characterized in that: The data analysis module determines the adjustment amount of the feed rate according to the temperature inside the tube of each tubular reactor based on the determination result of adjusting the feed parameters of the reaction raw materials, and determines the adjustment amount of the feed amount according to the gas pressure inside the tube of each tubular reactor; The data analysis module adjusts the feeding sequence of the reaction raw materials based on a preset feeding sequence table based on the determination result of adjusting the feeding sequence of the reaction raw materials.

6. The reaction device for continuously producing thiothiazole intermediates according to claim 5, characterized in that: The data analysis module determines the corresponding tube temperature change curve based on the tube temperature of each tubular reactor, determines the corresponding current theoretical temperature based on each tube temperature change curve, and determines the adjustment amount of the feed rate based on the comparison result between the current theoretical temperature and the current tube temperature.

7. The reaction device for continuously producing thiothiazole intermediates according to claim 6, characterized in that: The data analysis module determines the adjustment amount of the feed amount based on the comparison result of the change of the gas pressure in the tube of each tubular reactor and the preset gas pressure change.

8. The reaction device for continuously producing thiothiazole intermediates according to claim 7, characterized in that: The temperature adjustment module determines adjustment parameters based on the temperature and gas pressure inside the tubes of each tubular reactor, determines a temperature increase or decrease amount based on the adjustment parameters and a set temperature, and determines a temperature increase rate or a temperature decrease rate based on the adjustment parameters and a set rate.

9. The reaction device for continuously producing thiothiazole intermediates according to claim 8, characterized in that: The liquid-liquid reaction module also includes: A pipeline mixer element mechanism, which is arranged inside each of the tubular reactors to mix the materials in the tubular reactor uniformly; A heat exchange mechanism, which is arranged outside each of the tubular reactors and connected to the temperature adjustment module, and is used to adjust the temperature inside each of the tubular reactors based on a determined temperature adjustment method; The heat preservation mechanism is arranged outside the heat exchange mechanism to form a heat preservation environment.

10. A method for using the reaction device according to any one of claims 1 to 9, characterized in that: include: The raw material conveying module conveys each reaction raw material to the corresponding tubular reactor and mixes them evenly; The detection module detects the temperature and gas pressure in each tubular reactor in real time, and obtains the liquid phase image in each tubular reactor; Determine the reaction degree of each tubular reactor based on the temperature change in each tubular reactor and the liquid phase image, and determine the temperature adjustment mode of each tubular reactor based on the reaction degree of each tubular reactor, including a heating mode and a cooling mode; The temperature increase amount and the temperature increase rate corresponding to the temperature increase mode are determined based on the temperature inside the tube and the gas pressure inside the tube of each tubular reactor, and the temperature reduction amount and the temperature reduction rate corresponding to the temperature reduction mode are determined based on the temperature inside the tube and the gas pressure inside the tube of each tubular reactor; Determining whether to adjust the feed sequence and / or feed parameters of the reaction raw materials based on the reaction degree of each tubular reactor; If adjustment is determined, the adjustment amount of the feed rate is determined according to the temperature inside the tube of each tubular reactor, the adjustment amount of the feed amount is determined according to the gas pressure inside the tube of each tubular reactor, and the feed order of the reaction raw materials is adjusted based on a preset feed order table.

Images