Fracturing bactericide macrolide derivative production process management method and system
By selecting high-quality raw materials, adjusting reaction conditions and accurately controlling the addition of monoethanolamine and catalyst, the problem of low purity of acid derivatives in the macrocyclic in the prior art is solved, and a higher purity and a more scientific preparation process is achieved.
Patent Information
- Application Number
- CN202510124628.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-26
- Publication Date
- 2025-03-07
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing macrocyclic acid derivative production management technology cannot accurately regulate the intensity of the reaction and the uniformity of the reaction, resulting in the low purity of the prepared macrocyclic acid derivative.
By selecting high-quality core raw materials and auxiliary raw materials, adjusting the reaction conditions, and analyzing the relationship between reaction rate and derivative purity based on historical monitoring data, the addition ratio of monoethanolamine and catalyst is accurately adjusted to ensure that the reaction is stable and uniform.
The purity of acid derivatives within the macrocycle is improved, the scientificity and effectiveness of the preparation process are ensured, and the problem of low purity in the prior art is solved.
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Figure CN119575918A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of production management, and in particular to a production process management method and system for macrolide derivatives of fracturing fungicides. Background Art
[0002] The production management technology of macrolide derivatives refers to the planning, monitoring and optimization methods for the production process of this type of compounds. This technology involves all stages of the production process, including raw material procurement, reaction condition design, production equipment selection and maintenance, quality control, and improvement of product purity and output.
[0003] The existing production management technology of macrolide acid derivatives usually directly reacts the core raw materials with the auxiliary raw materials to prepare the macrolide acid derivatives. The purity of the macrolide acid derivatives prepared in this way is usually low. The purity of the macrolide acid derivatives is related to many factors, including but not limited to the preparation environment, raw material purity, reaction intensity and reaction uniformity. They need to be precisely regulated to prepare macrolide acid derivatives with higher purity. The existing production management technology of macrolide acid derivatives does not regulate these factors, especially the reaction intensity and reaction uniformity. The preparation environment and raw material purity guarantee the lower limit of the purity of the macrolide acid derivatives, while the reaction intensity and reaction uniformity can increase the upper limit of the purity of the macrolide acid derivatives. If they are not regulated, the purity of the prepared macrolide acid derivatives will be low. The existing macrolide acid derivatives also have the problem that the regulation of the preparation environment, raw material purity, reaction intensity and reaction uniformity is not precise enough, resulting in the low purity of the prepared macrolide acid derivatives. Summary of the invention
[0004] The present invention aims to solve one of the technical problems in the prior art to a certain extent at least. The core raw materials and auxiliary raw materials for preparing macrolide derivatives are selected, and then the reaction conditions are adjusted. The core raw materials and auxiliary raw materials are placed in a reaction device for reaction. Based on historical monitoring data, the relationship between the reaction rate and the purity of the derivative is analyzed. Based on the historical monitoring data, the influence of the ratio of monoethanolamine and the catalyst on the reaction rate is analyzed. Based on the historical monitoring data, the influence of the ratio of monoethanolamine and the catalyst on the reaction uniformity is analyzed. Then, based on the relationship between the reaction rate and the purity of the derivative, the influence of the ratio of monoethanolamine and the catalyst on the reaction rate, and the influence of the ratio of monoethanolamine and the catalyst on the reaction uniformity, the addition of monoethanolamine and the catalyst is precisely regulated. Finally, after the reaction process is completed, the reaction product is separated and purified to obtain the final macrolide derivative, so as to solve the problem that the existing macrolide derivatives still have the problem that the preparation environment, raw material purity, reaction intensity and reaction uniformity are not precisely regulated, resulting in the low purity of the prepared macrolide derivatives.
[0005] To achieve the above objectives, in a first aspect, the present application provides a method for managing the production process of macrolide derivatives of fracturing fungicides, comprising the following steps: Selecting core raw materials and auxiliary raw materials for preparing macrolide derivatives; Adjust the reaction conditions and place the core raw materials and auxiliary raw materials in the reaction equipment for reaction; Monitor the reaction process in real time and precisely control the addition of core and auxiliary raw materials while ensuring a smooth and uniform reaction; After the reaction process is completed, the reaction product is separated and purified to obtain the final macrolide derivative; Adjusting the reaction conditions and placing the core raw materials and auxiliary raw materials in the reaction equipment for reaction includes the following sub-steps: Placing the core raw materials and the auxiliary raw materials in a reaction device, wherein the reaction device is a reactor; Performing an amidation reaction on the core raw material, placing the core raw material and the auxiliary raw material in a reaction device, and adjusting the reaction temperature of the reactor to a first temperature threshold; adjusting the reaction pressure in the reactor to a first pressure threshold; The pH value in the reactor is adjusted to a first pH threshold.
[0006] Furthermore, the selection of core raw materials and auxiliary raw materials for preparing macrolide derivatives includes the following sub-steps: The core raw material is monoethanolamine, and the auxiliary raw materials are catalysts, solvents and reaction aids; Selecting monoethanolamine with a purity greater than a first purity threshold as a core raw material; Ensure that the water content in the solvent is less than a first content threshold; When storing monoethanolamine, ensure that it is stored in dry and light-proof conditions to avoid hydrolysis or degradation; Catalysts and solvents must be stored separately to avoid cross contamination.
[0007] Furthermore, the reaction process is monitored in real time, and the addition of the core raw materials and auxiliary raw materials is precisely regulated while ensuring a smooth and uniform reaction, including the following sub-steps: Analyze the relationship between reaction rate and purity of derivatives based on historical monitoring data; Based on historical monitoring data, analyze the effect of the ratio of added monoethanolamine and catalyst on the reaction rate; Based on historical monitoring data, the effect of the ratio of monoethanolamine to catalyst on reaction uniformity was analyzed; Based on the relationship between the reaction rate and the purity of the derivative, the effect of the ratio of monoethanolamine to the catalyst on the reaction rate, and the effect of the ratio of monoethanolamine to the catalyst on the reaction uniformity, the addition of monoethanolamine and the catalyst is precisely controlled.
[0008] Furthermore, based on historical monitoring data, analyzing the relationship between reaction rate and purity of the derivative includes the following sub-steps: The reaction rate of monoethanolamine was calculated by the Arrhenius formula; The Arrhenius formula is , where K is the reaction rate constant, which can be used as the reaction rate, A is the frequency factor, e is the base of the natural logarithm, Ea is the activation energy, R is the molar gas constant, T is the absolute temperature, and the unit of T is Kelvin, not Celsius. The frequency factor is calculated by quantum chemical calculation method; Obtaining historical monitoring data, marked as monitoring historical data, the monitoring historical data includes historical reaction rate, historical derivative purity, historical frequency factor, historical addition ratio and historical reaction time, the historical addition ratio is the ratio of added monoethanolamine to catalyst, the historical reaction time is the time taken for monoethanolamine and catalyst to react completely and no longer send reaction; the set of historical reaction rate, historical derivative purity, historical frequency factor, historical addition ratio and historical reaction time constitutes one piece of monitoring historical data; A rectangular coordinate system is established with the historical reaction rate as the X-axis and the historical derived purity as the Y-axis, named the rate purity influence diagram, and the historical reaction rate and the historical derived purity are entered into the rate purity influence diagram; Perform regression analysis on the rate purity influence diagram to obtain the regression function with the smallest standard deviation, which is marked as the rate purity influence equation.
[0009] Furthermore, based on historical monitoring data, analyzing the effect of the ratio of adding monoethanolamine and catalyst on the reaction rate includes the following sub-steps: It is easy to know from the Arrhenius formula that, under the premise of ensuring the same reaction conditions, the only factor affecting the reaction rate is the frequency factor A. A rectangular coordinate system is established with the historical addition ratio as the X-axis and the historical frequency factor as the Y-axis, named the frequency influence diagram, and the historical addition ratio and the historical frequency factor are entered into the frequency influence diagram; Perform regression analysis on the frequency influence diagram to obtain the regression function with the smallest standard deviation, which is marked as the frequency influence equation.
[0010] Furthermore, based on historical monitoring data, analyzing the effect of the ratio of adding monoethanolamine and catalyst on the reaction uniformity includes the following sub-steps: Get the historical reaction rate and historical reaction time, get the minimum and maximum values of the historical reaction rate, marked as K respectively min and K max , get the minimum and maximum values of the historical reaction time, marked as S min and S max ; For any piece of historical monitoring data, the historical reaction rate is marked as KL, and the historical reaction time is marked as SL; By formula Calculate the reaction uniformity of the monitoring historical data, where RU is the reaction uniformity; A rectangular coordinate system is established with the historical addition ratio as the X-axis and the reaction uniformity as the Y-axis, named the uniformity influence diagram, and the reaction uniformity in the monitoring historical data is entered into the uniformity influence diagram according to the historical addition ratio; Perform regression analysis on the uniformity influence diagram to obtain the regression function with the smallest standard deviation, which is marked as the uniformity influence equation.
[0011] Furthermore, based on the relationship between the reaction rate and the purity of the derivative, the effect of the ratio of monoethanolamine to the catalyst on the reaction rate, and the effect of the ratio of monoethanolamine to the catalyst on the reaction uniformity, the precise control of the addition of monoethanolamine and the catalyst includes the following sub-steps: Get the rate purity influence equation, find the value of the X-axis corresponding to the maximum value of the Y-axis, mark it as the target rate, and represent it by the symbol TR; Based on the Arrhenius formula, the frequency factor is solved and marked as the target factor. The target factor is substituted into the frequency influence equation to solve the historical addition ratio and marked as the target addition ratio. The target addition ratio is increased by a first ratio to obtain a fluctuation upper limit, the target addition ratio is reduced by a first ratio to obtain a fluctuation lower limit, and a range interval between the fluctuation lower limit and the fluctuation upper limit is marked as a fluctuation interval; Set X in the uniformity influence equation and the frequency influence equation as the fluctuation lower limit, and mark the solved results as reference uniformity and reference frequency, represented by symbols CR and CF respectively; Get the minimum and maximum values of the Y axis in the uniformity influence equation, marked as CR respectively min and CR max ; By formula Calculate the rate stability index when X is set to the lower limit of fluctuation, where H is the rate stability index, KL is the historical reaction rate, and max() is the maximum value operator; Continue to increase the lower limit of fluctuation, and do not exceed the upper limit of fluctuation. Meanwhile, continue to calculate H, obtain the maximum value of H, mark it as the maximum index, and mark the value of X corresponding to the maximum index as the optimal addition ratio; Monoethanolamine and catalyst were added into the reactor according to the optimal addition ratio.
[0012] Furthermore, after the reaction process is completed, the reaction product is separated and purified to obtain the final macrolide derivative, which includes the following sub-steps: The macrolide derivatives were separated by liquid-liquid extraction; The macrolide derivative is purified by recrystallization to obtain the final macrolide derivative.
[0013] In a second aspect, the present application provides a production process management system for macrolide derivatives of fracturing fungicides, including a raw material preparation module, a condition adjustment module, a reaction control module and a separation and purification module; the raw material preparation module, the condition adjustment module and the separation and purification module are respectively connected to the reaction control module data; The raw material preparation module is used to select core raw materials and auxiliary raw materials for preparing macrolide derivatives; The condition adjustment module is used to adjust the reaction conditions and place the core raw materials and auxiliary raw materials in the reaction equipment for reaction; The reaction control module is used to monitor the reaction process in real time and accurately control the addition of core raw materials and auxiliary raw materials while ensuring a smooth and uniform reaction; The separation and purification module is used to separate and purify the reaction product after the reaction process is completed to obtain the final macrocyclic lactic acid derivative; Adjusting the reaction conditions and placing the core raw materials and auxiliary raw materials in the reaction equipment for reaction includes the following sub-steps: Placing the core raw materials and the auxiliary raw materials in a reaction device, wherein the reaction device is a reactor; Performing an amidation reaction on the core raw material, placing the core raw material and the auxiliary raw material in a reaction device, and adjusting the reaction temperature of the reactor to a first temperature threshold; adjusting the reaction pressure in the reactor to a first pressure threshold; The pH value in the reactor is adjusted to a first pH threshold.
[0014] Beneficial effects of the present invention: The present invention selects core raw materials and auxiliary raw materials for preparing macrolide derivatives, and then adjusts the reaction conditions, and places the core raw materials and auxiliary raw materials in a reaction device for reaction. The advantage is that the quality of the raw materials is screened when selecting the core raw materials and auxiliary raw materials, and only high-quality raw materials are selected for reaction. At the same time, the reaction environment is regulated to ensure the lower limit of the purity of the macrolide derivatives, thereby improving the scientificity and effectiveness of the purity of the preparation of the macrolide derivatives. The present invention analyzes the relationship between the reaction rate and the purity of the derivative based on historical monitoring data, analyzes the influence of the ratio of monoethanolamine to the catalyst on the reaction rate based on the historical monitoring data, and analyzes the influence of the ratio of monoethanolamine to the catalyst on the reaction uniformity based on the historical monitoring data. Then, based on the relationship between the reaction rate and the purity of the derivative, the influence of the ratio of monoethanolamine to the catalyst on the reaction rate, and the influence of the ratio of monoethanolamine to the catalyst on the reaction uniformity, the addition of monoethanolamine and the catalyst is precisely regulated. The method has the advantage that the ratio of monoethanolamine to the catalyst is precisely regulated based on the historical monitoring data, so as to ensure that the reaction of monoethanolamine and the catalyst is stable and uniform, increase the upper limit of the purity of the macrolide derivative, and further improve the scientificity and effectiveness of preparing the macrolide derivative. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] Figure 1 is a functional block diagram of the system of the present invention; Figure 2 It is the rate purity influence diagram of the present invention; Figure 3 It is the frequency influence diagram of the present invention; Figure 4 is the uniformity influence diagram of the present invention; Figure 5 The figure is a flow chart of the steps of the method of the present invention. DETAILED DESCRIPTION
[0016] 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.
[0017] Example 1, please refer to Figure 1 As shown, the present application provides a production process management system for macrolide derivatives of fracturing fungicides, including a raw material preparation module, a condition adjustment module, a reaction control module and a separation and purification module; the raw material preparation module, the condition adjustment module and the separation and purification module are respectively connected with the reaction control module data; The raw material preparation module is used to select core raw materials and auxiliary raw materials for preparing macrolide derivatives; The raw material preparation module is configured with raw material preparation strategies, which include: The core raw material is monoethanolamine, and the auxiliary raw materials are catalysts, solvents and reaction aids; Selecting monoethanolamine with a purity greater than a first purity threshold as a core raw material; Ensure that the water content in the solvent is less than a first content threshold; When storing monoethanolamine, ensure that it is stored in dry and light-proof conditions to avoid hydrolysis or degradation; Catalysts and solvents must be stored separately to avoid cross contamination; In practical applications, the existing macrolide derivative preparation technology usually has certain standards for the selection of raw materials. In this embodiment, core raw materials and auxiliary raw materials are selected according to the existing standards. The focus of this embodiment is to control the intensity and uniformity of the reaction process by controlling the ratio of monoethanolamine to catalyst addition, thereby increasing the upper limit of the purity of the macrolide derivative; in this embodiment, the first purity threshold is set to 99%, and the first content threshold is set to 0.1%. Ensuring that the water content in the solvent is less than the first content threshold is to avoid affecting the reaction efficiency.
[0018] The condition adjustment module is used to adjust the reaction conditions and place the core raw materials and auxiliary raw materials in the reaction equipment for reaction; The conditional adjustment module is configured with conditional adjustment strategies, which include: Placing the core raw materials and the auxiliary raw materials in a reaction device, wherein the reaction device is a reactor; Performing an amidation reaction on the core raw material, placing the core raw material and the auxiliary raw material in a reaction device, and adjusting the reaction temperature of the reactor to a first temperature threshold; adjusting the reaction pressure in the reactor to a first pressure threshold; Adjusting the pH value in the reactor to a first pH threshold; In practical applications, the reaction environment is regulated according to existing standards. Based on the existing macrolide derivative preparation technology, the first temperature threshold is set to 100°C, the first pressure threshold is set to 0.2 MPa, and the first pH threshold is set to 7.
[0019] The reaction control module is used to monitor the reaction process in real time and accurately control the addition of core raw materials and auxiliary raw materials while ensuring a smooth and uniform reaction; the reaction control module includes a rate purity analysis unit, a ratio rate analysis unit, a ratio uniformity analysis unit and a precision control unit; The rate purity analysis unit is used to analyze the relationship between reaction rate and purity of derivatives based on historical monitoring data; The rate purity analysis unit is configured with a rate purity analysis strategy, which includes: The reaction rate of monoethanolamine was calculated by the Arrhenius formula; The Arrhenius formula is , where K is the reaction rate constant, which can be used as the reaction rate, A is the frequency factor, e is the base of the natural logarithm, Ea is the activation energy, R is the molar gas constant, T is the absolute temperature, and the unit of T is Kelvin, not Celsius. The frequency factor is calculated by quantum chemical calculation method; In practical applications, quantum chemical calculation is an existing calculation method, which will not be explained in detail in this embodiment. The reaction rate finally obtained is only used to express the speed of the reaction rate by numerical value, and the method of removing the dimension and taking the quantity is adopted, and only the numerical value is referred to, not the unit; assuming that A=1.0×10 6 S -1 , Ea=50000 J / mol, R=8.314 J / (mol·K), T=373.15 K (the Kelvin temperature corresponding to 100°C Celsius), from which the value of the reaction rate constant K can be calculated to be 0.1001, and the calculation result is rounded to four decimal places; Obtaining historical monitoring data, marked as monitoring historical data, the monitoring historical data includes historical reaction rate, historical derivative purity, historical frequency factor, historical addition ratio and historical reaction time, the historical addition ratio is the ratio of added monoethanolamine to catalyst, the historical reaction time is the time taken for monoethanolamine and catalyst to react completely and no longer send reaction; the set of historical reaction rate, historical derivative purity, historical frequency factor, historical addition ratio and historical reaction time constitutes one piece of monitoring historical data; See also Figure 2As shown, a rectangular coordinate system is established with the historical reaction rate as the X-axis and the historical derived purity as the Y-axis, named as the rate purity influence diagram, and the historical reaction rate and the historical derived purity are entered into the rate purity influence diagram; Perform regression analysis on the rate purity influence diagram to obtain the regression function with the smallest standard deviation, which is marked as the rate purity influence equation; In practical applications, the core raw materials, auxiliary raw materials and reaction environment used in monitoring historical data are the same as those in this embodiment, and the rate purity influence diagram is constructed as shown in Figure 2 As shown, regression analysis is performed again. Regression analysis includes a variety of analysis methods, such as linear regression and power regression, and the standard deviation reflects the discreteness of coordinate points in different regression analyses. The smaller the discreteness, the better the regression effect. Therefore, the regression function with the smallest standard deviation is selected as the rate purity influence equation. In this embodiment, the rate purity influence equation obtained by regression is P=-947.83×K 3 +379.69×K 2 -8.8793×K+92.035, where P is the historical derivative purity and K is the historical reaction rate. The higher the reaction rate, the better. The higher the reaction rate, the more intense the reaction. In the case of an intense reaction, the purity of the macrolide derivative will decrease to a certain extent. Therefore, it is necessary to find a balance between the reaction rate and purity to ensure that the reaction produces the macrolide derivative with the highest purity. The ratio rate analysis unit is used to analyze the effect of the ratio of added monoethanolamine and catalyst on the reaction rate based on historical monitoring data; The ratio rate analysis unit is configured with a ratio rate analysis strategy, which includes: It is easy to know from the Arrhenius formula that, under the premise of ensuring the same reaction conditions, the only factor affecting the reaction rate is the frequency factor A. See also Figure 3 As shown, a rectangular coordinate system is established with the historical addition ratio as the X-axis and the historical frequency factor as the Y-axis, named the frequency influence diagram, and the historical addition ratio and the historical frequency factor are entered into the frequency influence diagram; Perform regression analysis on the frequency influence diagram to obtain the regression function with the smallest standard deviation, which is marked as the frequency influence equation; In practical applications, the historical addition ratio is the ratio of the amount of added monoethanolamine to the amount of added catalyst. The frequency influence diagram is constructed as follows: Figure 3 As shown, the frequency influence equation obtained by regression analysis is A=-16399×X 2 +509843×X-401123, where A is the historical frequency factor and X is the historical addition ratio; The ratio uniformity analysis unit is used to analyze the effect of the ratio of added monoethanolamine and catalyst on the reaction uniformity based on historical monitoring data; The ratio uniformity analysis unit is configured with a ratio uniformity analysis strategy, which includes: Get the historical reaction rate and historical reaction time, get the minimum and maximum values of the historical reaction rate, marked as K respectively min and K max , get the minimum and maximum values of the historical reaction time, marked as S min and S max ; In practical applications, the reaction rate is only a reference value and does not remain constant. This involves the determination of reaction uniformity. Generally, the greater the reaction rate, the less time it takes for a complete reaction. However, due to different reaction uniformities, historical reaction times do not completely follow this rule. For example, in the past, the addition ratio was unreasonable, resulting in too little monoethanolamine content, and the reaction rate was fast at a certain moment. However, after a period of time, due to the uneven reaction, the reaction rate changed significantly, thereby greatly increasing the reaction time. In this embodiment, K min and K max They are 0.0048 and 0.3355 respectively, S min and S max 2.25h and 8.75h respectively; For any piece of historical monitoring data, the historical reaction rate is marked as KL, and the historical reaction time is marked as SL; By formula Calculate the reaction uniformity of the monitoring historical data, where RU is the reaction uniformity; See also Figure 4 As shown, a rectangular coordinate system is established with the historical addition ratio as the X-axis and the reaction uniformity as the Y-axis, named the uniformity influence diagram, and the reaction uniformity in the monitoring historical data is entered into the uniformity influence diagram according to the historical addition ratio; Perform regression analysis on the uniformity influence diagram to obtain the regression function with the minimum standard deviation, which is marked as the uniformity influence equation; In practical applications, the denominator in the formula is added with one to prevent the denominator from being zero. Assuming that the historical reaction rate KL is 0.1001 and the historical reaction time SL is 5.2h, the reaction uniformity RU=0.6350 is obtained by calculation. The calculation result is retained to four decimal places. All the monitoring historical data are calculated and then the uniformity influence diagram is constructed as shown below: Figure 4 As shown in the figure, the uniformity influence equation obtained by regression analysis is RU=-0.0274×X 2 +0.9216×X-0.8362; The precise control unit is used to precisely control the addition of monoethanolamine and the catalyst based on the relationship between the reaction rate and the purity of the derivative, the effect of the ratio of monoethanolamine to the catalyst on the reaction rate, and the effect of the ratio of monoethanolamine to the catalyst on the reaction uniformity; The precise control and analysis unit is configured with precise control and analysis strategies, which include: Get the rate purity influence equation, find the value of the X-axis corresponding to the maximum value of the Y-axis, mark it as the target rate, and represent it by the symbol TR; Based on the Arrhenius formula, the frequency factor is solved and marked as the target factor. The target factor is substituted into the frequency influence equation to solve the historical addition ratio and marked as the target addition ratio. The target addition ratio is increased by a first ratio to obtain a fluctuation upper limit, the target addition ratio is reduced by a first ratio to obtain a fluctuation lower limit, and a range interval between the fluctuation lower limit and the fluctuation upper limit is marked as a fluctuation interval; In practical applications, the value of the X axis corresponding to the maximum value of the Y axis is 0.2669 when the rate purity influence diagram is obtained, that is, the target rate TR is 0.2669; Substitute K=0.2669 into the Arrhenius formula , the target factor is 2.665319×10 6 , and then A=2.665319×10 6 Substitute A = -16399 × X 2 +509843×X-401123, the target addition ratio is 15.79, and the calculation result is rounded to two decimal places; the first ratio is set to find a point near the target addition ratio where the reaction is stable and more uniform. The first ratio is set to 5%, and the upper limit of the fluctuation is 16.57, the lower limit of the fluctuation is 14.99, and the fluctuation range is [14.99, 16.57]; Set X in the uniformity influence equation and the frequency influence equation as the fluctuation lower limit, and mark the solved results as reference uniformity and reference frequency, represented by symbols CR and CF respectively; In practical applications, the uniformity influence equation and the frequency influence equation are RU=-0.0274×X 2 +0.9216×X-0.8362 and A=-16399×X 2 +509843×X-401123, set X to the fluctuation lower limit 14.99, solve for the reference uniformity CR to be 6.8218, solve for A to be 3556567, and substitute into the Arrhenius formula to solve for the reference frequency CF to be 0.3561. The calculation results are all retained to four decimal places; continue to increase the fluctuation lower limit and calculate the corresponding reference uniformity and reference frequency; Get the minimum and maximum values of the Y axis in the uniformity influence equation, marked as CR respectively min and CR max ; By formula Calculate the rate stability index when X is set to the lower limit of fluctuation, where H is the rate stability index, KL is the historical reaction rate, and max() is the maximum value operator; Continue to increase the lower limit of fluctuation, and do not exceed the upper limit of fluctuation. Meanwhile, continue to calculate H, obtain the maximum value of H, mark it as the maximum index, and mark the value of X corresponding to the maximum index as the optimal addition ratio; Adding monoethanolamine and catalyst into the reactor according to the optimal addition ratio; In actual application, CR is obtained min and CR max They are 0.3385 and 6.9133 respectively. With the fluctuation lower limit of 14.99, the calculated reference uniformity CR is 6.8218, the target rate TR is 0.2669, and the reference frequency CF is 0.3561. Substituting them into the calculation, the rate stability index H=1.9323 is obtained. The calculation result is retained to four decimal places. It is to calculate the degree of deviation between the reference frequency and the target rate; continue to increase the lower limit of fluctuation, and calculate H at the same time. The maximum index is 3.6988 through comparison, and the corresponding optimal addition ratio is 16.02. Monoethanolamine and catalyst are added to the reactor at a ratio of 16.02.
[0020] The separation and purification module is used to separate and purify the reaction product after the reaction process is completed to obtain the final macrocyclic lactic acid derivative; The separation and purification module is configured with a separation and purification strategy, which includes: The macrolide derivatives were separated by liquid-liquid extraction; Purifying the macrolide derivative by recrystallization to obtain the final macrolide derivative; In practical applications, the separation and purification of macrolide derivatives are carried out using existing technologies, which will not be described in detail in this embodiment.
[0021] Example 2, please refer to Figure 5 As shown, the present application provides a production process management method for macrolide derivatives of fracturing fungicides, comprising the following steps: Step S1, selecting core raw materials and auxiliary raw materials for preparing macrolide derivatives; Step S1 includes the following sub-steps: Step S101, the core raw material is monoethanolamine, and the auxiliary raw materials are catalysts, solvents and reaction aids; Step S102, selecting monoethanolamine with a purity greater than a first purity threshold as a core raw material; Step S103, ensuring that the water content in the solvent is less than a first content threshold; Step S104, when storing monoethanolamine, ensure that it is stored in a dry and light-proof condition to avoid hydrolysis or degradation; Step S105, the catalyst and solvent need to be stored separately to avoid cross contamination; Step S2, adjusting the reaction conditions, placing the core raw materials and the auxiliary raw materials in a reaction device for reaction; Step S2 includes the following sub-steps: Step S201, placing the core raw material and the auxiliary raw material in a reaction device, wherein the reaction device is a reactor; Step S202, performing an amidation reaction on the core raw material, placing the core raw material and the auxiliary raw material in a reaction device, and adjusting the reaction temperature of the reactor to a first temperature threshold; Step S203, adjusting the reaction pressure in the reactor to a first pressure threshold; Step S204, adjusting the pH value in the reactor to a first pH threshold; Step S3, real-time monitoring of the reaction process, and precise control of the addition of the core raw materials and auxiliary raw materials while ensuring a smooth and uniform reaction; Step S3 includes the following sub-steps: Step S301, analyzing the relationship between reaction rate and purity of the derivative based on historical monitoring data; Step S301 includes the following sub-steps: Step S3011, calculating the reaction rate of monoethanolamine by using the Arrhenius formula; Step S3012, the Arrhenius formula is , where K is the reaction rate constant, which can be used as the reaction rate, A is the frequency factor, e is the base of the natural logarithm, Ea is the activation energy, R is the molar gas constant, T is the absolute temperature, and the unit of T is Kelvin, not Celsius. The frequency factor is calculated by quantum chemical calculation method; Step S3013, obtaining historical monitoring data, marked as monitoring historical data, the monitoring historical data includes historical reaction rate, historical derived purity, historical frequency factor, historical addition ratio and historical reaction time, the historical addition ratio is the ratio of added monoethanolamine to catalyst, the historical reaction time is the time taken for monoethanolamine and catalyst to react completely and no longer send reaction; the set of historical reaction rate, historical derived purity, historical frequency factor, historical addition ratio and historical reaction time constitutes one piece of monitoring historical data; Step S3014, establishing a rectangular coordinate system with the historical reaction rate as the X-axis and the historical derived purity as the Y-axis, named as the rate purity influence diagram, and entering the historical reaction rate and the historical derived purity into the rate purity influence diagram; Step S3015, performing regression analysis on the rate purity influence diagram to obtain a regression function with the minimum standard deviation, which is marked as a rate purity influence equation; Step S302, analyzing the effect of the ratio of adding monoethanolamine and the catalyst on the reaction rate based on historical monitoring data; Step S302 includes the following sub-steps: Step S3021, it is easy to know from the Arrhenius formula that, under the premise of ensuring the same reaction conditions, the only factor affecting the reaction rate is the frequency factor A. Step S3022, establish a rectangular coordinate system with the historical addition ratio as the X-axis and the historical frequency factor as the Y-axis, name it as the frequency influence diagram, and enter the historical addition ratio and the historical frequency factor into the frequency influence diagram; Step S3023, performing regression analysis on the frequency influence diagram to obtain a regression function with the minimum standard deviation, which is marked as a frequency influence equation; Step S303, analyzing the effect of the ratio of adding monoethanolamine and catalyst on the reaction uniformity based on historical monitoring data; Step S303 includes the following sub-steps: Step S3031, obtain the historical reaction rate and the historical reaction time, and obtain the minimum and maximum values of the historical reaction rate, which are marked as K and K respectively. min and K max , get the minimum and maximum values of the historical reaction time, marked as S min and S max ; Step S3032: for any piece of monitoring history data, mark the history reaction rate as KL and the history reaction time as SL; Step S3033, by formula Calculate the reaction uniformity of the monitoring historical data, where RU is the reaction uniformity; Step S3034, establish a rectangular coordinate system with the historical addition ratio as the X-axis and the reaction uniformity as the Y-axis, named as the uniformity influence diagram, and enter the reaction uniformity in the monitoring historical data into the uniformity influence diagram according to the historical addition ratio; Step S3035, performing regression analysis on the uniformity influence diagram to obtain a regression function with the minimum standard deviation, which is marked as a uniformity influence equation; Step S304, based on the relationship between the reaction rate and the purity of the derivative, the effect of the ratio of monoethanolamine to the catalyst on the reaction rate, and the effect of the ratio of monoethanolamine to the catalyst on the reaction uniformity, the addition of monoethanolamine and the catalyst is precisely regulated; Step S304 includes the following sub-steps: Step S3041, obtaining the rate purity influence equation, finding the value of the X-axis corresponding to the maximum value of the Y-axis, marking it as the target rate, represented by the symbol TR; Step S3042, solving the frequency factor based on the Arrhenius formula, marking it as the target factor, substituting the target factor into the frequency influence equation to solve the historical addition ratio, marking it as the target addition ratio; Step S3043, increasing the target addition ratio by a first ratio to obtain a fluctuation upper limit, decreasing the target addition ratio by a first ratio to obtain a fluctuation lower limit, and marking a range between the fluctuation lower limit and the fluctuation upper limit as a fluctuation range; Step S3044, setting X in the uniformity influence equation and the frequency influence equation as the fluctuation lower limit, and marking the solved results as reference uniformity and reference frequency, respectively, represented by symbols CR and CF; Step S3045, obtaining the minimum value and maximum value of the Y axis in the uniformity influence equation, marked as CR and min and CR max ; Step S3046, by formula Calculate the rate stability index when X is set to the lower limit of fluctuation, where H is the rate stability index, KL is the historical reaction rate, and max() is the maximum value operator; Step S3047, continuously increase the fluctuation lower limit, and the maximum value does not exceed the fluctuation upper limit. Meanwhile, continuously calculate H, obtain the maximum value of H, mark it as the maximum index, and mark the value of X corresponding to the maximum index as the optimal addition ratio; Step S3048, adding monoethanolamine and catalyst into the reactor according to the optimal addition ratio; Step S4, after the reaction process is completed, the reaction product is separated and purified to obtain the final macrolide derivative; Step S4 includes the following sub-steps: Step S401, separating the macrolide derivative by liquid-liquid extraction; Step S402, purifying the macrolide derivative by recrystallization to obtain the final macrolide derivative.
[0022] Embodiment 3, the present application provides an electronic device, which may include: a processor, a communication interface, a memory and a communication bus, wherein the processor, the communication interface, and the memory communicate with each other through the communication bus. The memory stores computer-readable instructions, and the processor can call the instructions in the memory. When the computer-readable instructions are executed by the processor, the steps in the production process management method of a fracturing fungicide macrolide derivative are executed to achieve the following functions: select the core raw materials and auxiliary raw materials for preparing macrolide derivatives; adjust the reaction conditions, place the core raw materials and auxiliary raw materials in the reaction equipment for reaction; monitor the reaction process in real time, and accurately control the addition of the core raw materials and auxiliary raw materials while ensuring that the reaction is stable and uniform; separate and purify the reaction products after the reaction process to obtain the final macrolide derivative.
[0023] In addition, the logic instructions in the above-mentioned memory can be implemented in the form of software functional units and can be stored in a computer-readable storage medium when sold or used as an independent product. Based on this understanding, the technical solution of the present application can be essentially or partly embodied in the form of a software product that contributes to the prior art. The computer software product is stored in a storage medium, including several instructions to enable a computer device (which can be a personal computer, server, or network device, etc.) to execute all or part of the steps of the method described in each embodiment of the present application. The aforementioned storage medium includes: U disk, mobile hard disk, read-only memory (ROM, Read-Only Memory), random access memory (RAM, Random Access Memory), disk or optical disk, etc. Various media that can store program codes.
[0024] Example 4. The present application also provides a computer-readable storage medium. The present application provides a storage medium on which a computer program is stored. When the computer program is executed by a processor, the steps in the above method for managing the production process of macrolide derivatives of fracturing fungicides are executed to achieve the following functions: selecting core raw materials and auxiliary raw materials for preparing macrolide derivatives; adjusting reaction conditions, placing the core raw materials and auxiliary raw materials in a reaction device for reaction; monitoring the reaction process in real time, and precisely controlling the addition of core raw materials and auxiliary raw materials while ensuring a smooth and uniform reaction; separating and purifying the reaction products after the reaction process to obtain the final macrolide derivatives.
[0025] Through the description of the above implementation methods, the embodiments of the present invention can be provided as methods, systems or computer program products. Based on such an understanding, the above technical solutions can be essentially or partly contributed to the prior art in the form of software products, which can be stored in a computer-readable storage medium, such as ROM / RAM, a magnetic disk, an optical disk, etc., and include several instructions for enabling a computer device (which can be a personal computer, a server, or a network device, etc.) to execute the methods described in each embodiment or some parts of the embodiments.
[0026] In the embodiments provided in the present application, it should be understood that the disclosed system or method can be implemented in other ways. The embodiments described above are merely schematic. For example, the division of modules or units is only a logical function division. There may be other division methods in actual implementation. For example, multiple modules or units can be combined or integrated into another system, or some features can be ignored or not executed. Another point is that the mutual coupling or direct coupling or communication connection shown or discussed can be through some communication interfaces, and the indirect coupling or communication connection of systems, modules and units can be electrical, mechanical or other forms.
[0027] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present application.
Claims
1. A production process management method for macrolide derivatives of fracturing fungicides, characterized in that: The steps include: Selecting core raw materials and auxiliary raw materials for preparing macrolide derivatives; Adjust the reaction conditions and place the core raw materials and auxiliary raw materials in the reaction equipment for reaction; Monitor the reaction process in real time and precisely control the addition of core and auxiliary raw materials while ensuring a smooth and uniform reaction; After the reaction process is completed, the reaction product is separated and purified to obtain the final macrolide derivative; Adjusting the reaction conditions and placing the core raw materials and auxiliary raw materials in the reaction equipment for reaction includes the following sub-steps: Placing the core raw materials and the auxiliary raw materials in a reaction device, wherein the reaction device is a reactor; Performing an amidation reaction on the core raw material, placing the core raw material and the auxiliary raw material in a reaction device, and adjusting the reaction temperature of the reactor to a first temperature threshold; adjusting the reaction pressure in the reactor to a first pressure threshold; The pH value in the reactor is adjusted to a first pH threshold.
2. The method for managing the production process of a fracturing fungicide macrolide derivative according to claim 1, characterized in that: The selection of core raw materials and auxiliary raw materials for preparing macrolide derivatives includes the following sub-steps: The core raw material is monoethanolamine, and the auxiliary raw materials are catalysts, solvents and reaction aids; Selecting monoethanolamine with a purity greater than a first purity threshold as a core raw material; Ensure that the water content in the solvent is less than a first content threshold; When storing monoethanolamine, ensure that it is stored in dry and light-proof conditions to avoid hydrolysis or degradation; Catalysts and solvents must be stored separately to avoid cross contamination.
3. The method for managing the production process of a fracturing fungicide macrolide derivative according to claim 1, characterized in that: Real-time monitoring of the reaction process and precise control of the addition of core raw materials and auxiliary raw materials while ensuring a smooth and uniform reaction include the following sub-steps: Analyze the relationship between reaction rate and purity of derivatives based on historical monitoring data; Based on historical monitoring data, analyze the effect of the ratio of added monoethanolamine and catalyst on the reaction rate; Based on historical monitoring data, the effect of the ratio of monoethanolamine to catalyst on reaction uniformity was analyzed; Based on the relationship between the reaction rate and the purity of the derivative, the effect of the ratio of monoethanolamine to the catalyst on the reaction rate, and the effect of the ratio of monoethanolamine to the catalyst on the reaction uniformity, the addition of monoethanolamine and the catalyst is precisely controlled.
4. The method for managing the production process of a fracturing fungicide macrolide derivative according to claim 3, characterized in that: Based on historical monitoring data, the relationship between reaction rate and purity of derivatives is analyzed, including the following sub-steps: The reaction rate of monoethanolamine was calculated by the Arrhenius formula; The Arrhenius formula is , where K is the reaction rate constant, which can be used as the reaction rate, A is the frequency factor, e is the base of the natural logarithm, Ea is the activation energy, R is the molar gas constant, T is the absolute temperature, and the unit of T is Kelvin, not Celsius. The frequency factor is calculated by quantum chemical calculation method; Obtaining historical monitoring data, marked as monitoring historical data, the monitoring historical data includes historical reaction rate, historical derivative purity, historical frequency factor, historical addition ratio and historical reaction time, the historical addition ratio is the ratio of added monoethanolamine to catalyst, the historical reaction time is the time taken for monoethanolamine and catalyst to react completely and no longer send reaction; the set of historical reaction rate, historical derivative purity, historical frequency factor, historical addition ratio and historical reaction time constitutes one piece of monitoring historical data; A rectangular coordinate system is established with the historical reaction rate as the X-axis and the historical derived purity as the Y-axis, named the rate purity influence diagram, and the historical reaction rate and the historical derived purity are entered into the rate purity influence diagram; Perform regression analysis on the rate purity influence diagram to obtain the regression function with the smallest standard deviation, which is marked as the rate purity influence equation.
5. The method for managing the production process of a fracturing fungicide macrolide derivative according to claim 4, characterized in that: Based on historical monitoring data, the analysis of the effect of the ratio of added monoethanolamine and catalyst on the reaction rate includes the following sub-steps: It is easy to know from the Arrhenius formula that, under the premise of ensuring the same reaction conditions, the only factor affecting the reaction rate is the frequency factor A. A rectangular coordinate system is established with the historical addition ratio as the X-axis and the historical frequency factor as the Y-axis, named the frequency influence diagram, and the historical addition ratio and the historical frequency factor are entered into the frequency influence diagram; Perform regression analysis on the frequency influence diagram to obtain the regression function with the smallest standard deviation, which is marked as the frequency influence equation.
6. A method for managing the production process of a fracturing fungicide macrolide derivative according to claim 5, characterized in that: Based on historical monitoring data, the analysis of the effect of the ratio of added monoethanolamine and catalyst on the reaction uniformity includes the following sub-steps: Get the historical reaction rate and historical reaction time, get the minimum and maximum values of the historical reaction rate, marked as K respectively min and K max , get the minimum and maximum values of the historical reaction time, marked as S min and S max ; For any piece of historical monitoring data, the historical reaction rate is marked as KL, and the historical reaction time is marked as SL; By formula Calculate the reaction uniformity of the monitoring historical data, where RU is the reaction uniformity; A rectangular coordinate system is established with the historical addition ratio as the X-axis and the reaction uniformity as the Y-axis, named the uniformity influence diagram, and the reaction uniformity in the monitoring historical data is entered into the uniformity influence diagram according to the historical addition ratio; Perform regression analysis on the uniformity influence diagram to obtain the regression function with the smallest standard deviation, which is marked as the uniformity influence equation.
7. The method for managing the production process of a fracturing fungicide macrolide derivative according to claim 6, characterized in that: Based on the relationship between the reaction rate and the purity of the derivative, the effect of the ratio of monoethanolamine to the catalyst on the reaction rate, and the effect of the ratio of monoethanolamine to the catalyst on the reaction uniformity, precise control of the addition of monoethanolamine and the catalyst includes the following sub-steps: Get the rate purity influence equation, find the value of the X-axis corresponding to the maximum value of the Y-axis, mark it as the target rate, and represent it by the symbol TR; Based on the Arrhenius formula, the frequency factor is solved and marked as the target factor. The target factor is substituted into the frequency influence equation to solve the historical addition ratio and marked as the target addition ratio. The target addition ratio is increased by a first ratio to obtain a fluctuation upper limit, the target addition ratio is reduced by a first ratio to obtain a fluctuation lower limit, and a range interval between the fluctuation lower limit and the fluctuation upper limit is marked as a fluctuation interval; Set X in the uniformity influence equation and the frequency influence equation as the fluctuation lower limit, and mark the solved results as reference uniformity and reference frequency, represented by symbols CR and CF respectively; Get the minimum and maximum values of the Y axis in the uniformity influence equation, marked as CR respectively min and CR max ; By formula Calculate the rate stability index when X is set to the lower limit of fluctuation, where H is the rate stability index, KL is the historical reaction rate, and max() is the maximum value operator; Continue to increase the lower limit of fluctuation, and do not exceed the upper limit of fluctuation. Meanwhile, continue to calculate H, obtain the maximum value of H, mark it as the maximum index, and mark the value of X corresponding to the maximum index as the optimal addition ratio; Monoethanolamine and catalyst were added into the reactor according to the optimal addition ratio.
8. The method for managing the production process of macrolide derivatives as a fracturing fungicide according to claim 7, characterized in that: After the reaction process is completed, the reaction product is separated and purified to obtain the final macrolide derivative, which includes the following sub-steps: The macrolide derivatives were separated by liquid-liquid extraction; The macrolide derivative is purified by recrystallization to obtain the final macrolide derivative.
9. A fracturing fungicide macrolide derivative production process management system, used to implement a fracturing fungicide macrolide derivative production process management method according to any one of claims 1 to 8, characterized in that: It includes a raw material preparation module, a condition adjustment module, a reaction control module and a separation and purification module; the raw material preparation module, the condition adjustment module and the separation and purification module are respectively connected with the reaction control module data; The raw material preparation module is used to select core raw materials and auxiliary raw materials for preparing macrolide derivatives; The condition adjustment module is used to adjust the reaction conditions and place the core raw materials and auxiliary raw materials in the reaction equipment for reaction; The reaction control module is used to monitor the reaction process in real time and accurately control the addition of core raw materials and auxiliary raw materials while ensuring a smooth and uniform reaction; The separation and purification module is used to separate and purify the reaction product after the reaction process is completed to obtain the final macrocyclic lactic acid derivative; Adjusting the reaction conditions and placing the core raw materials and auxiliary raw materials in the reaction equipment for reaction includes the following sub-steps: Placing the core raw materials and the auxiliary raw materials in a reaction device, wherein the reaction device is a reactor; Performing an amidation reaction on the core raw material, placing the core raw material and the auxiliary raw material in a reaction device, and adjusting the reaction temperature of the reactor to a first temperature threshold; adjusting the reaction pressure in the reactor to a first pressure threshold; The pH value in the reactor is adjusted to a first pH threshold.
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