CN-121972110-A - Optimized regulation and control method for chloroacetone reaction preparation

CN121972110ACN 121972110 ACN121972110 ACN 121972110ACN-121972110-A

Abstract

The invention relates to the technical field of chloracetone fine reaction regulation and control, in particular to a chloracetone reaction preparation optimization regulation and control method, which comprises the following steps of S1, setting a regulation and control target and a reaction state judgment threshold, S2, collecting reaction liquid detection data, calculating to obtain chloracetone actual concentration, S3, substituting a chloracetone concentration correction logarithmic model, calculating to obtain chloracetone actual concentration, S4, substituting process adaptation type relative deviation into a chloracetone reaction state entropy scoring model, obtaining comprehensive scoring and defining a reaction grade, S5, substituting a chloracetone chlorine flow dynamic regulation and control model, calculating chlorine flow regulation, and S6, executing graded regulation and control according to the reaction grade, and finishing chloracetone product collection. The invention integrates the core factors of the chloroacetone gas-liquid two-phase reaction to realize multidimensional cooperative regulation and control, effectively solves the technical problems of regulation and control lag and unbalanced technological parameters in the traditional chloroacetone reaction regulation and control process, and remarkably improves the accuracy and real-time response capability of the chloroacetone reaction regulation and control.

Inventors

CHEN JIANQIANG
GONG LEI
WANG YONGFU
WANG CHONG
MA SHUAI
YAN HAO

Assignees

济宁正东化工有限公司

Dates

Publication Date: 20260505
Application Date: 20260202

Claims (8)

1. An optimized regulation method for preparing chloroacetone reaction is characterized by comprising the following steps: S1, determining a target concentration C 0 of chloroacetone, a reference reaction temperature T 0 , a reference mixture ratio S 0 of an acetone-choline chloride-urea eutectic solvent and an initial flow Q 0 of chlorine, incorporating a mass transfer coefficient K in a reaction kettle to construct a reaction characteristic set, and setting a regulation and control target and a reaction state judgment threshold; S2, introducing chlorine into the reaction kettle according to the initial flow to start chlorination reaction, collecting detection data of a reaction liquid, and calculating to obtain the measured concentration C m of the chloroacetone; S3, substituting the actually measured concentration C m of the chloroacetone into a chloroacetone concentration correction logarithmic model, superposing a mass transfer coefficient correction term to eliminate the cooperative interference of temperature, proportioning and mass transfer efficiency, and calculating to obtain the actual concentration C n of the chloroacetone; S4, converting the actual concentration, the real-time temperature, the real-time proportioning and the real-time mass transfer coefficient into process adaptation type relative deviation, substituting the relative deviation into a chloroacetone reaction state entropy scoring model, fusing the information entropy weight and the process core weight to obtain a comprehensive score S and defining a reaction grade; s5, matching regulation and control parameters based on reaction grades, substituting a dynamic regulation and control model of chlorine flow of chloroacetone, and superposing a chlorine dissolution coefficient The correction term is combined with the concentration deviation, the deviation change rate and the reaction state constraint factor to calculate the chlorine flow regulating quantity Q a ; And S6, performing grading regulation and control according to the reaction grade, rechecking the index and grade of the reaction characteristic set in real time, dynamically adjusting the chlorine flow, stopping chlorine introduction until the reaction reaches the standard, and completing the collection of the chloroacetone product.
2. The method for optimizing and controlling the preparation of the chloroacetone reaction according to claim 1, wherein the expression of the chloroacetone concentration correction logarithmic model in the step S3 is as follows: ; Wherein, the ; The value of the temperature correction coefficient is 0.09-0.13; The value of the correction coefficient is 0.05-0.07 for logarithmic proportioning; The correction coefficient of the logarithmic mass transfer coefficient is 0.03-0.05; as the reference mass transfer coefficient, Is a real-time mass transfer coefficient.
3. The method for optimizing and controlling the chloroacetone reaction preparation according to claim 1, wherein the calculation flow of the chloroacetone reaction state entropy scoring model in step S4 is as follows: First to the actual concentration Real-time temperature Real-time proportioning and real-time mass transfer coefficient Performing process adaptation type dimensionless treatment, and calculating objective entropy weight of each factor by adopting an information entropy weight method, wherein the information entropy calculation formula is as follows: ; Wherein, the , ; Comprises actual measurement values of mass transfer coefficients; wherein, the the core weight of the reaction concentration is more than or equal to 60 percent, and the core weight of the mass transfer coefficient is more than or equal to 15 percent; finally press The factors are calculated to couple the rights of the job, For the objective entropy weight, And (3) as the process core weight, coupling the sum of all factors to be 1, substituting the coupling weight into the index type scoring core to complete the comprehensive scoring calculation of the reaction state.
4. The method for optimizing and controlling the chloroacetone reaction preparation of claim 3, wherein in step S4, an exponential scoring core formula of the chloroacetone reaction state entropy scoring model is: ; Wherein, the , , , , Is the coupling right of concentration, temperature and proportion, For the coupling right of mass transfer coefficient, Is a concentration index-type sensitive factor, As a temperature-sensitive factor, the temperature-sensitive factor, In order to match the sensitive factor of the mixture, The mass transfer coefficient sensitivity factors are set according to the gradient of the importance of the chloroacetone process.
5. The method for preparing and optimally controlling the chloroacetone reaction according to claim 1, wherein in the step S5, a flow adjustment amount calculation formula of a dynamic chloroacetone chlorine flow adjustment model is as follows: ; Wherein, the Is used for adjusting and controlling the coefficient for the concentration deviation, For the deviation regulation and control coefficient of the mass transfer coefficient, Is used for regulating and controlling the coefficient of the temperature deviation, The chlorine dissolution coefficient is 0.85-0.95.
6. The method for preparing and optimally regulating and controlling the chloroacetone reaction according to claim 1, wherein in a dynamic regulation and control model of the flow rate of the chloroacetone chlorine, the reaction grade is divided into three grades, the one grade is normal (score is 90-100 minutes), and the flow rate of the chlorine is kept at an initial value The second level is early warning (score 70-89 points), and the second level is calculated according to a formula And small gradient regulation is carried out, the single flow regulation amplitude is less than or equal to 0.2m 3 /h, the three stages are abnormal (score <70 min), and the calculation is carried out according to a formula And performing large-scale gradient regulation, wherein the single flow regulation range is 0.2-0.5m3/h, and the reaction parameters are monitored in real time after regulation, and the reaction grade is rechecked every 30 seconds.
7. The method for optimizing and controlling the preparation of the chloroacetone according to claim 1, wherein the construction of the reaction characteristic set in the step S1 further comprises a chlorine dissolution coefficient The fluctuation threshold of each process parameter and the initial value of the model correction coefficient are set according to the process standard of the industrial production of the chloroacetone, the concentration fluctuation threshold is less than or equal to +/-0.05, the temperature fluctuation threshold is less than or equal to +/-2 ℃, the ratio fluctuation threshold is less than or equal to +/-0.03, and the mass transfer coefficient fluctuation threshold is less than or equal to +/-0.05.
8. The method for optimizing and regulating the reaction preparation of the chloroacetone according to claim 1, wherein the step S6 is characterized in that the step S6 further comprises auxiliary regulation and control of technological parameters, when the reaction grade is a secondary early warning, only the flow of chlorine is regulated, when the reaction grade is a tertiary abnormality, the stirring rate of the reaction kettle and the temperature of a heat exchange system are synchronously regulated while the flow of the chlorine is regulated, the stirring rate is regulated to be +/-50 r/min, and the temperature of the heat exchange system is regulated to be +/-3 ℃.

Description

Optimized regulation and control method for chloroacetone reaction preparation Technical Field The invention relates to the technical field of chloroacetone refining reaction regulation and control, in particular to an optimized regulation and control method for chloroacetone reaction preparation. Background The chloroacetone is an important fine chemical intermediate, is widely applied to the synthesis production in the fields of medicines, pesticides, dyes, fragrances and the like, and mainly adopts an acetone chlorination method in industrial preparation, wherein a core reaction is a gas-liquid two-phase electrophilic substitution reaction, and each technological parameter needs to be accurately regulated and controlled in the reaction process so as to ensure the purity, the yield and the production safety of a product. The traditional regulation and control mode of the chloroacetone reaction preparation is that an operator sets a reference temperature, a solvent ratio and an initial chlorine flow according to production experience, only monitors the concentration of the chloroacetone or a single parameter of the reaction temperature in the reaction process, and the chlorine flow is regulated by manual judgment, so that the concentration detection mostly adopts offline sampling analysis or simple online detection, and the reaction state is often judged to be accumulated depending on the experience of the operator. It can be seen that the existing method has the following disadvantages when in use: On one hand, apparent process parameters such as focusing temperature, proportion, concentration and the like in the traditional method do not consider the influence of gas-liquid two-phase reaction such as mass transfer coefficient, chlorine dissolution coefficient and the like in a reaction kettle, and the efficiency and stability of the chloridizing reaction of the chloroacetone are mainly determined by the gas-liquid two-phase mass transfer and dissolution process, so that the regulation and control action is disjointed from the actual reaction working condition, and the regulation and control scientificity and the accuracy are insufficient. On the other hand, the traditional concentration correction mostly adopts a linear correction method, and nonlinear interference generated by the cooperation of temperature, solvent ratio and mass transfer efficiency cannot be eliminated, so that the deviation between a concentration detection value and an actual reaction value is larger, the accuracy of subsequent reaction state judgment and parameter regulation is further influenced, and reaction fluctuation is easy to occur. Based on the method, a chloroacetone reaction preparation optimization regulation method capable of dynamically adapting to multiple production scenes is designed. Disclosure of Invention The invention aims to solve one of the technical problems, and adopts the technical scheme that the optimized regulation and control method for the chloroacetone reaction preparation comprises the following steps of S1, determining a chloroacetone target concentration C 0, a reference reaction temperature T 0, an acetone-choline chloride-urea eutectic solvent reference ratio S 0 and a chlorine initial flow Q 0, incorporating a mass transfer coefficient K in a reaction kettle to construct a reaction characteristic set, and setting a regulation and control target and a reaction state judgment threshold. S2, introducing chlorine into the reaction kettle according to the initial flow to start chlorination reaction, collecting detection data of the reaction liquid, and calculating to obtain the measured concentration C m of the chloroacetone. S3, substituting the actually measured concentration C m of the chloroacetone into a chloroacetone concentration correction logarithmic model, superposing a mass transfer coefficient correction term to eliminate the cooperative interference of temperature, proportioning and mass transfer efficiency, and calculating to obtain the actual concentration C n of the chloroacetone. S4, converting the actual concentration, the real-time temperature, the real-time proportioning and the real-time mass transfer coefficient into process adaptation type relative deviation, substituting the relative deviation into a chloroacetone reaction state entropy scoring model, fusing the information entropy weight and the process core weight to obtain a comprehensive score S and defining a reaction grade. S5, based on the reaction grade matching regulation and control parameters, substituting the regulation and control parameters into a dynamic regulation and control model of the chlorine flow of the chloroacetone, superposing a correction term of the chlorine dissolution coefficient phi, and calculating a chlorine flow regulating quantity Q a by combining the concentration deviation, the deviation change rate and the reaction state constraint factor. And S6, performing grading regulation and control a