High-yield horse oil ethyl ester preparation system based on continuous microreactor

Abstract

The invention relates to the technical field of biomass chemical industry, in particular to a high-yield horse oil ethyl ester preparation system based on a continuous microreactor, which comprises a raw material supply module, a continuous microreactor module, an online analysis module, a feedback control module and a product refining module, wherein the raw material supply module is used for providing horse oil and ethanol raw materials and removing solid impurities; the continuous microreactor module is used for carrying out esterification reaction to generate a reaction mixture; the online analysis module is used for analyzing the acid value and the free fatty acid content in real time; the feedback control module is used for calculating an optimal reaction parameter; and the product refining module is used for purifying through adsorption and distillation and outputting high-yield horse oil ethyl ester. According to the invention, by constructing a continuous micro-reaction esterification and precise purification linkage system, stable output of horse oil ethyl ester under the conditions of high conversion rate and high purity is realized, and the overall process efficiency and product quality are improved.

Description

Technical Field

[0001] This invention relates to the field of biomass chemical technology, and in particular to a high-yield horse oil ethyl ester preparation system based on a continuous microreactor. Background Technology

[0002] Horse oil, as an animal fat rich in saturated and unsaturated fatty acids, has wide applications in cosmetics, biological lubricants, and biodiesel. However, horse oil raw materials contain a high proportion of free fatty acids and impurities, which can easily lead to rancidity, increased corrosivity, or reduced product stability if used directly. Therefore, horse oil usually needs to be converted into ester derivatives to improve its stability and application performance.

[0003] Esterification is a common method for converting horse oil, but traditional batch reaction processes suffer from drawbacks such as long reaction times, large fluctuations in conversion rates, and low product purity, making it difficult to meet the demands for efficient, continuous, and controllable production. In particular, there is a significant gap in the real-time monitoring and feedback control of acid value and free fatty acids on a microreactor platform. Furthermore, the removal of residual impurities in the reaction products relies on multi-stage separation processes, which are cumbersome and result in low yields. Therefore, there is an urgent need for a high-yield horse oil ethyl ester preparation system based on a continuous microreactor to achieve high-yield, high-purity product output and meet the needs of practical industrial applications. Summary of the Invention

[0004] To achieve the above objectives, the present invention provides a high-yield horse oil ethyl ester preparation system based on a continuous microreactor.

[0005] A high-yield system for preparing ethyl horse oil based on a continuous microreactor includes a raw material supply module, a continuous microreactor module, an online analysis module, a feedback control module, and a product purification module; wherein: Raw material supply module: Used to supply horse oil and ethanol raw materials, and to perform preliminary filtration of the raw materials to remove solid impurities; Continuous microreactor module: connected to the raw material supply module, used to receive filtered raw materials and carry out esterification reaction to generate reaction mixture; Online analysis module: Connected to the continuous microreactor module, it is used to receive the reaction mixture and analyze its acid value and free fatty acid content in real time; Feedback control module: Connected to the online analysis module, it calculates the optimal reaction parameters based on the acid value and free fatty acid content obtained from the analysis, and outputs adjustment signals to the continuous microreactor module to dynamically adjust the reaction temperature and time; Product refining module: Connected to the continuous microreactor module, it receives the reaction mixture output by the continuous microreactor module under the control of adjusted reaction parameters, and purifies it through adsorption and distillation to output high-yield ethyl horse oil.

[0006] Optionally, the raw material supply module includes a raw material storage unit, a metering and conveying unit, and a pre-filtration unit; wherein: Raw material storage unit: used to store horse oil and ethanol raw materials separately, maintain the independent storage state of the raw materials through sealed storage tanks, and output horse oil and ethanol to downstream under predetermined pressure conditions; Metering and conveying unit: connected to the raw material storage unit, used to meter and control the flow rate of horse oil and ethanol according to the set ratio, and to send the two raw materials into the pre-filtration unit through independent conveying channels. Pre-filtration unit: Connected to the metering and conveying unit, it is used to perform preliminary filtration of the incoming horse oil and ethanol, removing solid particulate impurities through a filter screen structure with a fixed pore size.

[0007] Optionally, the continuous microreactor module includes a raw material mixing unit, a microchannel reaction unit, and an outlet collection unit; wherein: Raw material mixing unit: A pre-filtration unit connected to the raw material supply module, used to receive filtered horse oil and ethanol raw materials respectively, and to stably mix the two raw materials in the inlet section by setting the flow rate ratio, so that the composition of the material entering the reaction channel remains constant; Microchannel reaction unit: connected to the raw material mixing unit, used to carry out esterification reaction of mixed raw materials under continuous flow conditions to form a reaction mixture containing ethyl horse oil, unreacted raw materials and by-products; Outlet collection unit: Connected to the microchannel reaction unit, it is used to collect the reaction mixture fluid after the reaction has been completed at the microchannel outlet and stably deliver it to the online analysis module.

[0008] Optionally, the microchannel reaction unit includes: Heating control subunit: Used to provide a constant heating environment for the microchannel reaction zone. Through an electric heating structure arranged close to the microchannel wall, the reaction zone is maintained within the set esterification temperature range. Microchannel flow channel subunit: connected to the heating control subunit, its structure consists of multiple parallel microscale straight flow channels. Each flow channel has a fixed width and depth, which allows the mixed raw materials of horse oil and ethanol to be continuously advanced in a single direction in the flow channel and achieve sufficient interfacial contact under high specific surface area conditions, thereby continuously causing esterification reaction in the flow path and gradually generating a reaction fluid containing esterification products. Residence time adjustment subunit: connected to the outlet of the microchannel flow channel subunit. By adjusting the microchannel length and flow control mode, the reaction system is kept within the microchannel for a set residence time, so that the raw materials have completed the main esterification reaction and formed a reaction mixture by the time they flow to the outlet section.

[0009] Optionally, the online analysis module includes a sampling and dispensing unit, an acid value detection unit, and a free fatty acid detection unit; wherein: Sampling and dispensing unit: Connected to the outlet collection unit of the continuous microreactor module, it is used to extract the flowing sample in a proportional manner from the continuously output reaction mixture stream, and deliver the sample to the acid value detection unit and the free fatty acid detection unit in a fixed proportion through the internal dispensing structure. Acid value detection unit: connected to the sampling and dispensing unit, used to detect the acid value of the input sample in real time. It quantifies the concentration of acidic components in the sample through the built-in potentiometric titration measurement structure and generates corresponding acid value data based on the detection signal. Free fatty acid detection unit: Connected to the sampling and dispensing unit, it is used to analyze the free fatty acid content of the input sample in real time. It continuously measures the concentration of free fatty acids in the reaction mixture through a spectroscopic absorption spectrometer and outputs the corresponding content data.

[0010] Optionally, the acid value detection unit includes: Titration reaction subunit: Used to automatically titrate the input sample with a set concentration of alkaline titrant in a reaction cell, so that the acidic components in the sample react chemically with the titrant, thus creating stable reaction conditions for potential change detection; Titration electrode measurement subunit: used to detect the potential change of the reaction system in real time during titration, determine the endpoint state of titration by the potential difference between the built-in reference electrode and the indicator electrode, record the volume of titrant consumed to reach the titration endpoint, and generate the corresponding potential measurement signal; Acid value calculation subunit: Used to calculate the acid value of the sample based on the potential signal at the titration endpoint and the volume of titrant consumed. The formula is: ,in, The acid value of the sample; This refers to the concentration of the titrant. This represents the volume of titrant consumed when the titration reaches the endpoint. The value represents the sample mass; the value 56.1 is a constant for acid value conversion.

[0011] Optionally, the free fatty acid detection unit includes: Light source emission subunit: used to provide incident light within a stable wavelength range to the colorimetric channel containing the reaction mixture sample; Colorimetric reaction subunit: used to contact the incoming reaction mixture sample with a preset colorimetric reagent in the flow colorimetric cell, so that the free fatty acids and the colorimetric reagent undergo a quantitative colorimetric reaction to form a colorimetric solution with specific spectral absorption characteristics; Spectral acquisition subunit: used to continuously acquire the transmitted light intensity of the colorimetric solution at a position downstream of the colorimetric channel. The transmitted light is received by a photodetector set at the outlet of the colorimetric cell, and the light intensity signal is converted into the corresponding absorbance data sequence to form spectral measurement data related to free fatty acids. Content calculation subunit: Used to calculate the concentration of free fatty acids based on the collected absorbance data. It converts the absorbance and concentration of the sample based on the Beer-Lambert law to obtain the concentration of free fatty acids. .

[0012] Optionally, the feedback control module includes a data integration unit, a parameter determination unit, and a control command generation unit; wherein: Data integration unit: used to receive acid value data and free fatty acid content data, and to synchronously integrate the two according to the time series to form a dataset of the current reaction state; Parameter determination unit: Based on the integrated dataset, the reaction system state is judged. The acid value change trend and the deviation of free fatty acid content are analyzed through the preset reaction model to determine whether the current reaction is in the optimal range, and the appropriate reaction temperature and reaction residence time adjustment amount are derived accordingly. Control command generation unit: Used to generate corresponding control commands based on the determined reaction parameter adjustment amount, and output the control commands to the continuous microreactor module, so that the reaction temperature and flow control structure can be dynamically adjusted according to the adjustment amount.

[0013] Optionally, the parameter determination unit includes: Trend Analysis Subunit: Used to receive time series data of acid value and free fatty acid concentration from the data integration subunit, analyze their changing trends, and identify whether the current reaction is trending away from the stable range by calculating short-term and medium-term change rates. Deviation identification subunit: It is used to compare the currently collected acid value and free fatty acid concentration with the set optimal reference value, determine whether the current reaction state is within the preset tolerance range, and output the deviation direction and deviation magnitude. Adjustment Amount Derivation Subunit: Used to derive the required adjustment amount of reaction temperature and reaction residence time based on the deviation magnitude and trend direction. By calling the parameter adjustment mapping table and combining it with the current reaction parameters, it outputs the corresponding optimal combination of reaction parameters.

[0014] Optionally, the product refining module includes an adsorption purification unit and a distillation separation unit; wherein: Adsorption purification unit: connected to the outlet of the continuous microreactor module, used to introduce the reaction mixture fluid into the adsorption bed, and remove impurities and polar components in the mixture by fixing the adsorption material; the fixed adsorption material includes activated carbon particles, alumina or natural zeolite; Distillation and separation unit: connected to the adsorption and purification unit, used to heat and distill the purified mixture. By controlling the temperature of the column bottom and the gas-liquid balance in the column, ethyl horse oil is separated from residual ethanol and unreacted components, and the purified ethyl horse oil product is output at the top or side stream position.

[0015] The beneficial effects of this invention are: This invention, by constructing an integrated system including raw material supply, continuous microreactor, online analysis, feedback control and product refining, achieves stable supply of horse oil and ethanol raw materials, continuous esterification reaction in microchannels, real-time detection of acid value and free fatty acids, and dynamic adjustment of reaction parameters. This makes the esterification reaction process continuous, efficient and controllable, significantly improving the reaction conversion rate and process stability.

[0016] This invention, by setting up a purification process that combines adsorption purification and distillation separation, effectively removes polar impurities and byproducts from the reaction mixture, ensuring stable purity and good yield of ethyl horse oil product, and improving the overall automation level and industrial adaptability of the system. Attached Figure Description

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

[0018] Figure 1 This is a schematic diagram of the high-yield horse oil ethyl ester preparation system according to an embodiment of the present invention; Figure 2 This is a schematic diagram of the online analysis module in an embodiment of the present invention. Detailed Implementation

[0019] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments. It should also be noted that, to make the embodiments more comprehensive, the following embodiments are the best and preferred embodiments, and those skilled in the art can use other alternative methods to implement some well-known technologies; moreover, the accompanying drawings are only for more specific description of the embodiments and are not intended to specifically limit the present invention.

[0020] It should be noted that the use of terms such as "an embodiment," "an embodiment," "an exemplary embodiment," and "some embodiments" in the specification indicates that the described embodiment may include a specific feature, structure, or characteristic, but not every embodiment necessarily includes that specific feature, structure, or characteristic. Furthermore, when a specific feature, structure, or characteristic is described in connection with an embodiment, implementing such a feature, structure, or characteristic in conjunction with other embodiments (whether explicitly described or not) should be within the knowledge of those skilled in the art.

[0021] Generally, terms can be understood at least partly from their use in context. For example, depending at least partly on the context, the term "one or more" as used herein can be used to describe any feature, structure, or characteristic in a singular sense, or a combination of features, structures, or characteristics in a plural sense. Additionally, the term "based on" can be understood not necessarily to convey an exclusive set of factors, but rather, alternatively, depending at least partly on the context, to allow for the presence of other factors that are not necessarily explicitly described.

[0022] like Figures 1-2 As shown, a high-yield horse oil ethyl ester preparation system based on a continuous microreactor includes a raw material supply module, a continuous microreactor module, an online analysis module, a feedback control module, and a product refining module; wherein: Raw material supply module: Used to supply horse oil and ethanol raw materials, and to perform preliminary filtration of the raw materials to remove solid impurities; Continuous microreactor module: connected to the raw material supply module, used to receive filtered raw materials and carry out esterification reaction to generate reaction mixture; Online analysis module: Connected to the continuous microreactor module, it is used to receive the reaction mixture and analyze its acid value and free fatty acid content in real time; Feedback control module: Connected to the online analysis module, it calculates the optimal reaction parameters based on the acid value and free fatty acid content obtained from the analysis, and outputs adjustment signals to the continuous microreactor module to dynamically adjust the reaction temperature and time; Product refining module: Connected to the continuous microreactor module, it receives the reaction mixture output by the continuous microreactor module under the control of adjusted reaction parameters, and purifies it through adsorption and distillation to output high-yield ethyl horse oil.

[0023] The raw material supply module includes a raw material storage unit, a metering and conveying unit, and a pre-filtration unit; wherein: Raw material storage unit: used to store horse oil and ethanol raw materials separately, maintain the independent storage state of the raw materials through sealed storage tanks, and output horse oil and ethanol to downstream at a controllable flow rate under predetermined pressure conditions; Metering and conveying unit: connected to the raw material storage unit, used to meter and control the flow rate of horse oil and ethanol according to the set ratio, and to send the two raw materials into the pre-filtration unit through independent conveying channels to ensure the stability of the raw material ratio entering the continuous microreactor module. Pre-filtration unit: Connected to the metering and conveying unit, it is used to perform preliminary filtration on the incoming horse oil and ethanol. It removes solid particulate impurities through a filter screen structure with a fixed pore size, keeping the raw materials entering the continuous microreactor module in a clean fluid state. Through the above structural setup, the raw material supply module can form a stable raw material input link adapted to the continuous microreactor module through hierarchical management, metering and conveying, and continuous pre-filtration.

[0024] The continuous microreactor module includes a raw material mixing unit, a microchannel reaction unit, and an outlet collection unit; wherein: Raw material mixing unit: A pre-filtration unit connected to the raw material supply module, used to receive filtered horse oil and ethanol raw materials respectively, and to stably mix the two raw materials in the inlet section by setting the flow rate ratio, so that the composition of the material entering the reaction channel remains constant; Microchannel reaction unit: connected to the raw material mixing unit, used to carry out esterification reaction of mixed raw materials under continuous flow conditions. Its interior is composed of microscale flow channels with high specific surface area. The raw materials flow directionally along the microchannels under set temperature and residence time conditions, so that the esterification reaction is completed during the flow process, and a reaction mixture containing ethyl horse oil, unreacted raw materials and by-products is gradually formed. Outlet collection unit: Connected to the microchannel reaction unit, it is used to collect the reaction mixture fluid after the reaction has been completed at the microchannel outlet and stably deliver it to the online analysis module for subsequent acid value and free fatty acid content detection. With the above structural configuration, the continuous microreactor module can form a continuous reaction system suitable for subsequent online analysis and feedback control under the coordination of stable flow input, microchannel reaction propulsion and continuous product outflow.

[0025] The microchannel reaction unit includes: Heating control subunit: Used to provide a constant heating environment for the microchannel reaction zone. Through the electric heating structure arranged close to the microchannel wall, the reaction zone is maintained within the set esterification temperature range to ensure that the mixed raw materials are immediately in a stable reaction temperature state at the channel inlet. Microchannel flow channel subunit: connected to the heating control subunit, its structure consists of multiple parallel microscale straight flow channels. Each flow channel has a fixed width and depth, which allows the mixed raw materials of horse oil and ethanol to be continuously advanced in a single direction in the flow channel and achieve sufficient interfacial contact under high specific surface area conditions, thereby continuously causing esterification reaction in the flow path and gradually generating a reaction fluid containing esterification products. Residence time adjustment subunit: Connected to the outlet of the microchannel flow channel subunit, it maintains a set residence time within the microchannel by adjusting the microchannel length and flow control method, ensuring that the raw materials have completed the main esterification reaction and formed a reaction mixture by the time they flow to the outlet section. Based on the above structural setup, the microchannel reaction unit, through isothermal heating, directional flow channel reaction, and controllable continuous advancement of residence time, ensures that the esterification reaction is stably completed within the structured channel, providing a continuous and compositionally stable reaction mixture fluid for subsequent online analysis.

[0026] The online analysis module includes a sampling and dispensing unit, an acid value detection unit, and a free fatty acid detection unit; among which: Sampling and dispensing unit: Connected to the outlet collection unit of the continuous microreactor module, it is used to extract the flowing sample in a proportional manner from the continuously output reaction mixture stream, and deliver the sample to the acid value detection unit and the free fatty acid detection unit in a fixed proportion through the internal dispensing structure, so that the subsequent detection steps can maintain a stable sample source. Acid value detection unit: connected to the sampling and distribution unit, used to detect the acid value of the input sample in real time. It quantifies the concentration of acidic components in the sample through the built-in potentiometric titration measurement structure, and generates corresponding acid value data based on the detection signal for the feedback control module to perform parameter calculation. Free fatty acid detection unit: Connected to the sampling and distribution unit, it is used to analyze the free fatty acid content of the input sample in real time. It continuously measures the concentration of free fatty acids in the reaction mixture through a spectroscopic absorption measurement structure and outputs the corresponding content data, enabling the system to obtain the real-time fatty acid changes in the reaction system. Through the above structural settings, the online analysis module, through the synergistic effect of sampling and distribution and dual-channel independent detection, enables the acid value and free fatty acid content to be continuously quantified during the reaction process, providing reliable real-time analysis data for feedback control.

[0027] The acid value detection unit includes: Titration reaction subunit: Used to automatically titrate the input sample with a set concentration of alkaline titrant in a reaction cell, so that the acidic components in the sample react chemically with the titrant, thus creating stable reaction conditions for potential change detection; Titration electrode measurement subunit: used to detect the potential change of the reaction system in real time during titration, determine the endpoint state of titration by the potential difference between the built-in reference electrode and the indicator electrode, record the volume of titrant consumed to reach the titration endpoint, and generate the corresponding potential measurement signal; Acid value calculation subunit: Used to calculate the acid value of the sample based on the potential signal at the titration endpoint and the volume of titrant consumed. The formula is: ,in, The acid value of the sample; This refers to the concentration of the titrant. This represents the volume of titrant consumed when the titration reaches the endpoint. The value is the mass of the sample; the value 56.1 is the constant for acid value conversion; through the above structural settings, the acid value detection unit can stably quantify the acidic components in the reaction mixture through continuous operation of titration reaction, potential endpoint identification and acid value calculation, providing accurate acid value data input for the feedback control module.

[0028] The free fatty acid detection unit includes: Light source emission subunit: used to provide incident light within a stable wavelength range to the colorimetric channel containing the reaction mixture sample, and to illuminate the sample through the emission light path of the preset wavelength so that the light absorption characteristics of the free fatty acid and the colorimetric system can be stably excited. Colorimetric reaction subunit: Used to contact the incoming reaction mixture sample with a preset colorimetric reagent in the flow colorimetric cell, so that the free fatty acids and the colorimetric reagent undergo a quantitative colorimetric reaction to form a colorimetric solution with specific spectral absorption characteristics, and to maintain the stability of the material composition in the colorimetric reaction area under continuous flow conditions; Spectral acquisition subunit: used to continuously acquire the transmitted light intensity of the colorimetric solution at a position downstream of the colorimetric channel. The transmitted light is received by a photodetector set at the outlet of the colorimetric cell, and the light intensity signal is converted into the corresponding absorbance data sequence to form spectral measurement data related to free fatty acids. Content calculation subunit: Used to calculate the concentration of free fatty acids based on the collected absorbance data. It converts the absorbance and concentration of the sample based on the Beer-Lambert law to obtain the concentration of free fatty acids. The conversion formula is: ,in, This represents the concentration of free fatty acids. The absorbance value obtained by the spectral acquisition subunit; The pre-calibrated molar absorptivity; The optical path length of the colorimetric channel; through the above structural setup, the free fatty acid detection unit, through the continuous coordination of colorimetric reaction, spectral acquisition and content calculation, converts the concentration of free fatty acids in the reaction mixture into continuously output content data, providing a stable online detection input for the feedback control module.

[0029] The feedback control module includes a data integration unit, a parameter determination unit, and a control command generation unit; wherein: Data integration unit: Used to receive acid value data and free fatty acid content data, and to integrate the two in a synchronous manner according to the time series to form a dataset of the current reaction state, providing a unified data basis for the determination of subsequent reaction parameters; Parameter determination unit: Based on the integrated dataset, the reaction system state is judged. The acid value change trend and the deviation of free fatty acid content are analyzed through the preset reaction model to determine whether the current reaction is in the optimal range, and the appropriate reaction temperature and reaction residence time adjustment amount are derived accordingly. The control command generation unit is used to generate corresponding control commands based on the determined adjustment amount of the reaction parameters, and output the control commands to the continuous microreactor module. This enables the reaction temperature and flow control structure to be dynamically adjusted according to the adjustment amount, realizing closed-loop control of the reaction process parameters. Through the above structure, the feedback control module, through continuous processing of data integration, parameter judgment and command generation, enables the reaction conditions to be dynamically corrected based on real-time analysis results, ensuring that the subsequent continuous microreactor module is in a controllable reaction operation state.

[0030] The parameter determination unit includes: Trend Analysis Subunit: Receives time-series data on acid value and free fatty acid concentration from the data integration subunit, analyzes their trends, and identifies whether the current reaction is trending away from its stable range by calculating short-term and medium-term change rates. The trend change rate is calculated using the following formula: ; ;in, This represents the rate of change in acid value. This represents the rate of change in free fatty acids; The acid value at the current moment; Time interval The acid value before; This represents the current concentration of free fatty acids; Time interval The concentration of free fatty acids before; For time intervals; Deviation identification subunit: This unit compares the currently collected acid value and free fatty acid concentration with the set optimal reference values ​​to determine whether the current reaction state is within the preset tolerance range. It also outputs the direction and magnitude of the deviation to quantify the degree of non-optimality in the reaction state. The deviation magnitude is calculated using the following formula: ; ,in, This is due to acid value deviation; This refers to the deviation in free fatty acid concentration; This is a reference value for acid value; This is a reference value for free fatty acid concentration; The adjustment amount derivation subunit is used to derive the required adjustment amounts for the reaction temperature and residence time based on the deviation magnitude and trend direction. By calling the parameter adjustment mapping table and combining it with the current reaction parameters, it outputs the corresponding optimal combination of reaction parameters, providing control input for the control command generation subunit. The temperature adjustment amount and residence time adjustment amount are calculated using the following expressions: ; ;in, This is the amount to adjust the reaction temperature; This is an adjustment amount for the reaction residence time; This refers to the parameter adjustment coefficient; This is due to acid value deviation; The structured parameter determination mechanism, which calculates the trend change rate, quantifies the deviation, and derives the adjustment amount, enables the feedback control module to calculate and determine the adjustment amount based on real-time data, forming a clear basis for reaction regulation and realizing the adaptive update of continuous flow esterification reaction conditions.

[0031] The product refining module includes an adsorption purification unit and a distillation separation unit; wherein: Adsorption purification unit: Connected to the outlet of the continuous microreactor module, it is used to introduce the reaction mixture fluid into the adsorption bed, remove impurities and polar components in the mixture by fixing the adsorption material, so that the subsequent distillation material maintains a stable composition; the fixed adsorption material includes activated carbon particles, alumina or natural zeolite; Distillation and separation unit: Connected to the adsorption and purification unit, it is used to heat and distill the purified mixture. By controlling the temperature of the column bottom and the gas-liquid balance in the column, it separates ethyl oleate from residual ethanol and unreacted components, and outputs the purified ethyl oleate product at the top or side stream position. Based on the above structure, the product purification module can convert the reaction mixture into a high-purity ethyl oleate product that can be directly collected through continuous processing of adsorption to remove impurities and distillation to separate target components.

[0032] This invention encompasses any substitutions, modifications, equivalent methods, and solutions made within the spirit and scope of this invention. To provide the public with a thorough understanding of this invention, specific details are described in detail in the following preferred embodiments; however, those skilled in the art will fully understand the invention even without these details. Furthermore, to avoid unnecessary misunderstanding of the essence of this invention, well-known methods, processes, procedures, components, and circuits are not described in detail.

[0033] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A high yield horse oil ethyl ester preparation system based on a continuous microreactor, characterized by, The system comprises a raw material supply module, a continuous micro-reactor module, an online analysis module, a feedback control module, and a product refining module. The raw material supply module is used to provide horse oil and ethanol raw materials and to preliminarily filter the raw materials to remove solid impurities. The continuous micro-reactor module is connected to the raw material supply module and is used to receive the filtered raw materials and perform esterification reactions to generate a reaction mixture. The online analysis module is connected to the continuous micro-reactor module and is used to receive the reaction mixture and analyze its acid value and free fatty acid content in real time. The feedback control module is connected to the online analysis module and is used to calculate optimal reaction parameters based on the analyzed acid value and free fatty acid content and output adjustment signals to the continuous micro-reactor module to dynamically adjust the reaction temperature and time. The product refining module is connected to the continuous micro-reactor module and is used to receive the reaction mixture output by the continuous micro-reactor module under the control of the adjusted reaction parameters, purify the reaction mixture through adsorption and distillation, and output horse oil ethyl ester with high yield.

2. A high yield horse oil ethyl ester preparation system based on a continuous microreactor according to claim 1, characterized in that, The raw material supply module comprises a raw material storage unit, a metering and conveying unit, and a pre-filtering unit. The raw material storage unit is used to store horse oil and ethanol raw materials separately, maintain the independent storage state of the raw materials through sealed storage tanks, and output the horse oil and ethanol under predetermined pressure conditions. The metering and conveying unit is connected to the raw material storage unit and is used to meter and control the flow of horse oil and ethanol according to the set ratio, and send the two raw materials into the pre-filtering unit through independent conveying channels. The pre-filtering unit is connected to the metering and conveying unit and is used to preliminarily filter the incoming horse oil and ethanol, and remove solid particle impurities through a filter screen structure with fixed pore size.

3. A high yield horse oil ethyl ester preparation system based on a continuous microreactor according to claim 1, characterized in that, The continuous micro-reactor module comprises a raw material mixing unit, a micro-channel reaction unit, and an outlet collection unit. The raw material mixing unit is connected to the pre-filtering unit of the raw material supply module and is used to receive the filtered horse oil and ethanol raw materials separately and stably mix the two raw materials at the inlet section through a set flow ratio to maintain a constant composition of the material entering the reaction channel. The micro-channel reaction unit is connected to the raw material mixing unit and is used to perform esterification reactions on the mixed raw materials under continuous flow conditions to form a reaction mixture containing horse oil ethyl ester, unreacted raw materials, and by-products. The outlet collection unit is connected to the micro-channel reaction unit and is used to collect the reaction mixture fluid that has completed the reaction at the micro-channel outlet and stably convey it to the online analysis module.

4. The high yield horse oil ethyl ester preparation system based on continuous microreactor according to claim 3, characterized in that, The micro-channel reaction unit comprises: A heating control subunit is used to provide a constant heating environment for the micro-channel reaction zone by arranging an electric heating structure close to the micro-channel wall layer to maintain the reaction zone within a set esterification temperature range. A micro-channel flow channel subunit is connected to the heating control subunit and is composed of multiple parallel micro-scale straight flow channels, each flow channel having a fixed width and depth, so that the mixed raw materials of horse oil and ethanol continuously advance in a single direction within the flow channel and achieve sufficient interfacial contact under high specific surface area conditions, thereby continuously generating esterification reactions in the flow path to gradually generate a reaction fluid containing esterification products. Residence time adjusting subunit: connected with the outlet of the microchannel flow passage subunit, by adjusting the length of the microchannel and the flow control mode, the reaction system is kept in the microchannel for a set residence time, so that the raw materials complete the main esterification reaction and form a reaction mixture before flowing to the outlet section.

5. The high yield horse oil ethyl ester preparation system based on continuous microreactor according to claim 1, characterized in that, The online analysis module comprises a sampling distribution unit, an acid value detection unit and a free fatty acid detection unit; wherein: The sampling distribution unit is connected to the outlet collection unit of the continuous micro-reactor module, and is used for extracting a flow sample in a fixed proportion from the continuously output reaction mixture flow, and conveying the sample to the acid value detection unit and the free fatty acid detection unit in a fixed proportion through an internal distribution structure; The acid value detection unit is connected with the sampling distribution unit, and is used for real-time detection of the acid value of the input sample, quantifying the concentration of acidic components in the sample through the built-in potential titration measurement structure, and generating corresponding acid value data based on the detection signal; The free fatty acid detection unit is connected with the sampling distribution unit, and is used for real-time analysis of the free fatty acid content of the input sample, continuously measuring the concentration of free fatty acid in the reaction mixture through the spectral absorption measurement structure, and outputting the corresponding content data.

6. A high yield horse oil ethyl ester preparation system based on a continuous microreactor according to claim 5, characterized in that, The acid value detection unit comprises: The titration reaction subunit is used for automatic titration of the input sample with a set concentration of alkaline titrant in the reaction cell, so that the acidic components in the sample react with the titrant to form a stable reaction condition for potential change detection; The titration electrode measurement subunit is used for real-time detection of the potential change of the reaction system during titration, determines the end point state of titration through the potential difference between the built-in reference electrode and the indicating electrode, records the volume of titrant consumed to reach the titration end point, and generates corresponding potential measurement signal; Acid value calculation subunit: used to calculate the acid value of the sample according to the potential signal of the titration end point and the consumption volume of the titrant, the formula is: wherein, is the acid value of the sample; is the substance concentration of the titrant; is the consumption volume of the titrant when titration is to the end point; is the mass of the sample; the numerical value 56.1 is a constant for acid value conversion.

7. A high yield horse oil ethyl ester preparation system based on a continuous microreactor according to claim 6, characterized in that, The free fatty acid detection unit comprises: The light source emission subunit is used for providing incident light in a stable wavelength range to the colorimetric channel loaded with the reaction mixture sample; The colorimetric reaction subunit is used for contacting the flowing reaction mixture sample with the pre-set color developing reagent in the flow-through colorimetric cell, so that the free fatty acid reacts with the color developing reagent to form a colorimetric solution with specific spectral absorption characteristics; The spectral acquisition subunit is used for continuously collecting the transmitted light intensity of the colorimetric solution at the downstream position of the colorimetric channel, receiving the transmitted light through the photodetector arranged at the outlet position of the colorimetric cell, and converting the light intensity signal into corresponding absorbance data sequence to form the spectral measurement data related to the free fatty acid; The content calculation subunit is configured to calculate the free fatty acid concentration according to the collected absorbance data, convert the relationship between the absorbance of the sample and the concentration based on the Beer-Lambert law to obtain the substance concentration of the free fatty acid. .

8. The high yield horse oil ethyl ester preparation system based on continuous microreactor according to claim 1, characterized in that, The feedback control module comprises a data integration unit, a parameter determination unit and a control instruction generation unit; wherein: The data integration unit is used for receiving the acid value data and the free fatty acid content data, and synchronously integrating them according to the time sequence to form a data set of the current reaction state; The parameter determination unit judges the reaction system state based on the integrated data set, analyzes the acid value change trend and the free fatty acid content deviation through the pre-set reaction model, determines whether the current reaction is in the optimal interval, and deduces the adaptive reaction temperature and reaction residence time adjusting amount accordingly; The control instruction generation unit is configured to generate a corresponding control instruction according to the adjustment amount of the determined reaction parameter, and output the control instruction to the continuous micro-reactor module, so that the reaction temperature and flow control structure are dynamically adjusted according to the adjustment amount.

9. The high yield horse oil ethyl ester preparation system based on continuous microreactor according to claim 8, characterized in that, The parameter determination unit comprises: The trend analysis subunit is configured to receive the time series data of the acid value and the free fatty acid concentration transmitted by the data integration subunit, analyze the change trend thereof, identify whether the current reaction has a change trend deviating from the stable interval by calculating short-term and medium-term change rates, and output the deviation direction and the deviation amplitude. The deviation recognition subunit is configured to compare the currently collected acid value and free fatty acid concentration with the set optimal reference value, judge whether the current reaction state is within the preset tolerance range, and output the deviation direction and the deviation amplitude. The adjustment amount derivation subunit is configured to derive the required reaction temperature adjustment amount and reaction residence time adjustment amount according to the deviation amplitude and the trend direction, output the corresponding optimal reaction parameter combination by calling a parameter adjustment mapping table and combining the current reaction parameters.

10. The high yield horse oil ethyl ester preparation system based on continuous microreactor according to claim 1, characterized in that, The product refining module comprises an adsorption purification unit and a distillation separation unit; wherein: The adsorption purification unit is connected to the outlet of the continuous micro-reactor module, configured to guide the reaction mixture fluid into the adsorption bed layer, and remove the impurity polar components in the mixture by fixed adsorption material; the fixed adsorption material comprises activated carbon particles, aluminum oxide or natural zeolite; The distillation separation unit is connected with the adsorption purification unit, configured to heat and distill the purified mixture, separate the horse oil ethyl ester, residual ethanol and unreacted components by controlling the column bottom temperature and the column gas-liquid equilibrium, and output the purified horse oil ethyl ester product at the top or side line position.

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