Intelligent control method for continuous production of ceric ammonium nitrate precipitation process and application

By using intelligent control methods to monitor and adjust the dripping rates of hydrogen peroxide and ammonia in real time, the problem of unstable quality in the cerium ammonium nitrate precipitation process was solved, achieving stability and automated recovery of continuous production and ensuring product quality.

CN120871797AActive Publication Date: 2025-10-31LESHAN DONGCHEN ADVANCED MATERIAL

Patent Information

Application Number
CN202511394148.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-28
Publication Date
2025-10-31
Estimated Expiration
2045-09-28

AI Technical Summary

Technical Problem

The existing continuous production control methods for the cerium ammonium nitrate precipitation process suffer from unstable quality, difficulty in controlling sampling time, and slow analysis speed, resulting in a high frequency of product quality defects.

Method used

The system employs an intelligent control method, using a potential sensor to monitor the reaction process in real time. The server adjusts the dripping rate of hydrogen peroxide and ammonia based on the potential deviation, and combined with heating and valve control, it achieves automatic adjustment to ensure the stability of the reaction process.

Benefits of technology

Stable production of the cerium ammonium nitrate precipitation process was achieved, preventing unqualified products from entering the next process. Furthermore, production could be adjusted and restored in a timely manner under abnormal circumstances, ensuring the overall quality stability of the process.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses an intelligent control method for ceric ammonium nitrate precipitation process continuous production and application, and belongs to the field of intelligent production control, the intelligent control method comprises a hydrogen peroxide section intelligent control method and an ammonia water section intelligent control method, and the method comprises the steps that S1, a server receives V2; s2, a second potential sensor sends V2 ''; the server makes X2 = V2 '-V2, if the absolute value of X2 is within the threshold value, production continues, and if the absolute value of X2 is outside the threshold value, an alarm instruction is output; m1, the server receives the V3; and M2, the third potential sensor sends V3 ''to the server, the server makes X3 = V3''-V3, if the absolute value of X3 is within the threshold value, production continues, and if the absolute value of X3 is outside the threshold value, an alarm instruction is output. The reaction process is intelligently controlled, the process is adjusted in time, unqualified products are prevented from entering the next procedure, and stable quality of the whole procedure is guaranteed.
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Description

Technical Field

[0001] This invention relates to the field of intelligent production control, and more specifically, to an intelligent control method and application for continuous production of cerium ammonium nitrate precipitation process. Background Technology

[0002] Most existing cerium ammonium nitrate precipitation processes are batch processes, that is, hydrogen peroxide is added to the reactor first and reacted completely before ammonia is added to react. Very few use tubular reactors for continuous reactions.

[0003] The existing continuous reaction production, which is rare, controls the production by setting the flow rate of trivalent Ce ion solution per unit time, calculating the required hydrogen peroxide and ammonia drop rates based on theoretical values, taking samples from the discharge pipe of the tubular reactor for chemical analysis, and adjusting the hydrogen peroxide and ammonia drop rates based on the chemical analysis results. On the one hand, the sampling time is difficult to control, and on the other hand, the analysis speed is slow, resulting in unstable quality in subsequent processes and a high frequency of quality defects.

[0004] The above background information is provided to facilitate understanding of the present invention and is not intended to be publicly known technology disclosed to the general public prior to the application of this invention. Summary of the Invention

[0005] To address the aforementioned problems, this invention provides an intelligent control method for continuous production of cerium ammonium nitrate precipitation process. This method intelligently controls the reaction process, adjusts the process in a timely manner, prevents substandard products from entering the next process, and ensures the stability of the quality throughout the entire process.

[0006] A smart control method for continuous production of cerium ammonium nitrate precipitation process includes a smart control method for the hydrogen peroxide section and a smart control method for the ammonia section, wherein: The intelligent control method for the hydrogen peroxide section includes the following steps: S1, The server receives the set target potential value of the site after the hydrogen peroxide segment reaction, and the target potential value of the site after the hydrogen peroxide segment reaction is recorded as V2; S2, the second potential sensor sends the first real-time potential value of the second potential sensor to the server, the server receives the first real-time potential value of the second potential sensor, the first real-time potential value of the second potential sensor is recorded as V2"; the server sets X2 = V2" - V2, if the absolute value of X2 is within the threshold, production continues, if the absolute value of X2 is outside the threshold, an alarm command is output; The intelligent control method for the ammonia water section includes the following steps: M1, The server receives the set target potential value of the site after the ammonia water section reaction, and the target potential value of the site after the ammonia water section reaction is recorded as V3; M2, the third potential sensor sends the first real-time potential value of the third potential sensor to the server. The server receives the first real-time potential value of the third potential sensor, which is recorded as V3". The server sets X3 = V3" - V3. If the absolute value of X3 is within the threshold, production continues. If the absolute value of X3 is outside the threshold, an alarm command is output.

[0007] Optionally, the second potential sensor is used to detect the potential of the mixed solution after the hydrogen peroxide stage reaction, and the third potential sensor is used to detect the potential of the mixed solution after the ammonia stage reaction.

[0008] Optionally, in S1, the server also receives the set target potential value of the hydrogen peroxide section before reaction, which is denoted as V1; in S2, the first potential sensor sends the real-time potential value of the first potential sensor to the server, which is denoted as V1". The server sets X1 = V1" - V1. If the absolute value of X1 is within the threshold, production continues; if the absolute value of X1 is outside the threshold, an alarm command is output.

[0009] Optionally, the intelligent control method for the hydrogen peroxide section further includes the following steps: S3, When the absolute value of X2 is outside the threshold, if X2 is positive, the server sends a command to reduce the hydrogen peroxide drip rate to the hydrogen peroxide drip rate actuator. At the same time, the server also sends a heating command to the heater actuator of the liquid storage open tank installed on the intermediate discharge pipe. After receiving the command, the hydrogen peroxide drip rate actuator executes the command to reduce the hydrogen peroxide drip rate, and the heater actuator executes the command to heat. If X2 is negative, the server sends a command to increase the hydrogen peroxide drip rate to the hydrogen peroxide drip rate actuator. At the same time, the server sends a closing command to the first valve actuator installed on the intermediate discharge pipe and an opening command to the second valve actuator installed on the first return pipe. After receiving the command, the first valve actuator executes the command, the second valve actuator executes the command, and the hydrogen peroxide drip rate actuator executes the command to increase the hydrogen peroxide drip rate. S4, the second potential sensor continues to send its second real-time potential value to the server, denoted as V2". The server receives the second real-time potential value and sets X2" = V2" - V2. If the absolute value of X2" is within the threshold, and the production abnormality is caused by X2 being positive, a shutdown command is sent to the heater actuator. The heater actuator receives the command and shuts down the heater. If the production abnormality is caused by X2 being negative, the first valve actuator sends an opening command and a shutdown command to the second valve actuator. The first valve actuator receives the command and executes it, as does the second valve actuator. If the absolute value of X2" is outside the threshold, and X2" is positive while the hydrogen peroxide drip rate is reduced, the server sends a further reduction command to the hydrogen peroxide drip rate actuator. Drip rate command; if X2" is negative, the server sends an increase command to the hydrogen peroxide drip rate actuator, a close command to the first valve actuator, an open command to the second valve actuator, and a close command to the heater actuator; when the hydrogen peroxide drip rate is increased, if X2" is positive, the server sends a decrease command to the hydrogen peroxide drip rate actuator, an open command to the first valve actuator, a close command to the second valve actuator, and a heat command to the heater actuator; if X2" is negative, the server sends a command to the hydrogen peroxide drip rate actuator to continue increasing the hydrogen peroxide drip rate. Repeat S4 until X2" is within the threshold, and resume normal production under the new equilibrium. At this time, the first valve is in the open state, the second valve is in the closed state, and the heater is in the closed state.

[0010] Optionally, when the liquid is returned to the hydrogen peroxide section tubular reactor due to insufficient hydrogen peroxide, the increase in the hydrogen peroxide drip rate by the hydrogen peroxide drip rate actuator is positively correlated with the amount of hydrogen peroxide required to replenish the returned liquid and the absolute value of X2; when there is an excess of hydrogen peroxide, the decrease in the hydrogen peroxide drip rate by the hydrogen peroxide drip rate actuator is positively correlated with X2.

[0011] Optionally, in M2, when the absolute value of X3 is outside the threshold, if X3 is positive, the server sends an instruction to increase the ammonia drip rate to the ammonia drip rate actuator. At the same time, the server also sends a closing instruction to the third valve actuator installed on the discharge pipe and an opening instruction to the fourth valve actuator installed on the second return pipe. The third valve actuator executes the instruction after receiving it, and the ammonia drip rate actuator executes the instruction to increase the ammonia drip rate after receiving it. If X3 is negative, the server sends an instruction to decrease the ammonia drip rate to the ammonia drip rate actuator. At the same time, the server sends an acid addition instruction to the acid addition actuator installed on the discharge pipe. The acid addition actuator executes the instruction after receiving it. The intelligent control method for the ammonia section further includes the following steps: M3, the third potential sensor continues to send the second real-time potential value of the third potential sensor to the server, the second real-time potential value of the third potential sensor is recorded as V3"", the server receives the second real-time potential value of the third potential sensor, the server sets X3" = V3"" - V3; if the absolute value of X3" is within the threshold, the abnormality ends, and the reaction achieves equilibrium in the new state; if the production abnormality is caused by excessive ammonia, a shut-off dripping command is sent to the acid dripping actuator, the acid dripping actuator stops dripping after receiving the command, if rare earth ions are not completely precipitated, an open command is sent to the third valve actuator and a shut-off command is sent to the fourth valve actuator, the third valve actuator executes the command after receiving the command, the fourth valve actuator executes the command after receiving the command; if the absolute value of X3" is outside the threshold, under the condition of reducing the ammonia dripping rate, if X3" is positive, the server sends a command to the ammonia dripping rate actuator. The server sends an instruction to increase the hydrogen peroxide drip rate, a closing instruction to the third valve actuator, an opening instruction to the fourth valve actuator, and a stop instruction to the acid dripping actuator. If X3" is negative, the server sends an instruction to further decrease the ammonia drip rate to the ammonia dripping actuator. If X3" is positive while increasing the ammonia drip rate, the server sends an instruction to continue increasing the ammonia drip rate to the ammonia dripping actuator. If X3" is negative, the server sends an instruction to decrease the hydrogen peroxide drip rate to the ammonia dripping actuator, an opening instruction to the third valve actuator, a closing instruction to the fourth valve actuator, and an acid dripping instruction to the acid dripping actuator. Repeat M3 until X3 is within the threshold. Normal production resumes under the new equilibrium. At this time, the third valve is in the open state, the fourth valve is in the closed state, and the acid dropper is in the closed state.

[0012] Optionally, when the ammonia section of the tubular reactor is affected by insufficient ammonia, the increase in the ammonia dripping rate by the ammonia dripping rate actuator is positively correlated with the amount of ammonia required to be added to the returned liquid and the absolute value of X3; when there is an excess of ammonia, the decrease in the hydrogen peroxide dripping rate by the ammonia dripping rate actuator is positively correlated with X3.

[0013] Optionally, in M1, the server receives the set target pH value after the ammonia water reaction, and the target pH value is denoted as Q; In M2, the pH sensor sends a first real-time pH value to the server, which receives and records this value as Q". When the absolute value of X3 is within the threshold, the server sets Y = Q" - Q. If Y is within the threshold, production continues. If Y is outside the threshold, the server sends a command to the ammonia dripping rate actuator to reduce the ammonia dripping rate, and simultaneously sends an acid addition command to the acid addition actuator. The acid addition actuator receives and executes the command. The pH sensor continues to send a second real-time pH value to the server, which receives and records this value as Q". When the absolute value of X3 is within the threshold, the server sets Y" = Q"" - Q. If Y" is within the threshold, the server sends a command to the acid addition actuator to stop adding acid. The acid addition actuator receives and executes the command. If Y" is outside the threshold, the server continues to send commands to the acid addition actuator to reduce the ammonia dripping rate until Y" is within the threshold. When the absolute value of X3 is outside the threshold, the operation for when the absolute value of X3 is outside the threshold is executed.

[0014] Optionally, the second potential sensor is installed at the junction of the hydrogen peroxide section tubular reactor and the intermediate discharge pipe, the third potential sensor is installed at the junction of the ammonia section tubular reactor and the discharge pipe, and the pH sensor is installed at the junction of the ammonia section tubular reactor and the discharge pipe.

[0015] The present invention also provides an electronic device.

[0016] An electronic device includes a memory, a processor, and a computer program stored in the memory and executable on the processor, wherein the processor executes the program to implement the steps of the intelligent control method for continuous production of the cerium ammonium nitrate precipitation process as described above.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows: This invention provides intelligent control of the reaction process, timely adjustments to the process, and prevention of substandard products from entering the next process, ensuring stable quality throughout the entire process. Furthermore, it enables production to continue without stopping when abnormalities occur, intelligently recovering from production anomalies. It also solves the problem of gelation caused by excessively fast ammonia dripping speed due to misjudgment. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of this application 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 some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is an interactive diagram of the hydrogen peroxide segment of the present invention; Figure 2 This is the interaction diagram of the ammonia water section of the present invention; Figure 3 This is a schematic diagram showing the installation positions of the potential sensor and pH sensor of the present invention; Explanation of reference numerals in the attached diagram: 1. First potential sensor; 2. Second potential sensor; 3. Third potential sensor; 4. pH sensor; 11. Hydrogen peroxide section tubular reactor; 12. Trivalent Ce ion solution feed pipe; 13. Intermediate discharge pipe; 14. Ammonia section tubular reactor; 15. Discharge pipe; 16. Storage tank; 17. Heater actuator; 18. First valve actuator; 19. Second valve actuator; 10. Hydrogen peroxide drip rate actuator; 20. Ammonia drip rate actuator; 21. Third valve actuator; 22. Fourth valve actuator; 23. Acid dripping actuator. Detailed Implementation

[0020] The invention will now be further described with reference to the accompanying drawings.

[0021] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, an indirect connection via an intermediate medium, or the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0022] In the description of this invention, it should be understood that the terms "upper," "lower," "front," "rear," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this invention. In the description of this invention, "a plurality of" means two or more, unless otherwise precisely specified.

[0023] The terms “first,” “second,” “third,” “fourth,” etc. (if present) in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a particular order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of this application described herein can be implemented, for example, in orders other than those illustrated or described herein. Furthermore, the terms “comprising” and “having,” and any variations thereof, are intended to cover a non-exclusive inclusion; for example, a process, method, system, product, or apparatus that comprises a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or units not explicitly listed or inherent to such processes, methods, products, or apparatus.

[0024] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0025] Please refer to Figures 1-3 , Figure 1 This is an interactive diagram of the hydrogen peroxide segment of the present invention. Figure 2 This is the interaction diagram of the ammonia water section of the present invention. Figure 3 This is a schematic diagram showing the installation positions of the potential sensor and pH sensor of the present invention.

[0026] In this invention, the continuous reaction apparatus for the cerium ammonium nitrate precipitation process includes a hydrogen peroxide section tubular reactor 11, an ammonia section tubular reactor 14, a first reflux pipe, and a second reflux pipe. The hydrogen peroxide section tubular reactor 11 and the ammonia section tubular reactor 14 are connected by an intermediate discharge pipe 13. The discharge pipe 15 is connected to the tail end of the ammonia section tubular reactor 14. One end of the first reflux pipe is connected to the intermediate discharge pipe 13, and the other end is connected to the hydrogen peroxide section tubular reactor 11. One end of the second reflux pipe is connected to the discharge pipe 15, and the other end is connected to the ammonia section tubular reactor 14. The trivalent Ce ion solution feed pipe 12 is connected to the head of the hydrogen peroxide section tubular reactor 11. A liquid storage open tank 16 is installed on the intermediate discharge pipe 13. A second valve actuator 19 is installed on the liquid storage open tank 16. A first valve actuator 18 is installed on the intermediate discharge pipe 13, located in front of the liquid storage open tank 16 and behind the first reflux pipe. The second valve actuator 19 is installed on the first reflux pipe; the hydrogen peroxide drip rate actuator 10 is installed at the head of the hydrogen peroxide section tubular reactor 11; the ammonia drip rate actuator 20 is installed at the head of the ammonia section tubular reactor 14; the third valve actuator 21 and the acid dripping actuator 23 are installed on the discharge pipe 15; the third valve actuator 21 is located in front of the acid dripping actuator 23 and behind the second reflux pipe; the fourth valve actuator 22 is installed on the second reflux pipe; the first potential sensor 1 is installed at the junction of the hydrogen peroxide section tubular reactor 11 and the trivalent Ce ion solution feed pipe 12; the second potential sensor 2 is installed at the junction of the hydrogen peroxide section tubular reactor 11 and the intermediate discharge pipe 13; the third potential sensor 3 is installed at the junction of the ammonia section tubular reactor 14 and the discharge pipe 15; and the pH sensor 4 is installed at the junction of the ammonia section tubular reactor 14 and the discharge pipe 15.

[0027] A smart control method for continuous production of cerium ammonium nitrate precipitation process includes a smart control method for the hydrogen peroxide section and a smart control method for the ammonia section, wherein: The intelligent control method for the hydrogen peroxide section includes the following steps: S1, During the calibration phase: The server receives the target potential value of the site before the hydrogen peroxide reaction and the target potential value of the site after the hydrogen peroxide reaction, wherein the target potential value of the site before the hydrogen peroxide reaction is recorded as V1 and the target potential value of the site after the hydrogen peroxide reaction is recorded as V2.

[0028] S2, During the production stage: The first potential sensor 1 sends its real-time potential value to the server, and the second potential sensor 2 sends its first real-time potential value to the server. The server receives the real-time potential values ​​of the first and second potential sensors respectively. The real-time potential value of the first sensor is denoted as V1" and the first real-time potential value of the second sensor is denoted as V2". The server sets X1 = V1" - V1. If the absolute value of X1 is within the threshold, production continues; if the absolute value of X1 is outside the threshold, an alarm command is output. The server sets X2 = V2" - V2. If the absolute value of X2 is within the threshold, production continues; if the absolute value of X2 is outside the threshold, an alarm command is output.

[0029] The intelligent control method for the ammonia water section includes the following steps: M1, during the calibration phase: The server receives the target potential value of the site after the ammonia water section reaction, which is recorded as V3.

[0030] M2, during the production stage: The third potential sensor 3 sends the first real-time potential value of the third potential sensor to the server. The server receives the first real-time potential value of the third potential sensor, which is recorded as V3". The server sets X3 = V3" - V3. If the absolute value of X3 is within the threshold, production continues. If the absolute value of X3 is outside the threshold, an alarm command is output.

[0031] Furthermore, the intelligent control method for the hydrogen peroxide section also includes S3, during the production stage: when the absolute value of X2 is outside the threshold, the server also sends a speed adjustment command to the hydrogen peroxide drip rate actuator 10, a heating command to the heater actuator 17 (or sends a closing command to the first valve actuator 18 and an opening command to the second valve actuator 19).

[0032] Furthermore, the intelligent control method for the hydrogen peroxide section also includes S4, during the production stage: the second potential sensor 2 continues to send the second real-time potential value of the second potential sensor to the server, which is denoted as V2"". The server receives the second real-time potential value of the second potential sensor and sets X2" = V2"" - V2. If the absolute value of X2" is within the threshold, the abnormality ends, and a heating shutdown command is sent (or a first valve opening command is sent, and a second valve closing command is sent). If the absolute value of X2" is outside the threshold, a speed adjustment command is sent, and the process is repeated until the absolute value of X2" is within the threshold.

[0033] Furthermore, during the production stage, when the absolute value of X3 is outside the threshold, M2 also sends a speed adjustment command to the ammonia dripping speed actuator 20, a closing command to the third valve actuator 21, and an opening command to the fourth valve actuator 22 (or sends an acid addition command to the acid addition actuator 23).

[0034] Furthermore, the intelligent control method for the ammonia section also includes M3. During the production stage: the third potential sensor 3 continues to send the second real-time potential value of the third potential sensor to the server. The second real-time potential value of the third potential sensor is recorded as V3". The server receives the second real-time potential value of the third potential sensor and sets X3" = V3" - V3. If the absolute value of X3" is within the threshold, the abnormality ends, and commands such as shutting down acid addition are sent (i.e., sending an opening command to the third valve actuator 21 and a closing command to the fourth valve actuator 22 (or sending a stop acid addition command to the acid droplet actuator 23)). If the absolute value of X3" is outside the threshold, commands such as continuing speed adjustment are sent until X3" is within the threshold.

[0035] Further, in the calibration phase (M1), the server also receives the target pH value after the ammonia reaction, denoted as Q. In the production phase (M2), the pH sensor 4 sends a first real-time pH value to the server, which receives this value and denots it as Q". When the absolute value of X3 is within the threshold, the server sets Y = Q" - Q. If Y is within the threshold, production continues; if Y is outside the threshold, a speed adjustment command is sent, i.e., a speed adjustment command is sent to the ammonia dripping actuator 20, and an acid addition command is sent to the acid adding actuator 23. In the production phase, the pH sensor 4 continues to send a second real-time pH value to the server, which receives this value and denots it as Q". When the absolute value of X3 is within the threshold, the server sets Y" = Q"" - Q. If Y" is within the threshold, a stop acid dripping command is sent to the acid adding actuator 23; if Y" is outside the threshold, a speed adjustment command is sent to the ammonia dripping actuator 20 until Y" is within the threshold.

[0036] The technical solution of the present invention will be described in detail below with reference to specific embodiments. These specific embodiments can be combined with each other, and the same or similar concepts or processes may not be described again in some embodiments.

[0037] Example 1 Please refer to this again. Figures 1-3 .

[0038] A smart control method for continuous production of cerium ammonium nitrate precipitation process includes a smart control method for the hydrogen peroxide section and a smart control method for the ammonia section, wherein: The intelligent control method for the hydrogen peroxide section includes the following steps: S1, During the calibration phase: The server receives the target potential value of the site before the hydrogen peroxide reaction and the target potential value of the site after the hydrogen peroxide reaction, wherein the target potential value of the site before the hydrogen peroxide reaction is recorded as V1 and the target potential value of the site after the hydrogen peroxide reaction is recorded as V2.

[0039] S2, During the production stage: The first potential sensor 1 sends its real-time potential value to the server, and the second potential sensor 2 sends its first real-time potential value to the server. The server receives the real-time potential values ​​of the first and second potential sensors respectively. The real-time potential value of the first sensor is recorded as V1" and the first real-time potential value of the second sensor is recorded as V2". The server sets X1 = V1" - V1. If the absolute value of X1 is within the threshold, it indicates that the trivalent Ce ion solution in the hydrogen peroxide section is being fed correctly, and production continues. If the absolute value of X1 is outside the threshold, it indicates that there is an error in the feeding of the trivalent Ce ion solution in the hydrogen peroxide section, and an alarm command is output. The server sets X2 = V2" - V2. If the absolute value of X2 is within the threshold, it indicates that the mixture after the reaction in the hydrogen peroxide section meets the quality requirements, and the hydrogen peroxide dripping rate matches the reaction in the hydrogen peroxide section, and production continues. If the absolute value of X2 is outside the threshold, it indicates that the mixture after the reaction in the hydrogen peroxide section does not meet the quality requirements, and the hydrogen peroxide dripping rate does not match the reaction in the hydrogen peroxide section, and an alarm command is output.

[0040] The first potential sensor 1 is used to detect the potential of the trivalent Ce ion solution before the hydrogen peroxide stage reaction, and the second potential sensor 2 is used to detect the potential of the mixed solution after the hydrogen peroxide stage reaction.

[0041] Matching means that the hydrogen peroxide drop rate ensures that the reaction between the trivalent Ce ion solution and the hydrogen peroxide is complete when the mixture leaves the hydrogen peroxide section of the tubular reactor 11, with the error within acceptable limits.

[0042] The intelligent control method for the ammonia water section includes the following steps: M1, during the calibration phase: The server receives the target potential value of the site after the ammonia water section reaction, which is recorded as V3.

[0043] M2, during the production stage: The third potential sensor 3 sends the first real-time potential value of the third potential sensor to the server. The server receives the first real-time potential value of the third potential sensor, which is recorded as V3". The server sets X3 = V3" - V3. If the absolute value of X3 is within the threshold, it means that the mixture in the ammonia section meets the quality requirements, the ammonia dripping rate matches the ammonia section reaction, and production continues. If the absolute value of X3 is outside the threshold, it means that the mixture after the ammonia section reaction does not meet the quality requirements, the ammonia dripping rate does not match the ammonia section reaction, and an alarm command is output.

[0044] The third potential sensor 3 is used to detect the potential of the mixed solution after the ammonia reaction.

[0045] Matching means that the ammonia water droplet rate and the ammonia water precipitation mixture react completely when leaving the tubular reactor 14 in the ammonia water section, with the error within an acceptable range.

[0046] Example 2 Although Example 1 can be produced normally, when a mismatch occurs due to an abnormality, even if the trivalent Ce ion solution is fed correctly into the feed pipe 12, there are no other corresponding measures to continue continuous production except to output an alarm command to stop production.

[0047] Please refer to this again. Figures 1-3 Based on Example 1: S3, During the production stage: When the absolute value of X2 is outside the threshold, if X2 is positive, it indicates that hydrogen peroxide is excessive. The server sends a command to reduce the hydrogen peroxide drip rate to the hydrogen peroxide drip rate actuator 10. At the same time, the server also sends a heating command to the heater actuator 17 of the liquid storage open tank 16 installed on the intermediate discharge pipe 13. After receiving the command, the hydrogen peroxide drip rate actuator 10 executes the command to reduce the hydrogen peroxide drip rate, and after receiving the command, the heater actuator 17 executes the command to heat.

[0048] If X2 is negative, it indicates that the reaction is incomplete, and some trivalent Ce ions have not been converted. The server sends an instruction to increase the hydrogen peroxide drip rate to the hydrogen peroxide drip rate actuator 10. At the same time, the server sends a closing instruction to the first valve actuator 18 installed on the intermediate discharge pipe 13 and an opening instruction to the second valve actuator 19 installed on the first reflux pipe. The first valve actuator 18 executes the instruction after receiving it, the second valve actuator 19 executes the instruction after receiving it, and the hydrogen peroxide drip rate actuator 10 executes the instruction to increase the hydrogen peroxide drip rate after receiving it.

[0049] In this embodiment, when the reaction mixture leaves the hydrogen peroxide section tubular reactor 11, if there is an excess of hydrogen peroxide, the excess hydrogen peroxide is removed by heating to ensure that the solution quality reaching the ammonia section tubular reactor 14 meets the requirements; if trivalent Ce ions are still present, they are returned to the hydrogen peroxide section tubular reactor 11 to continue the reaction, ensuring that the solution quality reaching the ammonia section tubular reactor 14 meets the requirements.

[0050] Therefore, although an alarm is issued when an anomaly occurs, production does not stop.

[0051] S4, During the production stage: The second potential sensor 2 continues to send the second real-time potential value of the second potential sensor to the server. The second real-time potential value of the second potential sensor is recorded as V2"". The server receives the second real-time potential value of the second potential sensor and sets X2" = V2"" - V2.

[0052] If the absolute value of X2" is within the threshold, it indicates that the mixture after the hydrogen peroxide reaction meets the quality requirements, the abnormality ends, and the reaction reaches equilibrium under the new state. If the production abnormality is caused by excessive hydrogen peroxide, a shutdown command is sent to the heater actuator 17. After receiving the command, the heater actuator 17 shuts down the heating. If the abnormality is caused by incomplete conversion of trivalent Ce ions, the first valve actuator 18 sends an opening command and the second valve actuator 19 sends a shutdown command. After receiving the command, the first valve actuator 18 executes the command, and the second valve actuator 19 executes the command.

[0053] If the absolute value of X2" is outside the threshold, when the hydrogen peroxide drip rate is reduced, if X2" is positive, it indicates that there is still an excess of hydrogen peroxide, and the server sends a further reduction command to the hydrogen peroxide drip rate actuator 10; if X2" is negative, it indicates that there is insufficient hydrogen peroxide, and the server sends an increase command to the hydrogen peroxide drip rate actuator 10, a close command to the first valve actuator 18, an open command to the second valve actuator 19, and a close command to the heater actuator 17. When the hydrogen peroxide drip rate is increased, if X2" is positive, it indicates that there is an excess of hydrogen peroxide, and the server sends a reduction command to the hydrogen peroxide drip rate actuator 10, an open command to the first valve actuator 18, a close command to the second valve actuator 19, and a heating command to the heater actuator 17; if X2" is negative, the server sends a further increase command to the hydrogen peroxide drip rate actuator 10.

[0054] Repeat this step until X2" is within the threshold, and resume normal production under the new equilibrium. At this time, the first valve is in the open state, the second valve is in the closed state, and the heater is in the closed state.

[0055] M2, during the production stage: When the absolute value of X3 is outside the threshold, if X3 is positive, it indicates that the ammonia dripping rate is low. The server sends an instruction to increase the ammonia dripping rate to the ammonia dripping rate actuator 20. At the same time, the server also sends a closing instruction to the third valve actuator 21 installed on the discharge pipe 15 and an opening instruction to the fourth valve actuator 22 installed on the second return pipe. After receiving the instruction, the third valve actuator 21 executes the instruction. After receiving the instruction, the ammonia dripping rate actuator 20 executes the instruction to increase the ammonia dripping rate.

[0056] If X3 is negative, it indicates that the ammonia dripping rate is too high. The server sends a command to the ammonia dripping rate actuator 20 to reduce the ammonia dripping rate. At the same time, the server sends an acid addition command to the acid addition actuator 23 installed on the discharge pipe 15. After receiving the command, the acid addition actuator 23 executes the command to ensure that the product reaching the next process meets the quality requirements.

[0057] In this embodiment, when the flocculant leaves the tubular reactor 14 of the ammonia section after the precipitation reaction, if there is an excess of ammonia, the excess ammonia is removed by adding acid to solve the colloidal problem, so that the quality of the flocculant reaching the next process meets the requirements; if there are still unprecipitated rare earth ions, they are returned to the tubular reactor 14 of the ammonia section to continue the reaction, ensuring that the quality of the flocculant reaching the next process meets the requirements.

[0058] Therefore, although an alarm is issued when an anomaly occurs, production does not stop.

[0059] M3, during the production stage: The third potential sensor 3 continues to send the second real-time potential value of the third potential sensor to the server. The second real-time potential value of the third potential sensor is recorded as V3"". The server receives the second real-time potential value of the third potential sensor and sets X3" = V3"" - V3.

[0060] If the absolute value of X3" is within the threshold, it means that the ammonia water meets the quality requirements after the ammonia water reaction, the abnormality ends, and the reaction reaches equilibrium under the new state.

[0061] If the production abnormality is caused by excessive ammonia, a stop dripping command is sent to the acid dripping actuator 23. After receiving the command, the acid dripping actuator 23 stops the acid dripping. If the rare earth ions are not completely precipitated, an open command is sent to the third valve actuator 21 and a close command is sent to the fourth valve actuator 22. After receiving the command, the third valve actuator 21 executes the command, and the fourth valve actuator 22 executes the command.

[0062] If the absolute value of X3" is outside the threshold, when the ammonia dripping rate is reduced, if X3" is positive, the server sends an instruction to increase the hydrogen peroxide dripping rate to the ammonia dripping rate actuator 20, a closing instruction to the third valve actuator 21, an opening instruction to the fourth valve actuator 22, and a stop instruction to the acid dripping actuator 23; if X3" is negative, the server sends an instruction to further reduce the ammonia dripping rate to the ammonia dripping rate actuator 20.

[0063] When the ammonia dripping rate is increased, if X3" is positive, the server sends a command to the ammonia dripping rate actuator 20 to continue increasing the ammonia dripping rate; if X3" is negative, the server sends a command to the ammonia dripping rate actuator 20 to decrease the hydrogen peroxide dripping rate, sends an opening command to the third valve actuator 21, a closing command to the fourth valve actuator 22, and an acid dripping command to the acid dripping actuator 23.

[0064] Repeat this step until X3" is within the threshold, and resume normal production under the new equilibrium. At this time, the third valve is in the open state, the fourth valve is in the closed state, and the acid dropper is in the closed state.

[0065] Furthermore, in order to shorten the abnormal time, when the liquid is returned to the hydrogen peroxide section of the tubular reactor 11 due to insufficient hydrogen peroxide, the adjustment range of the hydrogen peroxide drip rate actuator 10 should take into account both the amount of hydrogen peroxide required to replenish the returned liquid and the absolute value of X2. The larger the absolute value of X2, the higher the adjustment range, and the two are positively correlated. When there is an excess of hydrogen peroxide, the adjustment range of the hydrogen peroxide drip rate actuator 10 should take into account the value of X2, and X2 is positively correlated with the adjustment range.

[0066] When the ammonia section of the tubular reactor 14 is insufficient due to ammonia water shortage, the ammonia water dripping rate actuator 20 should increase the ammonia water dripping rate by taking into account both the amount of ammonia water needed to be added to the returned liquid and the absolute value of X3. The larger the absolute value of X3, the higher the adjustment range, and the two are positively correlated. When the ammonia water is excessive, the ammonia water dripping rate actuator 20 should decrease the hydrogen peroxide dripping rate by taking into account the value of X3, and X3 is positively correlated with the adjustment range.

[0067] Example 3 Although Example 2 can not only issue an alarm, but also continue production without stopping when abnormal situations occur, and restore a new balance through automatic regulation, Example 2 still has the shortcoming that the potential sensor cannot accurately detect the excessive ammonia water, which leads to the dissolution of the gel.

[0068] Based on Example 2, please refer again Figure 2 .

[0069] In the intelligent control method for the ammonia water section: M1, during the calibration phase: The server receives the target pH value after the ammonia reaction, denoted as Q. Q=7.

[0070] In the production stage (M2): pH sensor 4 sends the first real-time pH value to the server. The server receives the first real-time pH value and records it as Q". When the absolute value of X3 is within the threshold, the server sets Y = Q" - Q. If Y is within the threshold, it indicates that the ammonia water mixture meets the quality requirements, the ammonia water dripping rate matches the ammonia water reaction, and production continues. If Y is outside the threshold, it indicates that the ammonia water dripping rate is too fast, and the flocculant exhibits peptization due to excessive ammonia water. The server sends a command to the ammonia water dripping rate actuator 20 to reduce the ammonia water dripping rate. Simultaneously, the server sends an acid addition command to the acid addition actuator 23. The acid addition actuator 23 receives and executes the command to ensure that the product reaching the next process meets the quality requirements.

[0071] During the production phase: pH sensor 4 continues to send a second real-time pH value to the server. The server receives the second real-time pH value, which is denoted as Q". When the absolute value of X3 is within the threshold, the server sets Y" = Q"" - Q. If Y" is within the threshold, the server sends a stop acid addition command to the acid addition actuator 23. The acid addition actuator 23 receives and executes the command. If Y" is outside the threshold, the server continues to send a command to the acid addition actuator 23 to reduce the ammonia dripping rate until Y" is within the threshold. When the absolute value of X3 is outside the threshold, the operation for when the absolute value of X3 is outside the threshold is executed.

[0072] By enabling real-time pH comparison with the target pH value when the absolute value of X3 is within the threshold, the gelation phenomenon caused by excessive ammonia water due to misjudgment of ammonia water droplet rate matching based on potential is avoided.

[0073] Those skilled in the art should know that, since Q" is at least greater than Q when the absolute value of X3 is within the threshold, Y cannot be negative.

[0074] pH sensor 4 is used to detect the pH value of the mixed solution after the ammonia reaction.

[0075] In this invention, for the purpose of accurate detection, a first potential sensor 1 is installed at the junction of the hydrogen peroxide section tubular reactor 11 and the trivalent Ce ion solution feed pipe 12, a second potential sensor 2 is installed at the junction of the hydrogen peroxide section tubular reactor 11 and the intermediate discharge pipe 13, a third potential sensor 3 is installed at the junction of the ammonia section tubular reactor 14 and the discharge pipe 15, and a pH sensor 4 is installed at the junction of the ammonia section tubular reactor 14 and the discharge pipe 15.

[0076] The present invention also provides an electronic device, including a memory, a processor, and a computer program stored in the memory and executable on the processor, wherein the processor executes the program to implement the steps of the intelligent control method for continuous production of the above-described cerium ammonium nitrate precipitation process.

[0077] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. An intelligent control method for continuous production of cerium ammonium nitrate precipitation process, characterized in that, This includes intelligent control methods for the hydrogen peroxide section and intelligent control methods for the ammonia section, wherein: The intelligent control method for the hydrogen peroxide section includes the following steps: S1, The server receives the set target potential value of the site after the hydrogen peroxide segment reaction, and the target potential value of the site after the hydrogen peroxide segment reaction is recorded as V2; S2, the second potential sensor sends the first real-time potential value of the second potential sensor to the server, the server receives the first real-time potential value of the second potential sensor, the first real-time potential value of the second potential sensor is recorded as V2"; the server sets X2=V2"-V2, if the absolute value of X2 is within the threshold, production continues, if the absolute value of X2 is outside the threshold, an alarm command is output; The intelligent control method for the ammonia water section includes the following steps: M1, The server receives the set target potential value of the site after the ammonia water section reaction, and the target potential value of the site after the ammonia water section reaction is recorded as V3; M2, the third potential sensor sends the first real-time potential value of the third potential sensor to the server. The server receives the first real-time potential value of the third potential sensor, which is recorded as V3". The server sets X3 = V3" - V3. If the absolute value of X3 is within the threshold, production continues. If the absolute value of X3 is outside the threshold, an alarm command is output.

2. The intelligent control method for continuous production of cerium ammonium nitrate precipitation process according to claim 1, characterized in that, The second potential sensor is used to detect the potential of the mixed solution after the hydrogen peroxide stage reaction, and the third potential sensor is used to detect the potential of the mixed solution after the ammonia stage reaction.

3. The intelligent control method for continuous production of the cerium ammonium nitrate precipitation process according to claim 1, characterized in that, In S1, the server also receives the set target potential value of the hydrogen peroxide section before reaction, which is denoted as V1; in S2, the first potential sensor sends the real-time potential value of the first potential sensor to the server, which is denoted as V1". The server sets X1 = V1" - V1. If the absolute value of X1 is within the threshold, production continues; if the absolute value of X1 is outside the threshold, an alarm command is output.

4. The intelligent control method for continuous production of the cerium ammonium nitrate precipitation process according to claim 1, characterized in that, The intelligent control method for the hydrogen peroxide section also includes the following steps: S3, When the absolute value of X2 is outside the threshold, if X2 is positive, the server sends a command to reduce the hydrogen peroxide drip rate to the hydrogen peroxide drip rate actuator. At the same time, the server also sends a heating command to the heater actuator of the liquid storage open tank installed on the intermediate discharge pipe. After receiving the command, the hydrogen peroxide drip rate actuator executes the command to reduce the hydrogen peroxide drip rate, and the heater actuator executes the command to heat. If X2 is negative, the server sends a command to increase the hydrogen peroxide drip rate to the hydrogen peroxide drip rate actuator. At the same time, the server sends a closing command to the first valve actuator installed on the intermediate discharge pipe and an opening command to the second valve actuator installed on the first return pipe. After receiving the command, the first valve actuator executes the command, the second valve actuator executes the command, and the hydrogen peroxide drip rate actuator executes the command to increase the hydrogen peroxide drip rate. S4, the second potential sensor continues to send its second real-time potential value to the server, denoted as V2". The server receives the second real-time potential value and sets X2" = V2" - V2. If the absolute value of X2" is within the threshold, and the production abnormality is caused by X2 being positive, a shutdown command is sent to the heater actuator. The heater actuator receives the command and shuts down the heater. If the production abnormality is caused by X2 being negative, the first valve actuator sends an opening command and a shutdown command to the second valve actuator. The first valve actuator receives the command and executes it, as does the second valve actuator. If the absolute value of X2" is outside the threshold, and X2" is positive while the hydrogen peroxide drip rate is reduced, the server sends a further reduction command to the hydrogen peroxide drip rate actuator. Drip rate command; if X2" is negative, the server sends an increase command to the hydrogen peroxide drip rate actuator, a close command to the first valve actuator, an open command to the second valve actuator, and a close command to the heater actuator; when the hydrogen peroxide drip rate is increased, if X2" is positive, the server sends a decrease command to the hydrogen peroxide drip rate actuator, an open command to the first valve actuator, a close command to the second valve actuator, and a heat command to the heater actuator; if X2" is negative, the server sends a command to the hydrogen peroxide drip rate actuator to continue increasing the hydrogen peroxide drip rate. Repeat S4 until X2" is within the threshold, and resume normal production under the new equilibrium. At this time, the first valve is in the open state, the second valve is in the closed state, and the heater is in the closed state.

5. The intelligent control method for continuous production of the cerium ammonium nitrate precipitation process according to claim 4, characterized in that, When the hydrogen peroxide is insufficient and the liquid is returned to the hydrogen peroxide section of the tubular reactor, the increase in the hydrogen peroxide drip rate by the hydrogen peroxide drip rate actuator is positively correlated with the amount of hydrogen peroxide required to replenish the returned liquid and the absolute value of X2; when there is an excess of hydrogen peroxide, the decrease in the hydrogen peroxide drip rate by the hydrogen peroxide drip rate actuator is positively correlated with X2.

6. The intelligent control method for continuous production of the cerium ammonium nitrate precipitation process according to claim 1, characterized in that, In M2, when the absolute value of X3 is outside the threshold, if X3 is positive, the server sends an instruction to increase the ammonia drip rate to the ammonia drip rate actuator. At the same time, the server also sends a closing instruction to the third valve actuator installed on the discharge pipe and an opening instruction to the fourth valve actuator installed on the second return pipe. The third valve actuator executes the instruction after receiving it, and the ammonia drip rate actuator executes the instruction to increase the ammonia drip rate. If X3 is negative, the server sends an instruction to decrease the ammonia drip rate to the ammonia drip rate actuator. At the same time, the server sends an acid addition instruction to the acid addition actuator installed on the discharge pipe. The acid addition actuator executes the instruction after receiving it. The intelligent control method for the ammonia section further includes the following steps: M3, the third potential sensor continues to send the second real-time potential value of the third potential sensor to the server, the second real-time potential value of the third potential sensor is recorded as V3"", the server receives the second real-time potential value of the third potential sensor, the server sets X3" = V3"" - V3; if the absolute value of X3" is within the threshold, the abnormality ends, and the reaction achieves equilibrium in the new state; if the production abnormality is caused by excessive ammonia, a shut-off dripping command is sent to the acid dripping actuator, the acid dripping actuator stops dripping after receiving the command, if rare earth ions are not completely precipitated, an open command is sent to the third valve actuator and a shut-off command is sent to the fourth valve actuator, the third valve actuator executes the command after receiving the command, the fourth valve actuator executes the command after receiving the command; if the absolute value of X3" is outside the threshold, under the condition of reducing the ammonia dripping rate, if X3" is positive, the server sends a command to the ammonia dripping rate actuator. The server sends an instruction to increase the hydrogen peroxide drip rate, a closing instruction to the third valve actuator, an opening instruction to the fourth valve actuator, and a stop instruction to the acid dripping actuator. If X3" is negative, the server sends an instruction to further decrease the ammonia drip rate to the ammonia dripping actuator. If X3" is positive while increasing the ammonia drip rate, the server sends an instruction to continue increasing the ammonia drip rate to the ammonia dripping actuator. If X3" is negative, the server sends an instruction to decrease the hydrogen peroxide drip rate to the ammonia dripping actuator, an opening instruction to the third valve actuator, a closing instruction to the fourth valve actuator, and an acid dripping instruction to the acid dripping actuator. Repeat M3 until X3 is within the threshold. Normal production resumes under the new equilibrium. At this time, the third valve is in the open state, the fourth valve is in the closed state, and the acid dropper is in the closed state.

7. The intelligent control method for continuous production of the cerium ammonium nitrate precipitation process according to claim 6, characterized in that, When the ammonia section of the tubular reactor is affected by insufficient ammonia, the increase in the ammonia dripping rate by the ammonia dripping rate actuator is positively correlated with the amount of ammonia required to be added to the returned liquid and the absolute value of X3; when there is an excess of ammonia, the decrease in the hydrogen peroxide dripping rate by the ammonia dripping rate actuator is positively correlated with X3.

8. The intelligent control method for continuous production of cerium ammonium nitrate precipitation process according to claim 6, characterized in that, In M1, the server receives the target pH value after the ammonia water reaction, and the target pH value is denoted as Q. In M2, the pH sensor sends the first real-time pH value to the server, and the server receives the first real-time pH value, which is recorded as Q". When the absolute value of X3 is within the threshold, the server sets Y = Q" - Q. If Y is within the threshold, production continues; if Y is outside the threshold, the server sends a command to the ammonia dripping rate actuator to reduce the ammonia dripping rate, and at the same time, the server sends an acid addition command to the acid addition actuator. The acid addition actuator receives the command and executes it. The pH sensor continues to send a second real-time pH value to the server. The server receives the second real-time pH value and records it as Q". When the absolute value of X3 is within the threshold, the server sets Y" = Q"" - Q. If Y" is within the threshold, the server sends a stop acid addition command to the acid addition actuator. The acid addition actuator receives and executes the command. If Y" is outside the threshold, the server continues to send a command to the acid addition actuator to reduce the ammonia dripping rate until Y" is within the threshold. When the absolute value of X3 is outside the threshold, the operation for when the absolute value of X3 is outside the threshold is executed.

9. The intelligent control method for continuous production of the cerium ammonium nitrate precipitation process according to claim 1, characterized in that, The second potential sensor is installed at the junction of the hydrogen peroxide section tubular reactor and the intermediate discharge pipe, the third potential sensor is installed at the junction of the ammonia section tubular reactor and the discharge pipe, and the pH sensor is installed at the junction of the ammonia section tubular reactor and the discharge pipe.

10. An electronic device comprising a memory, a processor, and a computer program stored in the memory and executable on the processor, characterized in that, When the processor executes the program, it implements the steps of the intelligent control method for continuous production of the cerium ammonium nitrate precipitation process as described in any one of claims 1 to 9.

Citation Information

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