Automatic processing system and method for rare earth titration detection

Abstract

The invention relates to the technical field of rare earth detection processing corollary equipment, in particular to an automatic processing system and method for rare earth titration detection, and the system comprises a computer, a microcomputer, a titration mechanism, an image acquisition device and at least one titration threshold database; initial data of the titration threshold database are obtained by summarizing data of manual titration detection results; the titration mechanism is used for feeding a titration solution and heating and oscillating the fed mixed solution, so that the sufficiently mixed titration solution is quickly obtained; the image acquisition device adopts a CMOS industrial camera to shoot a solution image, automatic identification of the solution color in the chemical reaction process is achieved, and the method has the effects that the steps of manual operation control are greatly reduced, the automatic determination process and result recording are achieved, the detection process is optimized, the detection efficiency is effectively improved, and the detection cost is reduced.

Description

Technical Field

[0001] This application relates to the technical field of supporting equipment for rare earth detection and processing, and particularly to an automatic processing system and method for rare earth titration detection. Background Art

[0002] The manufacturing process of the rare earth industry is long, the technological process is complex, the industrial mechanism complexity is high, and it has the characteristics of both process and discrete manufacturing, which is a typical hybrid manufacturing process.

[0003] After the rare earth raw ore is produced from the mine, it enters the separation and extraction process. The overall process is generally divided into seven links: acid dissolution, extraction, precipitation, washing, calcination, sieving, and mixing, and finally forms rare earth oxides. After wet smelting, each element in the rare earth is completely separated, and the finished product can form rare earth oxides with extremely high purity. In the separation and extraction process, rare earth elements exist in the mixed solution, and the rapid analysis and detection of the solution components directly affect the quality of the final product. Currently, most enterprises still adopt the method of sampling and sending for inspection. Although this method saves the cost of analytical instruments, it cannot provide real-time feedback on the relevant parameters of the current solution, has a serious lag, affects the production of real-time products, and when quality problems occur, they have already appeared in the finished products, which will lead to resumption of work and re-production, and the cost of re-melting and re-making is higher. Due to the high dispersion of rare earth detection equipment, and a single instrument alone cannot directly obtain the detection results, and it also requires testers to have a high level of experience accumulation to control various instruments and equipment to obtain the results. In the control of heating duration, titration speed, color change timing, etc., experience accumulation is particularly important, which leads to a large amount of the cost in the detection process being spent on labor. Therefore, developing an automatic analysis and detection equipment for the material components in the rare earth production process, effectively improving the detection efficiency of the solution components in the rare earth separation and extraction process, and at the same time reducing the labor cost, is of great significance for improving the intelligent level of the rare earth industry. Summary of the Invention

[0004] Aiming at the deficiencies of the prior art, the purpose of this application is to provide an automatic processing system and method for rare earth titration detection with accurate detection results, effectively reducing the steps of manual operation and control, realizing the automatic determination process and result recording, and effectively improving the detection efficiency and reducing the detection cost.

[0005] The above application purpose of this application is achieved through the following technical solutions: An automatic processing system and method for rare earth titration detection, including: a computer, a microcomputer, a titration mechanism, an image acquisition device, and at least one titration threshold database; The initial data of the titration threshold database is obtained by summarizing the data of manual titration detection results; The titration mechanism is used to input the titrant and heat and shake the mixed solution being input, so as to quickly obtain a well-mixed titration liquid; The image acquisition device uses a CMOS industrial camera to capture the solution image, realizes the automatic recognition of the solution color during the chemical reaction process, and converts it into digital information. Among them, the CMOS industrial camera uses the second-order moment threshold of color components and the number of pixel points to exclude the interference of the alternating change of the solution color; The computer is used to process the solution color data collected by the image acquisition device, and make a reference with the values near the threshold in the titration threshold database, and then control the operation of the microcomputer; when the titration color value is far from the vicinity of the threshold, the microcomputer controls the titration mechanism to accelerate the input of the titrant, and when the titration reaches the vicinity of the threshold data, slows down the input of the titrant by the titration mechanism; The computer is also used to establish an end point determination standard to facilitate the automatic determination of the titration end point; The titration threshold database manually inputs the result list of titration under a certain volume of this type of rare earth; The computer is also used to record the values when the color changes captured by the CMOS industrial camera, obtain the titration result, and send it through a message.

[0006] Optionally, the titration mechanism includes: a rotating rod device, a pretreatment device, a stirring device and a heating device; the rotating rod device is used to transfer the bottle body and adjust the angle of the imaging device, so that the position of the COMS industrial camera in the image acquisition device reaches the best angle to avoid reflection or weak chrominance of the captured image; the pretreatment device includes a switching valve and a stepping motor peristaltic pump, the switching valve is used to realize the rapid replacement of reagent types, and the stepping motor peristaltic pump is used to accurately add reagents quantitatively into the reagent sample; the stirring device is used to fully mix the solution after adding the reagent; the heating device is used to heat the mixed solution and maintain it at a certain temperature value.

[0007] Optionally, the titration threshold database recorded in the computer determines the titration end point based on the similarity obtained by histogram comparison, and can effectively and accurately realize the automatic recognition of the solution color during the chemical reaction process.

[0008] Optionally, through the research and analysis of the experience of traditional manual titration and a large number of titration experiments, the appropriate dropping amount of the reagent and the accurate threshold of the titration end point are obtained.

[0009] Optionally, the titration result message sent by the computer at the end of the titration contains at least information such as the volume of the titrant consumed in the titration, the concentration of the titrant consumed, the volume of the test sample, the titration duration, and the reaction temperature.

[0010] Optionally, during detection, a preprocessing process is also included. During the preprocessing process, the solution and reagents can be heated up, and various reagents are respectively injected into their respective stepper motor peristaltic pumps to improve efficiency.

[0011] Optionally, the titration threshold database can select data of continuous variable type or discrete variable type.

[0012] Optionally, the computer also records the result of each titration in the titration threshold database.

[0013] A rare earth titration detection method uses an automatic processing system for rare earth titration detection, including: S1: Prepare the reagents required for the test, adjust the positions of the beaker and the titration equipment, adjust the shooting distance between the camera and the sample, and supplement light to the liquid in the beaker so that the illumination conditions passing through the beaker to the image acquisition device are the same, and heat up the liquid in the beaker. S2: Put samples of each label with a certain mass into different reaction beakers respectively, and input the sample mass contained in the solution in each beaker and the solution concentration information used for titration into the computer. S3: Operate the computer to control the microcomputer to start, and the microcomputer controls the titration mechanism to start the titration work for each beaker. S4: Titrate until the color changes at the end point. The computer records the titration value when reaching the end point, controls the microcomputer to terminate the titration process of this beaker, calculates the sample concentration at the same time, and displays and records it. S5: Clean the instruments used for automatic titration.

[0014] The beneficial effects of the present invention are: An accurate color state of one or more solutions is obtained through the CMOS industrial camera in the image acquisition device, and the information is transmitted to the computer. The computer controls the work of the microcomputer and determines the end of titration according to the color feedback. The microcomputer is used to respectively regulate the working states of the internal components of the titration mechanism, enabling the computer to be more focused on data processing when receiving color information, controlling the working conditions of the microcomputer, sharing the work burden of the computer by the microcomputer, ensuring the processing quality of titration data, and optimizing the control process; The microcomputer can control the titration speed of the titration mechanism in different situations, record multiple groups of titration gradient control quantities, and directly control the drive modules of each variable respectively, with more precise control; After detecting a larger number of samples, the detection speed of various samples will be greatly improved, which helps to speed up the production progress and optimize the detection process. Description of the Drawings

[0015] Figure 1It is a block diagram of the automatic processing system for rare earth titration detection provided by this application; Figure 2 It is a block diagram of the pretreatment mechanism provided by this application. Detailed implementation manners

[0016] The following further elaborates on this application in conjunction with the accompanying drawings.

[0017] To more clearly understand the technical solutions presented in the embodiments of this application, first, the working principles of the existing processing systems and methods for rare earth titration detection will be introduced.

[0018] In the existing rare earth detection process, a step-by-step operation form is used. The items to be detected need to be separately subjected to titration tests. Regarding the temperature control and timing selection during titration, etc., the testers need to have relatively rich experience to achieve accurate measurement results. Although the existing instruments can realize the detection process, their efficiency is low. When it is necessary to temporarily detect the product status at night or other times, only temporary samples can be stored and sent for inspection the next day. This form does not meet the on-demand detection requirements of manufacturers. Therefore, it is necessary to improve the existing rare earth titration detection equipment to achieve automated and highly efficient detection.

[0019] In some feasible implementation manners: An automatic processing system for rare earth titration detection includes: a computer, a microcomputer, a titration mechanism, an image acquisition device, and at least one titration threshold database; among them, the early titration threshold database is obtained by sequentially inputting the data from normal detections into the computer. Among them, the data must include the weights of different types of rare earths sampled before testing, and the dosages of titrants with different concentrations used in titration; It should be noted that in some cases where operations such as extraction and calcination are required before measurement, the mass of the rare earth sample taken before extraction or other processing procedures is also recorded. This is because in subsequent determinations of the same type of process, the same type of processing is also required, and when the conditions are the same, the results remain unchanged.

[0020] The initial data of the titration threshold database is obtained by summarizing the data of manual titration detection results; in some special cases, when there is really no database, titration operations can still be carried out, but in this case, the computer cannot be used to optimize and shorten the titration duration. Therefore, it will be carried out at a normal speed at the front-end position near the threshold, and a relatively long time will be wasted if the time is long; when using, the input of data uses Visual Studio software to design the upper computer software to complete the data input interface, real-time observation interface, manual control interface, and data statistics interface, realizing the basic functions of human-computer interaction; the input data information is summarized and stored in the computer and called during subsequent measurement processes. When using the information, the data near the threshold will be preferentially determined to control the working speed of the titration mechanism.

[0021] The titration mechanism is used to introduce the titrant and heat and shake the mixed solution introduced, so as to quickly obtain a well-mixed titration liquid; the titration mechanism is divided into multiple groups, and can respectively connect the same types of titration pipelines to the same beaker. During the titration detection process, the installation and connection of each component are also important considerations. Therefore, during the installation of the titration mechanism, reliable locking and fixing are required for the support of components such as beakers and titrators. Thus, a special platform or support structure for installation and fixation needs to be set up; among them, the heating and vibration functions are respectively realized by existing heating tables, experimental vibration tables or magnetic force stirring devices, which belong to common technical means.

[0022] The image acquisition device uses a CMOS industrial camera to capture the solution image, realizes the automatic recognition of the solution color during the chemical reaction process, and converts it into digital information. Among them, the CMOS industrial camera uses the second-order moment threshold of color components and the number of pixel points to exclude the interference of the alternating change of the solution color, and observes the color change more accurately, which is more accurate than the human eye. The computer is used to process the solution color data collected by the image acquisition device, and make a reference with the numerical values near the threshold in the titration threshold database, and then control the operation of the microcomputer; when the titration color value is far from the threshold, the microcomputer controls the titration mechanism to accelerate the introduction of one or more titrants, and when the volume of the titrant reaches near the threshold data, slows down the speed of the titration mechanism to introduce the titrant. The computer is also used to establish an end point determination standard to facilitate the automatic determination of the titration end point, that is: each result will be statistically stored in the computer and summarized and classified with the original data to further optimize the titration process, making the titration speed faster and the accuracy higher.

[0023] The titration threshold database manually inputs the result list of titration under a certain volume of this type of rare earth. During the data input process, list-type information can be directly input.

[0024] The computer is also used to record the numerical value when the color captured by the CMOS industrial camera changes, obtain the titration result, and send it through a message. During the titration process, generally the color change is the target position tested by the titration, and there are also cases where the target value is obtained only after the color changes twice. Since the color change is fast, and the human eye is not sensitive enough to observe some color changes.

[0025] The CMOS industrial camera uses the second-order moment threshold of color and the color histogram similarity algorithm to determine the end point, uses an industrial camera to record the solution color data, and finally determines the color end point by the computer comparing the processed collected color data. The titration mechanism includes: a rotating rod device, a pretreatment device, a stirring device, and a heating device; the rotating rod device is used to transfer the bottle body and adjust the angle of the imaging device, so that the position of the CMOS industrial camera in the image acquisition device reaches the optimal angle to avoid reflection or weak chrominance in the captured image; the pretreatment device includes components such as a switching valve and a stepper motor peristaltic pump. Sometimes, manual operation is also required to add some reagents and adjust the state of some equipment. The switching valve is used to quickly change the type of reagent, and the stepper motor peristaltic pump is used to accurately add reagents quantitatively into the reagent sample and pour a certain amount of solvents and other raw materials into the beaker; the stirring device is used to fully mix the solution after adding the reagents, and its form can be selected from existing magnetic stirring or vibrating table and other mechanisms for mixing solutions; the heating device is used to heat up the mixed solution and then maintain it at a certain temperature value.

[0026] The titration threshold database recorded in the computer determines the titration endpoint based on the similarity obtained by histogram comparison. This determination is more in line with the comparison logic of the computer. Other comparison programs can also be used for operation. The purpose is to further achieve the automatic recognition of the solution color during the chemical reaction process and improve the test rate.

[0027] By studying and analyzing the experience of traditional manual titration and conducting a large number of titration experiments, the appropriate dropping amount of the reagent and the accurate threshold of the titration endpoint are obtained.

[0028] The titration result message sent by the computer at the end of titration contains at least information such as the volume of the titrant consumed in titration, the concentration of the titrant consumed, the volume of the test sample, the titration duration, and the reaction temperature.

[0029] The titration threshold database can select data of continuous variable type or discrete variable type.

[0030] The computer also records the result of each titration in the titration threshold database.

[0031] During the titration process, before starting the microcomputer to control the titration rhythm, the computer will quickly retrieve based on the data of the raw material mass filled in the corresponding beaker to obtain the titration threshold position of this type of sample. Then, within the interval before reaching the titration result, titration is carried out at double or triple speed. When approaching the titration threshold, the speed is adjusted to normal speed or slowed down to 0.8 times the speed. The determination of this distance is generally to adjust to the normal titration speed when there is still 3 ml left in the distance interval. Since 3 ml is generally 45 to 60 drops of liquid, the color change time can be extended and controlled within two minutes or even longer, which greatly improves the titration accuracy at this point. If the color observed by the image acquisition device does not change, the microcomputer will continue to control according to the logic of delaying the dropping speed near the threshold. If the color changes after the last drop of solution is dropped, the industrial camera immediately transmits the information to the computer. The computer then records the liquid value dropped at the corresponding titration position of the microcomputer at this moment and summarizes it to obtain the result. At the same time, a shutdown signal is sent to the microcomputer, and related operations such as heating, shaking, and titration stop, and the titration at this position ends. Under this control logic, the manual labor and the error of manual recording can be greatly reduced. At the same time, multiple samples can be recorded simultaneously, and the equipment cost is greatly reduced compared with the existing ones, and the efficiency is greatly improved. It can measure the data of multiple samples by one person at a time at night and other situations, and there is no need to stare at the data of each instrument in real time, which better meets the actual needs of enterprises and is more convenient to realize the automatic detection process.

[0032] A rare earth titration detection method uses an automatic processing system for rare earth titration detection, including S1: Prepare the reagents required for the test, adjust the positions of the beaker and the titration equipment, adjust the shooting distance between the camera and the sample, and supplement the light for the liquid in the beaker to make the light conditions passing through the beaker and reaching the image acquisition device the same, and perform a heating treatment on the liquid in the beaker. Furthermore, in the early stage of the operation, a special mounting rack needs to be customized, which can install at least five beakers and the supporting titration structure. In the design, it can be arranged in an arc shape, and the number that can be installed can be adjusted according to the actual production scale. If the scale is large, the number can be increased, but when installing the same component or device, each component or structure should be installed at the same level with an arc-shaped interval distribution, which is convenient for adding raw materials and installation. After supplementary lighting, the image acquisition device can further improve the perception accuracy of color changes. Among the existing industrial cameras, some cameras can monitor the color changes at multiple points, and some can monitor the color changes at a single position. Therefore, it can be flexibly selected according to the actual scenario.

[0033] S2: Put samples of each label with a certain mass into different reaction beakers respectively, and input the sample mass contained in the solution in each beaker and the information of the solution concentration used for titration into the computer. Further, when inputting data and pouring in samples, it is preferred to continuously install them sequentially from the edge. This is to facilitate the subsequent temporary addition of titration, which may affect the samples already in the testing process. The concentration of the titrant solution and the amount used in the titration can be temporarily recorded at the microcomputer and captured by the computer at the titration endpoint to record the final value.

[0034] S3: Operate the computer to control the microcomputer to start, and the microcomputer controls the titration mechanism to start the titration work for each beaker; Overall, the computer selects the starting process and sets the speed of the microcomputer. The microcomputer records the reagent speed and the amount of reagent input by the titration mechanism in real time and caches them for the computer to call. The computer can also modify the threshold endpoint during the titration process, thereby changing the titration operation of the microcomputer, such as advancing or delaying.

[0035] S4: Titrate until the endpoint changes color. The computer records the titration value at the endpoint and controls the microcomputer to terminate the titration process of this beaker. At the same time, it calculates the sample concentration and displays and records it; In the calculation of the concentration, the conventional volume ratio method is adopted. In the test, multiple beakers can also be titrated simultaneously with the same sample, and then the average value is taken to further reduce the error. Generally, when the deviation of the titrant is 3 - 5 drops, the small concentration consumed does not affect, that is, the result error is low and there is no impact. Dilute titrant can also be used to further improve the accuracy of the titration test.

[0036] S5: Clean the instruments used for automatic titration.

[0037] During this detection process, it is necessary to summarize the interference of non-rare earth metal ions, study the yellow titration endpoint determination algorithm problem, and optimize the chromaticity recognition effect; S6: After a batch of titrations, several samples can be selected for manual titration operations to verify the accuracy of the measurement results. During the verification process, directly calculate the required amount of reagent based on the result value determined by the computer and directly prepare it to the titration color change threshold to start the titration to shorten the titration time; During the verification operation, it can also be in the form of submitting for inspection, using the detection results of the same sample in other manufacturers as a comparison.

[0038] What also needs to be noted in the experiment is to set a safety threshold range, that is: a safety mechanism for alarming in cases such as beaker cracks and abnormal temperature rises. For example, when the temperature range exceeds the safety value, the computer sends a message to the tester and reminds through sound and light signals to ensure the safety of the laboratory and the tester.

[0039] The embodiments of this specific implementation manner are all preferred embodiments of this application, and do not limit the protection scope of this application. Therefore, all equivalent changes made according to the structure, shape, and principle of this application shall be covered within the protection scope of this application.

Claims

1. An automatic processing system for rare earth titration detection, characterized in that: include: A computer, a microcomputer, a titration mechanism, an image acquisition device and at least one titration threshold database; The initial data of the titration threshold database is obtained by summarizing the data of manual titration test results; The titration mechanism is used to add titration solution and heat and shake the mixed solution to quickly obtain a fully mixed titration liquid; The image acquisition device uses a CMOS industrial camera to capture the solution image, realizes the automatic recognition of the solution color during the chemical reaction, and converts it into digital information, wherein the CMOS industrial camera uses the second-order moment threshold of the color component and the number of pixels to eliminate the interference of the alternating color changes of the solution; The computer is used to process the solution color data collected by the image acquisition device and to refer to the values ​​near the threshold value in the titration threshold database, thereby controlling the operation of the microcomputer; When the titration color value is far from the threshold value, the microcomputer controls the titration mechanism to accelerate the addition of the titration solution, and when the titration reaches the threshold value, the microcomputer controls the titration mechanism to slow down the addition of the titration solution; The computer is also used to establish an endpoint determination standard to facilitate automatic determination of the titration endpoint; The titration threshold database uses a manual input of a titration result list of a certain volume of the type of rare earth; The computer is also used to record the numerical value of the color transition captured by the CMOS industrial camera, obtain the titration result, and send it through a message.

2. The automatic processing system for rare earth titration detection according to claim 1, characterized in that: The titration mechanism includes: a rotating rod device, a pre-processing device, a stirring device and a heating device; the rotating rod device is used to transfer the bottle body and adjust the angle of the camera device so that the position of the COMS industrial camera in the image acquisition device reaches the optimal angle to avoid reflection or weak color of the captured image; the pre-processing device includes a switching valve and a stepper motor peristaltic pump, the switching valve is used to quickly change the reagent type, and the stepper motor peristaltic pump is used to accurately add reagents to the reagent sample in a quantitative manner; the stirring device is used to fully mix the solution after the reagent is added; the heating device is used to heat the mixed solution and maintain it at a certain temperature value.

3. The automatic processing system for rare earth titration detection according to claim 1, characterized in that: The titration threshold database recorded in the computer determines the titration endpoint based on the similarity obtained by histogram comparison, and can effectively and accurately realize the automatic recognition of the solution color during the chemical reaction process.

4. The automatic processing system for rare earth titration detection according to claim 1, characterized in that: The titration result message sent by the computer after the titration is finished contains at least information on the volume of titration solution consumed in the titration, the concentration of the consumed titration solution, the volume of the test sample, the titration duration, and the reaction temperature.

5. The automatic processing system for rare earth titration detection according to claim 1, characterized in that: During the detection, a pre-treatment process is also included, during which the solution and reagents can be heated, and various reagents can be injected into their respective stepper motor peristaltic pumps to improve efficiency.

6. The automatic processing system for rare earth titration detection according to claim 1, characterized in that: The titration threshold database may use continuous variable type or discrete variable type data.

7. The automatic processing system for rare earth titration detection according to claim 1, characterized in that: The computer also records the results of each titration into a titration threshold database.

8. A rare earth titration detection method, using an automatic processing system for rare earth titration detection as described in claims 1-7, characterized in that: include, S1: Prepare the reagents required for the test and adjust the positions of the beaker and the titration device, adjust the shooting distance between the camera and the sample, and fill light for the liquid in the beaker so that the light conditions passing through the beaker to the image acquisition device are the same, and heat the liquid in the beaker; S2: Put a certain mass of samples of each label into different reaction beakers, and input the mass of the sample contained in the solution in each beaker and the concentration information of the solution used for titration into the computer; S3: The operation computer controls the microcomputer to start, and the microcomputer controls the titration mechanism to start the titration work on each beaker; S4: Titrate until the end point changes color, the computer records the titration value when the end point is reached, and controls the microcomputer to terminate the titration process of the beaker, and at the same time calculates the sample concentration, displays it and records it; S5: Clean the instruments used for automatic titration.

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