CN118209683A

CN118209683A - Titration method

Info

Publication number: CN118209683A
Application number: CN202410342606.7A
Authority: CN
Inventors: 王宇; 王鹏刚; 梁振兴; 顾鹏
Original assignee: Meishan Boya New Material Co ltd
Current assignee: Meishan Boya New Material Co ltd
Priority date: 2021-09-30
Filing date: 2021-09-30
Publication date: 2024-06-18
Also published as: CN113884619A; CN113884619B

Abstract

Embodiments of the present disclosure provide a titration method, comprising: for a first titration process, titrating a precipitant into a metal salt solution at a first titration rate; monitoring a first pH change rate of the solution in real time during a first titration process; the first pH change rate reaches a preset threshold and the first titration process is stopped. For an Nth titration process, wherein N is more than or equal to 2, determining an Nth titration rate; titrating the precipitant into the solution at an nth titration rate; and monitoring the NpH th change rate of the solution in real time in the Nth titration process, wherein the Nth titration rate enables the difference value between the Nth pH change rate and the first pH change rate to be in a preset range.

Description

Titration method

Description of the division

The application is a divisional application of patent application with the application number 202111159971.7, the application date 2021, 09, 30 and the name of a titration method.

Technical Field

The specification relates to the technical field of powder, in particular to a titration method in the powder preparation process.

Background

Powders are one of the important raw materials in the preparation of crystals (e.g., scintillation crystals) or ceramics (e.g., scintillation ceramics). The process of preparing the powder (e.g., titration process) can affect the quality of the powder, further affecting the quality of the crystal or ceramic. Therefore, it is necessary to provide a titration method to improve the quality of the powder.

Disclosure of Invention

One of the embodiments of the present specification provides a titration method, the titration method comprising: for a first titration process, titrating a precipitant into a metal salt solution at a first titration rate; monitoring a first pH change rate of the solution in real time during the first titration; the first pH change rate reaches a preset threshold value, and the first titration process is stopped; for an Nth titration process, wherein N is more than or equal to 2, determining an Nth titration rate; titrating the precipitant into solution at the nth titration rate; and monitoring the N pH change rate of the solution in real time in the N titration process, wherein the N titration rate enables the difference value between the N pH change rate and the first pH change rate to be in a preset range.

In some embodiments, the first titration process or the nth titration process is achieved by spraying the precipitant.

In some embodiments, the first titration rate is determined based at least on the concentration of the precipitant, the concentration of the metal salt solution, and the pH of the metal salt solution.

In some embodiments, the nth titration rate is greater than the (N-1) th titration rate.

In some embodiments, the determining the nth titration rate comprises: the nth titration rate is determined based at least on the first rate of change of pH and a rate determination model.

In some embodiments, the determining the nth titration rate based at least on the first rate of change of pH and the rate determination model comprises: determining the nth titration rate based on the first rate of change of pH, titration parameters of an (N-1) th titration process, and the rate determination model.

In some embodiments, the determining the nth titration rate based at least on the first rate of change of pH and the rate determination model comprises: determining the nth titration rate based on the first rate of change of pH, a related parameter, and the rate determination model, wherein the related parameter comprises: at least one of the concentration of the metal salt solution, the concentration of the precipitant, the first titration rate, the pH of the solution at the end of the first titration process, the concentration of the solution at the end of the first titration process, the reaction time of the first titration process, the titration rate of at least one of the second to (N-1) th titration processes, the pH of the solution at the end of at least one of the second to (N-1) th titration processes, the concentration of the solution at the end of at least one of the second to (N-1) th titration processes, or the reaction time of at least one of the second to (N-1) th titration processes.

In some embodiments, the relevant parameter further comprises a reaction temperature.

In some embodiments, the determining the nth titration rate based at least on the first rate of change of pH and the rate determination model comprises: determining a plurality of candidate titration rates; determining a plurality of candidate pH change rates corresponding to the plurality of candidate titration rates, respectively, based at least on the plurality of candidate titration rates and the rate determination model; the nth titration rate is selected from the plurality of candidate titration rates based on the plurality of candidate pH rates and the first pH rate of change.

In some embodiments, the method further comprises: after stopping the first titration process or the nth titration process, the solution is filtered.

Drawings

The present specification will be further elucidated by way of example embodiments, which will be described in detail by means of the accompanying drawings. The embodiments are not limiting, in which like numerals represent like structures, wherein:

FIG. 1 is a flow chart of an exemplary titration method as shown in accordance with some embodiments.

FIG. 2 is a flow chart illustrating an exemplary determination of an Nth titration rate in accordance with some embodiments.

FIG. 3A is a graph of pH over time without adjustment of the titration rate during titration.

Fig. 3B is a schematic diagram of pH over time during an exemplary titration process as shown in accordance with some embodiments.

FIG. 4 is a schematic diagram of a titration apparatus in accordance with some embodiments.

Detailed Description

In order to more clearly illustrate the technical solutions of the embodiments of the present specification, the drawings that are required to be used in the description of the embodiments will be briefly described below. It is apparent that the drawings in the following description are only some examples or embodiments of the present specification, and it is possible for those of ordinary skill in the art to apply the present specification to other similar situations according to the drawings without inventive effort. Unless otherwise apparent from the context of the language or otherwise specified, like reference numerals in the figures refer to like structures or operations.

As used in this specification and the claims, the terms "a," "an," "the," and/or "the" are not specific to a singular, but may include a plurality, unless the context clearly dictates otherwise. In general, the terms "comprises" and "comprising" merely indicate that the steps and elements are explicitly identified, and they do not constitute an exclusive list, as other steps or elements may be included in a method or apparatus.

A flowchart is used in this specification to describe the operations performed by the system according to embodiments of the present specification. It should be appreciated that the preceding or following operations are not necessarily performed in order precisely. Rather, the steps may be processed in reverse order or simultaneously. Also, other operations may be added to or removed from these processes.

Some embodiments of the present disclosure provide a titration method, which may include at least two titration processes, in each titration process, titrating a precipitant into a solution (a first titration process corresponds to an initial metal salt solution, a subsequent titration process corresponds to a solution after the precipitant reacts with the metal salt solution) at a specific titration rate, so that a difference between pH change rates of solutions of any two titration processes in the at least two titration processes is within a preset range, and further, the reaction rate or precipitation rate of the whole titration process is kept stable, so as to ensure that quality of a precipitate prepared by each titration process is as consistent as possible, thereby improving quality of a powder prepared finally. For convenience of description, some of the descriptions in this specification will be specifically described with reference to preparation of scintillating powder as an example. It should be noted that, the titration method described in the present specification may also be used to prepare other powders, and is not limited to preparing scintillating powder.

FIG. 1 is a flow chart of an exemplary titration method as shown in accordance with some embodiments. In some embodiments, the process 100 may be performed by one or more components in a titration apparatus (e.g., titration apparatus 400). In some embodiments, the process 100 may be performed automatically by a control system. For example, the process 100 may be implemented by control instructions, based on which a control system controls various components to perform various operations of the process 100. In some embodiments, the process 100 may be performed semi-automatically. For example, one or more operations of the process 100 may be performed manually by an operator. In some embodiments, upon completion of flow 100, one or more additional operations not described above may be added and/or one or more operations discussed herein may be pruned. In addition, the order of the operations shown in FIG. 1 is not limiting. As shown in fig. 1, the process 100 includes the following steps.

Step 110, for a first titration procedure, titrating a precipitant into a metal salt solution at a first titration rate.

In some embodiments, the metal salt solution may be obtained by dissolving a metal oxide and/or a metal salt (e.g., a metal oxide or a metal salt used to prepare the scintillating powder) in an acid solution. In some embodiments, the acid solution may include at least one of nitric acid, sulfuric acid, or hydrochloric acid. In some embodiments, the mass of the metal oxide and/or metal salt may be calculated based on the mass of the powder to be prepared.

Taking the example of preparing the GAGG scintillating powder, the metal oxide can include gallium oxide, gadolinium oxide, and aluminum oxide. The metal salts may include gallium salts (e.g., gallium nitrate, gallium sulfate, gallium chloride, etc.), gadolinium salts (e.g., gadolinium nitrate, gadolinium sulfate, gadolinium chloride, etc.), aluminum salts (e.g., aluminum nitrate, aluminum sulfate, aluminum chloride, aluminum ammonium sulfate, etc.), and the like.

In some embodiments, the pH of the metal salt solution is related to the nature of the metal oxide (or metal salt) and the acid (e.g., strong acid, weak acid). In some embodiments, the pH of the metal salt solution may be less than 7, equal to 7, or greater than 7.

In some embodiments, the amount of acid solution may be slightly excessive to allow for adequate dissolution of the metal oxide. In some embodiments, the pH of the metal salt solution may be in the range of 4-6. In some embodiments, the pH of the metal salt solution may be in the range of 4.2-5.8. In some embodiments, the pH of the metal salt solution may be in the range of 4.4-5.6. In some embodiments, the pH of the metal salt solution may be in the range of 4.6-5.4. In some embodiments, the pH of the metal salt solution may be in the range of 4.8-5.2.

In some embodiments, the type of precipitant may be determined based on the pH of the metal salt solution. In some embodiments, the precipitation agent may include a strong alkaline solution and/or a weak alkaline solution. In some embodiments, the precipitants may include sodium hydroxide, ammonia, ammonium bicarbonate, and the like. In some embodiments, the precipitant may be a single precipitant or a mixed precipitant. For example, the precipitant may be a mixed solution of ammonia and ammonium bicarbonate.

In some embodiments, the concentration of the precipitant may be determined based on the concentration of the metal salt solution and the pH of the metal salt solution.

In some embodiments, the concentration of the metal salt solution, the concentration of the acid, and the concentration of the precipitant may be determined based on empirical parameters. In some embodiments, the concentration of the metal salt solution, the concentration of the acid, and the concentration of the precipitant may also be determined by other means. For example, by means of user customization, statistics, etc.

The titration rate may refer to the volume or mass of precipitant added to the metal salt solution per unit time (e.g., 1 second, 1 minute) during the titration process. Accordingly, the first titration rate may refer to the volume or mass of precipitant added to the metal salt solution per unit time during the first titration. In some embodiments, the titration rate of the precipitant into the metal salt solution may be controlled and detected by a flow meter (e.g., ultrasonic flow meter, electromagnetic flow meter).

In some embodiments, the first titration rate can be determined in a variety of ways.

In some embodiments, the first titration rate can be determined based on the concentration of the precipitant, the concentration of the metal salt solution, and the pH of the metal salt solution. Taking GAGG scintillation powder as an example, the concentration of the precipitator ammonia water is 3mol/L, the concentration of the metal salt solution is 0.3mol/L, and when the pH value of the metal salt solution is less than 7, the first titration rate can be in the range of 8-12 mL/min; when the pH of the metal salt solution is in the range of 7-8, the first titration rate may be in the range of 4mL/min-6 mL/min.

In some embodiments, the first titration rate may also be determined by other means (e.g., empirical parameters, statistics, user customization, etc.).

In the initial stage of titration, because the concentration of the metal salt solution is relatively large, if the first titration rate is too large, the precipitant and the metal salt solution may form crystal nuclei due to the phenomenon of local over-concentration, and the crystal nuclei may affect the quality of the precipitate, thereby reducing the quality of the powder. In the present embodiment, the titration rate at which nuclei are formed may be referred to as a nuclei titration rate. In some embodiments, the first titration rate may be less than the crystal nucleus titration rate to avoid crystal nuclei from being generated during titration, thereby affecting the quality of the precipitate.

Step 120, monitoring a first rate of change of pH of the solution in real time during the first titration.

The rate of change of pH may refer to the amount of change in the pH of the solution per unit time. Accordingly, the first rate of change of pH may refer to the amount of change in pH of the solution per unit time during the first titration. In some embodiments, the pH value of the solution may be monitored in real time by a pH sensor, so as to obtain a change condition of the pH with time (for example, a curve of the change of the pH with time as shown in fig. 3A and 3B, where a slope of the curve corresponding to each time is an instantaneous pH change rate at the corresponding time).

The precipitant titrates into the metal salt solution, reacts with metal ions to form precipitate on one hand, and reacts with hydrogen ions contained in excessive acid to generate neutralization reaction on the other hand. Thus, the rate of pH change may reflect the rate of precipitation reaction.

In step 130, the first pH change rate reaches a preset threshold, stopping the first titration process.

In the initial stage of titration, the overall reaction is relatively rapid after the precipitant is added, due to the relatively large concentration of the metal salt solution. Accordingly, the rate of change of the pH of the solution gradually increases (or remains substantially stable). With the continuous addition of the precipitant, the metal ions in the solution continuously react with the precipitant to precipitate out. On the one hand, the generated precipitate can influence the continuous progress of the titration reaction, and on the other hand, the concentration of metal ions in the solution gradually decreases, so that the precipitation reaction rate decreases. Accordingly, the rate of change of the pH of the solution may begin to decrease after a certain threshold is reached. For example, as shown in fig. 3A, the slope of the curve gradually increases (or remains substantially stable) from the origin to time tm, and from time tm, the slope of the curve begins to decrease. Therefore, when the first pH change rate reaches a preset threshold (e.g., the pH change rate corresponding to tm time as shown in fig. 3A or the pH change rate threshold set according to the process requirement (e.g., the pH change rate corresponding to tm time)), it is necessary to stop the first titration process in time and determine and/or adjust the titration rate of the subsequent titration processes so that the pH change rate of each titration process is equivalent to ensure consistent quality of the precipitate.

In some embodiments, the preset threshold may correspond to a turning point (from increasing or substantially steady to decreasing turning point) of the rate of change of the pH of the solution. In some embodiments, the preset threshold may be set according to process requirements. In some embodiments, the preset threshold may be determined by empirical parameters, statistical data, user-defined, etc.

In some embodiments, after stopping the first titration process, the solution may also be filtered to obtain a precipitate generated by the first titration process, and the filtered solution may be continued for a subsequent titration process.

Step 140, for an Nth titration process (where N.gtoreq.2), an Nth titration rate is determined.

In connection with step 110, the nth titration rate may refer to the volume or mass of precipitant added to the metal salt solution per unit time during the nth titration.

Step 150, titrating the precipitant into the solution at an nth titration rate.

In some embodiments, after determining the nth titration rate, the precipitant may be titrated into the solution at the nth titration rate. For details of the precipitant and the titration of the precipitant into the solution, reference may be made to the description of step 110 of the present specification, and no further description is given here.

Step 160, monitoring the nth pH change rate of the solution in real time during the nth titration, wherein the nth titration rate is such that the difference between the nth pH change rate and the first pH change rate is within a preset range.

In some embodiments, the nth titration rate may be determined based at least on the first rate of change of pH and the rate determination model.

In some embodiments, the rate determination model may include a statistical model, an empirical model, a model determined by modeling, a model determined by data fitting, and the like.

In some embodiments, the rate determination model may include a machine learning model.

In some embodiments, the nth titration rate may also be determined based on the first rate of change of pH, the titration parameters of the (N-1) th titration process, and the rate determination model to achieve continuous control of the entire titration process.

In some embodiments, the titration parameters of the (N-1) th titration process may include, but are not limited to, the (N-1) th titration rate, the (N-1) th pH change rate, the reaction time of the (N-1) th titration process, the pH of the solution at the end of the (N-1) th titration process, the concentration of the solution at the end of the (N-1) th titration process, and the like.

In some embodiments, the nth titration rate may also be determined based on the first rate of change of pH, the related parameters, and the rate determination model to improve the accuracy and overall suitability of the nth titration rate.

In some embodiments, the relevant parameter may include a concentration of the metal salt solution, a concentration of the precipitant, a first titration rate, a pH of the solution at the end of the first titration process, a concentration of the solution at the end of the first titration process, a reaction time of the first titration process, a titration rate of at least one of the second to (N-1) th titration processes, a pH of the solution at the end of at least one of the second to (N-1) th titration processes, a concentration of the solution at the end of at least one of the second to (N-1) th titration processes, a reaction time of at least one of the second to (N-1) th titration processes, a concentration of the solution corresponding to any time of the entire titration process, a pH of the solution corresponding to any time of the entire titration process, or the like, or any combination thereof.

In some embodiments, the relevant parameters may also include reaction temperature. In some embodiments, the reaction temperature may include an average reaction temperature for each titration process, an instantaneous temperature for each moment in time, and the like.

In some embodiments, the relevant parameters may also include other parameters related to the titration process, such as reaction humidity, air index, etc.

In some embodiments, the model may be determined by multiple sample training rates. For convenience of description, the metal salt solution and the precipitant involved in the model training process are referred to as "sample metal salt solution" and "sample precipitant", respectively, and each parameter involved in the model training process is referred to as "sample parameter". In some embodiments, during model training, the input of the model may include any combination of any one or more of the sample parameters corresponding to the above parameters and a sample candidate titration rate; the output of the model may be the sample pH rate of change of the sample solution; training labels (model trained label) are the actual rate of pH change of the sample solution.

Accordingly, after model training is completed, the rate determination model may output solution pH change rates corresponding to a plurality of candidate titration rates based on the multidimensional relevant parameters associated with the metal salt solution. Further, a final nth titration rate may be screened from the plurality of candidate titration rates based on the first pH rate and the pH rate of change corresponding to the plurality of candidate titration rates.

In some embodiments, parameters of the rate determination model may also be dynamically updated based on the updated experimental data, enhancing the comprehensive learning capabilities of the rate determination model to determine a more appropriate nth titration rate.

For a description of determining the nth titration rate based at least on the first rate of change of pH and the rate determination model, reference may be made to other parts of the specification (e.g., fig. 2 and its associated description), which are not repeated here.

In some embodiments, the difference in the nth pH change rate and the first pH change rate may refer to the difference in the average pH change rate of the nth titration process and the average pH change rate of the first titration process. For example, as shown in fig. 3B, the difference between the second pH change rate and the first pH change rate may be the difference between the average pH change rate of the second titration process and the average pH change rate of the first titration process: AB/(t 2-t 1) -OA/t1.

In some embodiments, the difference in the nth pH change rate and the first pH change rate may refer to the difference in the instantaneous NpH th change rate at a time during the nth titration and the instantaneous first pH change rate at a time during the first titration (a time corresponding to a time during the nth titration). In some embodiments, it is assumed that the reaction time of the first titration process corresponds to the (XTn/T1) th time in the nth titration process with the reaction time of the nth titration process being T1 and Tn, respectively, wherein X is no greater than any value of T1. For example, the reaction time of the first titration process is 10 minutes and the reaction time of the nth titration process is 5 minutes, then the 4 th minute of the first titration process corresponds to the 2 nd minute of the nth titration process.

In some embodiments, the nth pH rate of change may reflect the reaction rate of the nth titration process. The difference value between the N pH change rate and the first pH change rate is controlled within a preset range by controlling the N titration rate, so that the reaction rate of the N titration process is close to that of the first titration process, and the precipitation reaction rate in each titration process is further kept stable, so that the quality of finally prepared powder is improved.

In some embodiments, the preset range may be determined by empirical parameters, statistical data, user-defined, etc.

In some embodiments, the titration rate during the same titration may be a fixed value or may be dynamically variable. For example, the nth titration rate may be dynamically adjusted such that the difference between the nth pH change rate and the first pH change rate is within a preset range.

With the continuous addition of the precipitant, the metal ions in the solution continuously react with the precipitant to precipitate out, and the concentration of the metal ions in the solution gradually decreases. Therefore, in some embodiments, the nth titration rate may be greater than the (N-1) th titration rate, so that the reaction rate of the metal ions and the precipitant in each titration process is kept as stable as possible without generating crystal nuclei, thereby reducing quality problems such as non-uniform particle size of the powder. For example, during the first titration, the concentration of metal ions in the metal salt solution may be maximized and the first titration rate may be minimized to prevent nucleation of the "local over-concentration" phenomenon. When entering the second titration process, a second titration rate may be used that is greater than the first titration rate due to the reduced concentration of metal ions in the solution. When entering the third titration process, the third titration rate may be greater than the second titration rate as the concentration of metal ions in the solution further decreases, and so on.

In some embodiments, similar to the first titration process, when the (N-1) th pH change rate reaches a preset threshold, the (N-1) th titration process may be stopped and the solution filtered to obtain a precipitate generated during the (N-1) th titration process, and the N-th titration process may be continued on the filtered solution. In some embodiments, the preset thresholds for the pH change rates for different titration processes may be the same or different. For example only, as shown in fig. 3B, at point a, the first rate of change of pH reaches a preset threshold, the first titration process (such as the OA segment curve shown in fig. 3) ends, and the second titration process is entered. At point B, the second pH change rate reaches a preset threshold, the second titration process (e.g., the AB segment curve shown in fig. 3) ends, and a third titration process is entered. The pH change rate shown in point a may be the same as or different from the pH change rate shown in point B.

In some embodiments, the first titration process or the nth titration process can be implemented by spraying the precipitant, so that the precipitant can contact and react with the metal salt solution in a mist form, the reaction surface area can be increased, and the reaction efficiency can be improved.

In some embodiments, during titration, the solution may be stirred to thoroughly mix the precipitant with the metal ions, facilitating the precipitation reaction. In some embodiments, the solution may be stirred in a fixed direction. In some embodiments, the direction of agitation may be periodically changed, for example, first for a period of time with clockwise agitation and then for a period of time with counter-clockwise agitation. Periodically changing the stirring direction can improve the mixing effect and promote the precipitation reaction.

In some embodiments, the stirring speed may be the same or different for different titration processes. For example, during the first titration, the solution may be stirred at a greater stirring speed. During the nth titration, the solution may be stirred at a slower stirring rate.

In some embodiments, after stopping the nth titration process, the solution may be filtered to collect the precipitate produced by the nth titration process. In some embodiments, the precipitate collected from each titration process may be aggregated and further processed (e.g., dried, milled, etc.) to produce a final powder.

It should be noted that the above description of the process 100 is for illustration and description only, and is not intended to limit the scope of applicability of the present disclosure. Various modifications and changes to the process 100 will be apparent to those skilled in the art in light of the present description. However, such modifications and variations are still within the scope of the present description. For example, during each titration, parameters other than pH (e.g., concentration of metal ions) may be monitored to provide a comparable rate of decrease in concentration of metal ions during each titration to ensure a steady rate of reaction during each titration. The examples herein are not limited to other parameters as long as they reflect the reaction rate of the titration process.

FIG. 2 is a flow chart illustrating an exemplary determination of an Nth titration rate in accordance with some embodiments. In some embodiments, the process 200 may be performed by a processing device of a control system. As shown in fig. 2, the process 200 includes the following steps.

At step 210, a plurality of candidate titration rates are determined.

In some embodiments, the candidate titration rates may be determined by statistical data, empirical parameters, or user customization. In some embodiments, the candidate titration rate may be determined based on the (N-1) th titration rate. For example, the candidate titration rate may be greater than the (N-1) th titration rate, and the difference between the two is within a preset range. In some embodiments, the preset range may be determined based on statistical data, empirical parameters, or user customization.

In some embodiments, the plurality of candidate titration rates may be arranged in an arithmetic progression. For example, the plurality of candidate titration rates may be 5ml/min, 10ml/min, 15ml/min, 20ml/min, etc. In some embodiments, the plurality of candidate titration rates can be arranged in an arithmetic progression of increasing or decreasing values. For example, 5ml/min, 6ml/min, 8ml/min, 11ml/min, 15ml/min, etc. The number of candidate titration rates may not be limited in the embodiments of the present specification. In some embodiments, the number of candidate titration rates may be increased appropriately in order to obtain a more appropriate nth titration rate.

Step 220, determining a plurality of candidate pH change rates corresponding to the plurality of candidate titration rates, respectively, based at least on the plurality of candidate titration rates and the rate determination model.

In some embodiments, as described in connection with fig. 1, a plurality of candidate titration rates and one or more associated parameters may be input into a rate determination model, which will output a plurality of candidate pH change rates for each of the plurality of candidate titration rates. For a particular candidate titration rate, the candidate pH change rate may represent a simulated solution pH change based on the particular candidate titration rate.

At step 230, an nth titration rate is selected from the plurality of candidate titration rates based on the plurality of candidate pH rates and the first pH rate of change.

In some embodiments, the differences between the plurality of candidate pH change rates and the first pH change rate may be calculated, respectively, and it may be determined whether the minimum difference is within a preset range. If so, determining the candidate titration rate corresponding to the minimum difference as the Nth titration rate. If not, further determining a plurality of other candidate titration rates, and repeating the steps.

In some embodiments, the next set of candidate titration rates can be adjusted based on the minimum difference described above. For example, if the minimum difference corresponding to the previous set of candidate titration rates still deviates from the preset range to a large extent, the next set of input candidate titration rates may be adjusted to a large extent. For another example, if the minimum difference corresponding to the previous set of candidate titration rates deviates from the preset range to a small extent, the next set of input candidate titration rates may be adjusted to a small extent.

It should be noted that the above description of the process 200 is for illustration and description only, and is not intended to limit the scope of applicability of the present disclosure. Various modifications and changes to flow 200 will be apparent to those skilled in the art in light of the present description. However, such modifications and variations are still within the scope of the present description.

FIG. 3A is a graph of pH over time without adjustment of the titration rate during titration. Fig. 3B is a schematic illustration of a graph of pH over time with adjustment of titration rate during titration, according to some embodiments of the present disclosure.

As shown in fig. 3A, the slope of the curve remains substantially constant throughout the titration period, starting at time tm and decreasing.

As shown in fig. 3B, according to some embodiments of the present disclosure, the titration rates of different titration processes are dynamically adjusted during the whole titration process, so that the slope of the curve corresponding to each titration process at a corresponding specific time (for example, the X-th time in the first titration process corresponds to the (XTn/T1) time in the nth titration process) is equivalent, and further, the reaction rate of the whole titration process can be kept stable.

As shown in fig. 4, the titration apparatus 400 may include at least two titration assemblies (illustrated as two titration assemblies, a first titration assembly 410 and an nth titration assembly 420, respectively, where N is an integer not less than 2) and a collection assembly 430.

The first titration assembly 410 may be used to perform a first titration process. In some embodiments, first titration assembly 410 may include first titration vessel 411 and first titration nozzle 412.

In some embodiments, the first titration vessel 411 may be an instrument that holds a metal salt solution, and may also provide a location for the precipitation agent and the metal salt solution to perform a first titration reaction. In some embodiments, the material of the first titration vessel 411 may include any material that does not react with the metal salt solution and the precipitant.

In some embodiments, a first titration nozzle 412 may be used to spray a precipitation agent into the first titration container 411. In some embodiments, first titration nozzle 412 may be located above the metal salt solution and within or above first titration container 411.

In some embodiments, the first titration assembly 410 may further include a first metal salt solution input conduit 413 for inputting the metal salt solution into the first titration vessel 411.

The nth titration component 420 can be used to perform an nth titration process. In some embodiments, the nth titration assembly 420 may include an nth titration vessel 421, a saline delivery tube 422, and an nth titration nozzle 423.

In some embodiments, the nth titration vessel 421 may be the same as or different from the first titration vessel 411. In some embodiments, the nth titration vessel 421 may be used to hold a salt solution, and may also provide a location for an nth titration reaction of a precipitant with the salt solution.

In some embodiments, saline delivery tube 422 may be used to input saline after the end of the (N-1) th titration process to Nth titration assembly 420.

In some embodiments, the nth titration nozzle 423 may be the same as or different from the first titration nozzle 412. In some embodiments, an nth titration nozzle 423 may be used to inject a precipitation agent into an nth titration container 421. In some embodiments, the nth titration nozzle 423 may be located above the saline solution.

In some embodiments, the Nth titration assembly 420 may also include an Nth filter 424 for filtering the saline solution generated by the (N-1) th titration process to collect the precipitate generated by the (N-1) th titration process.

The collection assembly 430 may be used to filter and collect sediment produced by the nth titration process. In some embodiments, collection assembly 430 may include a collection container 431, a collection line 432, and a collection filter 433.

In some embodiments, collection container 431 may be used to hold filtrate generated by filtering the saline solution of the nth titration process. In some embodiments, the collection container 431 may be the same as or different from the first titration container 411.

In some embodiments, collection line 432 may be used to input saline solution to collection assembly 430 after the end of the nth titration process.

In some embodiments, a collection filter 433 may be used to filter the salt solution produced by the nth titration process to collect the precipitate produced by the nth titration process.

In some embodiments, at least one of the at least two titration assemblies may further comprise a stirring component (not shown) for stirring the salt solution to substantially react the precipitant with the metal ions.

In some embodiments, the titration apparatus 400 may further include a pH sensor (not shown) for monitoring the pH of the saline solution.

In some embodiments, the titration apparatus 400 may further include a processing device for generating a pH-dependent relationship (e.g., a rate of change of pH) of the saline solution from the pH of the saline solution detected by the pH sensor. In some embodiments, the processing device may also determine an nth titration rate. In some embodiments, the processing device may also determine a rate determination model. For a description of determining the nth titration rate and determining the rate determination model, reference may be made to other portions of the specification (e.g., fig. 1,2 and their associated descriptions), which are not repeated here.

Possible benefits of embodiments of the present description include, but are not limited to: (1) The method comprises at least two titration processes, wherein each titration process titrates a precipitant into a salt solution at a specific titration rate, so that the difference value of the solution pH change rates of any two titration processes in the at least two titration processes is within a preset range, the reaction rate of the whole titration process can be kept stable, the quality of a precipitate prepared by each titration process is ensured to be as consistent as possible, and the quality of finally prepared powder is improved. (2) And through a rate determination model, synthesizing multidimensional parameters, simulating pH change conditions under different titration rates, thereby determining the Nth titration rate, and enabling the Nth titration rate to be more proper and accurate.

While the basic concepts have been described above, it will be apparent to those skilled in the art that the foregoing detailed disclosure is by way of example only and is not intended to be limiting. Although not explicitly described herein, various modifications, improvements, and adaptations to the present disclosure may occur to one skilled in the art. Such modifications, improvements, and modifications are intended to be suggested within this specification, and therefore, such modifications, improvements, and modifications are intended to be included within the spirit and scope of the exemplary embodiments of the present invention.

Meanwhile, the specification uses specific words to describe the embodiments of the specification. Reference to "one embodiment," "an embodiment," and/or "some embodiments" means that a particular feature, structure, or characteristic is associated with at least one embodiment of the present description. Thus, it should be emphasized and should be appreciated that two or more references to "an embodiment" or "one embodiment" or "an alternative embodiment" in various positions in this specification are not necessarily referring to the same embodiment. Furthermore, certain features, structures, or characteristics of one or more embodiments of the present description may be combined as suitable.

Furthermore, the order in which the elements and sequences are processed, the use of numerical letters, or other designations in the description are not intended to limit the order in which the processes and methods of the description are performed unless explicitly recited in the claims. While certain presently useful inventive embodiments have been discussed in the foregoing disclosure, by way of various examples, it is to be understood that such details are merely illustrative and that the appended claims are not limited to the disclosed embodiments, but, on the contrary, are intended to cover all modifications and equivalent arrangements included within the spirit and scope of the embodiments of the present disclosure. For example, while the system components described above may be implemented by hardware devices, they may also be implemented solely by software solutions, such as installing the described system on an existing server or mobile device.

Likewise, it should be noted that in order to simplify the presentation disclosed in this specification and thereby aid in understanding one or more inventive embodiments, various features are sometimes grouped together in a single embodiment, figure, or description thereof. This method of disclosure does not imply that the subject matter of the present description requires more features than are set forth in the claims. Indeed, less than all of the features of a single embodiment disclosed above.

In some embodiments, numbers describing the components, number of attributes are used, it being understood that such numbers being used in the description of embodiments are modified in some examples by the modifier "about," approximately, "or" substantially. Unless otherwise indicated, "about," "approximately," or "substantially" indicate that the number allows for a 20% variation. Accordingly, in some embodiments, numerical parameters set forth in the specification and claims are approximations that may vary depending upon the desired properties sought to be obtained by the individual embodiments. In some embodiments, the numerical parameters should take into account the specified significant digits and employ a method for preserving the general number of digits. Although the numerical ranges and parameters set forth herein are approximations that may be employed in some embodiments to confirm the breadth of the range, in particular embodiments, the setting of such numerical values is as precise as possible.

Each patent, patent application publication, and other material, such as articles, books, specifications, publications, documents, etc., referred to in this specification is incorporated herein by reference in its entirety. Except for application history documents that are inconsistent or conflicting with the content of this specification, documents that are currently or later attached to this specification in which the broadest scope of the claims to this specification is limited are also. It is noted that, if the description, definition, and/or use of a term in an attached material in this specification does not conform to or conflict with what is described in this specification, the description, definition, and/or use of the term in this specification controls.

Finally, it should be understood that the embodiments described in this specification are merely illustrative of the principles of the embodiments of this specification. Other variations are possible within the scope of this description. Thus, by way of example, and not limitation, alternative configurations of embodiments of the present specification may be considered as consistent with the teachings of the present specification. Accordingly, the embodiments of the present specification are not limited to only the embodiments explicitly described and depicted in the present specification.

Claims

1. A titration method for precipitation reactions for powder preparation, the titration method comprising:

For the first titration procedure, a second titration procedure was used,

Titrating the precipitant into the metal salt solution at a first titration rate; wherein,

The first titration rate is based at least on the concentration of the precipitant, the concentration of the metal salt solution, and the pH of the metal salt solution;

Monitoring a first pH change rate of the solution in real time during the first titration;

the first pH change rate reaches a preset threshold value, and the first titration process is stopped;

For the Nth titration process, where N.gtoreq.2,

Determining an nth titration rate;

titrating the precipitant into solution at the nth titration rate;

And monitoring the N pH change rate of the solution in real time in the N titration process, wherein the N titration rate enables the difference value between the N pH change rate and the first pH change rate to be in a preset range.

2. The titration method of claim 1, wherein the first titration process or the nth titration process is performed by spraying the precipitant.

3. The titration method of claim 1, wherein the nth titration rate is greater than the (N-1) th titration rate.

4. The titration method of claim 1, wherein the determining the nth titration rate comprises:

The nth titration rate is determined based at least on the first rate of change of pH and a rate determination model.

5. The titration method of claim 4, wherein the determining the nth titration rate based at least on the first rate of change of pH and the rate determination model comprises:

Determining the nth titration rate based on the first rate of change of pH, a related parameter, and the rate determination model, wherein the related parameter comprises:

At least one of the concentration of the metal salt solution, the concentration of the precipitant, the first titration rate, the pH of the solution at the end of the first titration process, the concentration of the solution at the end of the first titration process, the reaction time of the first titration process, the titration rate of at least one of the second to (N-1) th titration processes, the pH of the solution at the end of at least one of the second to (N-1) th titration processes, the concentration of the solution at the end of at least one of the second to (N-1) th titration processes, or the reaction time of at least one of the second to (N-1) th titration processes.

6. The titration method of claim 5, wherein the associated parameters further include reaction temperature.

7. The titration method of claim 5 or 6, wherein the rate determination model is generated by a model training process, the model training process comprising: the initial machine learning model is trained based on the sample related parameters, the sample candidate titration rate, the sample pH change rate of the sample solution, and the actual pH change rate of the sample solution as a training label, resulting in the rate determination model.

8. The titration method of claim 4, wherein the determining the nth titration rate based at least on the first rate of change of pH and the rate determination model comprises:

Determining a plurality of candidate titration rates;

determining a plurality of candidate pH change rates corresponding to the plurality of candidate titration rates, respectively, based at least on the plurality of candidate titration rates and the rate determination model;

the nth titration rate is selected from the plurality of candidate titration rates based on the plurality of candidate pH rates and the first pH rate of change.

9. The titration method of claim 1, wherein the method further comprises:

And after stopping the first titration process or the Nth titration process, filtering the solution obtained after the first titration process or the Nth titration process.

10. A titration device, comprising:

A first titration component and an Nth titration component, wherein N is more than or equal to 2,

The first titration assembly is for performing a first titration process for which the first titration assembly is for titrating a precipitant into a metal salt solution at a first titration rate; wherein the first titration rate is based at least on the concentration of the precipitant, the concentration of the metal salt solution, and the pH of the metal salt solution;

The nth titration component is used for performing an nth titration process for which the nth titration component titrates the precipitant into the solution at an nth titration rate;

a collection assembly for filtering and collecting the precipitate produced by the nth titration process;

a pH sensor for monitoring the pH of the salt solution; and

A processing device for generating a pH change rate of the salt solution according to the pH of the salt solution detected by the pH sensor; in the first titration process, monitoring a first pH change rate of the solution in real time, wherein the first pH change rate reaches a preset threshold value, and controlling a first titration assembly to stop the first titration process; determining an nth titration rate; and monitoring the N pH change rate of the solution in real time in the N titration process, wherein the N titration rate enables the difference value between the N pH change rate and the first pH change rate to be in a preset range.