Method and apparatus for controlling particle size of a synthetic product

Abstract

The application relates to the technical field of synthetic reaction, in particular to a particle size control method and particle size control equipment for precisely regulating the particle size of a synthetic product. The method comprises determining a process parameter X according to formula 1) n to control the particle size; De n , De n‑1 is the n-th, (n-1)-th measured particle size value De; Df n , Df n‑1 is the n-th, (n-1)-th measured particle size value Df; De t , Df t is a target particle size value De, Df; De and Df are particle size values corresponding to the cumulative particle size distribution percentage of the synthetic product reaching e%, f%, 0 n , K2 n are determined according to formula 2).

Description

Technical Field

[0001] This application relates to the field of synthetic reaction technology, and in particular to a method and equipment for particle size control of synthetic products. Background Technology

[0002] In synthetic reactions, various uncontrollable factors, such as temperature and feed flow rate, can lead to instability, causing the particle size of the synthesized product to deviate from the target value and thus affecting product quality. Existing particle size control methods suffer from imprecise relationships between influencing factors and particle size, resulting in poor control accuracy. For example, pH is not precisely correlated with particle size, and the rate of particle size change after pH adjustment is not considered, which negatively impacts the accurate control of the synthesized product's particle size. Summary of the Invention

[0003] This application discloses a method and equipment for controlling the particle size of synthesized products, in order to solve the problem that the particle size control methods of existing synthesized products have poor control accuracy.

[0004] To achieve the above objectives, this application provides the following technical solution:

[0005] In a first aspect, this application provides a method for controlling the particle size of a synthesized product, the method comprising the following steps:

[0006] The numerical value of the process parameter X is determined according to Equation 1). n To control the particle size of the synthesized product;

[0007]

[0008] Among them, De n Let De be the nth measured particle size value of the synthesized product. n-1 De is the (n-1)th measured particle size value of the synthesized product. t De is the target particle size value of the synthesized product; De is the particle size value corresponding to the cumulative particle size distribution percentage of the synthesized product reaching e%, 0 < e < 100;

[0009] Df n Let Df be the nth measured particle size value of the synthesized product. n-1 Df is the (n-1)th measured particle size value of the synthesized product. t Let e ​​be the target particle size value Df of the synthesized product; Df is the particle size value corresponding to the cumulative particle size distribution percentage of the synthesized product reaching f%, where 0 < f < 100, and e and f are different.

[0010] Among them, K1 n K2 n To determine Xn The variable coefficient value at time, K1 n K2 n The particle size change rate is determined based on the magnitude of the particle size change rate obtained from equation 2).

[0011]

[0012] K1 n K2 n The absolute value of Y1 n The absolute values ​​of are positively correlated; where i is selected from either the e value or the f value.

[0013] Furthermore, K1 n K2 n The magnitude of the particle size change rate determined according to Equation 2) includes:

[0014] (1) When And Di (n-1) >Di t At that time, K1 n ≥0, K2 n ≥0;

[0015] when And Di (n-1) <Di t At that time, K1 n ≥0, K2 n ≥0;

[0016] (2) When And Di (n-1) >Di t At that time, K1 n ≤0, K2 n ≤0;

[0017] when And Di (n-1) <Di t At that time, K1 n ≤0, K2 n ≤0.

[0018] Furthermore, the granularity control method also includes an optimization process, which includes:

[0019] The value of the storage process parameter is X. n Measured particle size value De n 、Df n The value of the process parameter is X. n-1 Measured particle size value De n-1 、Df n-1 and particle size change rate Y1 n ;

[0020] When Y1n When the first preset condition is met, the particle size change rate is determined to be Y1. n K1 corresponding to the time n-1 K2 n-1 De n-1 、Df n-1 The optimal adjustment value is set as K1. n-1 *、K2 n-1 *、De* n-1 、Df* n-1 ;

[0021] Within a preset storage period, multiple optimal adjustment values ​​form an optimal adjustment method database.

[0022] Furthermore, the first preset condition includes:

[0023]

[0024]

[0025] Where 0 < A ≤ 3, -3 ≤ B < 0.

[0026] Furthermore, the optimization process also includes determining K1 based on the optimal adjustment database. n K2 n Specifically, it includes the following steps:

[0027] Within the preset storage period, the measured granularity value De from the Nth time will be stored. n 、Df n De* in the optimal adjustment method database n 、Df* n Compare the values ​​to obtain the corresponding particle size deviation values. n df n ;

[0028] When de n df n When the second preset condition is met, K1 n K2 n The value of K1 is directly called from the optimal adjustment method database. n *、K2 n *

[0029] Furthermore, de n For De n and De* n The difference between De* n The ratio of df n For Df n and Df* n The difference between Df* nThe ratio; the second preset condition includes de n The absolute value is less than the first preset value, and df n The absolute value is less than the second preset value.

[0030] Furthermore, both the first and second preset values ​​are 3%.

[0031] Furthermore, the process parameters are the pH value, temperature, pressure, or feed flow rate of the synthesis reaction.

[0032] Secondly, this application provides a particle size control device, which includes an online monitoring system and a control system. The online monitoring system is used to acquire the measured particle size value of the synthesized product and the detection value of the process parameters, and transmit them to the control system so that the control system can execute the control process as in the particle size control method of the first aspect.

[0033] Furthermore, the online monitoring system includes an online particle size analyzer, which monitors the measured particle size of the synthesized product in real time and transmits it to the control system.

[0034] The beneficial effects of adopting the technical solution of this application are as follows:

[0035] Firstly, the particle size control method provided in this application regulates particle size by constructing a relationship function between process parameters and the particle size of the synthesized product. The variable coefficient of the aforementioned relationship function is determined by the particle size change rate of the synthesized product, thereby precisely regulating the particle size of the synthesized product by controlling the process parameters. This ensures that the particle size of the synthesized product stably approaches the target value, avoiding excessive particle size changes before and after regulation. Compared with existing control methods, this method can precisely regulate the particle size of the synthesized product, thereby improving work efficiency and product quality.

[0036] Secondly, the particle size control equipment provided in this application includes an online monitoring system that can monitor the particle size of the synthesized product and the measured values ​​of process parameters in real time, and transmit them to the control system so that the control system can execute the control process in the first aspect of this application. This particle size control equipment can monitor, analyze, and control the synthesis reaction to ensure that the particle size of the synthesized product is stably close to the target value, thereby improving production efficiency and product quality. Detailed Implementation

[0037] To make the objectives, technical solutions, and advantages of this application clearer, a further detailed description will be provided below. Obviously, the described embodiments are merely some, not all, of the embodiments described in this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0038] The application scenarios described in this application are for the purpose of more clearly illustrating the technical solutions of this application, and do not constitute a limitation on the technical solutions provided in this application. Those skilled in the art will understand that with the emergence of new application scenarios, the technical solutions provided in this application are also applicable to similar technical problems. In the description of this application, unless otherwise stated, "multiple" means two or more.

[0039] In synthetic reactions, various factors can lead to instability, causing the particle size of the synthesized product to deviate from the target value and thus affecting product quality. Existing particle size control methods lack precise understanding of the relationship between influencing factors and particle size, and do not consider the rate of particle size change after adjusting influencing factors, making precise control of the synthesized product particle size difficult.

[0040] In view of this, embodiments of this application provide a method for particle size control of a synthesized product, the method comprising the following steps:

[0041] The numerical value of the process parameter X is determined according to Equation 1). n To control the particle size of the synthesized product;

[0042]

[0043] Among them, De n Let De be the nth measured particle size value of the synthesized product. n-1 De is the (n-1)th measured particle size value of the synthesized product. t De is the target particle size value of the synthesized product; De is the particle size value corresponding to the cumulative particle size distribution percentage of the synthesized product reaching e%, 0 < e < 100;

[0044] Df n Let Df be the nth measured particle size value of the synthesized product. n-1 Df is the (n-1)th measured particle size value of the synthesized product. t Let e ​​be the target particle size value Df of the synthesized product; Df is the particle size value corresponding to the cumulative particle size distribution percentage of the synthesized product reaching f%, where 0 < f < 100, and e and f are different.

[0045] Among them, K1 n K2 n To determine X n The variable coefficient value at time, K1 n K2 n The particle size change rate is determined based on the magnitude of the particle size change rate obtained from equation 2).

[0046]

[0047] K1 n K2n The absolute value of Y1 n The absolute values ​​of are positively correlated; where i is selected from either the e value or the f value.

[0048] Considering the accuracy of particle size adjustment, the value of i is less than or equal to 30, and the value of i can be 5, 6, 8, 10, 15, 20, 25 or 30. Preferably, the value of i is 5 or 10.

[0049] It is understandable that e and f are different, 0 < e < 100, 0 < f < 100. Among them, one of e and f is preferably 50, because D50 has moderate sensitivity to the control of process parameters, and D50 is the center value of particle size, which is more important; the other of e and f is less than or equal to 30, because the particle size within the above range is more sensitive to the control of process parameters, thus allowing for more precise control of the particle size of the synthesized product.

[0050] Current particle size control methods typically involve manually sampling a portion of the slurry at regular intervals to test its particle size. Based on the particle size results, the reaction conditions are then manually adjusted. After a period of time, another sample is taken to confirm the particle size change, and the conditions are adjusted again, continuously refining the process until the particle size returns to normal. This existing manual particle size testing method not only increases the workload for employees but also reduces production efficiency.

[0051] In view of this, the particle size of the synthesized product is monitored by an online detection method in the embodiments of this application. By monitoring the measured particle size value of the synthesized product online in real time, manual operation is avoided and production efficiency is greatly improved.

[0052] In one embodiment of this application, K1 n K2 n The magnitude of the particle size change rate determined according to Equation 2) includes:

[0053] (1) When And Di (n-1) >Di t At that time, K1 n ≥0, K2 n ≥0;

[0054] when And Di (n-1) <Di t At that time, K1 n ≥0, K2 n ≥0;

[0055] (2) When And Di (n-1) >Di t At that time, K1 n ≤0, K2 n ≤0;

[0056] when And Di (n-1) <Di t At that time, K1 n ≤0, K2 n ≤0.

[0057] Among them, K1 n K2 n The absolute value of Y1 n The absolute values ​​are positively correlated. After judging according to Equation 2), we obtain K1. n K2 n The range of values ​​for K1 n K2 n For discrete values ​​within the corresponding interval, specifically, taking a ternary precursor as an example, when e = 10, f = 50, X n When the precipitant flow rate is given, let's take Equation 2) as an example for further explanation:

[0058] (1) When And Di (n-1) ≥Di t At that time, K1 n >0.200, K2 n >0.300;

[0059] when And Di (n-1) ≤Di t At that time, K1 n >0.200, K2 n >0.300;

[0060] (2) When And Di (n-1) ≥Di t When 0.080 < K1 n <0.150, 0.120 <K2 n <0.225;

[0061] when And Di (n-1) ≤Di t When 0.080 < K1 n <0.150, 0.120 <K2 n <0.225;

[0062] (3) When And Di (n-1) ≥Di t When 0.028 < K1 n <0.050, 0.042 <K2 n <0.075;

[0063] when And Di (n-1) ≤Di t When 0.028 < K1 n <0.050, 0.042 <K2 n <0.075;

[0064] (4) When And Di (n-1) ≥Di t When 0.009 < K1 n <0.015, 0.0135 <K2 n <0.0225;

[0065] when And Di (n-1) ≤Di t When 0.009 < K1 n <0.015, 0.0135 <K2 n <0.0225;

[0066] (5) When And Di (n-1) ≥Di t When 0 < K1 n <0.009, 0 < K2 n <0.0135;

[0067] when And Di (n-1) ≤Di t When 0 < K1 n <0.009, 0 < K2 n <0.0135;

[0068] (6) When And Di (n-1) <Di t At that time, K1 n <-0.200, K2 n <-0.300;

[0069] when And Di (n-1) >Di t At that time, K1 n <-0.200, K2 n <-0.300;

[0070] (7) When And Di (n-1) <Di t When -0.150 < K1 n <-0.080, -0.225<K2 n <-0.120;

[0071] when And Di (n-1) >Di t When -0.150 < K1 n <-0.080, -0.225<K2 n <-0.120;

[0072] (8) When And Di (n-1) <Di t When -0.050 < K1 n <-0.028, -0.075<K2 n <-0.042;

[0073] when And Di (n-1) >Di t When -0.050 < K1 n <-0.028, -0.075<K2 n <-0.042;

[0074] (9) When And Di (n-1) <Di t When -0.015 < K1 n <-0.009, -0.0225<K2 n <-0.0135;

[0075] when And Di (n-1) >Di t When -0.015 < K1 n <-0.009, -0.0225<K2 n <-0.0135;

[0076] (10) When And Di (n-1) <Di t When -0.009 < K1 n <0, -0.0135<K2 n <0;

[0077] when And Di (n-1) >Di t When -0.009 < K1 n <0, -0.0135<K2 n <0.

[0078] In one embodiment of this application, when n=1, K11 and K21 are determined according to De1 and Det The relative size, and Df1 and Df t The determination of relative size includes:

[0079] (1) If De1-De t >0, Df1-Df t >0, 0≤K11≤0.2, 0≤K21≤0.3;

[0080] (2) If De1-De t >0, Df1-Df t <0, 0≤K11≤0.2, -0.3≤K21≤0;

[0081] (3) If De1-De t <0, Df1-Df t <0, 0≤K11≤0.2, 0≤K21≤0.3;

[0082] (4) If De1-De t <0, Df1-Df t >0, 0≤K11≤0.2, -0.3≤K21≤0.

[0083] Understandably, K1 n K2 n The value of can be any value within the range of values ​​under the corresponding conditions.

[0084] After judging according to Equation 2), K1 is obtained. n K2 n The range of values ​​for K1 n K2 n For discrete values ​​within the corresponding interval, specifically, taking a ternary precursor as an example, when e = 10, f = 50, X n For pH, let's take Equation 2) as an example for further explanation:

[0085] (1) When And Di (n-1) ≥Di t At that time, K1 n >0.040, K2 n >0.060;

[0086] when And Di (n-1) ≤Di t At that time, K1 n >0.040, K2 n >0.060;

[0087] (2) When And Di (n-1) ≥Dit When 0.015 < K1 n <0.022, 0.0225 <K2 n <0.033;

[0088] when And Di (n-1) ≤Di t When 0.015 < K1 n <0.022, 0.0225 <K2 n <0.033;

[0089] (3) When And Di (n-1) ≥Di t When 0.007 < K1 n <0.010, 0.0105 <K2 n <0.015;

[0090] when And Di (n-1) ≤Di t When 0.007 < K1 n <0.010, 0.0105 <K2 n <0.015;

[0091] (4) When And Di (n-1) ≥Di t When 0.0024 < K1 n <0.0040, 0.0036 <K2 n <0.0060;

[0092] when And Di (n-1) ≤Di t When 0.0024 < K1 n <0.0040, 0.0036 <K2 n <0.0060;

[0093] (5) When And Di (n-1) ≥Di t When 0 < K1 n <0.0024, 0 < K2 n <0.0036;

[0094] when And Di (n-1) ≤Di t When 0 < K1 n <0.0024, 0 < K2 n <0.0036.

[0095] (6) When And Di (n-1) <Di t At that time, K1 n <-0.040, K2 n <-0.060;

[0096] when And Di (n-1) >Di t At that time, K1 n <-0.040, K2 n <-0.060;

[0097] (7) When And Di (n-1) <Di t When -0.022 < K1 n <-0.015, -0.033<K2 n <-0.0225;

[0098] when And Di (n-1) >Di t When -0.022 < K1 n <-0.015, -0.033<K2 n <-0.0225;

[0099] (8) When And Di (n-1) <Di t When -0.010 < K1 n <-0.007, -0.015<K2 n <-0.0105;

[0100] when And Di (n-1) >Di t When -0.010 < K1 n <-0.007, -0.015<K2 n <-0.0105;

[0101] (9) When And Di (n-1) <Di t When -0.004 < K1 n <-0.0024, -0.006<K2 n <-0.0036;

[0102] when And Di (n-1) >Di t When -0.004 < K1n <-0.0024, -0.006<K2 n <-0.0036;

[0103] (10) When And Di (n-1) <Di t When -0.0024 < K1 n <0, -0.0036<K2 n <0;

[0104] when And Di (n-1) >Di t When -0.0024 < K1 n <0, -0.0036<K2 n <0.

[0105] In one embodiment of this application, when n=1, K11 and K21 are determined according to De1 and De t The relative size, and Df1 and Df t The determination of relative size includes:

[0106] (1) If De1-De t >0, Df1-Df t >0, 0≤K11≤0.04, 0≤K21≤0.06;

[0107] (2) If De1-De t >0, Df1-Df t <0, 0≤K11≤0.04, -0.06≤K21≤0;

[0108] (3) If De1-De t <0, Df1-Df t <0, 0≤K11≤0.04, 0≤K21≤0.06;

[0109] (4) If De1-De t <0, Df1-Df t >0, 0≤K11≤0.04, -0.06≤K21≤0.

[0110] Understandably, K1 n K2 n The value of can be any value within the range of values ​​under the corresponding conditions.

[0111] In one embodiment of this application, the granularity control method further includes an optimization process, which includes:

[0112] The value of the storage process parameter is X. nMeasured particle size value De n 、Df n The value of the process parameter is X. n-1 Measured particle size value De n-1 、Df n-1 and particle size change rate Y1 n ;

[0113] When Y1 n When the first preset condition is met, the particle size change rate is determined to be Y1. n K1 corresponding to the time n-1 K2 n-1 De n-1 、Df n-1 The optimal adjustment value is set as K1. n-1 *、K2 n-1 *、De* n-1 、Df* n-1 ;

[0114] Within a preset storage period, multiple optimal adjustment values ​​form an optimal adjustment method database.

[0115] In one embodiment of this application, the first preset condition includes:

[0116]

[0117]

[0118] Where 0 < A ≤ 3, -3 ≤ B < 0.

[0119] Understandably, Y1 n The rate of change is not limited to between -3% and 3%, but can also be other numerical ranges, such as between -1.5% and 1.5%, between -2% and 2%, or between -1% and 1%.

[0120] In one embodiment of this application, the optimization process further includes determining K1 based on the optimal adjustment database. n K2 n Specifically, it includes the following steps:

[0121] Within the preset storage period, the measured granularity value De from the Nth time will be stored. n 、Df n De* in the optimal adjustment method database n 、Df* n Compare the values ​​to obtain the corresponding particle size deviation values. n df n ;

[0122] When de n dfn When the second preset condition is met, K1 n K2 n The value of K1 is directly called from the optimal adjustment method database. n *、K2 n * The optimal adjustment database may contain more than one set of optimal adjustment values. During comparison, the first retrieved optimal adjustment value that meets the second preset condition is directly selected. This optimization process can significantly improve production efficiency.

[0123] This application does not limit the length of the data storage period, which can be set according to the amount of data, such as 1 month, 2 months, 5 months or 1 year. Similarly, this application does not limit the interval for particle size sampling tests, which can be set according to the type of synthesized product, such as 30 min, 60 min, 90 min, 150 min, 200 min or 300 min.

[0124] In one embodiment of this application, de n For De n and De* n The difference between De* n The ratio of df n For Df n and Df* n The difference between Df* n The ratio; the second preset condition includes de n The absolute value is less than the first preset value, and df n The absolute value is less than the second preset value. Examples of the first preset value are 1%, 1.5%, 2%, and 2.5%, with 3% being preferred. Examples of the second preset value are 1%, 1.5%, 2%, and 2.5%, with 3% being preferred.

[0125] In one embodiment of this application, the process parameters are the pH value, temperature, pressure, or feed flow rate of the synthesis reaction. Preferably, the process parameters are the pH value or feed flow rate of the synthesis reaction. Wherein, when the synthesis product is A... m B n When synthesizing the product, the preferred process parameter is the flow rate of the anion B.

[0126] Based on the same inventive concept, embodiments of this application provide a particle size control device, which includes an online monitoring system and a control system. The online monitoring system is used to acquire the measured particle size value of the synthesized product and the detection value of the process parameters, and transmit them to the control system so that the control system executes the control process as in the particle size control method of the first aspect.

[0127] The control system can be a distributed control system (DCS), which can automatically regulate the synthesis reaction by updating process parameters through process control based on data from the online monitoring system.

[0128] In one embodiment of this application, the online monitoring system includes an online particle size analyzer, a flow meter, an online stirring speed meter, and an oxygen analyzer. The online particle size analyzer monitors the measured particle size of the synthesized product in real time and transmits it to the control system. The flow meter monitors the raw material flow of the synthesis reaction and transmits it to the control system. The online stirring speed meter can stir the reaction solution, monitor the speed of the synthesis reaction, and transmit it to the control system. The oxygen analyzer monitors the oxygen content of the synthesis reaction and transmits it to the control system.

[0129] The granularity control method of this application will be further described in detail below with reference to specific embodiments and comparative examples.

[0130] Example 1

[0131] This embodiment is a granularity control method, including the following steps:

[0132] Step A) Prepare a mixed solution of nickel, cobalt, and manganese salts;

[0133] Step B) Configure the control system, including the following aspects:

[0134] a) Input target granularity: D10 t =4.00μm, D50 t =10.30μm;

[0135] b) Determine process parameters: pH adjustment is used, that is, the process parameter is pH value;

[0136] c) Set De to D10, the particle size deviation value corresponding to the optimal adjustment value. n The value is 2%, Df is D50, and the granularity deviation value df corresponding to the optimal adjustment value is... n It is 1.5%;

[0137] d) When n=1, set the values ​​of K11 and K21:

[0138] (1) If De1-De t >0, Df1-Df t Given that K11 > 0 and K21 > 0, assign initial values ​​K11 = 0.03 and K21 = 0.05.

[0139] (2) If De1-De t >0, Df1-Df t<0, K11≥0, K21≤0, assign initial values ​​K11=0.03, K21=-0.05;

[0140] (3) If De1-De t <0, Df1-Df t <0, K11≥0, K21≥0, assign initial values ​​K11=0.03, K21=0.05;

[0141] (4) If De1-De t <0, Df1-Df t Given that K11 > 0, K21 ≤ 0, assign initial values ​​K11 = 0.03, K21 = -0.05;

[0142] When n≥2, set the values ​​of K11 and K21 as follows:

[0143] (1) When And Di (n-1) ≥Di t At that time, K1 n It can be 0.05, K2 n It can be 0.08;

[0144] when And Di (n-1) ≤Di t At that time, K1 n It can be 0.05, K2 n It can be 0.08;

[0145] (2) When And Di (n-1) ≥Di t At that time, K1 n It can be 0.020, K2 n It can be 0.030;

[0146] when And Di (n-1) ≤Di t At that time, K1 n It can be 0.020, K2 n It can be 0.030;

[0147] (3) When And Di (n-1) ≥Di t At that time, K1 n It can be 0.008, K2 n It can be 0.012;

[0148] when And Di (n-1) ≤Di t At that time, K1 nIt can be 0.008, K2 n It can be 0.012;

[0149] (4) When And Di (n-1) ≥Di t At that time, K1 n It can be 0.003, K2 n It can be 0.005;

[0150] when And Di (n-1) ≤Di t At that time, K1 n It can be 0.003, K2 n It can be 0.005;

[0151] (5) When And Di (n-1) ≥Di t At that time, K1 n It can be 0.002, K2 n It can be 0.003;

[0152] when And Di (n-1) ≤Di t At that time, K1 n It can be 0.002, K2 n It can be 0.003;

[0153] (6) When And Di (n-1) <Di t At that time, K1 n It can be -0.05, K2 n It can be -0.08;

[0154] when And Di (n-1) >Di t At that time, K1 n It can be -0.05, K2 n It can be -0.08;

[0155] (7) When And Di (n-1) <Di t At that time, K1 n It can be -0.02, K2 n It can be -0.03;

[0156] when And Di (n-1) >Di t At that time, K1 n It can be -0.02, K2 nIt can be -0.03;

[0157] (8) When And Di (n-1) <Di t At that time, K1 n It can be -0.008, K2 n It can be -0.012;

[0158] when And Di (n-1) >Di t At that time, K1 n It can be -0.008, K2 n It can be -0.012;

[0159] (9) When And Di (n-1) <Di t At that time, K1 n It can be -0.003, K2 n It can be -0.005;

[0160] when And Di (n-1) >Di t At that time, K1 n It can be -0.003, K2 n It can be -0.005;

[0161] (10) When And Di (n-1) <Di t At that time, K1 n It can be -0.001, K2 n It can be -0.002;

[0162] when And Di (n-1) >Di t At that time, K1 n It can be -0.001, K2 n It can be -0.002.

[0163] f) The particle size change rate in the first preset condition is set to 1.0%;

[0164] g) Set the data storage period to 1 month and the particle size sampling test interval to 1 hour;

[0165] Step C) Add the raw material solution and excipient solution for the synthesis reaction to the synthesis reactor, maintain the synthesis reaction temperature at 60℃, and start the synthesis reaction. After the online particle size analyzer has been running for 2 hours, perform particle size testing. After the first particle size test, the online particle size analyzer transmits the test values ​​to the control system. The control system then determines the particle size based on the measured particle size values ​​D101, D501, and the target particle size value D10. t D50 t Confirm K11 and K21, and then perform the first automatic adjustment of process parameters based on the values ​​of K11 and K21;

[0166] Step D) The online particle size analyzer performs a second sampling test and transmits the data to the control system. The control system stores the second measured particle size values ​​D102 and D502 and the first measured particle size values ​​D101 and D501, calculates the particle size change rate, and determines the values ​​of K12 and K22 based on the particle size change rate. Then, the process parameters are automatically adjusted for the second time based on the values ​​of K12 and K22.

[0167] Step E) The online particle size analyzer performs the third and subsequent sampling tests according to the set sampling test interval. The control system stores and analyzes the measured particle size values ​​and records the optimal adjustment values ​​to form an optimal adjustment mode database.

[0168] In subsequent tests, the control system compared the measured granularity values ​​with data from the optimal adjustment mode database. When de n df n When the second preset condition is met, K1 n K2 n The value is directly retrieved from the corresponding value in the optimal adjustment method database;

[0169] The particle size test values, particle size change rate, relevant parameter values, and optimal adjustment values ​​for each test are shown in Table 1.

[0170] Table 1

[0171]

[0172] As can be seen from the data in Table 1, the particle size control method in the embodiments of this application can accurately control the particle size of the synthesized product.

[0173] The above are merely specific embodiments of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. A method for particle size control of a nickel-cobalt-manganese ternary precursor, characterized in that, Includes the following steps: The numerical value of the process parameter X is determined according to Equation 1). n To control the particle size of the nickel-cobalt-manganese ternary precursor; X n =( K1 n + K2 n +1) X n-1 Formula 1) Among them, De n De is the nth measured particle size value of the nickel-cobalt-manganese ternary precursor. n-1 De is the (n-1)th measured particle size value of the nickel-cobalt-manganese ternary precursor. t The target particle size value De for the nickel-cobalt-manganese ternary precursor; De is the particle size value corresponding to the cumulative particle size distribution percentage of the nickel-cobalt-manganese ternary precursor reaching e%, 0 < e < 100; the process parameter is the pH value of the synthesis reaction; Df n Df is the nth measured particle size value of the nickel-cobalt-manganese ternary precursor. n-1 Df is the (n-1)th measured particle size value of the nickel-cobalt-manganese ternary precursor. t Df is the target particle size value of the nickel-cobalt-manganese ternary precursor; Df is the particle size value corresponding to the cumulative particle size distribution percentage of the nickel-cobalt-manganese ternary precursor reaching f%, 0 < f < 100, and e and f are different; Among them, K1 n K2 n To determine the X n The variable coefficient value at time, K1 n K2 n The particle size change rate is determined based on Equation 2); Y1 n = Formula 2) K1 n K2 n The absolute value of Y1 n The absolute values ​​are positively correlated; where i is selected from either the e value or the f value; The particle size control method includes: Step A) Prepare a mixed solution of nickel, cobalt, and manganese salts; Step B) Configure the control system, including the following aspects: a) Input target granularity: D10 t = 4.00 μm, D50 t =10.30μm; b) Determine process parameters: pH adjustment is used, that is, the process parameter is pH value; c) Set De to D10, the particle size deviation value corresponding to the optimal adjustment value. n The value is 2%, Df is D50, and the granularity deviation value df corresponding to the optimal adjustment value is... n It is 1.5%; d) When n=1, set the values ​​of K11 and K21: (1) If De1-De t >0, Df1-Df t Given that K11 > 0, K21 ≥ 0, assign initial values ​​K11 = 0.03, K21 = 0.05; (2) If De1-De t >0, Df1-Df t Given K11 < 0, K21 ≥ 0, and K21 ≤ 0, assign initial values ​​K11 = 0.03 and K21 = -0.

05. (3) If De1-De t <0, Df1-Df t <0, K11≥0, K21≥0, assign initial values ​​K11=0.03, K21=0.05; (4) If De1-De t <0, Df1-Df t Given that K11 > 0, K21 ≤ 0, assign initial values ​​K11 = 0.03, K21 = -0.05; e) When n≥2, set the values ​​of K11 and K21: (1) When 20% and Di (n-1) ≥Di t At that time, K1 n K2 is 0.

05. n It is 0.08; when <-20% and Di (n-1) ≤Di t At that time, K1 n K2 is 0.

05. n It is 0.08; (2) When 10% < <20% and Di (n-1) ≥Di t At that time, K1 n K2 is 0.

020. n It is 0.030; When -20% < <-10% and Di (n-1) ≤Di t At that time, K1 n K2 is 0.

020. n It is 0.030; (3) When 5% < <10% and Di (n-1) ≥Di t At that time, K1 n K2 is 0.

008. n It is 0.012; When -10% < <-5% and Di (n-1) ≤Di t At that time, K1 n K2 is 0.

008. n It is 0.012; (4) When 3% < <5% and Di (n-1) ≥Di t At that time, K1 n K2 is 0.

003. n It is 0.005; When -5% < <-3% and Di (n-1) ≤Di t At that time, K1 n K2 is 0.

003. n It is 0.005; (5) When <3% and Di (n-1) ≥Di t At that time, K1 n K2 is 0.

002. n It is 0.003; When -3% < And Di (n-1) ≤Di t At that time, K1 n K2 is 0.

002. n It is 0.003; (6) When >20% and Di (n-1) <Di t At that time, K1 n K2 is -0.

05. n It is -0.08; when <-20% and Di (n-1) >Di t At that time, K1 n K2 is -0.

05. n It is -0.08; (7) When 20% > >10% and Di (n-1) <Di t At that time, K1 n K2 is -0.

02. n It is -0.03; When -20% < <-10% and Di (n-1) >Di t At that time, K1 n K2 is -0.

02. n It is -0.03; (8) When 10% > >5% and Di (n-1) <Di t At that time, K1 n K2 is -0.

008. n It is -0.012; When -10% < <-5% and Di (n-1) >Di t At that time, K1 n K2 is -0.

008. n It is -0.012; (9) When 5% > >3% and Di (n-1) <Di t At that time, K1 n K2 is -0.

003. n It is -0.005; When -5% < <-3% and Di (n-1) >Di t At that time, K1 n K2 is -0.

003. n It is -0.005; (10) When 3% > And Di (n-1) <Di t At that time, K1 n K2 is -0.

001. n It is -0.002; when <-3% and Di (n-1) >Di t At that time, K1 n K2 is -0.

001. n It is -0.002; f) The particle size change rate in the first preset condition is set to 1.0%; g) Set the data storage period to 1 month and the particle size sampling test interval to 1 hour; Step C) Add the raw material solution and auxiliary material solution for the synthesis reaction to the synthesis reactor, maintain the synthesis reaction temperature at 60℃, and start the synthesis reaction. After the online particle size analyzer has been running for 2 hours, perform particle size testing. After the first particle size test, the online particle size analyzer transmits the test values ​​to the control system. The control system then determines the particle size based on the measured particle size values ​​D101, D501, and the target particle size value D10. t D50 t Confirm K11 and K21, and then perform the first automatic adjustment of process parameters based on the values ​​of K11 and K21; Step D) The online particle size analyzer performs a second sampling test and transmits the data to the control system. The control system stores the second measured particle size values ​​D102 and D502 and the first measured particle size values ​​D101 and D501, calculates the particle size change rate, and determines the values ​​of K12 and K22 based on the particle size change rate. Then, the process parameters are automatically adjusted for the second time based on the values ​​of K12 and K22. Step E) The online particle size analyzer performs the third and subsequent sampling tests according to the set sampling test interval. The control system stores and analyzes the measured particle size values ​​and records the optimal adjustment values ​​to form an optimal adjustment mode database. In subsequent tests, the control system compared the measured granularity values ​​with data from the optimal adjustment mode database. When de n df n When the second preset condition is met, K1 n K2 n The value is obtained by directly calling the corresponding value in the optimal adjustment method database.

2. A particle size control device, characterized in that, include: An online monitoring system and a control system, wherein the online monitoring system is used to acquire the measured particle size value of the nickel-cobalt-manganese ternary precursor and the detected value of the process parameters, and transmit them to the control system so that the control system executes the adjustment process in the particle size control method as described in claim 1.

3. The particle size control device according to claim 2, characterized in that, The online monitoring system includes an online particle size analyzer, which monitors the measured particle size of the nickel-cobalt-manganese ternary precursor in real time and transmits it to the control system.

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