Method for detecting agglomeration type of slurry
By performing particle size testing and ultrasonic treatment on the negative electrode slurry of lithium-ion batteries, combined with particle size numerical comparison, the problem of the inability to detect slurry agglomeration type in the prior art is solved, and accurate distinction of slurry agglomeration type and guidance on battery production technology are achieved.
Patent Information
- Application Number
- CN202510374338.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-27
- Publication Date
- 2025-07-11
AI Technical Summary
The prior art cannot effectively detect the agglomeration type in the negative electrode slurry of lithium-ion batteries, resulting in the impact of coating quality and production progress.
By performing particle size testing and sonication on the slurry to be tested, combined with comparison of particle size values and difference analysis, the agglomeration type of slurry, including soft agglomeration and hard agglomeration.
能够准确区分浆料中的颗粒团聚类型,指导后续浆料应用和电池生产工艺,提高检测结果的准确性和效率。
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Figure CN120293785A_ABST
Abstract
Description
Technical Field
[0001] This application belongs to the technical field of slurry detection, and specifically provides a method for detecting the agglomeration type of slurry. Background Art
[0002] Lithium-ion batteries have the characteristics of high energy density, long cycle life, no memory effect, etc., and have been widely used in fields such as 3C, power, and energy storage. Currently, the mainstream cathode materials for lithium-ion batteries include lithium iron phosphate, ternary materials, or lithium iron manganese phosphate, etc.; and carbon-based materials represented by artificial graphite are the main materials used for the negative electrode of lithium-ion batteries. Currently, graphite materials occupy 95% of the market share of the negative electrode. In the actual application process, the negative electrode sheet is mainly composed of graphite active material, binder, dispersant, and water, which are mixed and dispersed and then evenly coated on both sides of the copper foil, and then dried and rolled to play the role of deintercalating / inserting lithium ions.
[0003] The negative electrode slurry-making process, as an important link in the manufacturing process of lithium-ion batteries, plays a crucial role in the quality of the negative electrode sheet and the consistency of the battery cells. However, in the actual manufacturing process, problems such as unqualified slurry fineness, blockage of the filter screen filter element, and unstable coating pump pressure often occur, seriously affecting the coating quality and production progress. Conventional analysis methods need to carry out a series of verifications and analyses in combination with people, machines, materials, methods, and the environment, and cannot quickly lock the cause of the problem to meet the requirements of high-efficiency production capacity.
[0004] The prior art usually evaluates the slurry by testing the viscosity, solid content, fineness, and 24-hour slurry stability of the slurry. This method can only detect the dispersion uniformity and sedimentation characteristics of the slurry, but cannot actually detect whether there is an agglomeration phenomenon in the slurry and cannot effectively identify the agglomeration type.
[0005] Correspondingly, the field needs a new technical solution to solve the above technical problems. Summary of the Invention
[0006] This application aims to solve the above technical problems, that is, to solve the problem that the prior art cannot detect the agglomeration type of slurry.
[0007] This application provides a method for detecting the agglomeration type of slurry. The method includes the following steps: S1: Perform a particle size test on the slurry to be tested to obtain the value D0 of the particle size D50 of the slurry to be tested; S2: Perform at least one ultrasonic treatment on the material to be tested. After each ultrasonic treatment, perform a particle size test on the material to be tested to obtain the corresponding values D1, D2....D n , where n is the number of ultrasonic treatments; S3: Determine the agglomeration type of the slurry to be tested according to D0, D1, D2,...., D n , where the material to be tested is the filter residue after filtering the slurry to be tested.
[0008] In a preferred technical solution of the above method for detecting the agglomeration type of the slurry, the number of ultrasonic treatments is 1 time. Step S2 specifically includes: subjecting the material to be tested to ultrasonic treatment, and then performing a particle size test to obtain a value D1 of the particle size D50; Step S3 includes: determining the agglomeration type of the slurry to be tested according to D0 and D1; the agglomeration type includes a soft agglomeration type and a hard agglomeration type. Step S3 specifically includes: S31: judging whether D1 is less than D0; S32: if D1 is less than D0, determining that the agglomeration type of the slurry to be tested is the soft agglomeration type; S33: if D1 is not less than D0, determining that the agglomeration type of the slurry to be tested is the hard agglomeration type; or, the agglomeration type includes a soft agglomeration type and a hard agglomeration type. Step S3 specifically includes: S31: calculating the difference ΔD between D0 and D1, ΔD = D0 - D1; S32: comparing ΔD with a set value; S33: if ΔD is greater than the set value, determining that the agglomeration type of the slurry to be tested is the soft agglomeration type; S34: if ΔD is not greater than the set value, determining that the agglomeration type of the slurry to be tested is the hard agglomeration type.
[0009] In a preferred technical solution of the above method for detecting the agglomeration type of the slurry, the number of ultrasonic treatments is 2 times or more. Step S2 specifically includes: S21: subjecting the material to be tested to the first ultrasonic treatment, and then performing a particle size test to obtain a value D1 of the particle size D50; S22: subjecting the material to be tested after the first ultrasonic treatment to the second ultrasonic treatment, and then performing a particle size test to obtain a value D2 of the particle size D50;...... S2n: subjecting the material to be tested after the (n - 1)th ultrasonic treatment to the nth ultrasonic treatment, and then performing a particle size test to obtain a value D of the particle size D50 n ; Step S3 specifically includes: according to D0 and D n calculating the ratio D nb , to obtain D 1b , D 2b ...... D nb , where D nb = (D0 - D n ) / D0; according to D 1b , D 2b ...... D nb , determining the agglomeration type of the slurry to be tested; or, Step S3 specifically includes: according to D n-1 and D n calculating the difference ΔD m , to obtain ΔD1, ΔD2...... ΔD m , where ΔD m = D n-1 - D n , m = n; according to ΔD1, ΔD2...... ΔD m, determine the agglomeration type of the slurry to be measured.
[0010] In a preferred technical solution of the above method for detecting the agglomeration type of the slurry, the number of ultrasonic treatments is 2 times, and step S3 specifically includes: S31: Calculate the first ratio D according to D0 and D1 1b , D 1b =(D0 - D1) / D0; S32: Calculate the second ratio D according to D0 and D2 2b , D 2b =(D0 - D2) / D0; S33: Determine the agglomeration type of the slurry to be measured according to D 1b and D 2b .
[0011] In a preferred technical solution of the above method for detecting the agglomeration type of the slurry, the agglomeration type includes a hard agglomeration type, a soft agglomeration type, and a combined soft and hard agglomeration type. Step S33 specifically includes: S331: Judge whether D 1b is greater than a first preset value, and judge whether D 2b is greater than a second preset value; S3321: If D 1b is not greater than the first preset value and D 2b is not greater than the second preset value, then determine that the agglomeration type of the slurry to be measured is the hard agglomeration type; S3322: If D 1b is greater than the first preset value and D 2b is greater than the second preset value, then determine that the agglomeration type of the slurry to be measured is the soft agglomeration type; S3323: If D 1b is not greater than the first preset value and D 2b is greater than the second preset value or D 1b is greater than the first preset value and D 2b is not greater than the second preset value, then determine that the agglomeration type of the slurry to be measured is the combined soft and hard agglomeration type; wherein, the second preset value is not less than the first preset value.
[0012] In a preferred technical solution of the above method for detecting the agglomeration type of the slurry, the first preset value is 0% - 5%, preferably the first preset value is 5%; and / or, the second preset value is 5% - 10%, preferably the second preset value is 10%.
[0013] In a preferred technical solution of the above method for detecting the agglomeration type of the slurry, in the case of n≥2, the ultrasonic time T n-1 of the (n - 1)th ultrasonic treatment and the ultrasonic time T n of the nth ultrasonic treatment satisfy the following relationship: T n-1 ≤T n; and / or, in the case of n≥2, the ultrasonic amplitude A of the (n - 1)th ultrasonic treatment n-1 and the ultrasonic amplitude A of the nth ultrasonic treatment n satisfy the following relationship: A n-1 ≤ A n .
[0014] In a preferred technical solution of the above method for detecting the type of slurry agglomeration, the ultrasonic time T1 of the first ultrasonic treatment is not less than 3 min; and / or, the ultrasonic time T of the nth ultrasonic treatment n is not greater than 20 min; and / or, the ultrasonic amplitude A1 of the first ultrasonic treatment is not less than 20 kHz; and / or, the ultrasonic amplitude A of the nth ultrasonic treatment n is not greater than 100 kHz.
[0015] In a preferred technical solution of the above method for detecting the type of slurry agglomeration, T n - T n-1 ≥ 2 min; and / or, A n - A n-1 ≥ 10 kHz.
[0016] In a preferred technical solution of the above method for detecting the type of slurry agglomeration, the material to be tested in step S1 is prepared by the following steps: washing the filter residue after filtering the slurry to be tested with water and then drying it to obtain the material to be tested.
[0017] In a preferred technical solution of the above method for detecting the type of slurry agglomeration, the number of washing times is not less than 2 times, and preferably not less than 5 times.
[0018] In a preferred technical solution of the above method for detecting the type of slurry agglomeration, before performing step S2, the method further includes the following steps: S11: obtaining the preset value D of the slurry particle size D50 x ; S12: judging whether the slurry to be tested has agglomeration according to D0 and D x , and selectively performing step S2 according to the agglomeration situation.
[0019] In a preferred technical solution of the above method for detecting the type of slurry agglomeration, step S12 specifically includes: S121: calculating the actual floating ratio X according to D0 and D x , X = |D0 - D x | / D x ; S122: comparing the actual floating ratio X with the standard floating ratio Y; S123: if X is less than Y, it is judged that the slurry to be tested has not agglomerated, and step S2 is not performed; S124: if X is not less than Y, it is judged that the slurry to be tested has agglomerated, and step S2 is performed.
[0020] In the case of adopting the above technical solution, for the method of detecting the agglomeration type of the slurry in this application, first perform a particle size test on the slurry to be tested to obtain D0, and then perform at least one ultrasonic treatment on the material to be tested (the filter residue after filtering the slurry to be tested), and perform a particle size test on the material to be tested after each ultrasonic treatment to obtain the corresponding numerical values D1, D2....D of the particle size D50 n , and finally determine the agglomeration type of the slurry to be tested according to D0, D1, D2,...., D n . This method can effectively distinguish the types of particle agglomeration in the slurry, and has guiding significance for the subsequent application of the slurry and the battery production process.
[0021] Furthermore, set the number of ultrasonic treatments to 2 or more. By the difference between the numerical values of two adjacent particle sizes D50 or the ratio D n of D0 to D nb to determine the agglomeration type of the slurry to be tested, which can improve the accuracy of the detection result. In addition, it is preferably to set the number of ultrasonic treatments to 2 times, which can not only ensure the relative accuracy of the detection result, but also minimize the number of ultrasonic treatments as much as possible, thereby saving the time required for detection.
[0022] Still further, calculate the first ratio D 1b according to D0 and D1, D 1b =(D0 - D1) / D0, calculate the second ratio D 2b according to D0 and D2, D 2b =(D0 - D2) / D0, compare D 1b with the first preset value, compare D 2b with the second preset value, and determine the agglomeration type of the slurry to be tested according to the two comparison results. Specifically, when D 1b is not greater than the first preset value and D 2b is not greater than the second preset value, determine that the agglomeration type of the slurry to be tested is the hard agglomeration type. When D 1b is greater than the first preset value and D 2b is greater than the second preset value, determine that the agglomeration type of the slurry to be tested is the soft agglomeration type. When D 1b is not greater than the first preset value and D 2b is greater than the second preset value or D 1b is greater than the first preset value and D 2b is not greater than the second preset value, determine that the agglomeration type of the slurry to be tested is the combined type of soft agglomeration and hard agglomeration. The agglomeration type of the slurry to be tested determined by such a determination process is more accurate.
[0023] Furthermore, let the first preset value be 0% - 5% and the second preset value be 5% - 10%. Preferably, the first preset value is 5% and the second preset value is 10%. This can be applied to most slurries, making the test results more in line with the actual situation.
[0024] Furthermore, in the case of n≥2, let the ultrasonic time T of the (n - 1)-th ultrasonic treatment n-1 and the ultrasonic time T of the n-th ultrasonic treatment n satisfy the following relationship: T n-1 ≤T n , so as to extend the ultrasonic time with the increase of the number of ultrasonic treatments, so that there is enough time to break up the agglomerates of the soft agglomeration type, thereby improving the detection accuracy.
[0025] Furthermore, in the case of n≥2, the ultrasonic amplitude A of the (n - 1)-th ultrasonic treatment n-1 and the ultrasonic amplitude A of the n-th ultrasonic treatment n satisfy the following relationship: A n-1 ≤A n , so as to increase the ultrasonic amplitude with the increase of the number of ultrasonic treatments, so as to improve the ultrasonic intensity of the ultrasonic treatment, making it easier to break up the agglomerates of the soft agglomeration type, thereby improving the detection accuracy.
[0026] Furthermore, before performing step S2, it further includes S11: obtaining the preset value D of the slurry fineness D50 x , and judging whether there is agglomeration in the slurry to be tested according to D0 and D x , and selectively performing step S2 according to the agglomeration situation. In this setting method, before actually performing the ultrasonic treatment, it is first judged whether there is agglomeration in the slurry to be tested, and if there is agglomeration in the slurry to be tested, then step S2 is continued to further determine the specific agglomeration type, so as to avoid wasting time by directly performing steps S2 to S3 when there is no agglomeration in the slurry to be tested. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] The preferred embodiments of the present application will be described below with reference to the accompanying drawings, in which:
[0028] Figure 1 is a flowchart of the main steps of the method for detecting the agglomeration type of the slurry in the present application;
[0029] Figure 2 is a flowchart of the first embodiment of the method for detecting the agglomeration type of the slurry in the present application;
[0030] Figure 3 is a flowchart of the second embodiment of the method for detecting the agglomeration type of the slurry in the present application;
[0031] Figure 4It is a flowchart of the third implementation manner of the method for detecting the type of slurry agglomeration in this application. Specific implementation manner
[0032] The preferred implementation manners of this application will be described below with reference to the accompanying drawings. Those skilled in the art should understand that these implementation manners are only used to explain the technical principle of this application and are not intended to limit the protection scope of this application.
[0033] In this application, the term "and / or" describes the association relationship of associated objects and indicates that three relationships can exist. For example, A and / or B can represent: A exists alone, A and B exist simultaneously, and B exists alone. Among them, A and B can be singular or plural. The character " / " generally represents an "or" relationship between the front and rear associated objects.
[0034] In this application, "at least one" means one or more, and "a plurality" means two or more. "At least one of the following items (pieces)" or its similar expressions refer to any combination of these items, including any combination of single items (pieces) or plural items (pieces). For example, "at least one of a, b, or c", or, "at least one of a, b, and c" can both represent: a, b, c, a - b (that is, a and b), a - c, b - c, or a - b - c, where a, b, and c can be single or multiple respectively.
[0035] It should be understood that in various embodiments of this application, the magnitude of the sequence numbers of the above processes does not mean the order of execution. Some or all steps can be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation to the implementation process of the embodiments of this application.
[0036] The terms used in the embodiments of this application are only for the purpose of describing specific embodiments and are not intended to limit this application. The singular forms "a", "the", and "said" used in the embodiments of this application and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise.
[0037] The weight of the relevant components mentioned in the specification of the embodiments of this application can not only refer to the specific content of each component, but also represent the ratio relationship of the weights between the components. Therefore, as long as the content of the relevant components in the specification of the embodiments of this application is enlarged or reduced according to the ratio, it is within the scope disclosed in the specification of the embodiments of this application. Specifically, the mass described in the specification of the embodiments of this application can be mass units well-known in the chemical industry such as μg, mg, g, kg, etc.
[0038] The terms "first" and "second" are for descriptive purposes only, used to distinguish objects such as substances from each other, and should not be construed as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. For example, without departing from the scope of the embodiments of the present application, the first XX may also be referred to as the second XX, and similarly, the second XX may also be referred to as the first XX. Thus, the features defined with "first" and "second" may explicitly or implicitly include one or more of such features.
[0039] The experimental methods in the following embodiments are all conventional methods unless otherwise specified, and the materials, reagents, etc. used in the following embodiments can all be obtained from commercial channels unless otherwise specified.
[0040] Based on the problem pointed out in the background art that the prior art cannot detect the agglomeration type of the slurry.
[0041] The present application provides a method for detecting the agglomeration type of a slurry. First, perform a particle size test on the slurry to be tested to obtain D0, and then perform at least one ultrasonic treatment on the material to be tested (the filter residue after filtering the slurry to be tested), and perform a particle size test on the material to be tested after each ultrasonic treatment to obtain the corresponding particle size D50 values D1, D2....D n According to D0, D1, D2,...., D n Determine the agglomeration type of the slurry to be tested. This method can effectively distinguish the particle agglomeration types in the slurry, and has guiding significance for the subsequent application of the slurry and the battery production process.
[0042] Specifically, please refer to Figure 1 The method for detecting the agglomeration type of the slurry in the present application mainly includes the following steps:
[0043] S1: Perform a particle size test on the slurry to be tested to obtain the value D0 of the particle size D50 of the slurry to be tested.
[0044] S2: Perform at least one ultrasonic treatment on the material to be tested, and perform a particle size test on the material to be tested after each ultrasonic treatment to obtain the corresponding particle size D50 values D1, D2....D n , where n is the number of ultrasonic treatments.
[0045] S3: According to D0, D1, D2,...., D n Determine the agglomeration type of the slurry to be tested.
[0046] Among them, the material to be tested is the filter residue after filtering the slurry to be tested.
[0047] Agglomeration types generally include hard agglomeration and soft agglomeration. Soft agglomeration in the slurry is caused by electrostatic attraction or van der Waals force between particles. Such agglomerates are easily redispersed into individual particles when subjected to external forces. Hard agglomeration, on the other hand, is formed by chemical bonding or sintering necks between particles. Such agglomerates are relatively stable and difficult to disperse by external forces. Ultrasonic treatment can use the cavitation effect and mechanical effect generated by sound waves to break soft agglomerates. Soft agglomerates can be depolymerized as the ultrasonic time prolongs, and the particle size gradually decreases. Hard agglomerates are difficult to be broken by ultrasonic and mechanical effects, and the particle size does not change significantly as the ultrasonic time prolongs. The particle size of the agglomerates can be detected by a laser particle size analyzer. Therefore, the material to be tested can be ultrasonically treated, and then the agglomeration type in the slurry can be determined according to the particle size change after treatment, so as to further optimize the pulping material or process.
[0048] For the method for detecting the agglomeration type of the slurry in this application, first perform a particle size test on the slurry to be tested to obtain D0, and then perform at least one ultrasonic treatment on the material to be tested (the filter residue after filtering the slurry to be tested), and perform a particle size test on the material to be tested after each ultrasonic treatment to obtain the corresponding numerical values D1, D2....D of the particle size D50 n , according to D0, D1, D2,...., D n to determine the agglomeration type of the slurry to be tested. This method can effectively distinguish the particle agglomeration type in the slurry and has guiding significance for the subsequent application of the slurry and the battery production process.
[0049] Specifically, the ultrasonic treatment in this application is specifically to disperse the material to be tested in a solvent (ethanol) for ultrasonic treatment.
[0050] This application uses a Malvern 3000 laser particle size analyzer to test the particle size of the material to be tested or the slurry to be tested. The specific operation is to directly take a certain amount of the slurry to be tested or the dispersion of the material to be tested (that is, the dispersion after ultrasonic treatment of the material to be tested) and drop it into the Malvern 3000 laser particle size analyzer for testing.
[0051] Specifically, the material to be tested in step S2 is prepared through the following steps: wash the filter residue after filtering the slurry to be tested with water and then dry it to obtain the material to be tested.
[0052] Preferably, the number of washing times is not less than 2 times.
[0053] More preferably, the number of washing times is not less than 5 times.
[0054] When preparing the material to be tested, the number of washing times after filtering the filter residue is not less than 2 times, preferably not less than 5 times, which can effectively remove the conductive agent and binder remaining on the surface of the filter residue to improve the accuracy of the detection result.
[0055] It should be noted that this application does not impose any restrictions on the number of ultrasonic treatments. In practical applications, those skilled in the art can set the number of ultrasonic treatments according to actual needs. For example, the number of ultrasonic treatments can be 1 time, or 2 times, or 3 times, and so on. Adjustments and changes to the number of ultrasonic treatments do not deviate from the basic principle of this application and should all be within the protection scope of this application.
[0056] It should be noted that this application does not impose any restrictions on the treatment time and ultrasonic parameters of ultrasonic treatment. In practical applications, those skilled in the art can set the treatment time and specific ultrasonic parameters of each ultrasonic treatment according to actual needs. Adjustments and changes to the ultrasonic time and ultrasonic parameters do not deviate from the basic principle of this application and should all be within the protection scope of this application.
[0057] Preferably, in the case of n≥2, the ultrasonic time T of the (n - 1)-th ultrasonic treatment n-1 and the ultrasonic time T of the n-th ultrasonic treatment n satisfy the following relationship: T n-1 ≤T n .
[0058] In some preferred embodiments, the ultrasonic time T1 of the first ultrasonic treatment is not less than 3 min, and the ultrasonic time T of the n-th ultrasonic treatment n is not greater than 20 min.
[0059] In some preferred embodiments, T n -T n-1 ≥2 min.
[0060] Exemplarily, in a specific embodiment, the number of ultrasonic treatments is 2 times, T1 = 5 min, and T2 = 10 min.
[0061] Exemplarily, in a specific embodiment, the number of ultrasonic treatments is 3 times, T1 = 3 min, T2 = 8 min, and T3 = 12 min.
[0062] In the above setting method, the ultrasonic time is extended as the number of ultrasonic treatments increases, so as to have enough time to break up the soft agglomerated aggregates and improve the detection accuracy. In addition, the ultrasonic time of the first ultrasonic treatment is controlled to be not less than 3 min, so that the ultrasonic treatment can play a role and avoid the ultrasonic treatment time being too short to achieve a good breaking-up effect.
[0063] Preferably, in the case of n≥2, the ultrasonic amplitude A of the (n - 1)-th ultrasonic treatment n-1 and the ultrasonic amplitude A of the n-th ultrasonic treatment n satisfy the following relationship: A n-1 ≤An 。
[0064] In some preferred embodiments, the ultrasonic amplitude A1 of the first ultrasonic treatment is not less than 20 kHz, and the ultrasonic amplitude A of the nth ultrasonic treatment n is not greater than 100 kHz.
[0065] In some preferred embodiments, A n -A n-1 ≥10 kHz.
[0066] Exemplarily, in a specific embodiment, the number of ultrasonic treatments is 2, A1 = 40 kHz, and A2 = 60 kHz.
[0067] Exemplarily, in a specific embodiment, the number of ultrasonic treatments is 3, A1 = 20 kHz, A2 = 50 kHz, and A3 = 80 kHz.
[0068] With the above setting method, the ultrasonic amplitude is further increased as the number of ultrasonic treatments increases, so as to increase the ultrasonic intensity of the ultrasonic treatment, making it easier to break up the agglomerates of soft agglomeration and improve the detection accuracy. In addition, the ultrasonic amplitude of the first ultrasonic treatment is controlled to be not less than 20 kHz, so that the ultrasonic treatment can play a role and avoid the ultrasonic treatment intensity being too low to achieve a good dispersion effect.
[0069] In a feasible embodiment, please refer to Figure 2 , the agglomeration types include soft agglomeration type and hard agglomeration type, and the number of ultrasonic treatments is 1, that is, n = 1. The method for detecting the agglomeration type of the slurry in this embodiment specifically includes the following steps:
[0070] S1: Perform a particle size test on the slurry to be tested to obtain the value D0 of the D50 of the slurry to be tested.
[0071] S2: Perform ultrasonic treatment on the material to be tested, and then perform a particle size test to obtain the value D1 of the D50 of the particle size.
[0072] S3: Determine the agglomeration type of the slurry to be tested according to D0 and D1.
[0073] In a feasible embodiment, please continue to refer to Figure 2 , step S3 "Determine the agglomeration type of the slurry to be tested according to D0 and D1" specifically includes:
[0074] S31: Judge whether D1 is less than D0.
[0075] S32: If D1 is less than D0, then determine that the agglomeration type of the slurry to be tested is the soft agglomeration type.
[0076] S33: If D1 is not less than D0, determine that the agglomeration type of the slurry to be measured is the hard agglomeration type.
[0077] In this embodiment, directly compare the magnitudes of D0 and D1, and determine the agglomeration type of the slurry to be measured according to the comparison result thereof. The judgment process is simple.
[0078] In another feasible embodiment, step S3 "determine the agglomeration type of the slurry to be measured according to D0 and D1" specifically includes:
[0079] S31: Calculate the difference ΔD between D0 and D1, ΔD = D0 - D1;
[0080] S32: Compare ΔD with a set value;
[0081] S33: If ΔD is greater than the set value, determine that the agglomeration type of the slurry to be measured is the soft agglomeration type;
[0082] S34: If ΔD is not greater than the set value, determine that the agglomeration type of the slurry to be measured is the hard agglomeration type.
[0083] It should be noted that when the number of ultrasonic treatments is 1 time, the specific execution steps of the above step S3 "determine the agglomeration type of the slurry to be measured according to D0 and D1" can be set according to actual needs. Those skilled in the art can set it to any one of the above two embodiments, or adopt other judgment steps. Adjustments and changes to the specific execution steps of the above step S3 do not deviate from the basic principle of this application and should all be limited within the protection scope of this application.
[0084] In some other feasible embodiments, the number of ultrasonic treatments is 2 times or more, that is, n≥2. The method for detecting the agglomeration type of the slurry in this embodiment specifically includes the following steps:
[0085] S1: Perform a particle size test on the slurry to be measured to obtain the value D0 of the particle size D50 of the slurry to be measured.
[0086] S21: Perform the first ultrasonic treatment on the material to be measured, and then perform a particle size test to obtain the value D1 of the particle size D50.
[0087] S22: Perform the second ultrasonic treatment on the material to be measured after the first ultrasonic treatment, and then perform a particle size test to obtain the value D2 of the particle size D50. ......
[0089] S2n: Perform the nth ultrasonic treatment on the material to be measured after the (n - 1)th ultrasonic treatment, and then perform a particle size test to obtain the value D of the particle size D50 n 。
[0090] S3: Determine the agglomeration type of the slurry to be measured according to D0, D1, D2,...., D n , and determine the agglomeration type of the slurry to be measured.
[0091] Specifically, in a feasible implementation manner, step S3 "determine the agglomeration type of the slurry to be measured according to D0, D1, D2,...., D n , and determine the agglomeration type of the slurry to be measured" specifically includes: Calculate the ratio D n , and obtain D nb , D 1b , D 2b ......D nb , where D nb = (D0 - D n ) / D0; Determine the agglomeration type of the slurry to be measured according to D 1b , D 2b ......D nb . For example: The agglomeration type of the slurry to be measured can be directly determined according to the numerical values of D 1b , D 2b ......D nb , or the agglomeration type of the slurry to be measured can also be judged according to the magnitude of the difference between adjacent two numerical values of D 1b , D 2b ......D nb . Regarding the specific implementation steps of step S3, those skilled in the art can adjust and change according to actual needs without departing from the basic principle of this application, and all should be limited within the protection scope of this application.
[0092] Specifically, in another feasible implementation manner, step S3 "determine the agglomeration type of the slurry to be measured according to D0, D1, D2,...., D n , and determine the agglomeration type of the slurry to be measured" includes: Calculate the difference ΔD n-1 according to D n and D m , and obtain ΔD1, ΔD2......ΔD m , where ΔD m = D n-1 - D n , m = n; Determine the agglomeration type of the slurry to be measured according to ΔD1, ΔD2......ΔD m . For example: The agglomeration type of the slurry to be measured can be directly determined according to the numerical values of ΔD1, ΔD2......ΔD m , or ΔD1, ΔD2......ΔD mCompare with different preset values respectively to determine the agglomeration type of the slurry to be tested. Regarding the specific implementation steps of step S3, those skilled in the art can adjust and change according to actual needs without departing from the basic principle of the present application, and all should be limited within the protection scope of the present application.
[0093] Certainly, in some preferred embodiments, the number of ultrasonic treatments is 2 times, which can not only ensure relatively accurate detection results, but also minimize the number of ultrasonic treatments as much as possible, thereby saving the time required for detection. The following will be combined with Figure 3 to specifically introduce this preferred embodiment.
[0094] Specifically, please refer to Figure 3 , the agglomeration types include hard agglomeration type, soft agglomeration type, and the combination type of soft agglomeration and hard agglomeration. The number of ultrasonic treatments is 2 times, that is, n = 2. The method for detecting the agglomeration type of the slurry in this embodiment specifically includes the following steps:
[0095] S1: Perform particle size testing on the slurry to be tested to obtain the value D0 of the particle size D50 of the slurry to be tested.
[0096] S21: Perform the first ultrasonic treatment on the material to be tested, and then perform particle size testing to obtain the value D1 of the particle size D50.
[0097] S22: Perform the second ultrasonic treatment on the material to be tested after the first ultrasonic treatment, and then perform particle size testing to obtain the value D2 of the particle size D50.
[0098] S3: Determine the agglomeration type of the slurry to be tested according to D0, D1, and D2.
[0099] Among them, the material to be tested is the filter residue after filtering the slurry to be tested.
[0100] Specifically, please continue to refer to Figure 3 , step S3 specifically includes:
[0101] S31: Calculate the first ratio D 1b , D 1b =(D0 - D1) / D0.
[0102] S32: Calculate the second ratio D 2b , D 2b =(D0 - D2) / D0.
[0103] S33: Determine the agglomeration type of the slurry to be tested according to D 1b and D 2b .
[0104] Specifically, please continue to refer to Figure 3 , step S33 specifically includes:
[0105] S331: Determine whether D 1b is greater than a first preset value, and determine whether D 2b is greater than a second preset value.
[0106] S332: Based on the determination result of D 1b and the first preset value, and the determination result of D 2b and the second preset value, determine the agglomeration type of the slurry to be measured.
[0107] Among them, the second preset value is not less than the first preset value.
[0108] Specifically, please continue to refer to Figure 3 , step S332 specifically includes:
[0109] S3321: If D 1b is not greater than the first preset value and D 2b is not greater than the second preset value, then determine that the agglomeration type of the slurry to be measured is a hard agglomeration type.
[0110] S3322: If D 1b is greater than the first preset value and D 2b is greater than the second preset value, then determine that the agglomeration type of the slurry to be measured is a soft agglomeration type.
[0111] S3323: If D 1b is not greater than the first preset value and D 2b is greater than the second preset value, or D 1b is greater than the first preset value and D 2b is not greater than the second preset value, then determine that the agglomeration type of the slurry to be measured is a combination type of soft agglomeration and hard agglomeration.
[0112] It should be noted that this application does not impose any restrictions on the specific values of the first preset value and the second preset value. In practical applications, those skilled in the art can set the specific values of the first preset value and the second preset value according to actual needs. Adjustments and changes to the specific values of the first preset value and the second preset value do not deviate from the basic principle of this application and should all be limited within the scope protected by this application.
[0113] Preferably, the first preset value is 0% - 5%.
[0114] In some preferred embodiments, the first preset value is 5%.
[0115] Preferably, the second preset value is 5% - 10%.
[0116] In some preferred embodiments, the second preset value is 10%.
[0117] In addition to the single hard agglomeration type and soft agglomeration type, the agglomeration type of the slurry to be measured may also have both hard agglomeration type and soft agglomeration type (i.e., the combined type of soft agglomeration and hard agglomeration). In this preferred embodiment, the number of ultrasonic treatments is set to 2 times, and the first ratio D is calculated according to D0 and D1 1b , D 1b =(D0 - D1) / D0, the second ratio D is calculated according to D0 and D2 2b , D 2b =(D0 - D2) / D0, D 1b is compared with the first preset value, D 2b is compared with the second preset value, and the agglomeration type of the slurry to be measured is determined according to the two comparison results. Specifically, when D 1b is not greater than the first preset value and D 2b is not greater than the second preset value, it is determined that the agglomeration type of the slurry to be measured is the hard agglomeration type. When D 1b is greater than the first preset value and D 2b is greater than the second preset value, it is determined that the agglomeration type of the slurry to be measured is the soft agglomeration type. When D 1b is not greater than the first preset value and D 2b is greater than the second preset value or D 1b is greater than the first preset value and D 2b is not greater than the second preset value, it is determined that the agglomeration type of the slurry to be measured is the combined type of soft agglomeration and hard agglomeration. The agglomeration type of the slurry to be measured determined by such a determination process is more accurate.
[0118] It should be noted that although in this preferred embodiment, step S3 is set to determine the agglomeration type of the slurry to be measured by comparing the first ratio with the first preset value, comparing the second ratio with the second preset value, and according to the two comparison results, in actual applications, those skilled in the art can also set step S3 to other judgment methods. For example, the agglomeration type of the slurry to be measured can be determined by directly comparing the numerical sizes of D0, D1, and D2; or, the difference between D0 and D1 and the difference between D1 and D2 can also be calculated, and the agglomeration type of the slurry to be measured can be determined according to the two differences. These adjustments and changes to the specific implementation steps of step S3 do not deviate from the basic principle of this application and should all be limited within the protection scope of this application.
[0119] Of course, it is still preferred to compare the first ratio with the first preset value and compare the second ratio with the second preset value in the above preferred embodiment, and determine the agglomeration type of the slurry to be measured according to the two comparison results. In this judgment method, both the first ratio and the second ratio are calculated based on D0, that is, the corresponding ratios are calculated by comparing with the initial value D0 after multiple ultrasounds. Compared with other judgment methods (for example: determining the agglomeration type of the slurry to be measured according to the difference or directly according to the numerical sizes of D0, D1, and D2), it can better reflect the changes brought by each ultrasound and can minimize the probability of misjudgment to the greatest extent.
[0120] In addition, preferably, please refer to Figure 4 , before performing step S2 in the method for detecting the agglomeration type of the slurry in this application, the following steps are further included:
[0121] S11: Obtain the preset value D of the slurry particle size D50 x .
[0122] Specifically, the preset value D of the slurry particle size D50 x is specifically the value of D50 corresponding to the slurry with the same raw material ratio under the condition of uniform dispersion, and can be determined through experiments specifically.
[0123] S12: Determine whether the slurry to be measured has agglomeration according to D0 and D x , and selectively execute step S2 according to the agglomeration situation.
[0124] Specifically, please continue to refer to Figure 4 , step S12 specifically includes:
[0125] S121: Calculate the actual floating ratio X according to D0 and D x , X = |D0 - D x | / D x .
[0126] S122: Compare the actual floating ratio X with the standard floating ratio Y.
[0127] S123: If X is less than Y, it is determined that the slurry to be measured has not agglomerated, and step S2 is not executed.
[0128] S124: If X is not less than Y, it is determined that the slurry to be measured has agglomerated, and step S2 is executed.
[0129] It should be noted that this application does not impose any restrictions on the specific value of the standard floating ratio Y. In actual applications, those skilled in the art can set the value of the standard floating ratio Y according to actual needs. Regarding the adjustment and change of the standard floating ratio Y, as long as it does not deviate from the basic principle of this application, it should be limited within the protection scope of this application.
[0130] Preferably, the standard floating ratio Y is 0.02 - 0.05.
[0131] Before performing step S2 in this embodiment, it is first determined whether the slurry to be measured has agglomeration. In the case where the slurry to be measured agglomerates, step S2 is performed to further determine the specific agglomeration type, so as to avoid wasting time by performing steps S2 to S3 when the slurry to be measured does not have agglomeration.
[0132] The following describes in detail the method for detecting the agglomeration type of the slurry of the present application through several specific embodiments.
[0133] In the following examples and comparative examples, the slurries A, B, C, and D are the anode slurries of different batches of lithium batteries prepared from the same raw materials according to the same formula and method. Among them, the preset value D of the particle size D50 of the anode slurry x = 7.4 μm.
[0134] Example 1
[0135] This embodiment detects the agglomeration type of slurry A according to the following steps, and its specific steps include:
[0136] S1: Perform a particle size test on slurry A to obtain the value D0 of the particle size D50 of slurry A, where D0 = 10.8 μm.
[0137] S11: Obtain the preset value D of the slurry particle size D50 x , D x = 7.4 μm.
[0138] S121: Calculate the actual floating ratio X according to D0 and D x X = |D0 - D x | / D x = (10.8 - 7.4) ÷ 7.4 = 0.46.
[0139] S122: Determine whether the actual floating ratio X is less than the standard floating ratio Y, where the standard floating ratio Y = 0.02.
[0140] S123: 0.46 is greater than 0.02, that is, X is not less than Y, then it is determined that slurry A has agglomerated, and step S2 is performed, where step S2 includes S20, S21, and S22.
[0141] S20: Prepare the slurry A into the material to be measured A: Wash the filter residue after filtering slurry A with deionized water 6 times and dry it to obtain the material to be measured A.
[0142] S21: Perform the first ultrasonic treatment on the material A to be measured, and then conduct a particle size test to obtain the value D1 of the particle size D50, where D1 = 10.5 μm. Among them, the time T1 of the first ultrasonic treatment is 5 min, and the amplitude A1 is 40 kHz.
[0143] S22: Perform the second ultrasonic treatment on the material A to be measured after the first ultrasonic treatment, and then conduct a particle size test to obtain the value D2 of the particle size D50, where D2 = 10.1 μm. Among them, the time T2 of the second ultrasonic treatment is 10 min, and the amplitude A2 is 60 kHz.
[0144] S31: Calculate the first ratio D 1b ,D 1b =(D0 - D1) / D0 = (10.8 - 10.5)÷10.8 = 0.028 = 2.8%.
[0145] S32: Calculate the second ratio D 2b ,D 2b =(D0 - D2) / D0 = (10.8 - 10.1)÷10.8 = 0.067 = 6.7%.
[0146] S331: Judge whether D 1b is greater than the first preset value, and judge whether D 2b is greater than the second preset value, where the first preset value is 5% and the second preset value is 10%.
[0147] S332: 2.8% is less than 5%, and 9.3% is less than 10%, that is, D 1b is not greater than the first preset value and D 2b is not greater than the second preset value, then determine that the agglomeration type of the slurry A is the hard agglomeration type.
[0148] Example 2
[0149] This embodiment detects the agglomeration type of the slurry B according to the following steps, and the specific steps include:
[0150] S1: Conduct a particle size test on the slurry B to obtain the value D0 of the particle size D50 of the slurry B, where D0 = 11.5 μm.
[0151] S11: Obtain the preset value D x of the slurry particle size D50, D x = 7.4 μm.
[0152] S121: Calculate the actual floating ratio X according to D0 and D x , X = |D0 - D x | / D x=(11.5 - 7.4)÷7.4 = 0.55.
[0153] S122: Determine whether the actual floating ratio X is less than the standard floating ratio Y, where the standard floating ratio Y = 0.02.
[0154] S123: Since 0.55 is greater than 0.02, that is, X is not less than Y, it is determined that the slurry B has agglomerated, and step S2 is executed, where step S2 includes S20, S21, and S22.
[0155] S20: Prepare the slurry B into the material B to be tested: Wash the filter residue after filtering the slurry B with deionized water 6 times and dry it to obtain the material B to be tested.
[0156] S21: Perform the first ultrasonic treatment on the material B to be tested, and then conduct a particle size test to obtain the value D1 of the particle size D50, D1 = 9.6μm. Among them, the time T1 of the first ultrasonic treatment = 5min, and the amplitude A1 = 40kHz.
[0157] S22: Perform the second ultrasonic treatment on the material B to be tested after the first ultrasonic treatment, and then conduct a particle size test to obtain the value D2 of the particle size D50, D2 = 7.5μm. Among them, the time T2 of the second ultrasonic treatment = 10min, and the amplitude A2 = 60kHz.
[0158] S31: Calculate the first ratio D according to D0 and D1 1b , D 1b =(D0 - D1) / D0 = (11.5 - 9.6)÷11.5 = 0.165 = 16.5%.
[0159] S32: Calculate the second ratio D according to D0 and D2 2b , D 2b =(D0 - D2) / D0 = (11.5 - 7.5)÷11.5 = 0.348 = 34.8%.
[0160] S331: Determine whether D 1b is greater than the first preset value, and determine whether D 2b is greater than the second preset value, where the first preset value is 5%, and the second preset value is 10%.
[0161] S332: Since 16.5% is greater than 5% and 34.8% is greater than 10%, that is, D 1b is greater than the first preset value and D 2b is greater than the second preset value, it is determined that the agglomeration type of the slurry B is the soft agglomeration type.
[0162] Example 3
[0163] This embodiment detects the agglomeration type of slurry C according to the following steps, and the specific steps include:
[0164] S1: Perform a particle size test on slurry C to obtain the value D0 of the D50 of slurry C, where D0 = 12.3 μm.
[0165] S11: Obtain the preset value D of the slurry particle size D50 x , D x = 7.4 μm.
[0166] S121: Calculate the actual floating ratio X according to D0 and D x X = |D0 - D x | / D x = (12.3 - 7.4) ÷ 7.4 = 0.66.
[0167] S122: Determine whether the actual floating ratio X is less than the standard floating ratio Y, where the standard floating ratio Y = 0.02.
[0168] S123: Since 0.66 is greater than 0.02, that is, X is not less than Y, it is determined that slurry C has agglomerated, and step S2 is executed, where step S2 includes S20, S21, and S22.
[0169] S20: Prepare the slurry C into the test material C: Wash the filter residue after filtering slurry C with deionized water 6 times and dry it to obtain the test material C.
[0170] S21: Perform the first ultrasonic treatment on the test material C, and then perform a particle size test to obtain the value D1 of the D50 of the particle size, D1 = 11.5 μm. Among them, the time T1 of the first ultrasonic treatment = 5 min, and the amplitude A1 = 40 kHz.
[0171] S22: Perform the second ultrasonic treatment on the test material C after the first ultrasonic treatment, and then perform a particle size test to obtain the value D2 of the D50 of the particle size, D2 = 11.4 μm. Among them, the time T2 of the second ultrasonic treatment = 10 min, and the amplitude A2 = 60 kHz.
[0172] S31: Calculate the first ratio D according to D0 and D1 1b , D 1b = (D0 - D1) / D0 = (12.3 - 11.5) ÷ 12.3 = 0.065 = 6.5%.
[0173] S32: Calculate the second ratio D according to D0 and D2 2b , D 2b = (D0 - D2) / D0 = (12.3 - 11.4) ÷ 12.3 = 0.073 = 7.3%.
[0174] S331: Determine D 1b whether it is greater than the first preset value, and determine whether D 2b is greater than the second preset value, where the first preset value is 5% and the second preset value is 10%.
[0175] S332: 6.5% is greater than 5%, 7.3% is less than 10%, that is, D 1b is not greater than the first preset value and D 2b is greater than the second preset value, then determine that the agglomeration type of slurry C is a combination of soft agglomeration and hard agglomeration.
[0176] Example 4
[0177] This embodiment detects the agglomeration type of slurry D according to the following steps, and the specific steps include:
[0178] S1: Perform a particle size test on slurry D to obtain the value D0 of the particle size D50 of slurry D, where D0 = 7.5 μm.
[0179] S11: Obtain the preset value D of the slurry particle size D50 x , D x = 7.4 μm.
[0180] S121: Calculate the actual floating ratio X according to D0 and D x X = |D0 - D x | / D x = (7.5 - 7.4) ÷ 7.4 = 0.013.
[0181] S122: Determine whether the actual floating ratio X is less than the standard floating ratio Y, where the standard floating ratio Y = 0.02.
[0182] S123: 0.013 is less than 0.02, that is, X is less than Y, then it is determined that slurry D does not agglomerate and step S2 is not executed.
[0183] Experimental verification
[0184] Verification Example 1
[0185] In this verification example, after step S22 of slurry A in Embodiment 1 is completed, step S23 and step S24 are executed again.
[0186] S23: Perform a third ultrasonic treatment on the material to be tested after the second ultrasonic treatment, and then perform a particle size test to obtain the value D3 of the particle size D50, D3 = 10.1 μm. Among them, the time T3 of the third ultrasonic treatment is 12 min and the amplitude A3 is 70 kHz.
[0187] S24: Subject the material to be tested after the third ultrasonic treatment to a fourth ultrasonic treatment, and then conduct a particle size test to obtain the value D4 of the particle size D50, where D4 = 10.1 μm. Among them, the time T4 of the fourth ultrasonic treatment is 14 min, and the amplitude A4 is 80 kHz.
[0188] Among them, from D2, D3, and D4, it can be seen that after the third ultrasonic treatment and the fourth ultrasonic treatment, the particle size of the material to be tested has not changed. In addition, D2, D3, and D4 are much larger than D x , and there is still agglomeration in slurry A, and the agglomerates cannot be broken up even through multiple ultrasonic treatments. From this, it can be seen that there is still a hard agglomeration type in slurry A.
[0189] It can be seen from this verification example that the results measured by the method of Example 1 are accurate.
[0190] Verification Example 2
[0191] In this verification example, after slurry B in Example 2 finishes step S22, steps S23 and S24 are executed again.
[0192] S23: Subject the material to be tested after the second ultrasonic treatment to a third ultrasonic treatment, and then conduct a particle size test to obtain the value D3 of the particle size D50, where D3 = 7.5 μm. Among them, the time T3 of the third ultrasonic treatment is 12 min, and the amplitude A3 is 70 kHz.
[0193] S24: Subject the material to be tested after the third ultrasonic treatment to a fourth ultrasonic treatment, and then conduct a particle size test to obtain the value D4 of the particle size D50, where D4 = 7.4 μm. Among them, the time T4 of the fourth ultrasonic treatment is 14 min, and the amplitude A4 is 80 kHz.
[0194] Among them, from D2, D3, and D4, it can be seen that after the third ultrasonic treatment and the fourth ultrasonic treatment, the particle size of the material to be tested has not changed. In addition, D2 and D3 are close to D x , and D4 is equal to D x , and there is no agglomeration in slurry B at this time, and the agglomerates can be broken up through the first ultrasonic treatment and the second ultrasonic treatment. From this, it can be seen that the agglomeration type of slurry B is a soft agglomeration type.
[0195] It can be seen from this verification example that the results measured by the method of Example 2 are accurate.
[0196] Verification Example 3
[0197] In this verification example, after slurry C in Example 3 finishes step S22, steps S23 and S24 are executed again.
[0198] S23: The material to be tested after the second ultrasonic treatment is subjected to a third ultrasonic treatment, and then particle size testing is carried out to obtain the value D3 of the particle size D50, D3 = 11.4 μm. Among them, the time T3 of the third ultrasonic treatment is 12 min, and the amplitude A3 is 70 kHz.
[0199] S24: The material to be tested after the third ultrasonic treatment is subjected to a fourth ultrasonic treatment, and then particle size testing is carried out to obtain the value D4 of the particle size D50, D4 = 11.4 μm. Among them, the time T4 of the fourth ultrasonic treatment is 14 min, and the amplitude A4 is 80 kHz.
[0200] Among them, from D2, D3 and D4, it can be seen that after the third ultrasonic treatment and the fourth ultrasonic treatment, the particle size of the material to be tested has not changed. In addition, D2, D3 and D4 are much larger than D x , there is still agglomeration in slurry C, and all the agglomerates cannot be broken up by multiple ultrasonic treatments. From this, it can be seen that there is still a hard agglomeration type in slurry C at this time. In addition, some agglomerates can be broken up after the first ultrasonic treatment, so there is also a soft agglomeration type in slurry C. From this, it can be seen that the agglomeration type of slurry C is a combination of soft agglomeration and hard agglomeration.
[0201] It can be seen from this verification example that the results measured by the method of Example 3 are accurate.
[0202] From the above examples and verification examples, it can be seen that the method for detecting the agglomeration type of the slurry in the present application can effectively detect the agglomeration type of the slurry, which has guiding significance for the subsequent application of the slurry and the battery production process. For example, if there is a soft agglomeration type in the slurry, the slurry is further stirred and dispersed to break up the agglomerates therein; if there is a hard agglomeration type in the slurry, it is necessary to subsequently confirm whether key indicators such as oversize and particle size distribution are abnormal, and at the same time feedback to the supplier to check the raw material manufacturing process.
[0203] So far, the technical solution of the present application has been described in combination with the preferred embodiments shown in the drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present application is obviously not limited to these specific embodiments. Without departing from the principle of the present application, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present application.
Claims
1. A method for detecting the type of slurry agglomeration, characterized in that, It includes the following steps: S1: Conduct a particle size test on the slurry to be tested, and obtain the value D0 of the particle size D50 of the slurry to be tested; S2: Perform ultrasonic treatment on the material to be tested at least once. After each ultrasonic treatment, perform particle size testing on the material to be tested to obtain corresponding values D1, D2....D of the particle size D50 n , where n is the number of times of the ultrasonic treatment; S3: Determine the agglomeration type of the slurry to be measured according to D0, D1, D2,...., D n , and determine the agglomeration type of the slurry to be measured; Wherein, the material to be tested is the filter residue after filtering the slurry to be tested.
2. The method for detecting the type of slurry agglomeration according to claim 1, characterized in that, The number of ultrasonic treatments is 1 time. Step S2 specifically includes: subjecting the material to be tested to ultrasonic treatment, and then conducting a particle size test to obtain the value D1 of the particle size D50; Step S3 includes: determining the agglomeration type of the slurry to be tested according to D0 and D1; The agglomeration types include soft agglomeration type and hard agglomeration type. Step S3 specifically includes: S31: Judge whether D1 is less than D0; S32: If D1 is less than D0, determine that the agglomeration type of the slurry to be tested is the soft agglomeration type; S33: If D1 is not less than D0, determine that the agglomeration type of the slurry to be tested is the hard agglomeration type; Or, The agglomeration types include soft agglomeration type and hard agglomeration type. Step S3 specifically includes: S31: Calculate the difference ΔD between D0 and D1, ΔD = D0 - D1; S32: Compare ΔD with the set value; S33: If ΔD is greater than the set value, determine that the agglomeration type of the slurry to be tested is the soft agglomeration type; S34: If ΔD is not greater than the set value, determine that the agglomeration type of the slurry to be tested is the hard agglomeration type.
3. The method for detecting the type of slurry agglomeration according to claim 1, wherein The number of ultrasonic treatments is 2 times or more than 2 times. Step S2 specifically includes: S21: Subject the material to be tested to the first ultrasonic treatment, and then conduct a particle size test to obtain the value D1 of the particle size D50; S22: Subject the material to be tested after the first ultrasonic treatment to the second ultrasonic treatment, and then conduct a particle size test to obtain the value D2 of the particle size D50; ...... S2n: Subject the material to be measured after the (n - 1)-th ultrasonic treatment to the n-th ultrasonic treatment, and then conduct a particle size test to obtain the value D of the particle size D50 n ; Step S3 specifically includes: According to D0 and D n calculate the ratio D nb , to obtain D 1b , D 2b ...... D nb , where D nb = (D0 - D n ) / D0; According to D 1b , D 2b ...... D nb , determine the agglomeration type of the slurry to be measured; Or, Step S3 specifically includes: According to D n-1 and D n calculate the difference ΔD m , to obtain ΔD1, ΔD2......ΔD m , where, ΔD m = D n-1 - D n , m = n; According to ΔD1, ΔD2......ΔD m , determine the agglomeration type of the slurry to be measured.
4. The method for detecting the type of slurry agglomeration according to claim 3, characterized in that, The number of ultrasonic treatments is 2 times. Step S3 specifically includes: S31: Calculate the first ratio D based on D0 and D1 1b , D 1b = (D0 - D1) / D0; S32: Calculate the second ratio D according to D0 and D2 2b , D 2b = (D0 - D2) / D0; S33: Determine the agglomeration type of the slurry to be measured according to D 1b and D 2b to determine the agglomeration type of the slurry to be measured.
5. The method for detecting the type of slurry agglomeration according to claim 4, wherein The agglomeration types include hard agglomeration type, soft agglomeration type, and the combination type of soft agglomeration and hard agglomeration. Step S33 specifically includes: S331: Determine D 1b whether it is greater than the first preset value, and determine D 2b whether it is greater than the second preset value; S3321: If D 1b is not greater than the first preset value and D 2b is not greater than the second preset value, then determine that the agglomeration type of the slurry to be measured is the hard agglomeration type; S3322: If D 1b is greater than the first preset value and D 2b is greater than the second preset value, then determine that the agglomeration type of the slurry to be measured is the soft agglomeration type; S3323: If D 1b is not greater than the first preset value and D 2b is greater than the second preset value, or D 1b is greater than the first preset value and D 2b is not greater than the second preset value, then determine that the agglomeration type of the slurry to be measured is the combined type of soft agglomeration and hard agglomeration; Wherein, the second preset value is not less than the first preset value.
6. The method for detecting the type of slurry agglomeration according to claim 5, wherein, The first preset value is 0% - 5%, and preferably the first preset value is 5%; And / or, the second preset value is 5% - 10%, and preferably the second preset value is 10%.
7. The method for detecting the type of slurry agglomeration according to claim 3, wherein, In the case of n≥2, the ultrasonic time T of the (n - 1)-th ultrasonic treatment n-1 and the ultrasonic time T of the n-th ultrasonic treatment n satisfy the following relationship: T n-1 ≤T n ; And / or, in the case of n≥2, the ultrasonic amplitude A of the (n - 1)-th ultrasonic treatment n-1 and the ultrasonic amplitude A of the n-th ultrasonic treatment n satisfy the following relationship: A n-1 ≤A n .
8. The method for detecting the type of slurry agglomeration according to claim 7, characterized in that, The ultrasonic time T1 of the first ultrasonic treatment is not less than 3 min; and / or, the ultrasonic time T of the nth ultrasonic treatment n not greater than 20 min; And / or, the ultrasonic amplitude A1 of the first ultrasonic treatment is not less than 20 kHz; and / or, the ultrasonic amplitude A of the nth ultrasonic treatment n not greater than 100 kHz.
9. The method for detecting the type of slurry agglomeration according to claim 8, wherein T n -T n-1 ≥ 2 min; and / or, A n -A n-1 ≥10 kHz.
10. The method for detecting the type of slurry agglomeration according to any one of claims 1 to 9, characterized in that, Before performing step S2, the method further includes the following steps: S11: Obtain the preset value D of the slurry particle size D50 x ; S121: Calculate the actual floating ratio X based on D0 and D x where X = |D0 - D x | / D x ; S122: Compare the actual floating ratio X with the standard floating ratio Y; S123: If X is less than Y, determine that the slurry to be tested has not agglomerated, and do not perform step S2; S124: If X is not less than Y, determine that the slurry to be tested has agglomerated, and perform step S2.