Search

KR-20260064493-A - METHOD FOR ACQUIRING REPRESENTATIVE PARTICLE SIZE USING TURBIDITY METER IN CRYSTALLIZATION APPARATUS AND SYSTEM FOR ACQUIRING REPRESENTATIVE PARTICLE SIZE

KR20260064493AKR 20260064493 AKR20260064493 AKR 20260064493AKR-20260064493-A

Abstract

(Problem) The present invention aims to obtain a method for obtaining the particle size of a generated particle in a crystallization device in a crystallization process using a single correlation equation from turbidity, the concentration of the generated particle, and the amount of raw material supplied. (Means of solution) A correlation equation for these variables is prepared in advance from basic data including the representative particle size of the generated particles obtained by a particle size distribution measuring device, the turbidity of the dispersion of the generated particles, the concentration of the generated particles in the dispersion of the generated particles, and the supply amount of metal derived from the metal salt. In the crystallization process, the representative particle size of the generated particles is obtained using the correlation equation from the turbidity, the concentration of the generated particles, and the supply amount of metal derived from the metal salt obtained by measuring the dispersion of the generated particles.

Inventors

  • 야이로 마코토

Assignees

  • 츠키시마 기카이 가부시키가이샤

Dates

Publication Date
20260507
Application Date
20250818
Priority Date
20241031

Claims (10)

  1. A method for obtaining a representative particle size of a generated particle in a crystallization process in which an aqueous solution containing each of a plurality of metal salts is supplied to a crystallization device and particles are generated by contacting them, A step of acquiring basic data including the representative particle size of the generated particles obtained by a particle size distribution measuring device, the turbidity of the dispersion of the generated particles, the concentration of the generated particles in the dispersion of the generated particles, and the supply amount of metal derived from the metal salt; A step of creating a correlation equation representing the relationship between the representative particle size of the generated particles, the turbidity of the dispersion of the generated particles, the concentration of the generated particles in the dispersion of the generated particles, and the supply amount of one or more types of the metal selected from the metal, obtained in the step of acquiring the basic data above; and In the crystallization process, a step of obtaining the turbidity of the dispersion of the generated particles, the concentration of the generated particles, and the supply amount of metal derived from multiple types of metal salts, and A step of obtaining a representative particle size of the generated particles by the correlation equation based on the respective numerical values of the turbidity of the dispersion of the generated particles obtained in the above standard process, the concentration of the generated particles, and the supply amount of one or more types of metals selected from the metals derived from the metal salt. A method for obtaining a representative particle size of a generated particle in a crystallization apparatus equipped with
  2. In Article 1, In the step of creating the above correlation equation, There are three types of the aforementioned metal salts of multiple species, and When the turbidity of the dispersion of the generated particles is X 1 NTU, the concentration of the generated particles is X 2 mass%, the supply amount of the metal is X 3 moles, X 4 moles, X 5 moles, and the representative particle size of the generated particles is Y μm, In the following equation representing the relationship between Y and X1 , X2 , X3 , X4 , and X5 , the correlation equation is determined by obtaining each coefficient a, b, c, d, and e by the least squares method. A method for obtaining the representative particle size of a generated particle in a crystal apparatus. [Mathematical Formula 1]
  3. In Article 2, In the step of creating the above correlation equation, There are three types of the aforementioned metal salts of multiple species, and A method for obtaining a representative particle size of the generated particles in a crystallization apparatus, wherein the turbidity of the dispersion of the generated particles is X 1 NTU, the concentration of the generated particles is X 2 mass%, X 3 is the number of moles of cobalt ions, X 4 is the number of moles of manganese ions, and X 5 is the number of moles of nickel ions.
  4. In any one of paragraphs 1 to 3, A method for obtaining a representative particle size of the generated particles in a crystallization apparatus, wherein the concentration of the generated particles is 1 to 40 mass%.
  5. In any one of paragraphs 1 to 3, A method for obtaining the representative particle size of the generated particles in the crystallization apparatus, wherein the turbidity is obtained by measurement by a turbidity meter installed in-line in the crystallization apparatus.
  6. In any one of paragraphs 1 to 3, In constructing the above correlation equation, regarding d10, d50, and d90 based on the volume of the generated particles obtained by the particle size distribution measuring device, The value of (d90 - d10)/d50 is 1.5 or less, A method for obtaining the representative particle size of the generated particles in a standard apparatus.
  7. In any one of paragraphs 1 to 3, A method for obtaining a representative particle size of the generated particles in a crystallization apparatus, wherein the crystallization process for obtaining the generated particles is a batch type or a continuous type.
  8. A crystallization apparatus that supplies aqueous solutions each containing multiple types of metal salts to a crystallization apparatus and generates particles by contacting them, wherein a system for obtaining a representative particle size of the generated particles, In the above-mentioned crystallization device, a turbidity acquiring unit for acquiring the turbidity of a dispersion of generated particles, and A particle concentration acquisition unit for acquiring the concentration of the generated particles in a dispersion of the generated particles, and A metal supply amount acquiring unit that acquires a supply amount of metal derived from the above metal salt, and A correlation formula generating unit that stores a correlation formula representing the relationship between the representative particle size of the generated particles acquired by a particle size distribution measuring device, the turbidity of the dispersion of the generated particles, the concentration of the generated particles in the dispersion of the generated particles, and the supply amount of one or more types of metals selected from the metals derived from the metal salt, and A representative particle size calculation unit that obtains the representative particle size of the generated particles by the correlation equation, based on the respective numerical values of the turbidity of the dispersion of the generated particles obtained from the turbidity acquisition unit, the concentration of the generated particles obtained from the generated particle concentration acquisition unit, and the supply amount of one or more types of metals selected from the metal salts derived from the metal supply amount obtained from the metal supply amount acquisition unit. A system for acquiring the representative particle size of generated particles in a crystallization device having
  9. In Article 8, The above correlation formula generation unit is, There are three types of the aforementioned metal salts of multiple species, and When the turbidity of the dispersion of the generated particles is X 1 NTU, the concentration of the generated particles is X 2 mass%, the supply amount of the metal is X 3 moles, X 4 moles, X 5 moles, and the representative particle size of the generated particles is Y μm, In the following equation representing the relationship between Y and X₁ , X₂ , X₃ , X₄ , and X₅ , constructing and remembering the correlation equation by finding the respective coefficients a, b, c, d, and e using the least squares method, System for acquiring the representative particle size of generated particles in a standard device. [Mathematical Formula 1]
  10. In Article 9, A system for obtaining the representative particle size of a generated particle in a crystallization apparatus, wherein X3 is the number of moles of cobalt ions, X4 is the number of moles of manganese ions, and X5 is the number of moles of nickel ions.

Description

Method for Acquiring Representative Particle Size Using Turbidimeter in Crystallization Apparatus and System for Acquiring Representative Particle Size The present invention relates to a method for obtaining the representative particle size of a crystal material generated during crystallization and a system for measuring the representative particle size. Crystallization is an operation that precipitates crystals from a liquid phase or the like. Crystallization occurs by creating a supersaturated state, and a supersaturated state can be obtained by cooling, evaporation, reaction, or pressurization. For example, when a supersaturated state is created by a reaction and product particles are formed, it is called reaction crystallization. In conventional crystallization operations, it is necessary to produce crystals with a specified representative particle size and particle size distribution. Crystallization is used in the manufacture of lithium-ion battery positive electrode precursors, various inorganic materials, and cosmetic materials; for these applications, the representative particle size and particle size distribution are important physical properties for the materials obtained through crystallization to exhibit performance. Therefore, obtaining information regarding the particle size of the generated particles is crucial for ensuring performance. Methods for measuring the particle size of micron and sub-micron order particles include dynamic light scattering, laser diffraction/scattering, centrifugal sedimentation, and image analysis; however, all of these methods require expensive measuring instruments or require time for measurement. Meanwhile, a method for enabling efficient particle size measurement at low cost has been proposed (Patent Document 1). The disclosed method comprises the steps of: mixing a predetermined amount of suspended material having a known average particle size with water according to the average particle size to prepare a suspension according to the average particle size; measuring the turbidity of the suspension according to the average particle size according to the average particle size and determining the correspondence between the average particle size and the turbidity; measuring the turbidity of a target suspension containing the suspended material to be measured, and comparing the measured turbidity with the correspondence, thereby determining the average particle size of the suspended material contained in the target suspension. Specifically, a graph of turbidity and particle size is created for each amount (concentration) of suspended matter, and the turbidity of the target suspension is compared to the turbidity-average particle size relationship graph. In this case, a graph is created for each concentration of suspended matter, and the concentration of the target suspension needs to be matched to the concentration of suspended matter in the graph created above. In addition, Patent Document 1 discloses creating graphs for kaolin (white), slate (gray), and basic volcanic rocks (brown) according to color and concentration, and determining the average particle size of a suspension containing a target suspension having a hue among white, gray, and brown by comparing the turbidity of the target suspension with the graph of the corresponding color among the turbidity-average particle size relationship graphs. In this case as well, it is necessary to match the concentration of the target suspension to the concentration of the suspension in the graph created above. In addition, it is necessary to select a turbidity-average particle size relationship graph according to the color of the suspension. Figure 1 is a schematic diagram of the entire crystal apparatus. Figure 2 is a schematic diagram of a reactor. Figure 3 is a flowchart showing the acquisition of representative particle diameters. Figure 4 is the system configuration. Figure 5 is a graph showing the calculated and measured values of representative particle sizes according to the method of the example. Figure 6 is a graph showing the calculated and measured values of representative particle sizes by the method of the comparative example. Next, an embodiment for carrying out the present invention will be described. A method for obtaining the particle size of a generated particle will be described, along with an example of an apparatus. (Standard device) A typical example of a crystallization apparatus related to the present invention is a reaction crystallization apparatus for obtaining metal particle generation particles. One specific example is intended for producing generation particles using transition metals such as Ni, Co, and Mn. However, since the method for carrying out reaction crystallization is widely and generally applicable, it may be used for metals other than the above transition metals or other materials. FIG. 1 shows an example of a standard apparatus related to the present invention, and FIG. 2 show