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Method for determining multi-component resultant in multivariant anode material precursor based on EDTA back titration-automatic titration method

A positive electrode material and automatic titration technology, which is applied in the direction of chemical analysis by titration, analysis by making materials undergo chemical reactions, and material analysis by observing the impact on chemical indicators, etc., which can solve the difficulties in judging the end point and inaccurate determination. Accurate, time-consuming and labor-intensive problems, to achieve the effect of improving the level of automatic detection and reliability, high precision and accuracy, and good repeatability

Active Publication Date: 2016-12-21
GEM WUXI ENERGY MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following defects: (1) under the same test conditions, EDTA has different complexation stability constants with different metal elements, which may cause inaccurate measurement due to incomplete complexation during direct titration; (2) the end point Difficult to judge, large measurement error; (3) low titration accuracy, large human error; (4) manual titration, time-consuming and laborious, not suitable for multi-batch sample testing in large-scale industrial production

Method used

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  • Method for determining multi-component resultant in multivariant anode material precursor based on EDTA back titration-automatic titration method
  • Method for determining multi-component resultant in multivariant anode material precursor based on EDTA back titration-automatic titration method
  • Method for determining multi-component resultant in multivariant anode material precursor based on EDTA back titration-automatic titration method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] (1) Sample dissolution: Accurately weigh ~1.0000g (1.0001g) nickel-cobalt-manganese ternary material precursor type 111 sample (abbreviated as 1# sample), add 15mL 1+1 hydrochloric acid, heat and decompose on the electric furnace, and wait for the test After the material is completely dissolved, cool down, transfer to a 250mL volumetric flask and dilute to the mark with ultrapure water to obtain the sample solution.

[0059] (2) Excess EDTA complexed ternary compound amount: accurately pipette 25mL of the above sample solution into a plastic cup for an automatic titration device, add 2mL of 5% ascorbic acid solution, 30mL of 0.05M EDTA-2Na solution, 1mL of 1+1 hydrochloric acid, 20-30mL boric acid-sodium borate buffer solution, adjust the pH to 9.0, record the volume of EDTA-2Na as V 1 .

[0060] (3) Back titration: Use ultrapure water to adjust the volume of the sample solution in step (2) to 160mL so that it is completely submerged in the effective part of the sensin...

Embodiment 2

[0066] (1) Sample dissolution: Accurately weigh ~1.0000g (1.0001g) nickel-cobalt-manganese ternary material precursor type 523 sample (referred to as 2# sample), add 15mL 1+1 hydrochloric acid, put it on the electric furnace and heat it to decompose, and wait for the test After the material is completely dissolved, cool down, transfer to a 250mL volumetric flask and dilute to the mark with ultrapure water to obtain the sample solution.

[0067] (2) Excess EDTA complexed ternary compound amount: accurately pipette 25mL of the above sample solution into a plastic cup for an automatic titration device, add 2mL of 5% ascorbic acid solution, 30mL of 0.05M EDTA-2Na solution, 1mL of 1+1 hydrochloric acid, 20-30mL boric acid-sodium borate buffer solution, adjust the pH to 9.0, record the volume of EDTA-2Na as V1.

[0068] (3) Back titration: Use ultrapure water to adjust the volume of the sample solution in step (2) to 160mL so that it is completely submerged in the effective part of ...

Embodiment 3

[0074] (1) Sample dissolution: Accurately weigh ~1.0000g (1.0001g) nickel-cobalt-manganese ternary material precursor type 622 sample (abbreviated as 3# sample), add 15mL 1+1 hydrochloric acid, heat and decompose on the electric furnace, and wait for the test After the material is completely dissolved, cool down, transfer to a 250mL volumetric flask and dilute to the mark with ultrapure water to obtain the sample solution.

[0075] (2) Excess EDTA complexed ternary compound amount: accurately pipette 25mL of the above sample solution into a plastic cup for an automatic titration device, add 2mL of 5% ascorbic acid solution, 30mL of 0.05M EDTA-2Na solution, 1mL of 1+1 hydrochloric acid, 20-30mL boric acid-sodium borate buffer solution, adjust the pH to 9.0, record the volume of EDTA-2Na as V1.

[0076] (3) Back titration: Use ultrapure water to adjust the volume of the sample solution in step (2) to 160mL so that it is completely submerged in the effective part of the sensing a...

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Abstract

The invention discloses a method for determining a multi-component resultant in a multivariant anode material precursor based on an EDTA back titration-automatic titration method. Excessive EDTA standard solution is added to a prepared precursor sample solution to complex multi-component metal elements; in a boric acid-sodium borate buffer solution, an automatic titration device is utilized to dropwise add a Zn <2+> solution for back titration of the excessive EDTA; a zinc reagent serves as an indicator, the sudden change of the luminosity intensity is sensed by using a luminosity sensor with the light filter wavelength of 650 nm, and a terminal point is automatically judged; according to sample mass, the recorded volume and concentration of the EDTA standard solution and the volume and concentration of the consumed Zn <2+> solution, the multi-component resultant in a nickel and cobalt (manganese / aluminum and the like) multivariant anode material are calculated. The method can accurately, rapidly and stably detect the multi-component resultant in various types of multi-component precursors, is especially suitable for multi-batch testing in large-scale industrialized production and greatly improves automated detecting level and reliability in the field.

Description

technical field [0001] The invention relates to a method for determining the amount of multiple components in a precursor of multiple positive electrode materials based on an EDTA back titration-automatic titration method, and belongs to the technical field of new detection methods. Background technique [0002] The precursor of multiple cathode materials refers to nickel hydroxide, cobalt, manganese, aluminum, magnesium, etc., which are used to produce ternary cathode materials (such as nickel-cobalt lithium manganese oxide LNCM, nickel-cobalt-aluminum-lithium NCA ternary cathode materials) and binary cathode materials (such as nickel-cobalt binary cathode material LNC) is the most important raw material. With the large-scale application of lithium-ion batteries produced by NCM, NCA, NC and other multi-component cathode materials in mobile phones, digital cameras, computers, electric tools, electric vehicles and other fields, the demand for precursors of multi-component cat...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N21/79
CPCG01N21/79G01N31/16
Inventor 李军秀张文艳闫国真黄孝伟严子人
Owner GEM WUXI ENERGY MATERIAL CO LTD
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