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Method for detecting content of free amine in NMP

A detection method, the technology of free amine, applied in the field of chemical detection, can solve the problems of battery self-discharge, inability to evaluate NMP performance, no effective and fast detection method for free amine, etc., and achieve the effect of not easy oxidation and stable chemical properties

Inactive Publication Date: 2019-06-07
刘洪河
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, due to its production process, NMP contains a small amount of free amine as a raw material, but it is an impurity in the finished product. If the content is too high, it will affect the quality of lithium batteries and cause problems such as battery self-discharge.
At present, there is no effective and fast detection method for the detection of free amines in NMP, and it is impossible to accurately evaluate the performance of NMP.

Method used

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  • Method for detecting content of free amine in NMP
  • Method for detecting content of free amine in NMP
  • Method for detecting content of free amine in NMP

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1, a kind of detection method to free amine in NMP, comprises the steps:

[0045] (1) Material preparation: hydrochloric acid standard solution, bromocresol green-methyl red indicator, absolute ethanol (content ≥ 99.7%), NMP finished product;

[0046] (2) Preparation of indicator solution:

[0047] Solution Ⅰ: Accurately weigh 0.1g of bromocresol green, dissolve it in absolute ethanol, and dilute to 100mL with absolute ethanol;

[0048] Solution II: Accurately weigh 0.2g of methyl red, dissolve in absolute ethanol, and dilute to 100mL with absolute ethanol;

[0049] Take 30ml of solution Ⅰ and 10ml of solution Ⅱ and mix them evenly.

[0050] Solution Ⅲ: Preparation of hydrochloric acid solution

[0051] Measure the corresponding amount of hydrochloric acid according to the provisions in the table below, use a volumetric flask to set the volume to 1000mL, and shake well.

[0052] The concentration of hydrochloric acid standard titration solution c...

Embodiment 2

[0094] Embodiment 2, original alcohol and isopropanol are done the comparative experiment of free amine

[0095] 1. The purpose of the experiment: to analyze the difference between alcohol and isopropanol as free amine

[0096] 2. Experimental equipment: balance, 250ml Erlenmeyer flask

[0097] 3. Experimental procedure: select 10 different samples as free amines.

[0098] The amount of free amine added is divided into: 30ml NMP+30ml alcohol; 30ml NMP+30ml isopropanol;

[0099] 4. Experimental results

[0100] Alcohol blank titration is 0.05ml; isopropanol blank titration is 0.5ml

[0101]

[0102] 5. Data processing, see appendix figure 1 , the average range is: 0.383

[0103] 6. Experimental conclusion: When making free amine, when adding 30ml alcohol and 30ml isopropanol, the detection error is within a reasonable range.

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Abstract

The invention relates to a method for detecting content of free amine in NMP. The method comprises the following steps: 1) carrying out material preparation; 2) preparing an indicator solution; 3) placing a conical flask on an electronic balance, carrying out peeling, measuring 50mL NMP with a measuring cylinder and pouring the measured NMP into the conical flask to accurately obtain the mass, recorded as m, of the NMP; 4) adding 50mL absolute ethyl alcohol and 3-4 drops of bromocresol green-methyl red indicators into the conical flask in sequence and then, smoothly shaking the conical flask to make the mixture uniform; 5) carrying out titration with a 0. 01mol / L hydrochloric acid standard solution till the solution is turned from green to light yellow and keeping for 30s till the color does not fade, and recording the consumption volume V of the hydrochloric acid standard solution; 6) carrying out blank test and recording consumption volume V0 of the hydrochloric acid standard solution; and 7) carrying out calculation. The method for detecting the content of free amine in the NMP adopts the absolute ethyl alcohol as a diluent instead of isopropanol adopted as the diluent in the previous method; and compared with other diluents, the absolute ethyl alcohol has the advantages of safety, environmental protection, low toxicity, stable chemical properties, not easy oxidation and lowcost and the like, and is a good diluent for detection of the free amine in the NMP.

Description

technical field [0001] The invention belongs to the technical field of chemical detection and relates to the detection of raw materials in the lithium battery industry, in particular to a detection method for free amine content in NMP. Background technique [0002] At present, the national policy support for the new energy industry is developing rapidly, and the development of new energy batteries as the core is also advancing by leaps and bounds. Regardless of whether PVDF is used as a binder or the main material of the negative electrode, graphite and conductive agent, the raw material NMP (N-methyl The role of pyrrolidone) in the middle can effectively dissolve PVDF to make it have better adhesion. Adding a small amount of NMP to the graphite material can also improve the wettability of graphite, making it better mixed with the binder, and finally improving The quality of the battery. [0003] However, due to its production process, NMP contains a small amount of free am...

Claims

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Application Information

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IPC IPC(8): G01N31/16
Inventor 刘洪河刘同兴郑之朋
Owner 刘洪河
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