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Method for measuring hydroxyl value of polycaprolactone triol by utilizing 1H nuclear magnetic resonance spectra

A technology of hydrogen nuclear magnetic resonance spectroscopy and polycaprolactone, which is applied in the fields of nuclear magnetic resonance analysis, climate sustainability, water resources assessment, etc., can solve the problem of rapid detection of hydroxyl value of polycaprolactone polyols that has not been seen , low analysis efficiency, high temperature requirements, etc., to achieve good environmental protection benefits, improve analysis efficiency, and improve product quality

Active Publication Date: 2019-12-27
PREAMSOLUTIONS INFORMATION TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires high temperature and complicated operation, and some human errors are prone to occur in the analysis process; at the same time, the entire analysis process takes a long time and the analysis efficiency is low
However, there is no relevant report on the use of 60MHz nuclear magnetic resonance analyzer to quickly detect the hydroxyl value and other indicators of polycaprolactone polyols.

Method used

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  • Method for measuring hydroxyl value of polycaprolactone triol by utilizing 1H nuclear magnetic resonance spectra
  • Method for measuring hydroxyl value of polycaprolactone triol by utilizing 1H nuclear magnetic resonance spectra
  • Method for measuring hydroxyl value of polycaprolactone triol by utilizing 1H nuclear magnetic resonance spectra

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Embodiment 1

[0033] Analysis of hydroxyl value of polycaprolactone triol (sample 1)

[0034] 1. Sample Analysis

[0035] Taking the polycaprolactone triol (sample 1) of a domestic chemical company as an example, the calculation process of the hydroxyl value of the polycaprolactone triol sample is explained. The steps are as follows:

[0036] (1) Add the analysis sample to the NMR tube.

[0037](2) Place the NMR tube in the NMR analyzer, select the corresponding analysis plan, scan the sample, and obtain the H NMR spectrum of the sample;

[0038] (3) Integrate the characteristic peak areas of the five regions of -0.55~0.93ppm, 0.93~1.89ppm, 1.89~2.79ppm, 2.79~3.64ppm, 3.64~5.11ppm in the sample hydrogen nuclear magnetic resonance spectrum, and calculate and obtain -0.55~ The total area of ​​three characteristic peaks in the 2.79ppm region X 1 is 67.190, the total area of ​​two characteristic peaks in the region of 2.79~5.11ppm X 2 is 31.763, then the ratio of the total number of H atoms...

Embodiment 2

[0045] Analysis of hydroxyl value of polycaprolactone triol (sample 2)

[0046] 1. Sample Analysis

[0047] Select polycaprolactone triol (sample 2), another domestic chemical company, to analyze the hydroxyl value of its polycaprolactone triol sample, the steps are as follows:

[0048] (1) Add the analysis sample to the NMR tube.

[0049] (2) Place the NMR tube in the NMR analyzer, select the corresponding analysis plan, scan the sample, and obtain the H NMR spectrum of the sample;

[0050] (3) Integrate the characteristic peak areas of the five regions of -0.55~0.93ppm, 0.93~1.89ppm, 1.89~2.79ppm, 2.79~3.64ppm, 3.64~5.11ppm in the sample hydrogen nuclear magnetic resonance spectrum, and calculate and obtain -0.55~ The total area of ​​three characteristic peaks in the 2.79ppm region X 1 is 69.267, the total area of ​​two characteristic peaks in the region of 2.79~5.11ppm X 2 is 31.543, then the ratio of the total number of H atoms in each structure in the two regions is t...

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Abstract

The invention provides a method for measuring hydroxyl value of polycaprolactone triol by utilizing 1H nuclear magnetic resonance spectra. The method comprises the following steps of (1) adding an analysis sample into a nuclear magnetic tube; (2) placing the nuclear magnetic tube in a nuclear magnetic resonance analyzer, selecting a corresponding analysis scheme, and scanning a sample to obtain a1H nuclear magnetic resonance spectra of the sample; (3) integrating characteristic peak areas of all structures in the 1H nuclear magnetic resonance spectra of the sample, calculating the average polymerization degree n of the sample according to the relation between the H atom number ratio of all structures and the characteristic peak intensity ratio, and further calculating the average relativemolecular mass and specific hydroxyl value of the polycaprolactone triol sample. The method disclosed by the invention has the characteristics of being simple and quick in analysis process, high in accuracy of analysis results, stable in operation of analysis equipment and the like, and a simple, quick and accurate detection method is provided for the calculation of the hydroxyl value of the polycaprolactone triad sample.

Description

technical field [0001] The invention belongs to the field of analysis of polycaprolactone trihydric alcohols, and in particular relates to a method for measuring the hydroxyl value of polycaprolactone trihydric alcohols by proton nuclear magnetic resonance spectrum. Background technique [0002] Polycaprolactone triol is a kind of polycaprolactone polyol (Poly-ε-caprolactone glycol, referred to as PCL), which plays an important role in industry. For example, in the main aspects of elastomers, coatings, adhesives, etc., various aspects such as elastic optical fibers, pottery sealants, coatings, foams, resins, microcellular elasticity / foam, sealants, shoe materials, tubular materials, etc. can be widely used application. It can improve the performance of coatings, elastomers and adhesives in many aspects such as abrasion resistance and hydrolysis resistance. [0003] Generally, polycaprolactone polyol is formed by ring-opening polymerization of caprolactone monomer, initiato...

Claims

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Application Information

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IPC IPC(8): G01N24/08
CPCG01N24/08Y02A90/30
Inventor 刘阳王晓宇
Owner PREAMSOLUTIONS INFORMATION TECH BEIJING
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