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Method for analyzing SEBS hydrogenation degree of butadiene styrene rubber by using nuclear magnetic resonance technology

A technology of styrene-butadiene rubber and nuclear magnetic resonance, which is applied in the direction of analysis by nuclear magnetic resonance, material analysis through resonance, and material analysis. It can solve the problem of long analysis period and the analysis and detection of hydrogenation degree of styrene-butadiene rubber products and other issues, to achieve the effect of improving economic benefits, good environmental protection benefits, and reducing work intensity

Pending Publication Date: 2020-05-15
PREAMSOLUTIONS INFORMATION TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the halogenation method can only be manually sampled for off-line analysis, and the analysis period is slightly longer. It is often difficult to provide sample property data for production in time, and there is a certain lag.
However, there is no relevant report on the analysis and detection of the hydrogenation degree of styrene-butadiene rubber products using a 60MHz nuclear magnetic resonance analyzer.

Method used

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  • Method for analyzing SEBS hydrogenation degree of butadiene styrene rubber by using nuclear magnetic resonance technology
  • Method for analyzing SEBS hydrogenation degree of butadiene styrene rubber by using nuclear magnetic resonance technology
  • Method for analyzing SEBS hydrogenation degree of butadiene styrene rubber by using nuclear magnetic resonance technology

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Experimental program
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Effect test

Embodiment 1

[0040] Analysis of hydrogenation degree of styrene-butadiene rubber SEBS (sample 1)

[0041] 1. Sample Analysis

[0042] Taking the styrene-butadiene rubber SEBS product of a domestic chemical company (sample 1, w% (styrene) = 34%, w% (butadiene) = 66%, hydrogenation reaction for about 10 minutes under certain conditions) as an example, the The analysis process of its degree of hydrogenation is described, and the steps are as follows:

[0043] (1) Add the analysis sample to the NMR tube.

[0044] (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 (as attached figure 1 shown);

[0045] (3) Integrate the characteristic peak areas in the two regions of 6.23-7.28ppm and 5.01-5.50ppm in the sample hydrogen NMR spectrum, and calculate the characteristic peak areas S in the two regions 1 , S 2 are 0.3101 and 0.1012 respectively, then according to the hydrogenation degree calculation for...

Embodiment 2

[0052] Analysis of hydrogenation degree of styrene-butadiene rubber SEBS (sample 2)

[0053] 1. Sample Analysis

[0054] Taking another styrene-butadiene rubber SEBS product of a domestic chemical company (sample 2, w% (styrene) = 34%, w% (butadiene) = 66%, hydrogenation reaction for about 20 minutes under certain conditions) as an example, The analysis process of its degree of hydrogenation is described, and the steps are as follows:

[0055] (1) Add the analysis sample to the NMR tube.

[0056] (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 (as attached figure 2 shown);

[0057] (3) Integrate the characteristic peak areas in the two regions of 6.23-7.28ppm and 5.01-5.50ppm in the sample hydrogen NMR spectrum, and calculate the characteristic peak areas S in the two regions 1 , S 2 are 0.4199 and 0.0340 respectively, then according to the hydrogenation degree calculation fo...

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Abstract

The invention provides a method for analyzing the SEBS hydrogenation degree of butadiene styrene rubber by using a nuclear magnetic resonance technology. The method comprises the following steps: (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 the sample to obtain a nuclear magnetic resonance hydrogen spectrum of the sample; and (3) integrating the area of each structural characteristic peak in the nuclear magnetic resonance hydrogen spectrum of the sample, and calculating the relative content of double bonds before and after the reaction of the butadiene styrene rubber sample according to the area of the corresponding structural characteristicpeak, thereby further calculating the hydrogenation degree of the sample. According to the method, rapid analysis can be carried out in the presence of a solvent, the accuracy of the analysis resultis high, analysis equipment operates stably, and a simple, rapid and accurate detection method is provided for detecting the hydrogenation degree of the styrene butadiene rubber SEBS sample.

Description

technical field [0001] The invention belongs to the field of analysis of rubber products, in particular to a method for analyzing the hydrogenation degree of styrene-butadiene rubber (SEBS) by nuclear magnetic resonance technology. Background technique [0002] Styrene-butadiene rubber SEBS is a linear three-block copolymer with polystyrene as the terminal block and ethylene-butene copolymer obtained by hydrogenation of polybutadiene as the middle elastic block. It is composed of block copolymer SBS ( Styrene-butadiene-styrene) is prepared by selective hydrogenation. The so-called selective hydrogenation refers to the hydrogenation of the polybutadiene segment mainly, while the benzene ring of the polystyrene segment is basically not hydrogenated. [0003] In SEBS products, the double bonds of the polybutadiene segment are hydrogenated, and only a small amount of unhydrogenated saturation, so its performance not only has the unique properties of thermoplastic elastomers suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/087G01N24/088
Inventor 刘阳
Owner PREAMSOLUTIONS INFORMATION TECH BEIJING
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