NMR Analysis to Identify Biuret Groups in Common Polyureas

Wei-Guang Qiu; Fei-Long Zhang; Xu-Bao Jiang; Xiang-Zheng Kong

doi:10.1007/s10118-018-2130-y

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NMR Analysis to Identify Biuret Groups in Common Polyureas

ARTICLE | Updated：2021-02-18

- NMR Analysis to Identify Biuret Groups in Common Polyureas
- Chinese Journal of Polymer Science Vol. 36, Issue 10, Pages: 1150-1156(2018)
- Affiliations：
  
  College of Chemistry and Chemical Engineering, University of Jinan, Jinan 250022, China
- Author bio：
  
  chm_jiangxb@ujn.edu.cn (X.B.J.)
  xzkong@ujn.edu.cn (X.Z.K.)
- Funds：
- DOI：10.1007/s10118-018-2130-y
  CLC：
- Received：24 January 2018，
  
  Revised：2018-1-24，
  
  Accepted：19 February 2018，
  
  Online First：12 April 2018，
  
  Published：2018-10
- Accepted：
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Citation: Qiu, W. G.; Zhang, F. L.; Jiang, X. B.; Kong, X. Z. NMR Analysis to Identify Biuret Groups in Common Polyureas. Chinese J. Polym. Sci. 2018, 36(10), 1150–1156.

Wei-Guang Qiu, Fei-Long Zhang, Xu-Bao Jiang, et al. NMR Analysis to Identify Biuret Groups in Common Polyureas[J]. Chinese Journal of Polymer Science, 2018, 36(10): 1150-1156.
Citation: Qiu, W. G.; Zhang, F. L.; Jiang, X. B.; Kong, X. Z. NMR Analysis to Identify Biuret Groups in Common Polyureas. Chinese J. Polym. Sci. 2018, 36(10), 1150–1156. DOI： 10.1007/s10118-018-2130-y.

Wei-Guang Qiu, Fei-Long Zhang, Xu-Bao Jiang, et al. NMR Analysis to Identify Biuret Groups in Common Polyureas[J]. Chinese Journal of Polymer Science, 2018, 36(10): 1150-1156. DOI： 10.1007/s10118-018-2130-y.

摘要

Abstract

Polyureas (PU) are well known as a class of high impact engineering materials

and widely used also in emerging advanced applications. As a general observation

most of them are only soluble in a very limited number of highly protonic solvents

which makes their chemical structure analysis a great challenge. Besides the presence of abundant hydrogen bonding

the poor solubility of PU in common organic solvents is often ascribed to the formation of biuret crosslinking in their molecular chains. To clarify the presence of biuret groups in PU has been of great interest. To this end

two samples

based on hexamethylene diisocyanate (HDI) and toluene diisocyanate (TDI) respectively

were synthesized by precipitation polymerization of each of these diisocyanates in water-acetone at 30 °C. Their chemical structures were analyzed by high resolution magic angle spinning (HR-MAS) NMR

and through comparison of their NMR spectra with those of specially prepared biuret-containing polyurea oligomers

it was concluded that biuret group was absent in all the PU prepared at 30 °C. In addition

this NMR analysis was also applied to a PU obtained by copolymerization of TDI with ethylene diamine (EDA) and water at 65 °C in EDA aqueous solution. It was confirmed that biuret unit was also absent in this PU and that EDA was more active than water towards TDI. The presence of EDA was crucial to the formation of uniform PU microspheres. This study provides therefore a reliable method for the analysis of PU chemical structure.

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references

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