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Development of the technique for quality control of 1,3-bis(3,4-dicyanophenoxy)benzene by HPLC

https://doi.org/10.32362/2410-6593-2021-16-1-88-98

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Abstract

Objectives. Determination of target products and byproducts is necessary for the quality control of phthalonitrile monomer synthesis as well as production scaling and performing related kinetic studies. High-performance liquid chromatography (HPLC) is a simple and affordable method for quantitative chemical analysis, which also verifies the quality of raw materials. The objective of this study was to develop an HPLC technique for determining the composition of the reaction mixture in the synthesis of 1,3-bis(3,4-dicyanophenoxy)benzene (DPB).

Methods. Reversed-phase HPLC was used to quantitatively analyze the reaction mixture.

Results. A simple and rapid method for the quantitative HPLC analysis of phthalonitrile monomers and their mixtures with reagents was developed. Reaction times and the accumulation of byproducts were also studied.

Conclusions. The successful performance of the developed technique allows us to recommend it for practical applications. The results obtained for reactors of different sizes have good convergence, and DPB synthesis was successfully scaled up to intermediate scale equipment.

About the Authors

Z. N. Shchekoldina
Moscow State University
Russian Federation

Zinaida N. Shchekoldina, Postgraduate Student, Department of Chemical Technology and New Materials

1–11, Leninskie Gory, Moscow, 119991



A. A. Bogolyubov
Moscow State University
Russian Federation

Alexey A. Bogolyubov, Cand. Sci. (Chem.), Engineer, Department of Chemical Technology and New Materials

1–11, Leninskie Gory, Moscow, 119991



A. Yu. Zakharov
Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences
Russian Federation

Alexander Yu. Zakharov, Postgraduate Student, Laboratories of Crystal Chemistry and X-Ray Structural Analysis

31, Leninsky prospect, Moscow, 119991



B. A. Bulgakov
Moscow State University
Russian Federation

Boris A. Bulgakov, Cand. Sci. (Chem.), Senior Science Master, Department of Chemical Technology and New Materials

1–11, Leninskie Gory, Moscow, 119991



A. V. Babkin
Moscow State University
Russian Federation

Alexander V. Babkin, Cand. Sci. (Chem.), Senior Science Master, Department of Chemical Technology and New Materials. Scopus Author ID 56258683200

1–11, Leninskie Gory, Moscow, 119991



A. V. Kepman
Moscow State University
Russian Federation

Alexey V. Kepman, Cand. Sci. (Chem.), Head Scientist Researcher, Department of Chemical Technology and New Materials

1–11, Leninskie Gory, Moscow, 119991



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Supplementary files

1. Fig. 4. 3D spectrum plotted during column washing.
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2. This is to certify that the paper titled Development of the technique for quality control of 1,3-bis(3,4-dicyanophenoxy)benzene by HPLC commissioned to us by Zinaida N. Shchekoldina, Alexey A. Bogolyubov, Alexander Yu. Zakharov, Boris A. Bulgakov, Alexander V. Babkin, Alexey V. Kepman. has been edited for English language and spelling by Enago, an editing brand of Crimson Interactive Inc.
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  • A simple and rapid method for the quantitative HPLC analysis of phthalonitrile monomers and their mixtures with reagents was developed.
  • Reaction times and the accumulation of byproducts were studied.
  • The synthesis was successfully scaled up from laboratory to intermediate scale equipment.

For citation:


Shchekoldina Z.N., Bogolyubov A.A., Zakharov A.Yu., Bulgakov B.A., Babkin A.V., Kepman A.V. Development of the technique for quality control of 1,3-bis(3,4-dicyanophenoxy)benzene by HPLC. Fine Chemical Technologies. 2021;16(1):88-98. https://doi.org/10.32362/2410-6593-2021-16-1-88-98

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ISSN 2410-6593 (Print)
ISSN 2686-7575 (Online)