The modern chemical industry is increasingly facing a contradiction: on the one hand, the need for complex chemical compounds is growing — from medicines to polymers, on the other, the requirements for environmental friendliness, energy efficiency and quality control are increasing. In these conditions, it is especially important not just to start chemical reactions, but to understand exactly how they proceed at the molecular level.

One of these key reactions is hydroformylation, a fundamental process of organic synthesis widely used in industry to convert olefins into aldehydes. Despite decades of research, it remains difficult to control: intermediates exist for fractions of a second, and traditional methods of analysis require stopping the reaction and sampling, which does not always reflect the real picture of what is happening.

This is exactly the problem that the study solves, the results of which are published in the reputable international journal Analytical Chemistry. A team of scientists from three research centers — the International Research Institute of Intelligent Materials of the Southern Federal University, the Faculty of Chemistry of Moscow State University and the International Tomographic Center of the Siberian Branch of the Russian Academy of Sciences — proposed using in-line nuclear magnetic resonance (NMR) to monitor hydroformylation directly inside a microfluidic reactor in a segmented flow mode. Each of the teams has made a key contribution. For example, SFedU specialists developed and implemented a microfluidic installation, and ensured that experiments were conducted under high pressure and controlled conditions. The researchers of the ITC SB RAS provided in-line NMR experiments on a high-field spectrometer, adapted the recording technique in a flow mode without stopping the reaction. Dmitry Gorbunov's team from Moscow State University synthesized a catalyst, prepared reaction mixtures, and analyzed the products using gas chromatography and ex situ NMR.

This approach made it possible to track the concentrations of reagents and products in real time, as well as study the kinetics of the reaction without having to use expensive deuterated solvents — ordinary toluene was used instead. This not only simplifies and reduces the cost of analysis, but also brings laboratory conditions closer to industrial ones.

The ability to observe a chemical reaction in real time fundamentally changes the approach to its study and optimization. In-line NMR allows you not only to record the result, but to understand the process itself — step by step. This is especially important for pressure reactions, where traditional sampling is laborious and can distort the picture," notes Alexander Guda, Doctor of Physics and Mathematics, Head of the research laboratory "Microfluidic Technologies for Accelerated Synthesis of Materials" at the SFedU.

Smart Materials Research Institute.

The development of in-line NMR diagnostics is a step towards "smart chemistry," where decisions are made based on accurate data rather than assumptions. Such technologies not only increase the efficiency of scientific research, but also shape the future of sustainable chemical production.

The results of the study, supported by a grant from the Russian Science Foundation (RNF project #25-12-00424 and 25-13-00053), are published in the scientific journal Analytical Chemistry.