Synthesis of chemical compounds is the process of creating new substances from raw materials. There are many ways to control the parameters of a chemical reaction, of which microfluidics is the most promising. Microfluidic technologies are focused on controlling the flow of liquids and gases at the microscopic level inside capillaries with a diameter of less than 1 mm. Unlike traditional methods of synthesis in a flask, microfluidics allows you to work with volumes of reagents in the range from microliters to picoliters, perform rapid mixing (on the order of milliseconds) and increase the contact area of two immiscible phases (for example, gas-liquid). Due to this, materials are created with very precise control of composition, morphology, and structure.

"First of all, microfluidics as a synthesis method has many advantages over traditional methods. It allows precise control of reaction conditions such as pressure, temperature and flow rate, which improves reaction kinetics and increases product yield. The use of even explosive mixtures of gases is safe in conditions of thin capillaries. High pressure and a large contact area with the liquid increase the efficiency of saturation of the solution with synthesis gas molecules and thereby accelerate the chemical reaction. In addition, some reactions occur only at high pressures and temperatures, for example hydroformylation, which has not previously been studied in this mode using X–ray spectral methods," said Eid Mahmoud Elsayed Abdelaziz, a postdoc at the SFedU from Egypt.

Mahmoud Elsayed Abdelaziz is a young scientist originally from Egypt. Since October 2023, he has been actively working at the International Research Institute of Intellectual Materials of the Southern Federal University under the postdoctoral program within the framework of the Priority 2030 Development Program (national project "Science and Universities") and under the guidance of Doctor of Physical and Mathematical Sciences Alexander Guda. The subject of his research is related to the project "Fast and Furious of materials" by the federal program "Priority 2030", within which he is engaged in expanding the field of applicability of microfluidic systems to high pressures. Together with colleagues from MIIIM and Moscow State University (Gorbunov PhD group), Mahmoud Elsayed Abdelaziz developed a new microfluidic system and cell for flow diagnostics of the reaction mixture using X-ray and Raman spectroscopy methods. This development has a number of key features that distinguish it from existing analogues.

The system is built on chemically inert capillaries made of PEEK material, and provides constant and stable pressure during the synthesis process due to a special back pressure regulator, which is an upgrade of a foreign commercial analog, the hydroformylation reaction [catalytic addition used for the production of aldehydes from alkenes]. The in-situ diagnostic cell is universal and allows monitoring both the state of the catalyst by X-ray absorption spectroscopy (XAS) and the concentration of reaction products by Raman spectroscopy. The in situ measurement cell, as well as high-precision syringe pumps for supplying reagents under pressure, were manufactured at the Institute.

"The system has a number of advantages: it accelerates the kinetics of reactions, ensures uniform mixing, reduces the risk of dangerous reactions and allows you to receive immediate feedback. These characteristics make it especially useful in the production of aldehydes and alcohols, which are later used in many branches of chemical production in the production of solvents and detergents," said Alexander Guda, PhD, Associate Professor, Deputy Director of the SFedU Research Institute.

A scientific paper published in the journal Q1 "Industrial & Engineering Chemistry Research" describes the successful application of the system for the analysis of a catalytic reaction in the presence of Rh/amine complexes active in the reductive hydroformylation of olefins to produce alcohols. Experimental studies and theoretical modeling have shown that under hydroformylation conditions, the presence of amines prevents the formation of rhodium nanoclusters and leads to the formation of rhodium monomers and dimers coordinated by a nitrogen atom.

At the next stage of the project, the scientists plan to create a metal gas-liquid separator for high-pressure sampling and use in situ Raman scattering to screen reaction parameters. The updates will allow hundreds of measurements to be carried out in a short time, which will allow the use of machine learning methods to control reaction parameters.

Mahmoud Elsayed Abdelaziz also noted that the conditions created at the SFedU Research Institute played an important role in supporting this research, providing the necessary resources and a favorable working environment. He was invited to the Institute by Professor, Doctor of Physico-Mathematical Sciences, head of the frontier laboratory of X-ray spectral Nanometrology of the Center for High-Tech Instrumentation of the Southern Federal University, scientific director of the Materials Science and Synchrotron-Neutron Research department of the Southern Federal University Alexander Soldatov to participate in the development of new approaches to accelerated production of functional materials under the control of artificial intelligence. The work at SFedU has made it possible to achieve significant success in the development and testing of a new microfluidic system, and its recognition at the international level further emphasizes the relevance of innovations in the field of microfluidics and their potential to advance research at the intersection of science and industry, especially in the production of specialized chemicals.