Effect of Process Conditions on the Properties of Resorcinol-Formaldehyde Aerogel Microparticles Produced via Emulsion-Gelation Method

Organic aerogels in the form of powder, microgranules and microsized particles receive considerable attention due to their easy fabrication, low process time and costs compared to their monolithic form. Here, we developed resorcinol-formaldehyde (RF) aerogel microparticles by using an emulsion-gelation method. The main objective of this study is to investigate the influence of curing time, stirring rate, RF sol:oil ratio and initial pH of the sol in order to control the size and properties of the microparticles produced. The emulsion-gelation of RF sol prepared with sodium carbonate catalyst in an oil phase at 60 °C was explored. RF microparticles were washed with ethanol to remove the oil phase followed by supercritical and ambient pressure drying. The properties of the dried RF microparticles were analyzed using FT-IR, N2 adsorption isotherm, gas pycnometry, wide angle X-ray scattering and scanning electron microscope. RF microparticles with high surface area up to 543 m2/g and large pore volume of 1.75 cm3/g with particle sizes ranging from 50–425 µm were obtained.

Improvement of Solvent Exchange for Supercritical Dried Aerogels

The solvent exchange as one of the most important steps during the manufacturing process of organic aerogels was investigated. This step is crucial as a preparatory step for the supercritical drying, since the pore solvent must be soluble in supercritical carbon dioxide to enable solvent extraction. The development and subsequent optimization of a suitable system with a peristaltic pump for automatic solvent exchange proved to be a suitable approach. In addition, the influence of zeolites on the acceleration of the process was found to be beneficial. To investigate the process, the water content in acetone was determined at different times using Karl Fischer titration. The shrinkage, densities, as well as the surface areas of the aerogels were analyzed. Based on these, the influence of various process parameters on the final structure of the obtained aerogels was investigated and evaluated. Modeling on diffusion in porous materials completes this study.

Investigation of Aerogel Production Processes: Solvent Exchange under High Pressure Combined with Supercritical Drying in One Apparatus

This work aims to contribute to the theoretical and experimental research of supercritical processes for intensification and combination in one apparatus. Investigation is carried out to improve production technology of organic alginate aerogels. It is proposed within the investigation to carry out the solvent exchange stage, an important stage of organic aerogels production, under pressure in a carbon dioxide medium in the same apparatus used for supercritical drying. The phase behavior in the system “carbon dioxide–water–2-propanol”, which arises during such a solvent exchange stage, is studied theoretically. An experimental study of the process of step-by-step solvent exchange under pressure was carried out through multiphase and homogeneous regions of the phase diagram of such a system. As a result, new highly efficient technology for the production of organic aerogels was proposed, which can be implemented by combining the two main stages of the process.

Organic Aerogels Based on Epoxy Resins: Synthesis and Properties

The aim of this work was to develop methods for the synthesis of organic aerogels based on epoxy resins and to investigate their properties. Aerogels based on DGEBA-epoxy resin were obtained by CO2-supercritical drying of gel samples prepared from acetone solutions of epoxy resin with different amount of catalyst and solvents. As a result, aerogels of different density were obtained; the dependence of density on the solvent content in the samples was revealed. The aerogels were characterized by infrared spectroscopy to define the degree of conversion of the epoxy groups, by SEM to confirm nanoscale morphology of aerogels, as well as by the BET method to determine the specific surface area of the samples and its dependence on the catalyst content and curing conditions.

Ferrocene Introduced into 5-Methylresorcinol-Based Organic Aerogels

The polycondensation sol–gel reaction of 5-methylresocinol and formaldehyde with additional compounds in reaction media is a relatively simple way to produce modified aerogels. In order to obtain aerogels with a large surface area and high porosity, the conditions for gel formation, the solvent exchange process before drying, and the supercritical drying process were optimized. A successful attempt was made to introduce ferrocene units into 5-methylresocinol-formaldehyde-based aerogels. The resulting aerogels are amorphous substrates, and no aggregated ferrocene units were found in their structures. All of the aerogel samples that were obtained are structurally similar despite differences in the original ferrocene units and their initial concentration. It was found that the inclusion limit of ferrocene structural blocks into an aerogel is ~6% wt. The structures of the inclusions in which all of the Fe atoms in the aerogel substrates were present in ferrocene/ferrocenium at an approximate ratio of 60/40 to 55/45 were confirmed by X-ray photoelectron spectroscopy and Mössbauer spectroscopy. Aerogels with ferrocene/ferrocenium inclusions are likely to exhibit reversible redox activity in reactions with gaseous reagents.