Magnetically Recyclable Borane Lewis Acid Catalyst for Hydrosilylation of Imines and Reductive Amination of Carbonyls.

Fluorinated arylborane-based Lewis acid catalysts have shown remarkable activity and serve as ideal examples of transition metal-free catalysts for diverse organic transformations. However, their homogeneous nature poses challenges in terms of recyclability and separation from reaction mixtures. This work presents an efficient technique for the heterogenization of boron Lewis acid catalysts by anchoring Piers' borane to allyl-functionalized iron oxide. This catalyst demonstrates excellent activity in the hydrosilylation of imines and the reductive amination of carbonyls using various silanes as reducing agents under mild reaction conditions. The catalyst exhibits broad tolerance towards a wide range of functional substrates. Furthermore, it exhibits good recyclability and can be easily separated from the products using an external magnetic field. This work represents a significant advance in the development of sustainable heterogenous metal-free catalysts for organic transformations.

On the Mechanical Properties of Microfibre-Based 3D Chitinous Scaffolds from Selected Verongiida Sponges.

Skeletal constructs of diverse marine sponges remain to be a sustainable source of biocompatible porous biopolymer-based 3D scaffolds for tissue engineering and technology, especially structures isolated from cultivated demosponges, which belong to the Verongiida order, due to the renewability of their chitinous, fibre-containing architecture focused attention. These chitinous scaffolds have already shown excellent and promising results in biomimetics and tissue engineering with respect to their broad diversity of cells. However, the mechanical features of these constructs have been poorly studied before. For the first time, the elastic moduli characterising the chitinous samples have been determined. Moreover, nanoindentation of the selected bromotyrosine-containing as well as pigment-free chitinous scaffolds isolated from selected verongiids was used in the study for comparative purposes. It was shown that the removal of bromotyrosines from chitin scaffolds results in a reduced elastic modulus; however, their hardness was relatively unaffected.

Metallodendrimers Unveiled: Investigating the Formation and Features of Double-Decker Silsesquioxane-Based Silylferrocene Dendrimers.

Dendrimers exhibiting reversible redox properties have attracted extensive attention for their potential as electron transfer mediators, catalysts, and molecular sensors. In this study, we introduce intriguing G1 and G2 dendrimers featuring double-decker silsesquioxane cores and silylferrocene moieties. Through a carefully orchestrated sequence of condensation, reduction, and hydrosilylation reactions, these compounds were synthesized and comprehensively characterized spectroscopically and spectrometrically. Our investigation also encompassed the examination of their properties, including thermal stability, solubility in common organic solvents, and electrochemical behavior. We determined that these dendrimers possess the capability to form monolayers on platinum electrodes, which we conclusively demonstrated through the probing of cyclic voltammetry, electrochemical impedance spectroscopy, and scanning electron microscopy imaging. Notably, this study marks the first-ever example of modifying double-decker silsesquioxane cores with ferrocene groups while simultaneously representing one of the scarce instances of dendrimers exhibiting an open double-decker silsesquioxane core.

Precipitation of Pt, Pd, Rh, and Ru Nanoparticles with Non-Precious Metals from Model and Real Multicomponent Solutions.

This article presents studies on the precipitation of Pt, Pd, Rh, and Ru nanoparticles (NPs) from model and real multicomponent solutions using sodium borohydride, ascorbic acid, sodium formate, and formic acid as reducing agents and polyvinylpyrrolidone as a stabilizing agent. As was expected, apart from PGMs, non-precious metals were coprecipitated. The influence of the addition of non-precious metal ions into the feed solution on the precipitation yield and catalytic properties of the obtained precipitates was studied. A strong reducing agent, NaBH4 precipitates Pt, Pd, Rh, Fe and Cu NPs in most cases with an efficiency greater than 80% from three- and four-component model solutions. The morphology of the PGMs nanoparticles was analyzed via SEM-EDS and TEM. The size of a single nanoparticle of each precipitated metal was not larger than 5 nm. The catalytic properties of the obtained nanomaterials were confirmed via the reaction of the reduction of 4-nitrophenol (NPh) to 4-aminophenol (NAf). Nanocatalysts containing Pt/Pd/Fe NPs obtained from a real solution (produced as a result of the leaching of spent automotive catalysts) showed high catalytic activity (86% NPh conversion after 30 min of reaction at pH 11 with 3 mg of the nanocatalyst).

Scanning Electron Microscope Examination as an Alternative to Classical Microbiology in the Diagnostics of Catheter-Related Sepsis?

Central venous catheters are essential elements enabling the treatment of intensive care unit patients. However, these catheters are sometimes colonised by both bacteria and fungi, and thus, they may become a potential source of systemic infections-catheter-related bloodstream infections (CRBSI). The identification of the pathogen responsible for CRBSI is a time-consuming process. At the same time, the relationship between the quick identification of the pathogen and the implementation of targeted antibiotic therapy is of key importance for controlling the clinical symptoms of sepsis and septic shock in the patient. Quick diagnosis is of key importance to reduce morbidity and mortality in this group of patients. In our study, we attempted to create a catalogue of images of the most commonly cultured pathogens responsible for CRBSI. An FEI Quanta 250 FEG Scanning Electron Microscope (SEM) was used for measurements. SEM images obtained during the analysis were included in this study. Images of SEM are three-dimensional and comparable to the images seen with the human eye and are a tool used for research and measurement whenever it is necessary to analyse the state of the surface and assess its morphology. The method described in our study will not replace the current procedures recognised as the gold standard, i.e., pathogen culturing, determination of the count of microorganisms (CFU -colony forming units), and assessment of drug sensitivity. However, in some cases, the solution proposed in our study may aid the diagnosis of patients with suspected catheter-related bloodstream infections leading to sepsis and septic shock.

Fluorocarbosilane-Based Protective Coatings for Concrete.

The effectiveness of protective coatings based on 3-(2,2,3,3,4,4,5,5-octafluoropentyloxy)propyltriethoxysilane (OFTES) in protecting concrete surfaces against water was tested. For the synthesis of OFTES, 2,2,3,3,4,4,5,5-octafluoropentanol, which is a by-product in the synthesis of poly(tetrafluoroethylene), was used. The proposed silane is a cheaper alternative to the fluorinated organosilicon compounds currently used. The coatings were deposited by the sol-gel method. As a result of the creation of chemical bonds between the concrete surface and the silane, a coating was created that permanently increases the hydrophobicity of the concrete. Fluorine chains attached to silicon atoms are an effective barrier that prevents access to water and limits its impact on the concrete surface. As a result of the proposed silanization, the concrete surface obtained a hydrophobic character at contact angles of up to 126°, and the water absorption of the concrete decreased by up to 96%.

Siloxane resins as hydrophobic self-cleaning layers for silicon and dye-sensitized solar cells: material and application aspects.

The aim of this study has been to examine in depth three siloxane resins (R1-R3) and two silanes (S1-S2) as hydrophobic self-cleaning layers for silicon and dye-sensitized solar cells. Herein, we focused on creating an active self-cleaning surface system using a combination of material and technical aspects. Siloxane resins were obtained via the hydrolytic polycondensation of methyltrimethoxysilane (R1) or the hydrolytic co-polycondensation of methyltrimethoxysilane, isobutyltrimethoxysilane and 3-methacroiloxypropyltrimethoxysilane (R2) or methyltrimethoxysilane n-octyltriethoxysilane and 3-methacroiloxypropyltrimethoxysilane (R3) under alkaline conditions using tetrahydrofuran. All layers under study did not significantly affect the original optical properties of the glass support, confirming that all these compounds can be used as protective layers on glass surfaces. The hydrophobic nature of formed layers was confirmed by static water contact angle measurements for hexane- and/or dibutyl ether-based starting solutions at various concentrations. The structural defects in created layers were studied via atomic force microscopy and thermal imaging, revealing RMS roughness (R q) values in the range of 0.76-5.25 nm, which varied for different materials. The current-voltage curves of different hydrophobic coatings showed conductive behaviour, demonstrating that principally non-conductive coatings mixed with silver conductive paste showed a certain level of conductivity. This finding suggests that the hydrophobic coating resembles a porous structure, enabling the formation of electrically conductive pathways. Finally, the influence of the presence of a coating layer on silicon and dye-sensitized solar cells was studied, and no negative effect on their photovoltaic parameters was observed after the durability test.

Elevated CD4 + T-cell glucose metabolism in HIV+ women with diabetes mellitus.

OBJECTIVE: Immune dysfunction and chronic inflammation are characteristic of HIV infection and diabetes mellitus, with CD4 + T-cell metabolism implicated in the pathogenesis of each disease. However, there is limited information on CD4 + T-cell metabolism in HIV+ persons with diabetes mellitus. We examined CD4 + T-cell glucose metabolism in HIV+ women with and without diabetes mellitus. DESIGN: A case-control study was used to compare CD4 + T-cell glucose metabolism in women with HIV with or without diabetes mellitus. METHODS: Nondiabetic (HIV+DM-, N = 20) or type 2 diabetic HIV+ women with (HIV+DM+, N  = 16) or without (HIV+DMTx+, N  = 18) antidiabetic treatment were identified from the WIHS and matched for age, race/ethnicity, smoking status and CD4 + cell count. CD4 + T-cell immunometabolism was examined by flow cytometry, microfluidic qRT-PCR of metabolic genes, and Seahorse extracellular flux analysis of stimulated CD4 + T cells. RESULTS: HIV+DM+ displayed a significantly elevated proportion of CD4 + T cells expressing the immunometabolic marker GLUT1 compared with HIV+DMTx+ and HIV+DM- ( P  = 0.04 and P  = 0.01, respectively). Relative expression of genes encoding key enzymes for glucose metabolism pathways were elevated in CD4 + T cells of HIV+DM+ compared with HIV+DMTx+ and HIV+DM-. T-cell receptor (TCR)-activated CD4 + T cells from HIV+DM+ showed elevated glycolysis and oxidative phosphorylation compared with HIV+DM-. CONCLUSION: CD4 + T cells from HIV+DM+ have elevated glucose metabolism. Treatment of diabetes mellitus among women with HIV may partially correct CD4 + T-cell metabolic dysfunction.

Machine Learning Approach for Application-Tailored Nanolubricants' Design.

The fascinating tribological phenomenon of carbon nanotubes (CNTs) observed at the nanoscale was confirmed in our numerous macroscale experiments. We designed and employed CNT-containing nanolubricants strictly for polymer lubrication. In this paper, we present the experiment characterising how the CNT structure determines its lubricity on various types of polymers. There is a complex correlation between the microscopic and spectral properties of CNTs and the tribological parameters of the resulting lubricants. This confirms indirectly that the nature of the tribological mechanisms driven by the variety of CNT-polymer interactions might be far more complex than ever described before. We propose plasmonic interactions as an extension for existing models describing the tribological roles of nanomaterials. In the absence of quantitative microscopic calculations of tribological parameters, phenomenological strategies must be employed. One of the most powerful emerging numerical methods is machine learning (ML). Here, we propose to use this technique, in combination with molecular and supramolecular recognition, to understand the morphology and macro-assembly processing strategies for the targeted design of superlubricants.

Poly(vinylbenzyl Pyridinium Salts) as Novel Sorbents for Hazardous Metals Ions Removal.

Novel efficient complexing resins-poly(vinylbenzyl pyridinium salts) fabricated through poly(vinylbenzyl halogene-co-divinylbenzene) quaternization of N-decyloxy-1-(pyridin-3-yl)ethaneimine and N-decyloxy-1-(pyridin-4-yl)ethaneimine-were tested as adsorbents of Pb(II), Cd(II), Cu(II), Zn(II), and Ni(II) from aqueous solutions. The structure of these materials was established by 13C CP-MAS NMR, X-ray photoelectron spectroscopy, elemental analysis, and Fourier transform infrared spectroscopy, as well as thermogravimetric and differential thermal analyses. The textural properties were determined using scanning electron microscopy and low-temperature N2 sorption. Based on the conducted sorption studies, it was shown that the uptake behavior of the metal ions towards novel resins depended on the type of functionalities, contact time, pH, metal concentrations, and the resin dosage. The Langmuir model was investigated to be the best one for fitting isothermal adsorption equilibrium data, and the corresponding adsorption capacities were predicted to be 296.4, 201.8, 83.8, 38.1, and 39.3 mg/g for Pb(II), Zn(II), Cd(II), Cu(II), and Ni(II), respectively. These results confirmed that owing to the presence of the functional pyridinium groups, the resins demonstrated proficient metal ion removal capacities. Furthermore, VBBr-D4EI could be successfully used for the selective uptake of Pb(II) from wastewater. It was also shown that the novel resins can be regenerated without significant loss of their sorption capacity.

Predicting the risk of Alaria alata infestation in wild boar on the basis of environmental factors.

Alaria alata is an emerging parasite that poses a potential risk for those consuming game, pork, snails and frogs. One paratenic host of A. alata that is known to play an important role in its spread through its feeding habitats is the wild boar. However, no statistical analysis of the influence of aquatic environments and carnivores on the occurrence of A. alata in wild boars has yet been performed. The present study combines a small-scale analysis based on hunting districts in the Mazowieckie province with a large-scale analysis based on data for all provinces in Poland. We applied various modeling approaches, including logistic regression and a generalized linear model in order to determine the presence, intensity and prevalence of A. alata. We used the Alaria mesocercariae migration technique (AMT) to estimate the risk of A. alata among wild boar in a given hunting district or province. The small-scale analysis found that mesopredators (red fox (Vulpes vulpes)) and racoon dog (Nyctereutes procyinoides) were likely to influence A. alata infestation of wild boar; however, the effect was weak, probably as a result of the large home range size of these animals. The large-scale analysis found that wetlands influence the prevalence of A. alata in wild boar, with the estimated risk increasing in the north of the country; this finding is consistent with other studies. Our findings indicate that the occurrence of A. alata in wild boar requires analysis on many levels, and environmental factors play a key role in risk assessment.

Novel Mesoporous Organosilicas with Task Ionic Liquids: Properties and High Adsorption Performance for Pb(II).

Removal of toxic contaminants such as Pb(II) from waste solutions is environmentally requested. Therefore, in this paper, for potential novel sorbents, mesoporous ionic liquid-functionalized silicas were synthesized and tested for the removal of Pb(II) from aqueous solutions. The successful synthesis of the adsorbents was proved by nuclear magnetic resonance (29Si and 13C NMR), Fourier transform infrared spectroscopy (FTIR), and elemental analysis. The structural and textural properties were determined using scanning electron microscopy (SEM), X-ray diffraction (XRD), high-resolution transmission electron microscopy (TEM), and low-temperature N2 sorption, and the result showed that the applied procedure made it possible to obtain highly ordered particles with a two-dimensional mesostructure. The effects of several parameters including initial pH, contact time, adsorption temperature, and Pb(II) concentration were studied in detail and were discussed to evaluate the adsorption properties of the fabricated materials towards Pb(II). The obtained results confirmed a very high potential of the sorbents; however, the adsorption properties depend on the structure and amounts of the functional group onto fabricated materials. The sample ILS-Ox3-40 showed fast kinetics (equilibrium reached within 10 min) and capacity of 172 mg/g, and that makes it a promising sorbent for the cleanup of water contaminated by lead. It was also indicated that, regardless on structure of the tested materials, the Pb(II) removal was spontaneous and exothermic. The fabricated mesoporous silicas exhibited that they were easy to regenerate and had excellent reusability.

The Friction of Structurally Modified Isotactic Polypropylene.

The purpose of studies was to analyse an impact of heterogeneous nucleation of modified isotactic polypropylene (iPP) on its tribological properties. The iPP injection molded samples, produced by mold temperature of 20 and 70 °C, were modified with compositions of two nucleating agents (NA's), DMDBS creating α-form and mixture of pimelic acid with calcium stearate (PACS) forming ß-phase of iPP, with a total content 0.2 wt.% of NA's. A polymorphic character of iPP, with both, monoclinic (α) and pseudo-hexagonal (ß) crystalline structures, depending on the NA's ratio, was verified. The morphology observation, DSC, hardness and tribological measurements as test in reciprocating motion with "pin on flat" method, were realized, followed by microscopic observation (confocal and SEM) of the friction patch track. It was found that Shore hardness rises along with DMBDS content, independent on mold temperature. The friction coefficient (COF) depends on NA's content and forming temperature-for upper mold temperature (70 °C), its value is higher and more divergently related to NA's composition, what is not the case by 20 °C mold temperature. The height of friction scratches and the width of patch tracks due to its plastic deformation, as detected by confocal microscopy, are related to heterogeneous nucleation modified structure of iPP.

Experimental Study of Single-Lap, Hybrid Joints, Made of 3D Printed Polymer and Aluminium Adherends.

This paper presents the results of an experimental study into single-lap joints. One part of the joint was made as a 3D printed polymer and had cylindrical tenons, while the other part was made of an aluminium flat bar having mortises whose diameter and distribution corresponded to the polymer tenons. In addition to the mechanical joint, a layer of double-sided VHB (Very High Bond) adhesive tape was also placed in the lap, thus creating a hybrid joint. In total, 80 specimens were made, which were divided into four groups: A-specimens with one tenon of different diameters, B-specimens with different number of tenons of the same diameter, C-specimens characterised by multi-stage operation and R-reference specimens, connected only by double-sided adhesive tape. The joints were subjected to uniaxial tensile tests. The force-displacement characteristics obtained and the energy required, up to the point of the failure of the joints, have been analysed in this paper. The four and six-stage joints designed can significantly increase the safety of the structures in which they will be used.

Novel Polymer Sorbents with Imprinted Task-Specific Ionic Liquids for Metal Removal.

In this paper, the potential of novel polymer sorbents with the imprinted IL-functional group for the removal of Cu(II), Cd(II), and Zn(II) from aqueous solutions was investigated by batch mode. The sorbents were fabricated by direct reaction of the prepared polymer matrix (poly(vinylbenzyl chloride-divinylbenzene), VBC, and poly(vinylbenzyl bromide-divinylbenzene), VBBr) with 1-(3- or 4-pyridyl)undecan-1-one and oxime of 1-(3- or 4-pyridyl)undecan-1-one. The Fourier Transform Infrared Spectroscopy (FT-IR), Raman Spectroscopy (Raman), Thermogravimetric Analysis (TG), Differential Scanning Calorimetry (DSC), and Scanning Electron Microscopy (SEM) techniques were used to show functionality and stability of the sorbents. The materials were also characterized by contact-angle goniometry, X-rayphotoelectron spectroscopy (XPS), and Zeta potential analysis. The removal of Cd(II), Cu(II), and Zn(II) was monitored and optimized under the influence of several operational controlling conditions and factors such as pH, shaking time, temperature, initial metal ions concentration, and counter-ions at the functional group. The results obtained confirmed the very high potential of the sorbents; however, the properties depend on the structure of the functional group. The tested sorbents showed fast kinetics, significant capacity at 25 °C (84 mg/g for the Zn(II) sorption with VBC-Ox4.10, 63 mg/g for the Cd(II) sorption with VBBr-Ox3.10, and 69 mg/g for the Cu(II) sorption with VBC-K3.10), and temperature dependence (even 100% increase in capacity values at 45 °C). The selected sorbent can be regenerated without a significant decrease in the metal removal efficiency.

A comparison of detection methods of Alaria alata mesocercariae in wild boar (Sus scrofa) meat.

Distomum musculorum suis (DMS), the mesocercariae of Alaria alata, is typically found accidently during examination of wild boar meat for Trichinella spp. The aim of the study was to compare DMS detection methods. Briefly, 232 wild boar meat samples were tested by mesocercariae migration technique (AMT) as a reference method; of these, 104 were found to be positive. Selected positive samples were tested again with the three other methods: compressorium method (Compressor), digestion with magnetic stirrer (Digestion) and by modified digestion with Pancreatin® bile and pancreatic enzymes (D + P). The results were analyzed by logistic regression, the non-parametric Kruskal-Wallis test and the Mann-Whitney U test. Of the 43 samples found positive by the AMT, 20 were found positive by Digestion and 25 by D + P. The Compressor identified DMS in seven of the 19 tested samples. The Digestion and D + P methods gave similar intensities (P = 0.506), i.e. 1.4 and 1.3 DMS respectively, but the AMT detected seven times higher number of parasites. The probability of detection of DMS in the meat sample by the Digestion or by D + P was higher than 0.5 when at least seven (Digestion) or five (D + P) DMS were present in the sample (AMT). The Compressor was the least sensitive method: at least 14 DMS must be present in the meat sample for detection. AMT should be considered the most accurate method of DMS detection.

Mechanisms of Fluorine-Induced Separation of Mass Interference during TOF-SIMS Analysis.

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is one of very few analytical techniques allowing sample chemical structure to be characterized in three-dimensional (3D) with nanometer resolution. Due to the excellent sensitivity in the order of ppm-ppb and capability of detecting all ionized elements and molecules, TOF-SIMS finds many applications for analyzing nanoparticle-containing systems and thin films used in microdevices for new energy applications, microelectronics, and biomedicine. However, one of the main drawbacks of this technique is potential mass interference between ions having the same or similar masses, which can lead to data misinterpretation. In this work, we present that this problem can be easily solved by delivering fluorine gas to a sample surface during TOF-SIMS analysis and we propose mechanisms driving this phenomenon. Our comprehensive studies, conducted on complex thin films made of highly mass-interfering elements, show that fluorine modifies the ionization process, leading to element-specific changes of ion yields (which can vary by several orders of magnitude), and affects the efficiency of metal hydride and oxide formation. In conjunction, these two effects can efficiently induce separation of mass interference, providing more representative TOF-SIMS data with respect to the sample composition and significant enhancement of chemical image resolution. Consequently, this can improve the chemical characterization of complex multilayers in nanoscale.

Medium-term response of the natural grassland soil biota to multiwalled carbon nanotube contamination.

Although the soil environment can potentially be exposed to contamination by carbon nanotubes (CNT), its impact on soil biology is poorly understood. In this study, we investigated the effect of the multiwalled CNT (MWCNT) contamination on different groups of soil organisms (microbial, micro- and mesofaunal communities) as well as the soil enzyme activity. The experimental mesocosms included the intact soil cores that were collected from a natural grassland. The MWCNTs that were pristine (pCNTs) and functionalised (fCNTs) at a concentration of 500 µg g-1 of soil were applied in the form of water suspensions to the surface of the mesocosms, while ensuring the soil was not mixed after the treatment. Soil samples were taken at 3, 6, and 15 weeks after CNT application. The CNT soil contamination highlighted differences in the community dynamics within the studied groups when compared to the control (non-contaminated soil). Among the faunal groups, nematodes were found to be more sensitive to the CNT impact than mites. The most pronounced response of the nematodes was observed in the subsoil at week 6, when their numbers were 3- (pCNTs) and 4-fold (fCNTs) higher than the control mesocosms. Both types of CNTs influenced the relative abundance of the bacterial- and hyphal-feeding nematodes, where pCNTs significantly and negatively affected the predatory nematodes. Moreover, CNTs temporarily, but significantly, decreased the diversity of the nematode communities. In addition, the values of the nematode Structure Index confirmed a strong transitional disturbance effect of CNTs in the soil food web, while the Channel Index in the pCNTs indicated an increasing share of fungi in the decomposition pathway. Hence, we can infer that although the impact of CNTs seems to be temporary, the shifts in the soil community abundance and structure that it induced may have long-term consequences for soil functioning, including nutrient cycling.

Trabecular bone remodelling in the femur of C57BL/6J mice treated with diclofenac in combination with treadmill exercise.

PURPOSE: Analgesic treatment with diclofenac deteriorates bone structure and decreases biomechanical properties. This bone loss has been though to be reversed by training. The impact of exercise on bone treated with diclofenac (DF) has reminded elusive. In the present study, we assayed the combined impact of exercises and DF on mouse femur. METHODS: The femur samples we obtained from 30 days treated C57BL/6J female mice. The training group ran on a horizontal treadmill at 12 m/min by 30 min a day (5% grade/slope). The group of ten mice treated with DF received the drug subcutaneously every day (5 mg/kg of body weight/day). The combined group ran on the treadmill and obtained DF. After 30 days, we sacrificed mice and studied their femurs using microcomputed tomography (µCT), dynamic mechanical analysis (DMA) and nanoindentation. RESULTS: We observed that treadmill running and DF decreased trabecular bone volume and mineral density. Combined effect of training and DF was not additive. A significant interaction of both parameters suggested protective effect of training on bone loss provoked by DF. The femur cortical bone shell remained untouched by the training and treatment. The training and the DF treatment did not alter the storage modulus E' significantly. The unchanged storage modulus would be suggesting on the unaltered bone strength. CONCLUSIONS: We concluded that even relatively short time of training with concomitant DF treatment could be protective on trabecular bone. Although viscoelastic properties of the entire femur were not modulated, femur trabecular tissue was thinned by treatment with DF and protected by training.

Phosphorus-Containing Silsesquioxane Derivatives as Additive or Reactive Components of Epoxy Resins.

Two phosphorus-containing cage-like silsesquioxane derivatives were synthesized as reactive or additive flame retardants for epoxy resin. The silsesquioxanes were obtained via an epoxide ring-opening reaction using a 10-hydroxy-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPA). In one derivative containing in its structure 4 glycidoxypropyl and 4 phosphate groups, denoted as 4P4GS, only half of the epoxy rings was reacted with phosphate to obtain a reactive additive, while in the second derivative containing 8 phosphate groups, denoted as 8PS, all epoxy groups were converted, thus an additive modifier was obtained. The silsesquioxanes containing phosphorus atoms and the reactive phosphorus-free silsesquioxane derivative (octakis[(3-glycidoxypropyl)dimethylsiloxy]octasilsesquioxane (8GS)) were used to prepare hybrid materials based on epoxy resin. To compare the impact of the structure of silsesquioxane derivatives on the properties of hybrid materials, a number of samples containing 1, 5, and 10% of the modifiers making a series of epoxy materials containing additive or reactive modifiers, were obtained. The modified epoxies were studied using scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM-EDS), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), nanoindentation, water contact angle, and cone calorimetry tests to assess the effects of the modifier structure on the physicochemical properties of the investigated materials.