The aim of the study was to investigate the effect of process parameters on the production of hydrogels with antisolvent precipitation using unpurified (UB) and purified (PB) birch outer bark betulin powder samples. Experimental activities are focused on the production of hydrogels using concentration of colloidal dispersions with filtration of UB or PB sample particles obtained by antisolvent precipitation method varying the dilution of saturated (at boiling temperature) ethanol solutions with different water content. During the study the maximum solubility in ethanol at boiling point of PB (22.0 g/L) and UB (55.0 g/L) was determined. For obtaining gel with the highest liquid content (absorption capacity 37.45 g per 1 g of dry matter) from PB by antisolvent precipitation the optimal saturated ethanol solution dilution with water was 12.5 vol%. In the case of UB hydrogel, by dilution of ethanol from 25 to 10 vol%, a gradual decrease of hydrogel dry matter yield and a simultaneous increase of the filtrate dry matter yield can be observed, which is related with leaching of the particles through the filter paper together with a solution and form a colloidal suspension of particles. For obtaining gels with high liquid content from UB the optimal saturated ethanol solution dilution with water was in the range from 20.0 to 12.5 vol% (absorption capacity in average 18 g per 1 g of dry matter). Comparing the chemical compositions of the raw materials and dry matter of hydrogels in the case of PB composition remains quite similar while in UB dry matter composition the betulin content increased from 52 to even 69 wt%. PB at the optimal dilution of 12.5 vol% of ethanol managed to achieve average particle size - 231.7 nm and with UB in the optimal dilution range from 20 to 12.5 vol% the range of average particle size was from 304.7 to 189.8 nm.
A wood residuesawdust of the mechanical processing of aspen (Populus tremula) woodwas used to obtain a short fibre filler in the form of the modified microparticles < 250 µm for polymeric composite materials. To reduce energy input for wood size reduction and the activation of the lignocellulosic matrix for modification, low temperature acid hydrolysis of the residue under mild conditions was carried out. The effect of the pre-treatment parameters (acid concentration, hydrolysis duration, hydromodulus) on the fractional and chemical composition as well as on the zeta potential and contact angle of the obtained filler were studied. A comparison of the mechanical properties (tensile, bending) of the composites filled with initial sawdust and hydrolysed microparticles modified with a non-stoichiometric polyelectrolyte complex showed a pronounced improvement of the mechanical properties of the composites filled with modified wood microparticles.
To decrease climate changes, more research focuses on decreasing waste wood biomass (WWB) burning and increasing its conversion into value-added products. The WWB was isolated from model wood processing wastewater with a new hybrid coagulant by the coagulation/flocculation method. This study is aimed to characterize the WWB and to investigate its effect in the composition of a hybrid lignocellulosic filler on the properties of recycled polypropylene (rPP)-based wood–plastic composites (WPCs). The waste biomass contained high-molecular lignin and hemicelluloses substances and represented a finely dispersed powder. It was hydrophobic and was characterized by enhanced thermal stability. To minimize the negative effect of polymer wastes on the environment, recycled polypropylene as a polymer matrix was used with the hybrid filler in fabricating WPC samples. The presence of the coagulated WWB in the hybrid filler composition positively affects the mechanical properties, water uptake and dimensional stability of the composite samples. Such a behavior of the waste biomass showed its function as a compatibilizer, which promoted the interfacial adhesion in the composite system.
A lignin-containing adhesion enhancer, a water-soluble polyelectrolyte complex (LPEC) composed of soda hardwood lignin (HASL) and polyethylenimine (PEI), and the effect of the treatment of hydrolyzed and ammoxidized aspen sawdust with the LPEC nanoparticles were studied relative to the properties of wood-plastic composites (WPCs) based on recycled polypropylene (rPP). The presence of the excess of free amine groups and salt bonds between PEI and soda lignin, forming hydrophobic sites in the LPEC structure, caused the enhanced surface activity of the LPEC. The treatment with the LPEC nanoparticles increased the content of the fixed nitrogen in the modified sawdust samples and was accompanied by decreasing their water sorption and increasing contact angles that favored the decrease in the polar part of their surface free energy. The decreasing wetting ability enhanced the mechanical and water sorption properties of the obtained WPC samples. The improvement of the interfacial adhesion between the nitrogen-containing groups of the treated sawdust and the oxygen-containing groups of rPP was explained by the formation of both covalent and physicochemical bonds.
Dynamic light scattering (DLS) is a well-established technique to analyze particle size in a liquid medium and sample preparation is an essential step of the analysis to obtain reliable data. In this study, the pretreatment of an aqueous suspension containing betulin particles was studied to characterize the colloidal betulin particles in supramolecular hydrogels obtained by the liquid antisolvent precipitation from purified and unpurified betulin samples. Parameters of two-step homogenization process using rotor and ultrasonic homogenizer, particle concentration, and pH were systematically varied to obtain stable aqueous suspensions that meet the requirements of DLS technique for good particle size analysis. It was found that the purified betulin particles have a higher tendency to agglomerate and their suspension is stable in a narrower concentration and pH range than unpurified. Particle size analysis in suspensions prepared independently shows good reproducibility of sample preparation.
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