Global sustainability challenges prompt the world to modify its strategies and shift from a fossil-fuel-based economy to a bio-resources-based one and to the production of renewable biomass chemicals. Depolymerized suberinic acids (SA) were considered as an alternative resource to develop bio-polyols that can be further used in polyurethane (PU) material production. Birch (Betula pendula) outer bark was used as a raw material to obtain the SA, extracted with ethanol, and depolymerized with potassium hydroxide ethanol solution. By acidifying the filtrate to pH 5.0, 3.0, and 1.0 and drying it at 50 °C and 130 °C, 12 different SA potential feedstocks were obtained and characterized using chemical (total phenolics content, solubility in DMSO, acid, hydroxyl, and saponification number) and instrumental analytical methods (GC-MS, SEC-RID, DSC, and FTIR). Several bio-polyols were synthesized from the SA sample acidified to pH 1 and dried at 130 °C. Acid number and hydroxyl number values, the apparent viscosity and moisture content were measured. It was concluded that SA have a high enough saponification and acid value to investigate the polyol synthesis route via the esterification reaction. Moreover, SA had OH groups in their structure, which can be exploited for PU material development. The majority of SA compounds had relatively low molecular weight with <1300 Da that are suited for bio-polyol synthesis applied for rigid PU foam development. The synthesized bio-polyols had high hydroxyl number values necessary for bio-polyols to be used for rigid PU foam production.
The birch (Betula spp.) outer bark is a valuable product rich in betulin. After removal of betulin extractives, suberin containing tissues are left. Suberin is a biopolyester built from α,ω-bifunctional fatty acids (suberinic acids), which after depolymerization together with lignocarbohydrate complex is a potential adhesive as a side-stream product (residue) from obtaining suberinic acids for polyol synthesis. In this work, we studied the utilization possibilities in particleboards of the said residue obtained by depolymerization in four different solvents (methanol, ethanol, isopropanol and 1-butanol). The adhesives were characterised by chemical (acid number, solubility in tetrahydrofuran, epoxy and ash content) and instrumental analytical methods (SEC-RID, DSC, TGA and FTIR). Based on the results of mechanical characteristics, ethanol was chosen as the most suitable depolymerization medium. The optimal hot-pressing parameters for particleboards were determined using the design of experiments approach: adhesive content 20 wt%; hot-pressing temperature 248 °C, and hot-pressing time 6.55 min.
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.
Global sustainability challenges prompt the world to modify their strategies and shift from a fossil-fuel-based economy to a bio-resources-based one and to the production of renewable biomass-based chemicals. Different processes exist that allow the transformation of raw biomass into desirable bio-based products and/or energy. Depolymerized suberinic acids (SA) can be considered as an alternative resource to different feedstocks for value-added product obtaining, for example to develop bio-polyols that can be further used in polymeric material production. Birch outer bark was used as a raw material for obtaining SA and was extracted with ethanol to remove extractives. Further extracted birch outer bark was depolymerized with potassium hydroxide ethanol/methanol/n-butanol/2-propanol solutions. Obtained SA suspension was dried by performing lyophilization or by drying at 100 °C. As a result, we obtained 8 SA samples, which were characterized using chemical (total phenolics content, solubility in DMSO, acid number, hydroxyl number, and saponification number) and instrumental analytical methods (GC-MS, SEC-RID, FTIR). The most suitable SA for obtaining value-added product, such as bio-polyol, were obtained by using ethanol as a solvent for depolymerization process. The corresponding SA had the best results in terms of dry matter content, yield, solubility in DMSO, epoxy groups, acid number and ash content. After GC-MS results it was concluded that the amount of diacids, hydroxyacids and extractives are dependent of the used alkanol for SA depolymerization as well as the drying method.
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