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Kunkel, Benny ; Seeburg, Dominik ; Kabelitz, Anke ; Witte, Steffen ; Gutmann, Torsten ; Breitzke, Hergen ; Buntkowsky, Gerd ; Guilherme Buzanich, Ana ; Wohlrab, Sebastian
The production of formaldehyde on industrial scale requires huge amounts of energy due to the involvement of reforming processes in combination with the demand in the megaton scale. Hence, a direct route for the transformation of (bio)methane to formaldehyde would decrease costs and puts less pressure on the environment. Herein, we report on the use of zinc modified silicas as possible support materials for vanadium catalysts and the resulting consequences for the performance in the selective oxidation of methane to formaldehyde. After optimization of the Zn content and reaction conditions, a remarkably high space-time yield of 12.4 kgCH2O⋅kgcat − 1 ⋅h− 1 was achieved. As a result of the extensive characterization by means of UV–vis, Raman, XANES and NMR spectroscopy it was found that vanadium is in the vicinity of highly dispersed zinc atoms which promote the formation of active vanadium species as supposed by theoretical calculations. This work presents a further step of catalyst development towards direct industrial methane conversion which may help to overcome current limitations in the future.
Ring-opening polymerizations (ROPs) of l-lactide (LA) were performed with ethyl l-lactate or 11-bromoundecanol as initiators (In) and tin(II) ethyl hexanoate (SnOct2) as catalyst (Cat) using four different LA/In ratios (20/1, 40/1, 60/1, and 100/1). One series of ROPs was conducted in bulk at 120 °C, yielding PLAs with low dispersities (Ð ~ 1.2–1.4), and a second series was conducted in bulk at 160 °C, yielding higher dispersities (Ð ~ 1.3–1.9). Samples from both series were annealed for 1 or 14 days at 140 °C in the presence of SnOct2. Both polycondensation and disproportionation reactions occurred, so that all four samples tended to form the same type of molar mass distribution below 10,000 Da, regardless of their initially different number average molar masses (Mn). Both initiators gave nearly identical results. The thermodynamic control of all reversible transesterification processes favored the formation of crystallites composed of chains with a Mn around 3500–3700, corresponding to a crystal thickness of 10–13 nm.
Solvent-free sample preparation offers some advantages over solvent-based techniques, such as improved accuracy, reproducibility and sensitivity, for matrix-assisted laser desorption/ionization (MALDI) analysis. However, little or no information is available on the application of solvent-free techniques for the MALDI analysis of polymer blends. Solvent-free sample preparation by ball milling was applied with varying sample-to-matrix ratios for MALDI time-of-flight mass spectrometry analysis of various polymers, including polystyrenes, poly(methyl methacrylate)s and poly(ethylene glycol)s. The peak intensity ratios were compared with those obtained after using the conventional dried droplet sample preparation method. In addition, solvent-assisted milling was also applied to improve sample homogeneities.
Depending on the sample preparation method used, different peak intensity ratios were found, showing varying degrees of suppression of the signal intensities of higher mass polymers. Ball milling for up to 30 min was required to achieve constant intensity ratios indicating homogeneous mixtures. The use of wet-assisted grinding to improve the homogeneity of the blends was found to be disadvantageous as it caused partial degradation and mass-dependent segregation of the polymers in the vials.The results clearly show that solvent-free sample preparation must be carefully considered when applied to synthetic polymer blends, as it may cause additional problems with regard to homogeneity and stability of the blends.
Hoogendoorn, Levi ; Huertas, Mauricio ; Nitz, Phillip ; Qi, Naiyu ; Baller, Johannes ; Prinz, Carsten ; Graeber, Gustav
AbstractSorbents are promising materials for applications in atmospheric water harvesting, thermal energy storage, and passive cooling, thereby addressing central challenges related to water scarcity and the global energy transition. Recently, hygroscopic hydrogel composites have emerged as high‐performance sorbents. However, many of these systems are fabricated with unsustainable and costly sorbent materials, which hinders their wide deployment. Here, the synthesis of high‐performance, cost‐efficient polyacrylamide hydrogels loaded with unprecedented amounts of calcium chloride is demonstrated. To this end, the swelling procedure of polyacrylamide hydrogels in aqueous calcium chloride solutions is optimized. The achievable salt loading in the hydrogel is characterized as a function of temperature, calcium chloride concentration in the swelling solution, and the hydrogel preparation conditions. The obtained hydrogel‐salt composites are shown to be stable under repeated sorption‐desorption cycling and enable water uptakes of 0.92 and 2.38 grams of water per gram of dry materials at 30% and 70% relative humidity, respectively. The resulting cost‐performance ratio substantially exceeds lithium chloride‐based systems. Further, the mechanistic insights on hydrogel salt interactions can guide the design of sustainable and low‐cost sorbent materials for future applications in water and energy.
A poly(L-lactide) with a trifluoroethyl ester end group and an average degree of polymerization (DP) of 50 was synthesized by ROP of L-lactide initiated with trifluoroethanol. Small-angle X-ray scattering (SAXS) in combination with differential scanning calorimetry (DSC) measurements revealed an average crystal thickness of 13 nm, corresponding to 45 repeat units. This suggests that most crystallites were formed by extended PLA chains, and both flat surfaces were covered by CF3 groups. The crystalline PLAs were annealed at 140 or 160 °C in the presence of two catalysts: tin(II) 2-ethylhexanoate, (SnOct2) or dibutyltin bis(pentafluorophenoxide) (BuSnPhF). The chemical reactions, such as polycondensation and cyclization, proceeded in the solid state and were monitored by matrix-assisted laser desorption/ionization time-offlight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC) measurements. Under optimal conditions a large fraction of linear chains was transformed into crystallites composed of extended cycles. Additionally, MALDI TOF MS analysis of GPC fractions from samples annealed for 28 or 42 days detected chain elongation of the linear species up to a factor of 20.
The Na salt of chloroacetic acid is condensed in suspension. Furthermore,glycolic acid is condensed in bulk or in concentrated solution by means of SnCl2 or 4-toluene sulfonic acid (TSA) as catalysts. The temperatures are varied from 160 to 200°C and the time from 1 to 5 days. Low molar mass cyclic poly(glycolic acid) (PGA) is detected by means of matrix-assisted laser desorption ionization time-of-flight (MALDI TOF) mass spectrometry in most PGAs. A predominance of certain cycles having an even number of repeat units is observed suggesting a thermodynamically favored formation of extended-ring crystals. Extremely high melting temperatures (up to 237.5°C)and high melting enthalpies are found for polycondensations with TSA in 1,2-dichlorobenzene.
Glycolide was polymerized in bulk with two cyclic catalysts − 2,2-dibutyl-2-stanna-1,3-dithiolane (DSTL) and 2-stanna-1,3-dioxa-4,5,6,7-dibenzepane (SnBiph). The monomer/initiator ratio, temperature (140 – 180 °C) and time (1–––4 days) were varied. The MALDI TOF mass spectra exclusively displayed peaks of cyclic polyglycolide (PGA) and revealed an unusual “saw-tooth pattern” in the mass range below m/z 2 500 suggesting formation of extended ring crystallites. The DSC measurements indicated increasing crystallinity with higher temperature and longer time, and after annealing for 4 d at 160 °C a hitherto unknown and unexpected glass transition was found in the temperature range of 170–185 °C. Linear PGAs prepared by means of metal alkoxides under identical conditions did not show the afore-mentioned features of the cyclic PGAs, neither in the mass spectra nor in the DSC measurements. All PGAs were also characterized by SAXS measurements, which revealed relatively small L-values suggesting formation of thin crystallites in all cases with little influence of the reaction conditions.