Different approaches towards hydrophobic modification of bacterial cellulose aerogels with the alkyl ketene dimer (AKD) reagent are presented. If AKD modification was performed in supercritical CO 2 , an unexpectedly high degree of loading was observed. About 15 % of the AKD was bound covalently to the cellulose matrix, while the other part consisted of re-extractable AKD-carbonate oligomers, which are novel chemical structures described for the first time. These oligomers contain up to six AKD and CO 2 moieties linked by enolcarbonate structures. The humidity uptake from environments with different relative humidity by samples equipped with up to 30 % AKD is strongly reduced, as expected due to the hydrophobization effect. Samples above 30 % AKD, and especially at very high loading between 100 and 250 %, showed the peculiar effect of increased humidity uptake which even exceeded the value of unmodified bacterial cellulose aerogels.
Conjugated polymers gain growing importance as conductive materials in industrial applications in various fields of electronic devices. Cellulose with its extraordinary supramolecular structure and material properties can help to awake the possibilities for conducting polymers in interplay of the two materials. The ability of additional derivatization, the stiff and oriented molecular structure and the inherent strength, stability and film-forming properties give cellulose a complementary role to the brittle conjugated polymers, cellulose imparting the features of a stable and robust carrier component. To go forward this way, making a composite out of cellulose and conducting polymers is a prerequisite. Different strategies to form composite materials of non-derivatized cellulose and conductive organic polymers were tested. Significant differences between various mixing strategies as well as between the conducting polymers polyaniline (PAni), polypyrrole (PPy), and polythiophen (PTh) were observed. In situ synthesis of the conducting polymers in cellulose solutions and microcellulose dispersions as well as blending of pre-synthesized conducting polymers in these cellulose systems were tested. Unexpectedly, not homogenous mixtures showed best results in respect to film formation and conductivity, but composites formed by heterogeneous mixtures of the conducting polymers within a cellulose gel. Best results were obtained with finely dispersed PAni. The results support development studies towards circuitry and photo-current systems based on cellulose carriers.
Analytical monitoring of xanthation in the viscose process along with xanthate group analysis in the viscose material is a long‐debated problem in cellulose chemistry. The task is rendered extremely intricate by the lability of the starting material and the harshness of the reaction medium, which adds to a lack of suitable analytical approaches. In a four‐years' endeavor in our lab, a method is being developed which allows to analyze the distribution of xanthate groups in viscoses relative to the anhydroglucose units and along the cellulose chain.In a first step the xanthate groups are stabilized by alkylation, which was optimized towards quantitative conversion. In a second step, the remaining free hydroxyl groups are protected by carbanilation, followed by selective removal of the stabilized xanthate groups. Steps two and three thus generate an inverse image of the initial xanthate pattern. In the forth and fifth step, the liberated hydroxyl groups are methylated, and the carbanilates are removed, so that in the overall process the xanthates were replaced by methyl groups. All reaction steps have been comprehensively tested with regard to completeness of conversion and orthogonality of the protecting groups.
In the course of the Ioncell-P process, hemicelluloses are extracted from wood pulps by a mild treatment with an ionic liquid (IL) water mixture, and the result is a high-purity dissolving pulp. The aim of the present work is to study the influence of pulp origin concerning different wood species and pulping processes on the resulting pulp purity and yield after extraction with IL/water, while the IL is 1-ethyl-3-methylimidazolium acetate ([emim][OAc]). The raw materials were chosen from commercial alkaline kraft and acid sulfite paper and dissolving pulps prepared from both hardwood (HW) and softwood (SW). The extraction was followed by a filtration step to separate the cellulose and the hemicellulose fractions. The hemicelluloses were precipitated from the IL/water filtrate. In general, the Ioncell-P process proved to be more selective toward the removal of xylan as compared to glucomannan indicating that HW pulps are easier to purify than those of SW. It was possible to reach high alpha pulp qualities by the extraction process.
Based on previous investigations on the substitution pattern of stabilized and fresh viscose, different viscoses were analyzed by gel permeation chromatography (GPC) with multiple-angle laser light scattering, refractive index (RI), and UV detection. Viscoses derivatized with N-methyl-N-phenyl-iodoacetanilide are stable over a long time and largely improve handling for analytical purposes. In addition, the derivatized xanthogenate groups exhibit UV absorbance that can be used to detect their distribution along the polymer molecule, once the polymer is dissolved. UV assay indicated that in technical viscoses the distribution of substituents is uniform. Enzymatic degradation with endoglucanases was followed by analysis of the degradation pattern by GPC. Even though the degree of substitution (DS) of xanthogenate groups ranged from gs0.4 to 0.6, endoglucanases were able to slightly degrade the viscose. Ultrasonic degradation resulted in a narrow molecular weight distribution (MWD), notably without cleavage of substituents, and was also used to improve the solubility of the stabilized viscoses for further analysis. The techniques applied provide more insight into the xanthogenate distribution along the MWD. Remarkable differences in the degradation behavior of both viscose samples were observed.
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