Synthesis and characterization of hydroxypropyl cellulose from bacterial cellulose

Bacterial cellulose produced by Acetobacter xylinum has been reacted with propyleneoxide to synthesize hydroxypropyl cellulose(HPC) under different reaction conditions while diluted by toluene. The effects of mass ratio of bacterial cellulose to propyleneoxide, dilutability of toluene, reaction temperature(T) and time(t) were investigated by series of experiments. The degree of substitution(DS), hydroxypropyl content(A) and yield(η) were compared. The optimized product exhibited cold-water solubility and hot-water gelatinization in aqueous medium. Further study was carried out with FTIR, TGA, XRD, SEM and 13C-NMR for characterization. The water/air contact angle measurement reveals that it is a good hydrophobic material with good mechanical properties.     

Synthesis and characterization of microcrystalline cellulose produced from bacterial cellulose

In this study, microcrystalline cellulose (MCC) was prepared from the acid hydrolysis of bacterial cellulose (BC) produced in culture medium of static Acetobacter xylinum. The MCC-BC produced an average particle size between 70 and 90 μm and a degree of polymerization (DP) of 250. The characterization of samples was performed by thermogravimetric analysis, X-ray diffraction, and scanning electron microscopy (SEM). The MCC shows a lower thermal stability than the pristine cellulose, which was expected due to the decrease in the DP during the hydrolysis process. In addition, from X-ray diffractograms, we observed a change in the crystalline structure. The images of SEM for the BC and MCC show clear differences with modifications of BC fiber structure and production of particles with characteristics similar to commercial MCC.     

Synthesis, characterization and thermal studies on cellulose acetate membranes with additive

Cellulose acetate (CA) membranes are used in ultrafiltration applications, although they show low chemical, mechanical and thermal resistance. In order to prepare membranes with improved properties, modification of cellulose acetate with polyethelene glycol (PEG 600) has been attempted. In this study, CA has been mixed with PEG 600 as an additive in a polar solvent. The effects of CA composition and additive concentration given by a mixture design of experiments on membrane compaction, pure water flux, water content and membrane hydraulic resistance have been studied and discussed. The efficiency of protein separation by the developed CA membranes have been quantified using model proteins such as pepsin, egg albumin (EA) and bovine serum albumin (BSA). The thermal stability of the developed membranes prepared with PEG 600 additive has also been investigated using thermogravimetric analysis and differential scanning calorimetry.     

Preparation and characterization of bacterial cellulose membranes with tailored surface and barrier properties

Modified bacterial cellulose membranes with tailored properties, regarding their surface and barrier properties were prepared by controlled heterogeneous esterification with hexanoyl chloride. The characterization of the esterified bacterial cellulose membranes was performed by FTIR spectroscopy, elemental analyses, X-ray diffraction, thermogravimetry and contact angle measurements. The esterified membranes showed an increased hydrophobic surface character, while preserving the bulk structure of the pristine material. The evaluation of the barrier properties was carried out through permeability measurements towards water vapor at different relative humidities and by the permeability towards humidified carbon dioxide, oxygen and nitrogen using the time-lag method. A decrease of roughly 50% in both water and gas permeation through bacterial cellulose membranes was observed after heterogeneous esterification. The bacterial cellulose membranes prepared are a good and interesting example of the development of bio-based materials with promising applications in the packaging industry.     

Synthesis of bacterial cellulose nitrates

Russian Chemical Bulletin - The conceptual possibility to synthesize bacterial cellulose nitrates with the use of commercial mixed acid was demonstrated. The initial bacterial cellulose was...     

Preparation and properties of photochromic bacterial cellulose nanofibrous membranes

The photochromic bacterial cellulose (BC) nanofibrous membranes containing 1′,3′,3′-trimethyl-6-nitrospiro(2H-1-benzopyran-2,2′-indoline) (NO₂SP) were successfully prepared by surface modification of BC nanofibers with spiropyran photochromes, and their physical and photochromic properties were characterized. The FTIR spectra indicated the interaction between BC and NO₂SP which leads to the uniform dispersion of NO₂SP in the nanofibrous membrane. SEM results demonstrated that the introduction of NO₂SP maintains the nanofibrous network structure of BC. UV/vis spectrometry of the resulting BC-NO₂SP revealed that the membranes show reversible photochromic property by changing their color from colorless to pink forming a merocyanine structure upon UV irradiation, and returning back again to colorless spiropyran structure by visible light. The contact angle of the BC-NO₂SP with water was found to be reversibly regulated due to the reversible isomerization of the spiropyran moieties in BC-NO₂SP. The result indicates that the surface modification with spiropyran photochromes expands new applications of BC nanofibers and such photochromic nanofibers with excellent photosensitivity have great potentials for sensitive displays, biosensors and other optical devices.     

Controlled release of amoxicillin from bacterial cellulose membranes

Bacterial cellulose (BC), a natural polymer with unique physical and mechanical properties, has several applications in the biomedical field, including drug loading and controlled drug delivery. For this study, a Box-Behnken experimental design was employed as a statistical tool to optimize the release of a model drug, amoxicillin, from BC membranes. Independent variables studied were the concentration of the drug (X₁), the concentration of glycerol (X₂) and the concentration of a permeation enhancer (X₃). From the variables studied, drug concentration had the highest effect on drug release. Among the other independent variables, th linear and quadratic X₂ terms, the linear X₃ term and the interaction term X₂X₃ were found to affect the release of amoxicillin from bacterial cellulose membranes.

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Preparation,thermal characterization,and DFT study of the bacterial cellulose

A bifunctional comonomer 3-aminocarbonyl-3-butenoic acid methyl ester (ABM) was designed and synthesized to prepare poly(acrylonitrile-co-3-aminocarbonyl-3-butenoic acid methyl ester) [P(AN-co-ABM)] copolymer which can be used as carbon fiber precursor instead of poly(acrylonitrile–acrylamide–methyl acrylate) [P(AN–AM–MA)] terpolymer. The stabilization mechanism and structural evolution of P(AN-co-ABM) and P(AN–AM–MA) during stabilization were studied by Fourier transform infrared spectroscopy, X-ray diffraction, differential scanning calorimetry, and thermogravimetry. The activation energy (E _a) of the cyclization reactions was calculated by Kissinger method and Ozawa method. The results show that the stabilization of P(AN-co-ABM) has been remarkably improved by ABM compared with P(AN–AM–MA) terpolymer, such as lower initiation temperature, broadened exothermic peak, larger extent of stabilization, and smaller E _a of cyclization, which is attributed to the initiation of ABM through ionic mechanism. Moreover, the spinnability of P(AN-co-ABM) is also improved by ABM due to the lubrication of ester groups in ABM. This study clearly shows that P(AN-co-ABM) copolymer is a better material used as carbon fiber precursor than P(AN–AM–MA) terpolymer.     

Synthesis and characterization of cellulose resins

A series of cellulose-phenol-formaldehyde (LCPF) and cellulose-urea-formaldehyde (CUF) resins were produced using banana waste. Detailed structure and quantitative information was provided by FT-IR and mass spectroscopy. The main interests were the ability to use banana waste as a source of cellulose in the condensation reaction. Functionality of CPF and structure of CUF were investigated. Copyright © 2003 John Wiley & Sons, Ltd.     

Synthesis and characterization of oxidized cellulose

Samples of oxidized cellulose (OC) with various carboxyl contents and degrees of crystallinity were obtained by the oxidation of native and mercerized cellulose with a solution of nitrogen(IV) oxide in CCl₄. A detailed characterization of these OC samples was performed. The effect of oxidation conditions (concentration of N₂O₄ in the solution and oxidation time) and starting cellulose material on OC characteristics (carboxyl, carbonyl and nitrogen content, degree of crystallinity and polymerization, surface area and swelling, and acidic properties) was investigated. Reactivity in the oxidation process was higher in mercerized cellulose than in native cellulose. The action of dilute solutions (10–15%) of N₂O₄ did not affect the degree of crystallinity of cellulose samples. Under these conditions, the oxidation took place mainly in amorphous regions and on the surface of crystallites. Oxidation in a concentrated (40%) N₂O₄ solution led to the destruction of crystallites, which increased the surface area and swelling of cellulose in water. The surface area and the swelling of OC samples increased with a decrease in the index of crystallinity. The acidic properties of OC were shown to increase with an increase of swelling in water. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 4785–4791, 2004     

Synthesis of mesoporous titania networks consisting of anatase nanowires by templating of bacterial cellulose membranes

Mesoporous titania networks consisting of interconnected anatase nanowires have been synthesized by using unique bacterial cellulose membranes as natural biotemplates; the titania networks exhibit enhanced photocatalytic activity compared with titania microfiber networks.     

Characterization of magnetic membranes based on bacterial and man-made cellulose

Ferrites were synthetized in situ in two different neutral cellulose gels: a never-dried bacterial cellulose membrane and a never-dried cast film using N-methylmorpholine-N-oxide as solvent. X-ray diffraction, transmission electron microscope (TEM), vibrating sample magnetometry (VSM) and Mossbauer spectroscopy were used to characterize the resulting magnetic nanocomposites. TEM micrographs showed the presence of ferrites in two different shapes, acicular and equiaxial, respectively hydrated ferric oxides (FeOOH) and the spinel oxides: maghemite (gamma-Fe2O3) or magnetite (Fe3O4). Thin sections of bacterial cellulose showed these particles to be located along the cellulose microfibrils, which are assumed to provide a site for their nucleation. Room temperature magnetization curves showed all samples to be superparamagnetic     

Synthesis and screening of peptoid arrays on cellulose membranes

Rapid synthesis and screening of compound libraries enables the accelerated identification of novel protein ligands in order to support processes like analysis of protein interactions, drug target discovery or lead structure discovery. SPOT synthesis—a well established method for the rapid preparation of peptide arrays—has recently been extended to the field of nonpeptides. In this contribution we report on the systematic evaluation of the SPOT technique for the assembly of N-alkylglycine (peptoid) library arrays. In the course of this investigation bromoacetic acid 2,4-dinitrophenylester (1a) was identified to be the most suited agent for bromoacetylation in terms of yield and N-selectivity enabling straightforward submonomer synthesis on hydroxy-group rich cellulose membranes. The potential of this method for the rapid identification of novel nonpeptidic protein ligands was demonstrated by synthesis and screening of a library consisting of 8000 peptoids and peptomers (i.e. their hybrids with α-substituted amino acids) allowing the identification of micromolar ligands for the monoclonal antibody Tab-2.     

Synthesis and characterization of cellulose acetate from cellophane industry residues. Application as acetaminophen controlled-release membranes

Journal of Thermal Analysis and Calorimetry - Cellophane film production generates cellulosic residues from scraps, edges, and low-quality films. In this work, cellophane was used as a raw material...     

Preparation and characterization of the bacterial cellulose/polyurethane nanocomposites

New nanocomposites based on bacterial cellulose nanofibers (BCN) and polyurethane (PU) prepolymer were prepared and characterized by SEM, FT-IR, XRD, and TG/DTG analyses. An improvement of the interface reaction between the BCN and the PU prepolymer was obtained by a solvent exchange process. FT-IR results showed the main urethane band at 2,270 cm^?1 to PU prepolymer; however, in nanocomposites new bands appear as disubstituted urea at 1,650 and 1,550 cm^?1. In addition, the observed decrease in the intensity of the hydroxyl band (3,500 cm^?1) suggests an interaction between BCN hydroxyls and NCO-free groups. The nanocomposites presented a non-crystalline character, significant thermal stability (up to 230 °C) and low water absorption when compared to pristine BCN.     

Synthesis and characterization of novel amino cellulose esters

The homogeneous conversion of cellulose dissolved in N-methyl-2-pyrrolidone/LiCl and 1-N-butyl-3-methylimidazolium chloride with N-methyl-2-pyrrolidone, ε-caprolactam, N-methyl-ε-caprolactam, and N-methyl-2-piperidone in the presence of p-toluenesulphonic acid chloride was studied. Depending on the reaction conditions, novel cellulose esters with degree of substitution (DS) values ranging from 0.12 to 1.17 could be prepared. The structure of the amino group containing cellulose esters was elucidated by elemental analysis, FTIR- and NMR spectroscopy. NMR spectroscopy revealed an almost complete esterification of position 6 of the anhydroglucose unit at DS of 1. The conversion can be conducted between room temperature and 40 °C, while side-reactions became predominant at 60 °C. Starting with DS of 0.24, the samples were soluble both in water and dimethyl sulphoxide. The derivatives described are capable of forming polyelectrolyte complexes. The samples were stable at room temperature in aqueous solution at pH 2 and 7. Lower viscosities were found for samples with higher DS in aqueous solution at comparable molar mass.     

Synthesis and characterization of carboxylate waterborne cellulose emulsion based on cellulose acetate

With cellulose acetate (CA) as a base material, a novel environmentally friendly carboxylate waterborne cellulose acetate (CWCA) emulsion was synthesized via the method of self-emulsification. Taking advantage of acrylic acid, hydroxyethyl acrylate as a modifier, and isophorone diisocyanate as a bridging agent, the molecular structural design of CWCA dispersion was completed successfully, and the structure was confirmed by Fourier transform infrared spectroscopy (FTIR). In this work, the particle size and distribution of the stable CWCA dispersion with solid content of 22.6% are 115.6 and 0.158 nm, respectively. It was found that the microstructure of emulsion particles is a core-shell structure containing a hydrophilic carboxylate group as the shell and hydrophobic cellulose acetate molecular as the core. In addition, the hydrophobic behavior of CWCA film is presented as a contact angle of 109.9°. Furthermore, CWCA film provided a higher thermal decomposition temperature of 345.42 °C than that of CA film at the largest mass loss rate.     

Surface characterization of TEMPO‐oxidized bacterial cellulose

In this study, we focused on the surface character of bacterial cellulose (BC) before and after oxidation mediated by 2,2,6,6‐tetramethylpiperidine‐1‐oxyl (TEMPO).Solid‐state ¹³C NMR, XPS, SEM, contact angle and surface free energy analyses were performed to investigate the effects of various parameters (reaction time and oxidant and catalyst concentrations) on the surface composition, morphology and polarity of the BC. The results provided by the combined use of these techniques showed that hydrogen bonds were disrupted on the BC surface after carboxylation occurred; therefore, the surface of oxidized BC was rougher than that of the original BC, and the surface free energy, especially the polar components, increased after oxidation. Copyright © 2013 John Wiley & Sons, Ltd.