Investigation on degradation and stability of oxidized regenerated cellulose

The selective oxidation of nitrogen dioxide in CCl₄ for regenerated cellulose to C6 oxidized regenerated cellulose (ORC) was proved using FTIR and NMR, and the ORC were dried under three different conditions, including vacuum-dried at high temperature, air-dried at room temperature and frozen-dried at low temperature. The degrees of polymerization (DP) of ORC gradually decreased with the increase of the oxidation time, which was probably due to the decarboxylation reaction. The DP of ORC further decreased and the color became deep as the increase of drying temperature, which was probably due to the ??-elimination reaction from C2 or C3-carbonyl group, and the yellow color of ORC was due to chromophoric enol structure. The final DP was determined by two kinds of degradation process based on the oxidation of C6 and little C2 or C3, respectively.     

Evaluation of the dyeability of the new eco-friendly regenerated cellulose

Three commercial dyes-direct, reactive, and vat dye-were applied to the new regenerated cellulose fiber which was prepared from cellulose acetate fiber through the hydrolysis of acetyl groups with an environmentally friendly manufacturing process. The effect of salt, alkali, liquor ratio, temperature, and leveling agent on the dyeing behavior and fastness were evaluated and compared with regular viscose rayon. From the results, we found that new regenerated cellulose fiber exhibited better dyeability and fastness than regular viscose rayon.     

Preparation,functional characterization and hemostatic mechanism discussion for oxidized microcrystalline cellulose and its composites

Effective and affordable hemostatic materials are of great interests in the development of biomaterials. Lignocellulose, which is a raw material for microcrystalline cellulose, is one of the most economical and readily available polymers in the nature. The oxidized microcrystalline cellulose particles prepared in NO₂/CCl₄ oxidation system may be a type of affordable, effective and nontoxic hemostatic biomaterial. The FT-IR and ¹³C solid state NMR results showed that the hydroxyl groups on C6 of cellulose were highly selectively oxidized. The increase of carboxyl content and Zeta potential of OMCC were highly dependent on the oxidation time at the first 64 h. XRD spectra indicated that the crystallinity changed from 70.01 % (MCC) to 60.63 % (OMCC-96 h), and the particle size decreased to 80 µm (OMCC-96 h). To composite with oxidized regenerated cellulose gauze, the OMCC-64 h was optimal, based on the dramatically reduced DP value after 64 h oxidization. The results showed this novel composite with negative charge exhibited good hemostatic property and antibacterial activity. The composite was possessed of both the good biocompatibility for mouse endothelial cells in vitro and the superior biodegradation for rabbits in vivo. Moreover, the data of enzyme-linked immunosorbent assay and blood coagulation tests in vitro suggested that the composite could adsorb and activate the platelets, and then the platelet glycoprotein (GPIIb/IIIa) receptor became competent to bind soluble fibrinogen. The composite also greatly accelerated the activation of the blood coagulation factor XII, and promoted the generation of thrombin, so that the extrinsic route of blood coagulation was initiated.     

Synthesis of non-water soluble polymeric guanidine derivatives and application in preparation of antimicrobial regenerated cellulose

In order to prepare antimicrobial regenerated cellulose fibers from blended spinning solutions, three non-water soluble polymeric guanidine derivatives, polyhexamethylene guanidine dodecyl benzene sulfonate (PHGDBS), polyhexamethylene guanidine dodecyl sulfate (PHGDSA), and polyhexamethylene guanidine laurylsulfonate (PHGLSO) were synthesized. And the chemical structure of these agents was verified by element analysis, Fourier transform infrared spectroscopy (FTIR), and proton nuclear magnetic resonance (¹H-NMR). The antimicrobial activity of the three agents as well as cellulose films containing PHGDBS was also studied. The results showed that the compounds we prepared had strong properties against both bacterial and fungus, including Staphylococcus aureus (S. aureus), Escherichia coli (E. coli), Candida albicans, and Aspergillus niger. Moreover, it was found that three antimicrobial agents were insoluble in water but they can dissolve in solvents of cellulose such as 1-butyl-3-methylimidazolium chloride ([BMIM]Cl) and N-methylmorpholine-N-oxide monohydrate (NMMO·H₂O). Meanwhile, it was also proved that [BMIM]Cl had little effect on the antimicrobial properties of these agents. The cellulose films containing only 1.0 wt% PHGDBS showed 99.94 % and 96.95 % bacterial reduction rates for S. aureus and E. coli, respectively. Moreover, still over 91 % of bacterial reduction was maintained after 15 laundering cycles. It suggests that the three agents will be suitable to prepare antimicrobial regenerated cellulose fibers or films.     

Preparation of regenerated cellulose fiber via carbonation. I. Carbonation and dissolution in an aqueous NaOH solution

Cellulose carbonate was prepared by the reaction of cellulose pulp and CO₂ with treatment reagents, such as aqueous ZnCl₂ (20–40 wt%) solution, acetone or ethyl acetate, at −5–0°C and 30–40 bar (CO₂) for 2 hr. Among the treatment reagents, ethyl acetate was the most effective. Cellulose carbonate was dissolved in 10% sodium hydroxide solution containing zinc oxide up to 3 wt% at −5–0°C. Intrinsic viscosities of raw cellulose and cellulose carbonate were measured with an Ubbelohde viscometer using 0.5 M cupriethylenediamine hydroxide (cuen) as a solvent at 20°C according to ASTM D1795 method. The molecular weight of cellulose was rarely changed by carbonation. Solubility of cellulose carbonate was tested by optical microscopic observation, UV absorbance and viscosity measurement. Phase diagram of cellulose carbonate was obtained by combining the results of solubility evaluation. Maximum concentration of cellulose carbonate for soluble zone was increased with increasing zinc oxide content. Cellulose carbonate solution in good soluble zone was transparent and showed the lowest absorbance and the highest viscosity. The cellulose carbonate and its solution were stable in refrigerator (−5°C and atmospheric pressure).     

Influence of residual ionic liquid on the thermal stability and electromechanical behavior of cellulose regenerated from 1-ethyl-3-methylimidazolium acetate

The regenerated cellulose films were prepared by dissolving cotton cellulose pulp directly in room temperature ionic liquid namely, 1-ethyl-3-methylimidazolium acetate at 80 °C, followed by washing/curing in different coagulants namely, methanol, deionized water, methanol-deionized water, and isopropyl alcohol-deionized water. It was found that the type of coagulants employed for curing the cellulose films has a significant influence on the amount of residual ionic liquid entrapped in the films. The amount of residual ionic liquids was 2.68, 1.01, 0.84, and 0.75 wt.% for the films cured with deionized water, isopropyl alcohol-deionized water, methanol, and methanol-deionized water, respectively. The DTG peaks of regenerated cellulose films showed two decomposition temperatures at 280 °C and 320 °C. Among all the cases studied, deionized water curing case showed the lowest decomposition temperature, attributed to entrapment of large residual ionic liquid in it. Electromechanical characteristic of the regenerated cellulose films was also investigated.     

Effect of degree of polymerization on the mechanical properties of regenerated cellulose fibers using synthesized 1-allyl-3-methylimidazolium chloride

1-Ally-3-methylimidazolium chloride ([AMIM]Cl) was successfully synthesized and was used as a green spinning solvent for cellulose. The celluloses of various degrees of polymerization (DP) were dissolved in the [AMIM]Cl to obtain 5 % (w/w) cellulose solutions, which were regenerated to cellulose fibers through wet spinning process. Of three different regenerated cellulose fibers with different DPs, a DP of 2,730 was gave the strongest regenerated fiber without drawing having a tensile strength of 177 MPa and an elongation at break of 9.6 % respectively, indicating that celluloses of higher molecular weight can be entangled and oriented more easily. Also maximum draw ratio of the as-spun fibers increased from 1.2 to 1.7 with increasing degree of polymerization leading to a tensile strength and modulus of 207 MPa and 48 GPa, respectively. Particularly the tensile modulus was substantially higher than those of lyocell and high performance viscose fibers of 20 GPa or less. The higher DP of pristine cellulose was critical in increasing the mechanical properties such as tensile strength and elongation at break of the as-spun fibers coupled with higher tensile modulus after drawing.     

Production and performance analysis of an antibacterial foot sweat pad

An antibacterial foot sweat pad was designed and produced by using materials of standard disposable absorbent hygienic products. Topsheet layer of the pad was modified by two volatile oils; cinnamaldehyde and geraniol and a standard zinc-based synthetic antibacterial agent. Physical properties of the sweat pad was arranged according to the sweat disposal amount and dimensions of a foot. Besides antibacterial performance of the topsheet layer of the pad, surface characteristics (friction test), bending rigidity of the modified topsheet layer, liquid absorption and transfer characteristics of the pad were also investigated. Subjective forearm test was conducted to determine effects of antibacterial coating materials on coolness and dampness to touch sensations created by the pads in dry and wet forms. According to the results, cinnamaldehyde created maximum antibacterial activity, which is better than the commonly used synthetic agent, on topsheet layer of the pads and geraniol had an acceptable performance. But cinnamaldehyde treated topsheet fabric became stiffer, rougher and its liquid absorption characteristics deteriorated significantly. Zinc-based synthetic antibacterial agent created higher coolness and dampness sensations during skin contact according to forearm test results.     

Deodorizing and antibacterial performance of cotton, silk and wool fabrics dyed with Punica granatum L. extracts

Natural dye extracts were obtained by extraction from Punica granatum L. using water as an extractant at 90 °C for 90 min with various liquor ratios (solid Punica granatum L.(wt.): solvent water(wt.); 1:100–1:5). Dyeing was carried out using a 1:50 dyeing bath ratio at 80 °C for 60 min by exhaustion method. This study focused on the effect of liquor ratio on dyeing properties and deodorizing/antibacterial performance of various fabrics (cotton, silk and wool) dyed with Punica granatum L. extract without mordants. The optimum liquor ratio was found to be 1:10. By IR, UV-visible spectroscopies and HPLC analysis, the main component in Punica granatum L. extract and the yellow colorant component were found to be ellagic acid. By GC/MS analysis, the major volatile components of pristine Punica granatum L. powder were found to be acetic acid (area: 25.84 %), ethanol (area: 17.97 %), acetoin (area: 13.11 %), acetaldehyde (area: 8.96 %), isobutanal (area: 4.90 %). All dyed fabrics (cotton, silk and wool fabrics) displayed outstanding deodorizing performance (99 %) against ammonia gas and excellent antibacterial performance (bacteriostatic reduction rate: 99.9 %) against Staphylococcu aureus and Klebsiella pneumoniae.     

TEMPO-mediated oxidation of microcrystalline cellulose: Influence of temperature and oxidation procedure on yields of water-soluble products and crystal structures of water-insoluble residues

A series of microcrystalline cellulose samples were reacted with catalytic amounts of 2, 2, 6, 6-tetramethyl-1-piperidine oxoammonium salt (TEMPO), sodium hypochlorite and sodium bromide in Na₂CO₃/NaHCO₃ buffer solution at different temperature (15 °C, 20 °C, 30 °C, 35 °C, 40 °C, 50 °C). The oxidation procedures included first and second oxidation. The first oxidation was a classical process for activating cellulose for the second oxidation. A substantial increase in the reactivity of the second oxidation cellulose samples was observed in comparison to those in the first oxidation and a relationship between oxidation procedures and accessibility of cellulose primary hydroxyl groups was directly established. For the characterization, we have used several methods, mainly XRD, FTIR. In all samples, the partial primary alcohol groups were selectively oxidized into carboxyl groups. The reaction during the first oxidation procedure mainly occurs in disordered regions of MCC and crystal surface. But the second oxidation procedure took place not only in disordered regions and crystal surface but inside crystalline region of cellulose I.     

Manufacture and performance of O-carboxymethyl chitosan sodium salt/cellulose fibers in N-methylmorpholine-N-oxide system

A series of O-carboxymethyl chitosan sodium salt (NaCMCh) with different degree of substitution (DS) of -CH₂COONa agent were successfully prepared by altering the reaction temperature and time. Both fourier transform infrared spectroscopy (FTIR) and ¹³C-Nuclear Magnetic Resonance (¹³C-NMR) were used to study the structure of NaCMCh. And the impact of DS on the antibacterial activity of NaCMCh was investigated. Then, the NaCMCh with optimal antibacterial activity was selected to prepare NaCMCh/cellulose fibers in N-methylmorpholine-N-oxide (NMMO) system. The structure, crystallization behavior, thermal property and morphology of obtained fibers were carefully studied with FTIR, Wide-angle X-ray diffraction (WAXD), differential scanning calorimetry (DSC), thermal gravimetric (TG) and scanning electron microscope (SEM), respectively. Meanwhile, the antibacterial activity as well as mechanical properties of resultant fibers was also investigated. The results demonstrated that the fibers had strong antibacterial activity against Escherichia coli (E. coli), acceptable mechanical properties and good water retention.     

Dyeing performance of disperse dyes based on 2-aminothiazole for cellulose triacetate and nylon fibers

A series of monoazo disperse dyes based on 2-amino-4-phenylthiazole was prepared using variousN,N-dialkylaniline derivatives as the coupling component. The dyes were characterized by IR spectral studies, visible absorption spectroscopy and elemental analysis. The dyeing performance of these dyes was assessed on cellulose triacetate and nylon fibers. These dyes were found to give a wide range of colour shades varying from bright red to royal blue with very good depth, brightness and levelness on fibers. The dyed fibers showed good to very good light fastness and very good to excellent fastness to washing, perspiration, rubbing and sublimation. The dyebath exhaustion and fixation on the fibers were found to be very good.     

Macro-micro structure,antibacterial activity,and physico-mechanical properties of the mulberry bast fibers

In this paper, the mulberry fibers were successfully obtained by a new pretreatment named alkali-assisted microwave plus biological enzymatic technique (AMBET). The morphology, microstructure, physico-mechanical and antibacterial properties of the mulberry bast fibers were investigated by means of scanning electron microscope (SEM), Fourier Transform-Infrared (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray diffraction (XRD), instron tensile tester and antibacterial testing. The results showed that impurities of the bast fibers could be removed by AMBET treatment. AMBET treated mulberry fiber was even, smooth and fine, and typical cellulose I in the mulberry fibers was confirmed by FTIR and XRD analysis. The crystallinity of the AMBET treated fibers was higher than that of the raw mulberry and chemical treated mulberry fibers. Thermal analysis indicated that the mulberry fibers had a good thermal stability. Moreover, the AMBET treated mulberry fibers showed excellent antimicrobial activities against S.aureus. The physical properties of the mulberry fibers indicated the AMBET treated mulberry fibers were ideal candidates for new textile materials.     

Application of silver nanoparticles as an antibacterial mordant in wool natural dyeing: Synthesis,antibacterial activity,and color characteristics

Madder is a natural colorant which is commonly applied with metal salts as a mordant to improve its affinity to fibers and color fastness. Madder produces an insoluble complex or lake in the presence of metal ions on mordanted fabric. In this study, wool fabric was pretreated with AgNPs (silver nanoparticles) as a mordant, then dyed with madder. The wool fabric samples were examined by scanning electron microscopy (SEM) and their colorimetric characteristics were evaluated. The formation of spherical silver nanoparticle was confirmed using UV-Visible spectroscopy, SEM images, and elemental analysis. The average size of synthesized silver nanoparticles on the surface of wool fibers is around 73 nm. The dyed wool samples were pretreated with different concentration of Ag⁺ ions or AgNPs, which showed higher color strength value compared to untreated dyed wool fabric. This pretreatment also presented good antibacterial activity.     

Fast separation and characterization of water-soluble proteins in wheat grains by reversed-phase ultra performance liquid chromatography (RP-UPLC)

Water-soluble proteins account for about 10% of total grain proteins in wheat (Triticum aestivum L.) and have specific functions in plant growth and development. In this study, a reversed-phase ultra performance liquid chromatography (RP-UPLC) method was trialed and the experimental conditions were optimized for rapidly separating and characterizing water-soluble proteins in wheat grains, and a comparative analysis with traditional RP-HPLC was performed. Under optimized separation conditions, fast, high resolution and reproducible RP-UPLC separation for water-soluble proteins could be obtained by gradually increasing eluting gradient from 21% to 47% in 30 min at 0.6 ml/min and 60 °C. Using this method, separation and characterization of water-soluble protein in wheat grains could be completed in less than 20 min for one sample, and the resolution and efficiency were significantly higher than those obtained with RP-HPLC. In addition, RP-UPLC consumed smaller amounts of samples and reagents as well. The optimized RP-UPLC could be used as an effective and alternative method for rapid separation and characterization of water-soluble proteins in wheat cultivar and germplasm evaluation, genetic and biochemical studies on grain proteins, and environmental influence analysis of water-soluble proteins.     

Antioxidant, antibacterial, and antiviral effects of Lactuca sativa extracts

Antioxidant, antibacterial and antiviral effects of aqueous and methanol extracts of Lactuca sativa var longifolia leaves were investigated. The antioxidant activity was evaluated using the DPPH assay. The effect of the extracts against 5 Gram-positive and 6 Gram-negative bacteria was tested. The antiviral activity was determined against human cytomegalovirus (HCMV) strain AD-169 (ATCC Ref. VR 538) and coxsackie B virus type 3 (CoxB-3) using a cytopathic effect (CPE) reduction assay. The methanol extract had the highest total phenolic contents (235.31 mg CE/g extract). It exhibited a significantly (p < 0.05) greater hydroxyl radical-scavenging activity (IC₅₀ = 3.5 μg/ml) than the aqueous extract (4.1 μg/ml). It was also the most effective extract with the lowest MIC (2.5 mg/ml) against all Gram negative and Gram positive bacteria. Methanol and aqueous extracts exhibited antiviral activity against HCMV and Cox-B3 viruses with IC₅₀ of 200 μg/ml.     

Miscibility, structural characteristics, and thermal behavior of wet spun regenerated silk fibroin/nylon 6 blend filaments

In this study, the regenerated silk fibroin (SF)/nylon 6 blend filaments were fabricated by the wet spinning and miscibility, structural characteristics, and thermal behavior of blend filaments were elucidated. The XRD results implied that the amount of crystalline region of each polymer did not change linearly with the blend ratio suggesting that there are some changes in the miscibility depending on the mixing ratio. The SEM observation revealed that the miscibility of blend decreased with an increase of nylon 6 resulting in a severe phase separation in 50/50 SF/nylon 6 filament. The miscibility governed the thermal behavior of blend filaments. The melting point of nylon 6 remained constant until 50 % nylon 6 content, whereas the melting point depression appeared in 30 % nylon 6 implying miscibility. Interestingly, the thermal decomposition of the nylon 6 component was accelerated by the presence of SF and the acceleration action of SF became stronger as the miscibility increased.     

Effects of Chitin and Sepia Ink Hybrid Hemostatic Sponge on the Blood Parameters of Mice

Chitin and sepia ink hybrid hemostatic sponge (CTSH sponge), a new biomedical material, was extensively studied for its beneficial biological properties of hemostasis and stimulation of healing. However, studies examining the safety of CTSH sponge in the blood system are lacking. This experiment aimed to examine whether CTSH sponge has negative effect on blood systems of mice, which were treated with a dosage of CTSH sponge (135 mg/kg) through a laparotomy. CTSH sponge was implanted into the abdominal subcutaneous and a laparotomy was used for blood sampling from abdominal aortic. Several kinds of blood parameters were detected at different time points, which were reflected by coagulation parameters including thrombin time (TT), prothrombin time (PT), activated partial thromboplatin time (APTT), fibrinogen (FIB) and platelet factor 4 (PF4); anticoagulation parameter including antithrombin III (AT-III); fibrinolytic parameters including plasminogen (PLG), fibrin degradation product (FDP) and D-dimer; hemorheology parameters including blood viscosity (BV) and plasma viscosity (PV). Results showed that CTSH sponge has no significant effect on the blood parameters of mice. The data suggested that CTSH sponge can be applied in the field of biomedical materials and has potential possibility to be developed into clinical drugs of hemostatic agents.     

粗纤维、透光率、pH值与乌龙茶品质关系初探

成品乌龙荣中的色、香、昧、形等品质因素的形成,是通过选择最佳嫩度的鲜叶,结合它的特殊制造工艺来实现的。鲜叶是茶叶品质的基础,做青时要求老微度适当,偏激或过于租者,咸菜品质都不好。人们通常是依靠感官审评来鉴定茶叶品质,本文拟通过测定菜叶粗纤维含量、茶汤的酸碱度及造光率,探讨它们与茶叶品质的关系。这对于开展菜叶的理化分析,减少人为审评误差且有现实意义。1材料与方法（1）主要测试仪器PHS－2型欧度计测定茶场的PH值;721型分光光度计（波长440微毫米）测定茶汤的透光率;用恒温干燥箱及分析天平测定茶叶粗纤维含量…     

Extraction, preparation and characterization of cellulose fibres and nanocrystals from rice husk

Cellulose fibres and cellulose nanocrystals were extracted from rice husk. Fibres were obtained by submitting the industrial rice crop to alkali (NaOH) and bleaching treatments. Nanocrystals were extracted from these fibres using sulphuric acid (H₂SO₄) hydrolysis treatment. The material obtained after each stage of the treatments was carefully characterized and its chemical composition was determined. Morphological investigation was performed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Fourier transform infrared (FTIR) spectroscopy showed the progressive removal of non-cellulosic constituents. X-ray diffraction (XRD) analysis revealed that the crystallinity increased with successive treatments. The thermal stability of the rice husk fibres and cellulose nanocrystals was also investigated using thermogravimetric analysis (TGA).