Bioglycerol-Based Sulfonic Acid-Functionalized Carbon Catalyst as an Efficient and Reusable Catalyst for One-Pot Synthesis of 3- Substituted-2H-1,4-Benzothiazines

Abstract

A simple and efficient synthetic protocol has been developed for the synthesis of 3-substituted-2H-1,4-benzothiazines by using bioglycerol-based sulfonic acid-functionalized carbon catalyst, devoid of corrosive acidic and basic reagents. The developed method has the advantages of good to excellent yields, short reaction times, operational simplicity, and a recyclable catalyst.     

Preparation of polyaniline grafted multiwalled carbon nanotubes and conductive application in polyetherimide

A methodology for improving antistatic property of polyetherimide (PEI) composite using polyaniline (PANI) grafted multi‐walled carbon nanotubes (MWNTs) as conductive medium was proposed. First, the MWNTs grafted with PANI (PANI‐g‐MWNTs) were prepared by in‐situ polymerization in an emulsion system. Subsequently, PANI‐g‐MWNTs were blended with PEI using N‐methyl‐2‐pyrrolidone as solvent. After removing the solvent, the PEI/PANI‐g‐MWNT composite was prepared. As assisted conductive medium, the grafted PANI molecular chains on MWNT surface were dispersed in the PEI matrix to decrease the percolation value of the antistatic composites. The structure and morphology of PANI‐g‐MWNTs were characterized by Fourier transform infrared spectroscopy, transmission electron microscope, thermogravimetric analysis, and X‐ray powder diffraction, respectively. The dispersion of PANI‐g‐MWNTs in PEI matrix was studied by scanning electron microscope. The electrical performance was characterized by highly resistant meter. The volume resistivity of the conductivity percolation threshold was 1.781 × 10^?8 S/cm when the loading of PANI‐g‐MWNTs was 1.0 wt%. The conductivity of PANI‐g‐MWNTs/PEI composites was found to be higher than that of pristine MWNTs/PEI composite. Copyright © 2012 John Wiley & Sons, Ltd.     

Structure-Property Dependence of Copolymers Prepared by Cationic Polymerization

α-Methylstyrene/isobutene, α-methylstyrene/diisobutene, cyclopentadiene/isobutene, and cyclopentadiene/α-methylstyrene were copolymerized by cationic polymerization techniques. Several properties of the copolymers such as softening ranges and oxidation stability depend on their constitutional composition, and were controlled by variation of the conditions of their synthesis.     

Preparation and Antibacterial Function of Quaternary Ammonium Salts Grafted Cellulose Fiber Initiated by Fe2 +-H2O2 Redox

The surface contact disinfecting technique is a newly developed method for water sterilization. In this paper, the grafted quaternary ammonium salts (QAS) antibacterial fibers were prepared and designed to apply for the surface contact disinfecting process in water treatment. The antibacterial fibers were directly prepared by grafting methacryloxylethyl benzyl dimethyl ammonium chloride (DMAE-BC) onto cellulose fiber using thiocarbonate-H₂O₂ redox system. All kinds of factors in the grafting reactions, such as reaction time, reaction temperature, monomer concentration, initiator concentration, which influence the percentage of grafting, were studied and optimized. The modified cellulose fibers were characterized by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscope(SEM). The effects of the percentage of grafting of the grafted cellulose fibers on bactericidal activity were also studied. The spread plate method was used to characterize the bactericidal activity. The disinfection process was further investigated by directly observing the morphology of the bacterial cells adsorbed on the antibacterial fibers with SEM and measuring extracelluar total protein concentration in suspension. The poly(DMAE-BC)-grafted cellulose ?ber was found to exhibit particularly high activity against E.coli.     

Anti‐static Agent Containing Zinc Oxide and its Modification for PA6 Fiber

A new anti‐static agent was synthesized from zinc oxide‐adipic acid‐polyethylene glycol and caprolactam by three‐step reactions. The antistatic agent (called poly(ether ester amide zinc oxide) or PEEAZ) was analyzed by IR and DSC. The results showed that zinc oxide existed in the main chain of PEEAZ. The glass temperature and melt temperature of poly(ether ester amide zinc oxide) (referred to as PEEAZ in the following) decreased with increasing poly(ether ester zinc oxide) increasing in PEEAZ. Antistatic PA6 fiber was obtained by adding PEEAZ 2–8% (wt/wt) to PA6 during blend spinning. The specific resistance and the static half‐value period of PA6 fiber was less than 10⁹Ω · cm and 60 sec, respectively. Excellent antistatic property remained after being washed 30 times.     

Study on Dyeing Properties of Functional Acrylic Fiber

Anti‐mite acrylic fiber is a new type of functional fiber which incorporates a small amount of anti‐mite agent. Basic dye can be used in the dyeing of the functional acrylic fiber. Compared with the dyeing properties of conventional fibers, the dyeing properties of the functional acrylic fiber have new characteristics such as different dyeing temperature, time, amount of leveling agent and pH level due to the rough surface and larger size of micro‐channels in the functional fiber structure that helps basic dye molecules to diffuse into the fiber.     

A Preliminary Study on Preparation of the Aromatic/Aliphatic Co‐polyurea as Spun Fibers

Aromatic‐aliphatic co‐polyurea has been synthesized from 4,4 prime‐diphenylmethane diisocyanate (MDI), m‐phenylene diamine (m‐PDA), and 1,6‐diaminohexane (HDA) in DMAc by solution polymerization. The chemical structure of the co‐polyurea has been characterized by ¹H‐NMR. The thermal properties of the copolymers were measured by DSC and TGA. The co‐polyurea solutions were spun into fibers by means of wet spinning. The effects of coagulation conditions on the morphologies and mechanical properties of the co‐polyurea as spun fibers are discussed.     

Diffusion Mechanism of As‐spun Polyacrylonitrile Fiber in a Dimethyl Sulfoxide‐Water Coagulation Bath

In this paper, the diffusion mechanism of as‐spun PAN fiber was investigated in dimethyl sulfoxide‐water by determining the dynamic compositions of the fibers and the diffusion coefficients of solvent and nonsolvent during coagulation. The diffusion process could be divided into two stages. Results showed that the first stage of the diffusion process was the most important during the whole process, which was fundamental to further study on the formation mechanism. Also, compared with wet spinning, the dry‐jet wet spinning method had the advantage of mild coagulating at a high jet‐stretch. At high concentrations, the diffusion coefficients increased and the ratio of solvent diffusion coefficient to nonsolvent diffusion coefficient decreased; an increasing temperature resulted in the increase of both diffusion coefficients with a decrease in their ratios. To some extent, for the PAN‐DMSO‐water system, the more the ratios D_s*/D_n* tended to 1, the more the cross‐section shapes of as‐spun PAN fiber tended to be circular.     

Effects of Ultra-sonification Assisting Polyethylene Glycol Pre-treatment on the Crystallinity and Accessibility of Cellulose Fiber

In order to prepare the advanced cellulosic super-absorbent polymer with high grafting level, we tried the novel ultrasound wave assisting polyethylene glycol (PEG) pre-treatment method to decrease the crystallinity and increase the accessibility of cellulose fiber. The effects of ultrasonification assisting PEG method on the crystallinity and swelling capacity of cellulose fiber were investigated. To optimize the experimental condition, the Taguchi method was employed in the treatment process. The influence factors such as ultrasonic wave power, ultrasonic wave time and PEG molecular weight relative to the crystallinity of cellulose fiber were studied systematically. The degree of crystallinity of cellulose fiber was measured by wide-angle X-ray diffraction (WAXD). The morphology of cellulose fiber was observed by environment scanning electron microscopy (ESEM). The effects of pre-treatment variables on the water absorbency and water retention values of cellulose fiber were also investigated. The research results revealed that, under the optimal experimental condition (ultrasonic powder, 500 W; ultrasonic time, 150 s; PEG molecular weight, 600 g/mol), the crystallinity of cellulose fiber decreased from 72.16 to 42.95%. Accordingly, the absorbency of cellulose fiber increased from 1.436 to 2.063 g/g, and the water retention value increased from 47.21 to 113.4%. However, the morphology of cellulose fiber did not change thoroughly compared with the original cellulose fiber. It can be hypothesized that the original inter- and intra-macromolecular hydrogen bonds in cellulose network were weakened, resulting from the high level dispersion of PEG within cellulose network without breaking the surface morphology of fiber.     

Effect of Polycondensation Reaction Conditions on the Properties of Thermotropic Liquid‐Crystalline Copolyester

In this study a range of wholly aromatic copolyesters based on kink m‐acetoxybenzoic acid (m‐ABA) monomer (33 mol%) and equimolar‐linear p‐acetoxybenzoic acid (p‐ABA), hydroquinone diacetate (HQDA) and terephthalic acid (TPA) monomers (67 mol%) have been synthesized by melt polycondensation reaction process at 280°C and 260°C for different time intervals. Characterization of copolyesters were performed by solution viscosity measurement, wide–angle X‐ray diffraction (WAXD), differential scanning calorimetry (DSC), hot‐stage polarized light microscopy, proton‐nuclear magnetic resonance analysis (¹H‐NMR). According to the results obtained, copolyesters showed thermotropic liquid crystalline behavior in an appropriate temperature range. The copolyesters were prepared in high yields. It was observed that the intrinsic viscosities of the copolyesters are increased regularly with increasing polymerization time and temperature. All the copolyesters were soluble in a trifluoroacetic acid/dichloromethane (30:70 v/v) except the copolyesters which were synthesized at 280°C in 5 h. According to the WAXD results; the degree of crystallinity of copolyesters were found to be between 5–15%. DSC and hot stage polarized light microscopy results showed that all the copolyesters are melt processable and a significant molecular interaction exist in a very broad temperature range (160°C and 165°C) in the nematic mesophase. The T_g values are increased with an increasing polycondensation reaction time and temperature and they were observed between 93–126°C. Fibers prepared by a hand‐spinning technique from the polymer melt exhibit well‐developed fibrillar structure parallel to the fiber axis.