A quick and green ionic liquid-mediated approach for the synthesis of high-performance, organosoluble and thermally stable polyimides

Three diamine monomers with different derivatives of imidazole heterocyclic ring and meta-linked aryl ethers were synthesized and used in polycodensation reaction with various commercial dianhydrides for preparation of a series of novel poly(ether-imide) (PEI)s. The polycodensation reactions were carried out by using conventional method and in a green medium of ionic liquid (IL) without using NMP-pyridine-acetic anhydride. The PEIs were obtained in good yields (80% 96%) with moderate viscosity (0.48 0.66 dL/g) in a shorter reaction time (10 h) in IL as compared with the conventional method (36 h). All of the polymers were amorphous in nature, showed excellent solubility in amide-type polar aprotic solvents with ability to form tough and flexible films, and excellent thermal stability with Tgs in the range of 212 340 ℃ and 10% weight loss temperature (T10) up to 570℃ in N 2 and 528 ℃ in air.     

“Living” radical graft polymerization of styrene to styrene butadiene rubber (SBR) with 2,2,6,6‐tetramethyl‐1‐piperidinyloxy (TEMPO)

Well‐defined graft copolymers with styrene butadiene rubber (SBR) backbones and polystyrene branches were synthesized by living free radical polymerization (LFRP) techniques. Thus 1‐ benzoyl‐2‐phenyl‐2‐(2′,2′,6′,6′‐tetramethyl‐piperidinyl‐1′‐oxy)ethane (BZ‐TEMPO) was synthesized and hydrolyzed to the corresponding 1‐hydroxyl derivative. This functional nitroxyl compound was coupled with brominated SBR (SBR‐Br). The resulting macroinitiator (SBR‐TEMPO) for “living” free radical polymerization was then heated in the presence of styrene for the formation of the controlled graft copolymer. ¹H‐NMR and IR spectroscopy were used to investigate the structure of the polymers. Copyright © 2004 John Wiley & Sons, Ltd.     

Development of a new fluorimetric bulk optode membrane based on 2,5-thiophenylbis(5-tert-butyl-1,3-benzexazole) for nickel(II) ions

A highly sensitive and selective fluorimetric optode membrane for the determination of ultra trace amounts of Ni²⁺ ions was prepared. The plasticized PVC-membrane incorporating potassium tetrakis(p-chlorophenyl)borate (KTpClPB) and 2,5-thiophenylbis(5-tert-butyl-1,3-benzexazole) (TTBB), as a highly fluorescent chromoionophore, displays a calibration response for Ni²⁺ ions over a wide concentration range of 1.0×10⁻³ to 1.0×10⁻⁸ M. It has a relatively fast response of <40 s. In addition to high stability and reproducibility, and relatively long working lifetime, the sensor possesses good selectivity for nickel ions over several common diverse ions. The fluorescence signal of the optode membrane can be easily recovered by immersion in EDTA solution. The optode was applied successfully to the determination of traces of Ni²⁺ ion in edible oil and a wastewater sample from nickel electroplating industries.     

Spectrophotometric study of the complexation of iodine with 1,7-diaza-15-crown-5 in chloroform solution

The complex formation reaction between iodine and 1,7-diaza-15-crown-5 (DA15C5) has been studied spectrophotometrically in chloroform at 25°C. The resulting 1:2 (DA15C5:I₂) molecular complex was formulated as (DA15C5...;I⁺)I ₃ ^– . The spectrophotometric results, as well as the conductivity measurements, revealed that the gradual release of triiodide ion from its contact ion paired form in the molecular complex into the solution is the rate determining step of the reaction. The rate constant was calculated ask=(8.8±0.2)×10^–3 min^–1. The formation constant of the molecular complex was evaluated from the computer fitting of the absorbance-mole ratio data as logK _f=6.89±0.09.     

A cost-effective form-stable PCM composite with modified paraffin and expanded perlite for thermal energy storage in concrete

Journal of Thermal Analysis and Calorimetry - High thermal conductivity in phase change materials (PCM) is preferred in thermal energy storage (TES) systems. Carbon additives are considered as...     

Ion pairing, H-bonding, and π–π interactions in copper(II) complex-organo-networks derived from a proton-transfer compound of the 1,10-phenanthroline-2,9-dicarboxylic acid

The one-pot reaction between the novel proton transfer compound (pydaH₂)²⁺(phendc)²⁻, LH₂, and Cu(II) afforded the compounds (pydaH)₂[Cu(phendc)₂]·10H₂O, 1, and (pydaH)₂[Cu(phendc)(phendcH)]₂·5H₂O, 2, where pyda=2,6-diaminopyridine, and phendcH₂=1,10-phenanthroline-2,9-dicarboxylic acid. The single crystal X-ray diffraction analysis of 1 and 2 revealed that these are two novel self-assembled 3D Cu(II) complex-organo-networks, in which (pydaH)⁺ ions and [Cu(phendc)₂]²⁻ or complex units are held together by ion pairing, H-bonding, and π–π interactions. Magnetic measurements over the temperature range 1.8–310 K revealed no significant magnetic coupling between Cu(II) centers in 1 or 2.     

Purification of L-Lysine in Simulated Moving Bed and Fixed-Bed Chromatography

 L-Lysine was produced by a microbial process utilizing a Corynebacterium glutamicum (ATCC 21799) strain. L-Lysine was purified from the cultivated medium by fixed-bed and simulated moving bed （SMB） chromatography. The separation conditions including pH, eluent concentration and Lys+ and Lys2+ adsorption isotherms were studied in batch adsorption. The column capacity, eluent flow rate and eluent concentration have been studied in fixed-bed chromatography. Maximum purification rate of lysine was obtained as 0.066 g/(g·h) (per gram resin and per hour) at an eluent flow rate of 10 mL/min in fixed-bed chromatography. The results obtained from SMB were 0.11 g/(g·h) for L-lysine purification rate and 96% for L-lysine recovery.     

Tribromoisocyanuric Acid (TBCA) and Oxone®‐MX Systems as Oxidizing Agents: Oxidative Coupling of Thiols to Their Corresponding Disulfides under Mild and Heterogeneous Conditions

Tribromoisocyanuric acid (TBCA) and Oxone^®‐MX systems were used as effective oxidizing agents for the oxidation of thiols to their corresponding disulfides under mild conditions at room temperature with good to excellent yields.     

Nitroxide mediated living radical polymerization of styrene onto poly (vinyl chloride)

Nitroxide‐mediated ‘living’ free radical polymerisation (LREP) was employed for the first time to prepare graft copolymer by having arylated poly (vinyl chloride) (PVC‐Ph) as a backbone and polystyrene (PS) as branches. The graft copolymerization of styrene was initiated by arylated PVC carrying 2,2,6,6‐tetramethyl‐1‐piperidinyloxy (TEMPO) groups as a macroinitiator. Thus, the arylated PVC was prepared in the mild conditions and these reaction conditions could overcome the problem of gelation and crosslinking in polymers. Then, 1‐hydroxy TEMPO was synthesized by the reduction of TEMPO with sodium ascorbate. This functional nitroxyl compound was coupled with brominated arylated PVC (PVC‐Ph‐Br). The resulting macro‐initiator (PVC‐Ph‐TEMPO) for ‘living’ free radical polymerization was then heated in the presence of styrene to form graft copolymer. DSC, GPC, ¹HNMR, and FT‐IR spectroscopy were employed to investigate the structure of the polymers. Copyright © 2007 John Wiley & Sons, Ltd.     

A Novel Hydrogen Peroxide Sensor Based on the Direct Electron Transfer of Catalase Immobilized on Nano‐Sized NiO/MWCNTs Composite Film

MWCNTs‐nanoNiO composite was used as a glassy carbon electrode modifier for construction of a novel catalase nanobiosensor for hydrogen peroxide. The immobilized catalase exhibited excellent electrocatalytic activity towards the reduction of H₂O₂. The resulting amperometric biosensor exhibited a linear response over a concentration range of 200 µM to 2.53 mM with a low detection limit of 19.0 µM. Electrochemical impedance measurements revealed that the modified electrode can be used for the sensitive detection of H₂O₂. The charge transfer resistance found to decrease significantly after enzymatic reaction of nanobiosensor with H₂O₂. The resulting impedance was highly sensitive to H₂O₂ over a linear range of 19–170 nM with a detection limit of 2.4 nM.