Conservation of [(C2H4NH3)3N]2·(ZrF7)2·H2O layers during the topotactic dehydration of [(C2H4NH3)3N]2·(ZrF7)2·9H2O

Tren amine cations [(C₂H₄NH₃)₃N]³⁺ and zirconate or tantalate anions adopt a ternary symmetry in two hydrates, [H₃tren]₂·(ZrF₇)₂·9H₂O and [H₃tren]₆·(ZrF₇)₂·(TaOF₆)₄·3H₂O, which crystallise in R32 space group with a_H = 8.871 (2) Å, c_H = 38.16 (1) Å and a_H = 8.758 (2) Å, c_H = 30.112 (9) Å, respectively. Similar [H₃tren]₂·(MX₇)₂·H₂O (M = Zr, Ta; X = F, O) sheets are found in both structures; they are separated by a water layer (O_w(2)-O_w(3)) in [H₃tren]₂·(ZrF₇)₂·9H₂O. Dehydration of [H₃tren]₂·(ZrF₇)₂·9H₂O starts at room temperature and ends at 90 °C to give [H₃tren]₂·(ZrF₇)₂·H₂O. [H₃tren]₂·(ZrF₇)₂·H₂O layers remain probably unchanged during this dehydration and the existence of one intermediate [H₃tren]₂·(ZrF₇)₂·3H₂O hydrate is assumed. O_w(1) molecules are tightly hydrogen bonded with -NH₃⁺ groups and decomposition of [H₃tren]₂·(ZrF₇)₂·H₂O occurs from 210 °C to 500 °C to give successively [H₃tren]₂·(ZrF₆)·(Zr₂F₁₂) (285 °C), an intermediate unknown phase (320 °C) and ZrF₄.     

Analytical study of Joule heating effects on electrokinetic transportation in capillary electrophoresis

Electric fields are often used to transport fluids (by electroosmosis) and separate charged samples (by electrophoresis) in microfluidic devices. However, there exists inevitable Joule heating when electric currents are passing through electrolyte solutions. Joule heating not only increases the fluid temperature, but also produces temperature gradients in cross-stream and axial directions. These temperature effects make fluid properties non-uniform, and hence alter the applied electric potential field and the flow field. The mass species transport is also influenced. In this paper we develop an analytical model to study Joule heating effects on the transport of heat, electricity, momentum and mass species in capillary-based electrophoresis. Close-form formulae are derived for the temperature, applied electrical potential, velocity, and pressure fields at steady state, and the transient concentration field as well. Also available are the compact formulae for the electric current and the volume flow rate through the capillary. It is shown that, due to the thermal end effect, sharp temperature drops appear close to capillary ends, where sharp rises of electric field are required to meet the current continuity. In order to satisfy the mass continuity, pressure gradients have to be induced along the capillary. The resultant curved fluid velocity profile and the increase of molecular diffusion both contribute to the dispersion of samples. However, Joule heating effects enhance the sample transport velocity, reducing the analysis time in capillary electrophoretic separations.     

Inductive effect for the phase stability in hydrogen bonded liquid crystals,x-(p/m)BA:9OBAs

A new series of hydrogen bonded liquid crystal (HBLC) complexes, made up with substituted benzoic acids (BAs) and nonyloxy benzoic acid, viz., x-(p/m)BA:9OBAs are reported for x = F, Cl, Br and –CH₃ substituted at para (p) or meta (m) positions of BA moiety. Proton nuclear magnetic resonance (¹H-NMR) spectrum confirms the HBLC complex. Infra red (IR) spectrum confirms linear, double and complementary type of hydrogen bonding (HB) between x-(p/m)BAs and 9OBA. The liquid crystal (LC) phases are characterised by polarisation optical microscopy (POM) and differential scanning calorimetry (DSC) techniques. x-(p/m)BA:9OBA exhibit N, C and G LC phase variance. HB induces tilted phases and enhances LC phase stability. The influence of configuration, size, electronegativity, electron directing capacity and inductive nature of substituent (x) is investigated for the stability of LC phases. An overview of the LC phase data indicates predominant ‘negative inductive effect’ in HBLCs with electron withdrawing substituents. Inductive effect operates effectively for para substitutions. Results are discussed in the wake of reports in other HBLCs.     

High-speed deposition of RE123 film with large current capacity by hot-wall type PLD system

We have studied a hot-wall heating system to produce GdBa₂Cu₃O_y (GdBCO) films with large critical currents (I_c) at a high production rate by a pulsed-laser-deposition (PLD) method. GdBCO films fabricated at a production rate of 30 m/h under the optimized conditions, especially a distance of 95 mm between the target and the substrate (T–S), exhibited high critical current densities (J_c) of about 3 MA/cm² and I_c over 300 A at a thickness of 1–2 μm. Furthermore, long GdBCO tapes prepared by repeated depositions at each tape-passing speed of 80 m/h showed uniform I_c distribution along the longitudinal direction, because the hot-wall system enabled to stabilize temperature within a few degrees at 800 °C. A 170 m long tape with I_c over 600 A was successfully fabricated at a production rate of 16 m/h using a laser power of 360 W.     

Preparation and Characterization of Quaternized Chitosan Under Microwave Irradiation

For the first time, N-(2-hydroxyl) propyl-3-trimethyl ammonium chitosan chloride (HTCC) was prepared through a fast, easy and efficient method with the assistance of microwave irradiation, and the quaternized chitosan was also degraded via the microwave irradiation. A comparative study was performed by using the conventional heating method to prepare HTCC. The structure and property of the quaternized chitosan obtained by these two methods were characterized by GPC, XRD, FTIR, NMR, TG and elemental analysis. It was shown that quaternized chitosan was successfully prepared within 50 min via microwave irradiation method, while a much longer time of 6–7 h was needed with the conventional heating method. The substitutions both occurred on the C2 position of chitosan with the two different methods, and their HTCC products had weight average similar molecular weight (Mw), structure and thermal stability. The HTCC prepared by the microwave irradiation method had a little lower degree of substitution (DS) than those prepared via conventional heating with the same mole ratio (6:1) of the intermediate to chitosan. The degradation study showed that the Mw of HTCC decreased rapidly from 4.6 × 10⁵ to 1.1 × 10⁵ in 1 h under microwave irradiation, while it only decreased from 4.6 × 10⁵ to 2.1 × 10⁵in 1 h through conventional heating degradation. These results revealed that microwave irradiation is a more efficient and environment-friendly way to obtain the water-soluble chitosan derivatives and their degraded products.     

Multicomponent Domino [4+1+1] Carbocyclization Providing an Efficient and Regioselective Strategy to Fluoren-9-ones

Concise and efficient three‐component domino [4+1+1] carbocyclization to highly substituted fluoren‐9‐one derivatives promoted by K₂CO₃ has been developed under microwave irradiation conditions. The direct bis‐cyanation and aryl amination residing in fluoren‐9‐one framework were achieved in a one‐pot operation. The reaction proceeds at fast rates and can be finished within 30 min, which makes workup convenient to give good to excellent chemical yields.     

Solvent-Free C-Benzoylation and N-Benzoylation Reactions Using Microwave Heating

An ecofriendly and efficient microwave-irradiated solvent-free benzoylation method was developed. The procedure for C-benzoylation used 50 mol% AlCl₃ as a Lewis acid catalyst at 130 °C and was completed in 10 min. The isolated yield was between 71% and 100%. N-benzoylation was conducted in a catalyst-free environment at 130 °C in 10 min. The isolated yield was between 80% and 100%.

Synthesis of Metal‐Free Phthalocyanines in Functionalized Ammonium Ionic Liquids

A convenient, fast, efficient, and ecofriendly synthesis of metal‐free phthalocyanines from various substituted phthalonitriles in different hydroxyalkylammonium ionic liquids in the presence of 1,8‐diazabicyclo‐[5,4,0]‐undec‐7‐ene (DBU) is reported in moderate yields. The effect of concentration of DBU and temperature on the synthesis of phthalocyanine in N‐(2‐hydroxyethyl)‐N,N‐dimethylbutylammonium bromide ionic liquid has been examined, and the ionic liquid has been recovered and reused conveniently.     

Microwave‐Assisted Synthesis and Characterization of CuO Nanocrystals

CuO feather‐like and flower‐like crystals have been synthesized by a fast microwave‐assisted solution approach using Cu(NO₃)₂ and NaOH. The morphology transformation of CuO could be achieved by ionic liquid 1‐n‐butyl‐3‐methyl imidazolium tetrafluoroborate ([BMIM]BF₄). With [BMIM]BF₄, flower‐like CuO were obtained, whereas without [BMIM]BF₄, feather‐like CuO were obtained. The possible formation mechanism of flower‐like CuO was discussed on the basis of experimental results. The products were characterized by XRD, FESEM/EDS, and TEM/SAED. In addition, the adsorption of [BMIM]BF₄ on flower‐like CuO was confirmed by FTIR and TG/DSC, and the band gap energies of the flower‐like CuO was estimated by UV‐vis spectra.     

New formal (3+3) cycloaddition of enaminones for forming tetracyclic indolo[2,3-b]quinolines under microwave irradiation

Concise and efficient base-promoted domino formal (3+3) cycloaddition has been established for the formation of tetracyclic indolo[2,3-b]quinoline derivatives under microwave heating. The present methodology shows attractive properties, such as the maximum efficiency of a process, short reaction periods, and operational simplicity, and it can avoid time-consuming and costly syntheses, tedious work-up and isolation of intermediate. This chemistry provides a facile and promising synthetic strategy to construction of tetracyclic indolo[2,3-b]quinoline skeleton.