Visible light irradiation promoted catalyst-free and solvent-free synthesis of pyrano[2,3-d]pyrimidine scaffolds at room temperature

A catalyst-free and solvent-free synthetic route for convenient one-pot synthesizing pyrano[2,3-d] pyrimidine scaffolds through Knoevenagel-Michael cyclocondensation is reported using visible light irradiation as a green promoter at room temperature based on green chemistry principles. Completing the reactions takes thoroughly less time while obtaining the products in outstanding yields. This green method includes the application of non-hazardous reaction circumstances, direct work-up without column chromatographic separation, catalyst-free, solvent-free, cost effective, simple synthesis, one-pot procedure, and high atom-economy.     

Investigation of dense slurry suspensions with coaxial mixers: Influences of design variables through tomography and mathematical modelling

The coaxial mixers enhance the suspension of concentrated slurries in an agitated reactor. In this research work, the complex slurry suspension and dissemination behavior in a coaxial slurry mixing system (comprised of a close clearance anchor rotating with a low speed and an inner axial impeller rotating with a high speed) was analyzed employing ERT (electrical resistance tomography, a non-intrusive flow visualization technique), and computational fluid dynamics (CFD). The numerical models were validated by comparing the axial solid concentration profiles generated using the ERT data and the CFD simulation results. The influences of various important parameters such as the diameter of the inner axial impeller, the inner impeller type, and the inner impeller spacing on the hydrodynamic characteristics of the slurry suspensions in a coaxial mixing vessel were thoroughly analyzed. The radial and axial velocity profiles of solid particles were generated using the validated mathematical models. The assessment of energy loss due to the solid–solid collisions, the particle–fluid frictions, and the particle–vessel wall collisions was conducted. The evaluation of optimum inner impeller clearance and inner impeller diameter is essential to attain a high degree of solids suspension and dissemination in a coaxial slurry mixing system.     

山楂叶中熊果酸提取工艺研究

以熊果酸的提取率为指标,采用单因素与正交实验相结合的方法对提取工艺进行了优化,得到最佳提取参数为:乙醇体积分数95%、提取温度85℃、提取时间110min、液固比5:1、提取次数3次。在该条件下,熊果酸提取率为93.47%。该工艺简单合理,为工业生产提供了理论参考。     

喷流冷却复合陶瓷薄片激光器的热特性仿真分析及实验研究

为分析喷流冷却复合陶瓷薄片激光器的热特性,设计用于冷却复合陶瓷薄片的喷流冷却系统.利用湍流换热理论和计算流体动力学仿真方法建立喷流冷却复合陶瓷薄片激光器的流固耦合热仿真模型,定义评价其冷却能力和冷却均匀性的定量参数.根据该仿真模型得到喷流冷却系统的最优设计参数,并进行实验验证.使用163孔喷板,流量为0.2kg/s,入口温度为20℃,在1200 W泵浦时获得359 W激光输出功率,并测得复合陶瓷薄片上表面的最高温度为92℃.激光输出功率与复合陶瓷薄片上表面温度均与泵浦功率呈近似正线性关系,且温度的实验值与仿真值相符度较高.     

Sonoelectrochemical hydrogenation of safrole: A reactor design,statistical analysis and computational fluid dynamic approach

In this work, ultrasound-assisted electrocatalytic hydrogenation (US-ECHSA) of safrole was carried out in water medium, using sacrificial anode of nickel. The ultrasonic irradiation was carried out at frequency of 20 kHz ± 500 Hz with a titanium cylindrical horn (MS 73 microtip; Ti-6AI-4V alloy; 3.0 mm diameter). The optimal conditions were analyzed by statistical experimental design (fractional factorial). The influence of the sonoelectrochemical reactor design was also investigated by using computational fluid dynamics as simulation tool. Among the five parameters studied: catalyst type, use of β-cyclodextrin as inverse phase transfer catalyst, sonoelectrochemical reactor design, ultrasound mode and the temperature of the solution, only the last three were significant. The hydrogenation product, dihydrosafrole, reached 94% yield, depending on the experimental conditions applied. Data of computational fluid dynamics showed that a wing shape tube added to the sonoelectrochemical reactor can work as a cooling apparatus, during the electrochemical process. The reactional solution temperature diminishes 14 °C when compared to the four-way-type reactor. Cooper cathode, absence of β-cyclodextrin, four-way-type reactor, ultrasound continuous mode (14 W) and absence of temperature control were the most effective reaction parameters for the safrole hydrogenation using US-ECHSA method. The proposed approach represents an important contribution for understanding the hydrodynamic behavior of sonoelectrochemical reactors designs and, consequently, for the reducing of the experimental costs inherent to the sonoelectrochemical process.     

The Influence of Synthesis Conditions on the Antioxidant Activity of Selenium Nanoparticles

Selenium nanoparticles (SeNPs) have attracted great attention in recent years due to their unique properties and potential bioactivities. While the production of SeNPs has been long reported, there is little news about the influence of reaction conditions and clean-up procedure on their physical properties (e.g., shape, size) as well as their antioxidant activity. This study takes up this issue. SeNPs were synthesized by two methods using cysteine and ascorbic acid as selenium reductants. The reactions were performed with and without the use of polyvinyl alcohol as a stabilizer. After the synthesis, SeNPs were cleaned using various procedures. The antioxidant properties of the obtained SeNPs were investigated using DPPH and hydroxyl radical scavenging assays. It was found that their antioxidant activity does not always depend only on the nanoparticles size but also on their homogeneity. Moreover, the size and morphology of selenium nanoparticles are controlled by the clean-up step.     

Intelligent Reflecting Surface–Assisted Wireless Secret Key Generation against Multiple Eavesdroppers

In this paper, we propose an improved physical layer key generation scheme that can maximize the secret key capacity by deploying intelligent reflecting surface (IRS) near the legitimate user aiming at improving its signal-to-noise ratio (SNR). We consider the scenario of multiple input single output (MISO) against multiple relevant eavesdroppers. We elaborately design and optimize the reflection coefficient matrix of IRS elements that can improve the legitimate user’s SNR through IRS passive beamforming and deteriorate the channel quality of eavesdroppers at the same time. We first derive the lower bound expression of the achievable key capacity, then solve the optimization problem based on semi-definite relaxation (SDR) and the convex–concave procedure (CCP) to maximize the secret key capacity. Simulation results show that our proposed scheme can significantly improve the secret key capacity and reduce hardware costs compared with other benchmark schemes.     

Synthesis and Crystal Structure of 3-Benzoyl-7,7-dimethyl-4-phenyl-2-phenylamino-4,6,7,8-tetrahydro-chromen-5-one

The title compound (C30H27NO3) was synthesized via a one-pot procedure starting from β-benzoylthioacetanilide, benzaldehyde and 5,5-dimethyl-1,3-cyclohexanedione, and its struc- ture was determined by single-crystal X-ray diffraction analysis. The crystal belongs to triclinic system, space group P, with a = 6.325(2), b = 11.243(3), c = 17.553(4) , α = 87.306(4), β = 80.822(4), γ = 77.798(4)°, V = 1204.2(5) 3, Z = 2, Mr = 449.53, Dc = 1.240 g/cm3, μ = 0.080 mm-1, F(000) = 476, the final R = 0.0459 and wR = 0.0970 for 2301 observed reflections with I > 2σ(I).     

State-crossing from a Locally Excited to an Electron Transfer State(SLEET) Model Rationalizing the Aggregation-induced Emission Mechanism of (Bi)piperidylanthracenes

Luminogens with aggregation-induced emission(AIE)characteristics(or AIEgens)have been widely used in various applications due to their excellent luminescent properties in molecular aggregates and the solid state.A deep understanding of the AIE mechanism is critical for the rational development of AIEgens.In this work,the“state-crossing from a locally excited to an electron transfer state”(SLEET)model is employed to rationalize the AIE phenomenon of two(bi)piperidylanthracenes.According to the SLEET model,an electron transfer(ET)state is formed along with the rotation of the piperidyl group in the excited state of(bi)piperidylan-thracene monomers,leading to fluorescence quenching.In contrast,a bright state exists in the crystal and molecular aggregates of these compounds,as the intermolecular interactions restrict the formation of the dark ET state.This mechanistic understanding could inspire the deployment of the SLEET model in the rational designs of various functional AIEgens.     

NARROW-DISPERSED CROSSLINKED CORE-SHELL POLYMER MICROSPHERES PREPARED BY SURFACE-INITIATED ATOM TRANSFER RADICAL POLYMERIZATION＊

Grafting of polystyrene with narrowly dispersed polymer microspheres through surface-initiated atom transfer radical polymerization (ATRP) was investigated. Polydivinylbenzene (PDVB) microspheres were prepared by dispersion polymerization with poly(N-vinyl pyrrolidone) (PVP) as stabilizer. The surfaces of PDVB microspheres were chloromethylated by chloromethyl methyl ether in the presence of zinc chloride as catalyst to form chloromethylbenzene initiating core sites for subsequent ATRP grafting of styrene using CuCl/bpy as catalytic system. Polystyrene was found to be grafted not only from the particle surfaces but also from within a thin shell layer, resulting in the formation of particles size increased from 2.38-2.58μm, which can further grow to 2.93μm during secondary grafting polymerization of styrene. This demonstrates that grafting polymerization proceeds through a typical ATRP procedure with living nature. All of the prepared microspheres have narrow particle size distribution with coefficient of variation around 10%.