雷芬那辛的合成工艺研究

以联苯-2-基氨基甲酸哌啶-4-基酯(SM-1)为起始物料，经亲核取代、脱苄基、和4-甲酰基苯甲酸脱水反应生成酰胺中间体，最后和哌啶-4-甲酰胺脱水反应先形成希夫氏碱再经三乙酰氧基硼氢化钠还原制备雷芬那辛。通过对反应条件的控制及纯化，所得产品纯度为99.5%,总收率为45.7%,目标产物的化学结构经质谱和核磁共振确证。该工艺反应条件温和、操作简便，为雷芬那辛的合成提供了一种新选择。     

Co?N graphene encapsulated cobalt catalyst for H2O2 decomposition under acidic conditions

Hydrogen peroxide (H₂O₂) has been listed as one of the 100 most important chemicals in the world. However, huge amount of residual H₂O₂ is hard to timely decomposed into O₂ and H₂O under acidic condition, easily resulting in explosion hazard. Here, we reported a core–shell structure catalyst, that is graphene with Co N structure encapsulated Co nanoparticles. Co N graphene shell serves as the active site for the H₂O₂ decomposition, and Co core further enhance this decomposition. Benefiting from it, the H₂O₂ decomposition were close to 100% after 6 cycles without pH adjustment, which increased 6 orders of magnitude compared with no catalyst. At the same time, the O₂ generation reached 99.67% in 2 h with little metal leaching, and ·OH has been greatly inhibited to only 0.08%. This work can cleanly remove H₂O₂ with little deep oxidation and protect the process of H₂O₂ utilization to achieve a safer world.     

A numerical model to predict the powder–binder separation during micro-powder injection molding

The micro-powder injection molding (micro-PIM) process has the potential to bridge the gap between the design and manufacturing of micro-components that are often used in small and handy devices. Numerical modeling helps to analyze and overcome various difficulties of micro-PIM. In the present work, a numerical model is developed to predict the powder–binder separation (a common defect in PIM and especially severe in micro-PIM) during the injection of an alumina feedstock. A powder–binder separation criterion is proposed dealing with applied injection pressure and friction force between the powder and binder. An indirect comparison of feedstock travel time between two locations is used to validate the model. The predicted segregation from the simulated result is supported by a qualitative experimental measurement. The developed model can be used to optimize injection parameters to get a defect-free product.     

Double pyrovanadates CaMgV2O7: Formation mechanism,phase structure,and thermodynamic properties

A double pyrovanadate CaMgV₂O₇ sample was synthesized via a facile solid-state route under an air atmosphere. The nonequilibrium formation pathways of the CaMgV₂O₇ were investigated via powder X-ray diffraction. A multistep reactions path (metavanadates–pyrovanadates–double pyrovanadate CaMgV₂O₇) was proposed to describe the formation of the CaMgV₂O₇ considering the thermodynamic and kinetic factors. The cell unit parameters of the CaMgV₂O₇ sample indicated the crystallization according to a monoclinic system with space group P12/c1(14), and the lattice parameters of a = 6.756 Å, b = 14.495 Å, c = 11.253 Å, β = 99.12, and V = 108.806 Å³. X-ray photoelectron spectroscopy also confirmed the +5 oxidation state vanadium in CaMgV₂O₇. The endothermic effects at 1033 and 1143 K were related to the incongruent melting and liquidus temperatures of CaMgV₂O₇, respectively. The comprehensive thermodynamic properties of CaMgV₂O₇ were established in both low- and high-temperature regions, utilizing a physical property measurement system and multi-high-temperature calorimetry (96 lines). The heat capacity (200 J mol K⁻¹) and entropy (198 J mol K⁻¹) at 298.15 K were computed based on the low-temperature heat capacity values, and the enthalpy of formation at 298.15 K was also estimated. The fitted high-temperature capacity can be used to obtain the changes in the enthalpy, entropy, and Gibbs free energy. This study is part of building a reliable thermodynamic database of the CaO–MgO–V₂O₅ system.     

A triptycene derived hypercrosslinked polymer for gas capture and separation applications

This work describes facile synthesis of a porous polymeric material ( T-HCP ) using readily available reagents. Specifically, T-HCP is a thermally stable and hypercrosslinked polymer (HCP) that is essentially microporous with a high BET specific surface area (940 m² g^?1). Triptycene based polymers are known to feature internal free volume. Thus, the incorporation of triptycene units and extensive crosslinking by an external cross-linker in T-HCP makes it a promising adsorbent for small gas capture applications. Experimental results show that T-HCP demonstrated good CO₂ capture capacity of 132 mg g^?1 (273 K, 1 bar). Molecular hydrogen storage capacity of T-HCP is estimated to be 17.7 mg g^?1 (77 K, 1 bar). T-HCP revealed high CO₂/N₂ selectivity (up to 63) as well as promising CO₂/CH₄ (up to 9.1) selectivity suggesting its potential applicability for CO₂ separation from flue and natural gases.     

高效液相色谱法测定化妆品中依克多因的含量

建立高效液相色谱法测定化妆品中依克多因的分析方法,采用Agilent Poroshell 120 EC-C₁₈色谱柱（100 mm×3.0 mm,2.7μm）分离,以甲醇和p H为3.0的40 mmol/L磷酸二氢钠-10 mmol/L 1-庚烷磺酸钠缓冲溶液梯度洗脱,流速0.8 m L/min,柱温30℃,检测波长210 nm。采用外标法定量测定化妆品中的依克多因含量。结果表明,依克多因在5～800 mg/L的质量浓度范围内呈现良好线性关系,相关系数为0.999 8,方法的检出限和定量限分别为0.3和1.0 mg/L。该方法具有分离效率高、分析时间短、节省溶剂等优点,解决了依克多因在C₁₈色谱柱上保留弱的问题。     

Study on the removal of olefins from naphtha by clay loaded with trifluoromethanesulfonic acid

Journal of Porous Materials - In this work, a trifluoromethanesulfonic acid (TFOH) modified clay (TFOH-Clay) was developed for the removal of trace olefins in heavy naphtha. 5%TFOH-Clay can...     

纯净美妆产品的设计理念

以消费者、行业专家、各品牌商以及全球各个美妆相关行业对纯净美妆的认识为依据,从配方设计、关键的原料筛选、生产过程、包材选择以及测试评估等方面,对如何实现纯净美妆产品进行了较为详细的阐述,无疑为纯净美妆的标准建立和定义提供很好的参考.     

Synthesis of Janus polyaniline–polyelectrolyte complex membrane via in situ confined polymerization

Polyelectrolyte complex (PEC) membranes prepared from poly(styrene sulfonate) (PSS) and poly(diallyldimethylammonium chloride) (PDADMAC) were modified by crossflow polymerization of aniline (ANI). The PEC membranes were used as separators in a two-compartment setup where ANI monomer and ammonium persulfate (APS) oxidant diffused through the membranes to form polyaniline (PANI). APS and ANI having different distributions throughout the membranes, the reaction led to the asymmetric polymerization of PANI on one face of each PEC membrane thus producing Janus membranes. Due to the excess PANI content, the membrane displayed distinct asymmetric electrical conductivities on each face. Interestingly, very different ANI polymerizations were obtained when nonstoichiometric PEC membranes having different molar ratio of cationic and anionic polyelectrolytes (P⁺:P^? represents PDADMAC:PSS) were used and transport of APS was fastest through the 2:1 PEC when compared to the 1:2 PEC. In all experiments, the polymerization was most intense on the ANI side of the membranes. Also, the influence of NaCl both during PEC fabrication and during polymerization was studied and found to have some effect on the solute permeability. Results showed that a higher content of PANI was formed on PEC membranes having excess P⁺ and with no NaCl added during PEC fabrication. Although X-ray diffraction confirmed the presence of PANI on both sides of each membrane, scanning electron microscopy images demonstrated that both sides of each membrane had different PANI content deposited. Electrical conductivity measurements using a four-point probe setup also showed that the PEC–PANI exhibits asymmetric electrical property on different sides. © 2021 Society of Industrial Chemistry.